# Electronic Supplementary Material (ESI) for Dalton Transactions. # This journal is © The Royal Society of Chemistry 2023 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_megm_lamgabra_0m _database_code_depnum_ccdc_archive 'CCDC 2173026' loop_ _audit_author_name _audit_author_address 'Lucia Alvarez Miguel' ;Universidad de Alcala Spain ; _audit_update_record ; 2022-06-09 deposited with the CCDC. 2023-02-22 downloaded from the CCDC. ; _audit_creation_date 2022-06-09 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C36 H46 Br Ga N2 O2' _chemical_formula_sum 'C36 H46 Br Ga N2 O2' _chemical_formula_weight 688.38 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7269(4) _cell_length_b 12.7417(6) _cell_length_c 14.5254(7) _cell_angle_alpha 84.461(2) _cell_angle_beta 78.992(2) _cell_angle_gamma 71.350(2) _cell_volume 1673.11(13) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9049 _cell_measurement_temperature 200.0 _cell_measurement_theta_max 27.15 _cell_measurement_theta_min 2.35 _shelx_estimated_absorpt_T_max 0.762 _shelx_estimated_absorpt_T_min 0.646 _exptl_absorpt_coefficient_mu 2.050 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0832 before and 0.0660 after correction. The Ratio of minimum to maximum transmission is 0.9185. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 716 _exptl_crystal_size_max 0.234 _exptl_crystal_size_mid 0.203 _exptl_crystal_size_min 0.14 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0909 _diffrn_reflns_av_unetI/netI 0.0400 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 93581 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.919 _diffrn_reflns_theta_min 2.253 _diffrn_ambient_temperature 200.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6089 _reflns_number_total 7986 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.562 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.070 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 391 _refine_ls_number_reflns 7986 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0391 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+1.0568P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.0943 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C7(H7), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C26(H26) 2.b Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B, H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C31(H31A, H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.23563(3) 0.63061(3) 0.23796(2) 0.04371(10) Uani 1 1 d . . . . . Ga1 Ga 0.42650(3) 0.53294(2) 0.31970(2) 0.02112(8) Uani 1 1 d . . . . . O1 O 0.58818(19) 0.58236(14) 0.26901(12) 0.0279(4) Uani 1 1 d . . . . . O2 O 0.53085(18) 0.39819(14) 0.26255(12) 0.0265(4) Uani 1 1 d . . . . . N1 N 0.3905(2) 0.62158(16) 0.43588(14) 0.0222(4) Uani 1 1 d . . . . . N2 N 0.3154(2) 0.44845(16) 0.41711(14) 0.0224(4) Uani 1 1 d . . . . . C1 C 0.6307(3) 0.6626(2) 0.29173(17) 0.0227(5) Uani 1 1 d . . . . . C2 C 0.7425(3) 0.6959(2) 0.22886(17) 0.0236(5) Uani 1 1 d . . . . . C3 C 0.7946(3) 0.7733(2) 0.25893(18) 0.0258(5) Uani 1 1 d . . . . . H3 H 0.873677 0.791398 0.218688 0.031 Uiso 1 1 calc R U . . . C4 C 0.7398(3) 0.8275(2) 0.34460(18) 0.0254(5) Uani 1 1 d . . . . . C5 C 0.6280(3) 0.7986(2) 0.40236(17) 0.0246(5) Uani 1 1 d . . . . . H5 H 0.586729 0.834057 0.460324 0.030 Uiso 1 1 calc R U . . . C6 C 0.5720(3) 0.71682(19) 0.37777(17) 0.0228(5) Uani 1 1 d . . . . . C7 C 0.4582(3) 0.69247(19) 0.44400(17) 0.0227(5) Uani 1 1 d . . . . . H7 H 0.428055 0.732015 0.500317 0.027 Uiso 1 1 calc R U . . . C8 C 0.7995(3) 0.6503(2) 0.13001(18) 0.0268(5) Uani 1 1 d . . . . . C9 C 0.6706(3) 0.6750(2) 0.07627(19) 0.0341(6) Uani 1 1 d . . . . . H9A H 0.594755 0.644987 0.112475 0.051 Uiso 1 1 calc R U . . . H9B H 0.705867 0.640565 0.015196 0.051 Uiso 1 1 calc R U . . . H9C H 0.628692 0.755396 0.066825 0.051 Uiso 1 1 calc R U . . . C10 C 0.8770(3) 0.5252(2) 0.1350(2) 0.0354(6) Uani 1 1 d . . . . . H10A H 0.966586 0.510543 0.161941 0.053 Uiso 1 1 calc R U . . . H10B H 0.902923 0.496461 0.071681 0.053 Uiso 1 1 calc R U . . . H10C H 0.810958 0.488452 0.174531 0.053 Uiso 1 1 calc R U . . . C11 C 0.9102(3) 0.7043(2) 0.0725(2) 0.0366(6) Uani 1 1 d . . . . . H11A H 0.863921 0.784711 0.068003 0.055 Uiso 1 1 calc R U . . . H11B H 0.941024 0.674852 0.009408 0.055 Uiso 1 1 calc R U . . . H11C H 0.996320 0.687790 0.103401 0.055 Uiso 1 1 calc R U . . . C12 C 0.8056(3) 0.9124(2) 0.37084(19) 0.0295(6) Uani 1 1 d . . . . . C13 C 0.9346(3) 0.8528(3) 0.4211(2) 0.0421(7) Uani 1 1 d . . . . . H13A H 0.899944 0.814463 0.478269 0.063 Uiso 1 1 calc R U . . . H13B H 0.977292 0.906850 0.437820 0.063 Uiso 1 1 calc R U . . . H13C H 1.009435 0.798603 0.379696 0.063 Uiso 1 1 calc R U . . . C14 C 0.8590(5) 0.9747(3) 0.2837(2) 0.0606(11) Uani 1 1 d . . . . . H14A H 0.942133 0.923354 0.244770 0.091 Uiso 1 1 calc R U . . . H14B H 0.890584 1.034015 0.302612 0.091 Uiso 1 1 calc R U . . . H14C H 0.778779 1.006931 0.247744 0.091 Uiso 1 1 calc R U . . . C15 C 0.6914(4) 0.9978(3) 0.4359(3) 0.0610(11) Uani 1 1 d . . . . . H15A H 0.606583 1.035550 0.404924 0.092 Uiso 1 1 calc R U . . . H15B H 0.735308 1.052376 0.450256 0.092 Uiso 1 1 calc R U . . . H15C H 0.659104 0.960401 0.494232 0.092 Uiso 1 1 calc R U . . . C16 C 0.2765(3) 0.6045(2) 0.50654(16) 0.0231(5) Uani 1 1 d . . . . . C17 C 0.2027(3) 0.6734(2) 0.58054(18) 0.0299(6) Uani 1 1 d . . . . . H17 H 0.227841 0.738167 0.586912 0.036 Uiso 1 1 calc R U . . . C18 C 0.0928(3) 0.6479(2) 0.64484(18) 0.0313(6) Uani 1 1 d . . . . . H18 H 0.042198 0.695390 0.695267 0.038 Uiso 1 1 calc R U . . . C19 C 0.0558(3) 0.5533(2) 0.63624(18) 0.0293(6) Uani 1 1 d . . . . . H19 H -0.019438 0.535943 0.681103 0.035 Uiso 1 1 calc R U . . . C20 C 0.1275(3) 0.4843(2) 0.56309(17) 0.0265(5) Uani 1 1 d . . . . . H20 H 0.102300 0.419274 0.557805 0.032 Uiso 1 1 calc R U . . . C21 C 0.2369(3) 0.5098(2) 0.49692(17) 0.0227(5) Uani 1 1 d . . . . . C22 C 0.2946(3) 0.3573(2) 0.39909(17) 0.0244(5) Uani 1 1 d . . . . . H22 H 0.226155 0.331369 0.443360 0.029 Uiso 1 1 calc R U . . . C23 C 0.3654(3) 0.2929(2) 0.31893(17) 0.0235(5) Uani 1 1 d . . . . . C24 C 0.3161(3) 0.2028(2) 0.30731(18) 0.0270(5) Uani 1 1 d . . . . . H24 H 0.240424 0.187881 0.353399 0.032 Uiso 1 1 calc R U . . . C25 C 0.3736(3) 0.1364(2) 0.23208(19) 0.0265(5) Uani 1 1 d . . . . . C26 C 0.4880(3) 0.1617(2) 0.16697(18) 0.0262(5) Uani 1 1 d . . . . . H26 H 0.528727 0.117030 0.113749 0.031 Uiso 1 1 calc R U . . . C27 C 0.5449(3) 0.2459(2) 0.17456(17) 0.0240(5) Uani 1 1 d . . . . . C28 C 0.4803(3) 0.31580(19) 0.25254(17) 0.0221(5) Uani 1 1 d . . . . . C29 C 0.6713(3) 0.2656(2) 0.10090(18) 0.0265(5) Uani 1 1 d . . . . . C30 C 0.7232(3) 0.1815(3) 0.0235(2) 0.0429(7) Uani 1 1 d . . . . . H30A H 0.754965 0.106355 0.051420 0.064 Uiso 1 1 calc R U . . . H30B H 0.805817 0.195514 -0.020563 0.064 Uiso 1 1 calc R U . . . H30C H 0.642059 0.188701 -0.010056 0.064 Uiso 1 1 calc R U . . . C31 C 0.8026(3) 0.2538(2) 0.1494(2) 0.0314(6) Uani 1 1 d . . . . . H31A H 0.772751 0.307422 0.199039 0.047 Uiso 1 1 calc R U . . . H31B H 0.883075 0.267905 0.103234 0.047 Uiso 1 1 calc R U . . . H31C H 0.835913 0.178515 0.176778 0.047 Uiso 1 1 calc R U . . . C32 C 0.6207(3) 0.3813(2) 0.0541(2) 0.0351(6) Uani 1 1 d . . . . . H32A H 0.536032 0.387779 0.024185 0.053 Uiso 1 1 calc R U . . . H32B H 0.701362 0.392795 0.006530 0.053 Uiso 1 1 calc R U . . . H32C H 0.592412 0.437474 0.101598 0.053 Uiso 1 1 calc R U . . . C33 C 0.3160(3) 0.0432(2) 0.2141(2) 0.0295(6) Uani 1 1 d . . . . . C34 C 0.2164(5) 0.0837(3) 0.1418(3) 0.0685(12) Uani 1 1 d . . . . . H34A H 0.135483 0.149477 0.164219 0.103 Uiso 1 1 calc R U . . . H34B H 0.176204 0.025279 0.131400 0.103 Uiso 1 1 calc R U . . . H34C H 0.272696 0.102798 0.082727 0.103 Uiso 1 1 calc R U . . . C35 C 0.2299(5) 0.0062(4) 0.3038(3) 0.0755(14) Uani 1 1 d . . . . . H35A H 0.292489 -0.016583 0.352207 0.113 Uiso 1 1 calc R U . . . H35B H 0.199393 -0.056317 0.290790 0.113 Uiso 1 1 calc R U . . . H35C H 0.142532 0.067925 0.325954 0.113 Uiso 1 1 calc R U . . . C36 C 0.4413(4) -0.0585(2) 0.1801(3) 0.0548(10) Uani 1 1 d . . . . . H36A H 0.493840 -0.041106 0.118954 0.082 Uiso 1 1 calc R U . . . H36B H 0.401876 -0.118834 0.174008 0.082 Uiso 1 1 calc R U . . . H36C H 0.509316 -0.081398 0.225354 0.082 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.03734(17) 0.0531(2) 0.03512(17) 0.00285(14) -0.01255(13) -0.00382(14) Ga1 0.02217(14) 0.02278(14) 0.01841(14) -0.00393(10) 0.00113(10) -0.00868(11) O1 0.0307(10) 0.0288(9) 0.0261(9) -0.0100(7) 0.0075(7) -0.0165(8) O2 0.0231(9) 0.0254(9) 0.0314(10) -0.0087(7) 0.0043(7) -0.0110(7) N1 0.0223(10) 0.0234(10) 0.0196(10) -0.0037(8) 0.0001(8) -0.0068(8) N2 0.0238(10) 0.0224(10) 0.0205(10) -0.0045(8) 0.0006(8) -0.0080(8) C1 0.0219(12) 0.0217(12) 0.0242(12) -0.0012(10) -0.0034(10) -0.0066(10) C2 0.0228(12) 0.0252(12) 0.0219(12) -0.0007(10) -0.0010(10) -0.0075(10) C3 0.0222(12) 0.0258(13) 0.0294(14) -0.0001(10) -0.0008(10) -0.0096(10) C4 0.0249(12) 0.0246(13) 0.0288(13) -0.0012(10) -0.0071(10) -0.0091(10) C5 0.0270(13) 0.0240(12) 0.0236(12) -0.0051(10) -0.0025(10) -0.0087(10) C6 0.0234(12) 0.0208(12) 0.0224(12) -0.0021(9) -0.0020(10) -0.0051(10) C7 0.0245(12) 0.0212(12) 0.0211(12) -0.0048(9) -0.0019(10) -0.0050(10) C8 0.0265(13) 0.0277(13) 0.0237(13) -0.0029(10) 0.0031(10) -0.0085(11) C9 0.0367(15) 0.0398(16) 0.0261(14) -0.0048(12) -0.0023(12) -0.0130(13) C10 0.0392(16) 0.0302(15) 0.0288(15) -0.0049(11) 0.0074(12) -0.0060(12) C11 0.0400(16) 0.0416(17) 0.0286(15) -0.0029(12) 0.0065(12) -0.0197(13) C12 0.0304(14) 0.0280(14) 0.0341(15) -0.0042(11) -0.0038(11) -0.0148(11) C13 0.0435(17) 0.0463(18) 0.0475(19) -0.0031(14) -0.0151(14) -0.0243(15) C14 0.102(3) 0.058(2) 0.048(2) 0.0152(17) -0.024(2) -0.059(2) C15 0.0443(19) 0.0432(19) 0.101(3) -0.037(2) 0.0009(19) -0.0182(16) C16 0.0223(12) 0.0280(13) 0.0185(12) -0.0015(10) -0.0022(9) -0.0076(10) C17 0.0311(14) 0.0305(14) 0.0284(14) -0.0071(11) 0.0002(11) -0.0113(11) C18 0.0261(13) 0.0411(16) 0.0229(13) -0.0105(11) 0.0034(10) -0.0066(12) C19 0.0251(13) 0.0403(15) 0.0206(13) 0.0000(11) 0.0017(10) -0.0109(11) C20 0.0259(13) 0.0296(13) 0.0242(13) -0.0005(10) -0.0035(10) -0.0097(11) C21 0.0223(12) 0.0239(12) 0.0200(12) -0.0018(9) -0.0025(9) -0.0047(10) C22 0.0243(12) 0.0257(13) 0.0236(13) -0.0013(10) -0.0015(10) -0.0095(10) C23 0.0237(12) 0.0233(12) 0.0238(13) -0.0036(10) -0.0018(10) -0.0081(10) C24 0.0259(13) 0.0251(13) 0.0306(14) -0.0020(10) -0.0020(11) -0.0101(10) C25 0.0251(13) 0.0218(12) 0.0334(14) -0.0037(10) -0.0067(11) -0.0067(10) C26 0.0264(13) 0.0243(13) 0.0274(13) -0.0069(10) -0.0028(10) -0.0066(10) C27 0.0222(12) 0.0246(12) 0.0239(13) -0.0011(10) -0.0028(10) -0.0058(10) C28 0.0206(12) 0.0197(12) 0.0253(13) -0.0034(9) -0.0024(10) -0.0052(9) C29 0.0275(13) 0.0262(13) 0.0252(13) -0.0059(10) 0.0027(10) -0.0101(10) C30 0.0471(18) 0.0439(18) 0.0362(17) -0.0147(14) 0.0126(14) -0.0196(15) C31 0.0220(13) 0.0311(14) 0.0378(15) 0.0013(12) 0.0009(11) -0.0079(11) C32 0.0395(16) 0.0372(16) 0.0298(15) 0.0023(12) -0.0057(12) -0.0145(13) C33 0.0276(13) 0.0248(13) 0.0392(15) -0.0070(11) -0.0055(11) -0.0107(11) C34 0.073(3) 0.048(2) 0.107(3) 0.005(2) -0.060(3) -0.0254(19) C35 0.108(3) 0.076(3) 0.064(3) -0.029(2) 0.028(2) -0.074(3) C36 0.0434(18) 0.0259(16) 0.097(3) -0.0153(17) -0.0082(18) -0.0115(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Ga1 2.3419(4) . ? Ga1 O1 1.8745(16) . ? Ga1 O2 1.8724(17) . ? Ga1 N1 2.0335(19) . ? Ga1 N2 2.048(2) . ? O1 C1 1.309(3) . ? O2 C28 1.323(3) . ? N1 C7 1.302(3) . ? N1 C16 1.417(3) . ? N2 C21 1.412(3) . ? N2 C22 1.299(3) . ? C1 C2 1.428(3) . ? C1 C6 1.417(3) . ? C2 C3 1.380(3) . ? C2 C8 1.536(3) . ? C3 H3 0.9500 . ? C3 C4 1.410(4) . ? C4 C5 1.368(3) . ? C4 C12 1.530(3) . ? C5 H5 0.9500 . ? C5 C6 1.421(3) . ? C6 C7 1.415(3) . ? C7 H7 0.9500 . ? C8 C9 1.534(4) . ? C8 C10 1.531(4) . ? C8 C11 1.533(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.522(4) . ? C12 C14 1.524(4) . ? C12 C15 1.529(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.388(3) . ? C16 C21 1.404(3) . ? C17 H17 0.9500 . ? C17 C18 1.379(4) . ? C18 H18 0.9500 . ? C18 C19 1.386(4) . ? C19 H19 0.9500 . ? C19 C20 1.376(4) . ? C20 H20 0.9500 . ? C20 C21 1.390(3) . ? C22 H22 0.9500 . ? C22 C23 1.421(3) . ? C23 C24 1.414(3) . ? C23 C28 1.416(3) . ? C24 H24 0.9500 . ? C24 C25 1.366(4) . ? C25 C26 1.417(3) . ? C25 C33 1.528(3) . ? C26 H26 0.9500 . ? C26 C27 1.376(3) . ? C27 C28 1.427(3) . ? C27 C29 1.537(3) . ? C29 C30 1.529(4) . ? C29 C31 1.532(4) . ? C29 C32 1.533(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.507(4) . ? C33 C35 1.529(4) . ? C33 C36 1.514(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 Br1 106.76(6) . . ? O1 Ga1 N1 90.10(7) . . ? O1 Ga1 N2 153.60(8) . . ? O2 Ga1 Br1 109.32(6) . . ? O2 Ga1 O1 87.61(7) . . ? O2 Ga1 N1 145.14(8) . . ? O2 Ga1 N2 88.24(8) . . ? N1 Ga1 Br1 104.63(6) . . ? N1 Ga1 N2 78.68(8) . . ? N2 Ga1 Br1 99.21(6) . . ? C1 O1 Ga1 131.87(16) . . ? C28 O2 Ga1 127.59(15) . . ? C7 N1 Ga1 124.23(16) . . ? C7 N1 C16 122.2(2) . . ? C16 N1 Ga1 113.50(15) . . ? C21 N2 Ga1 113.58(15) . . ? C22 N2 Ga1 122.70(17) . . ? C22 N2 C21 122.3(2) . . ? O1 C1 C2 119.3(2) . . ? O1 C1 C6 122.5(2) . . ? C6 C1 C2 118.2(2) . . ? C1 C2 C8 121.2(2) . . ? C3 C2 C1 117.7(2) . . ? C3 C2 C8 121.0(2) . . ? C2 C3 H3 117.4 . . ? C2 C3 C4 125.2(2) . . ? C4 C3 H3 117.4 . . ? C3 C4 C12 120.8(2) . . ? C5 C4 C3 116.5(2) . . ? C5 C4 C12 122.6(2) . . ? C4 C5 H5 119.2 . . ? C4 C5 C6 121.6(2) . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 120.6(2) . . ? C7 C6 C1 122.9(2) . . ? C7 C6 C5 116.4(2) . . ? N1 C7 C6 126.8(2) . . ? N1 C7 H7 116.6 . . ? C6 C7 H7 116.6 . . ? C9 C8 C2 109.7(2) . . ? C10 C8 C2 110.8(2) . . ? C10 C8 C9 109.8(2) . . ? C10 C8 C11 107.4(2) . . ? C11 C8 C2 112.1(2) . . ? C11 C8 C9 107.0(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C4 109.2(2) . . ? C13 C12 C14 109.3(3) . . ? C13 C12 C15 108.7(3) . . ? C14 C12 C4 110.9(2) . . ? C14 C12 C15 107.7(3) . . ? C15 C12 C4 111.0(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N1 125.5(2) . . ? C17 C16 C21 119.6(2) . . ? C21 C16 N1 114.9(2) . . ? C16 C17 H17 120.0 . . ? C18 C17 C16 120.0(2) . . ? C18 C17 H17 120.0 . . ? C17 C18 H18 119.8 . . ? C17 C18 C19 120.3(2) . . ? C19 C18 H18 119.8 . . ? C18 C19 H19 119.8 . . ? C20 C19 C18 120.3(2) . . ? C20 C19 H19 119.8 . . ? C19 C20 H20 120.0 . . ? C19 C20 C21 120.0(2) . . ? C21 C20 H20 120.0 . . ? C16 C21 N2 114.5(2) . . ? C20 C21 N2 125.7(2) . . ? C20 C21 C16 119.7(2) . . ? N2 C22 H22 117.2 . . ? N2 C22 C23 125.7(2) . . ? C23 C22 H22 117.2 . . ? C24 C23 C22 116.9(2) . . ? C24 C23 C28 120.3(2) . . ? C28 C23 C22 122.9(2) . . ? C23 C24 H24 118.9 . . ? C25 C24 C23 122.2(2) . . ? C25 C24 H24 118.9 . . ? C24 C25 C26 116.0(2) . . ? C24 C25 C33 123.5(2) . . ? C26 C25 C33 120.4(2) . . ? C25 C26 H26 117.4 . . ? C27 C26 C25 125.3(2) . . ? C27 C26 H26 117.4 . . ? C26 C27 C28 117.5(2) . . ? C26 C27 C29 121.4(2) . . ? C28 C27 C29 121.0(2) . . ? O2 C28 C23 121.6(2) . . ? O2 C28 C27 119.7(2) . . ? C23 C28 C27 118.6(2) . . ? C30 C29 C27 112.3(2) . . ? C30 C29 C31 107.7(2) . . ? C30 C29 C32 107.6(2) . . ? C31 C29 C27 108.8(2) . . ? C31 C29 C32 110.5(2) . . ? C32 C29 C27 110.0(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C25 C33 C35 111.5(2) . . ? C34 C33 C25 108.9(2) . . ? C34 C33 C35 109.1(3) . . ? C34 C33 C36 109.9(3) . . ? C36 C33 C25 111.2(2) . . ? C36 C33 C35 106.3(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Ga1 O1 C1 90.8(2) . . . . ? Br1 Ga1 O2 C28 -61.7(2) . . . . ? Ga1 O1 C1 C2 -167.36(18) . . . . ? Ga1 O1 C1 C6 13.9(4) . . . . ? Ga1 O2 C28 C23 -30.9(3) . . . . ? Ga1 O2 C28 C27 150.82(18) . . . . ? Ga1 N1 C7 C6 -3.5(4) . . . . ? Ga1 N1 C16 C17 -161.9(2) . . . . ? Ga1 N1 C16 C21 16.8(3) . . . . ? Ga1 N2 C21 C16 -14.8(3) . . . . ? Ga1 N2 C21 C20 164.7(2) . . . . ? Ga1 N2 C22 C23 12.1(3) . . . . ? O1 Ga1 O2 C28 -168.7(2) . . . . ? O1 C1 C2 C3 -173.9(2) . . . . ? O1 C1 C2 C8 8.0(4) . . . . ? O1 C1 C6 C5 175.9(2) . . . . ? O1 C1 C6 C7 -3.0(4) . . . . ? O2 Ga1 O1 C1 -159.8(2) . . . . ? N1 Ga1 O1 C1 -14.6(2) . . . . ? N1 Ga1 O2 C28 104.6(2) . . . . ? N1 C16 C17 C18 179.7(2) . . . . ? N1 C16 C21 N2 -1.2(3) . . . . ? N1 C16 C21 C20 179.2(2) . . . . ? N2 Ga1 O1 C1 -78.6(3) . . . . ? N2 Ga1 O2 C28 37.4(2) . . . . ? N2 C22 C23 C24 -173.5(2) . . . . ? N2 C22 C23 C28 6.6(4) . . . . ? C1 C2 C3 C4 -4.3(4) . . . . ? C1 C2 C8 C9 56.9(3) . . . . ? C1 C2 C8 C10 -64.5(3) . . . . ? C1 C2 C8 C11 175.6(2) . . . . ? C1 C6 C7 N1 -1.6(4) . . . . ? C2 C1 C6 C5 -2.8(4) . . . . ? C2 C1 C6 C7 178.2(2) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C2 C3 C4 C12 -179.8(2) . . . . ? C3 C2 C8 C9 -121.1(3) . . . . ? C3 C2 C8 C10 117.5(3) . . . . ? C3 C2 C8 C11 -2.4(3) . . . . ? C3 C4 C5 C6 1.0(4) . . . . ? C3 C4 C12 C13 -88.1(3) . . . . ? C3 C4 C12 C14 32.4(4) . . . . ? C3 C4 C12 C15 152.1(3) . . . . ? C4 C5 C6 C1 -0.2(4) . . . . ? C4 C5 C6 C7 178.8(2) . . . . ? C5 C4 C12 C13 90.8(3) . . . . ? C5 C4 C12 C14 -148.7(3) . . . . ? C5 C4 C12 C15 -29.0(4) . . . . ? C5 C6 C7 N1 179.5(2) . . . . ? C6 C1 C2 C3 4.9(3) . . . . ? C6 C1 C2 C8 -173.2(2) . . . . ? C7 N1 C16 C17 14.4(4) . . . . ? C7 N1 C16 C21 -166.9(2) . . . . ? C8 C2 C3 C4 173.8(2) . . . . ? C12 C4 C5 C6 -177.9(2) . . . . ? C16 N1 C7 C6 -179.4(2) . . . . ? C16 C17 C18 C19 0.3(4) . . . . ? C17 C16 C21 N2 177.6(2) . . . . ? C17 C16 C21 C20 -2.0(4) . . . . ? C17 C18 C19 C20 -0.5(4) . . . . ? C18 C19 C20 C21 -0.5(4) . . . . ? C19 C20 C21 N2 -177.8(2) . . . . ? C19 C20 C21 C16 1.7(4) . . . . ? C21 N2 C22 C23 177.8(2) . . . . ? C21 C16 C17 C18 1.0(4) . . . . ? C22 N2 C21 C16 178.3(2) . . . . ? C22 N2 C21 C20 -2.1(4) . . . . ? C22 C23 C24 C25 178.6(2) . . . . ? C22 C23 C28 O2 1.4(4) . . . . ? C22 C23 C28 C27 179.7(2) . . . . ? C23 C24 C25 C26 1.2(4) . . . . ? C23 C24 C25 C33 -175.8(2) . . . . ? C24 C23 C28 O2 -178.6(2) . . . . ? C24 C23 C28 C27 -0.3(4) . . . . ? C24 C25 C26 C27 0.7(4) . . . . ? C24 C25 C33 C34 99.8(3) . . . . ? C24 C25 C33 C35 -20.6(4) . . . . ? C24 C25 C33 C36 -139.0(3) . . . . ? C25 C26 C27 C28 -2.3(4) . . . . ? C25 C26 C27 C29 178.9(2) . . . . ? C26 C25 C33 C34 -77.1(3) . . . . ? C26 C25 C33 C35 162.5(3) . . . . ? C26 C25 C33 C36 44.1(4) . . . . ? C26 C27 C28 O2 -179.6(2) . . . . ? C26 C27 C28 C23 2.0(3) . . . . ? C26 C27 C29 C30 -1.0(4) . . . . ? C26 C27 C29 C31 -120.1(3) . . . . ? C26 C27 C29 C32 118.7(3) . . . . ? C28 C23 C24 C25 -1.4(4) . . . . ? C28 C27 C29 C30 -179.7(2) . . . . ? C28 C27 C29 C31 61.2(3) . . . . ? C28 C27 C29 C32 -60.0(3) . . . . ? C29 C27 C28 O2 -0.8(4) . . . . ? C29 C27 C28 C23 -179.2(2) . . . . ? C33 C25 C26 C27 177.8(2) . . . . ? _shelx_res_file ; TITL megm_lamgabra_0m_a.res in P-1 megm_lamgabra_0m.res created by SHELXL-2018/3 at 16:32:15 on 09-Jun-2022 REM Old TITL megm_lamgabra_0m_a.res in P-1 REM SHELXT solution in P-1: R1 0.120, Rweak 0.011, Alpha 0.039 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C36 Br2 N2 O2 CELL 0.71073 9.7269 12.7417 14.5254 84.461 78.992 71.35 ZERR 2 0.0004 0.0006 0.0007 0.002 0.002 0.002 LATT 1 SFAC C H Br Ga N O UNIT 72 92 2 2 4 4 L.S. 4 PLAN 8 SIZE 0.14 0.203 0.234 TEMP -73.15 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 1 -1 2 OMIT -1 1 0 REM REM REM WGHT 0.041700 1.056800 FVAR 0.36784 BR1 3 0.235626 0.630610 0.237963 11.00000 0.03734 0.05308 = 0.03512 0.00285 -0.01255 -0.00382 GA1 4 0.426504 0.532936 0.319702 11.00000 0.02217 0.02278 = 0.01841 -0.00393 0.00113 -0.00868 O1 6 0.588181 0.582362 0.269014 11.00000 0.03075 0.02882 = 0.02609 -0.00999 0.00746 -0.01648 O2 6 0.530846 0.398192 0.262547 11.00000 0.02311 0.02539 = 0.03140 -0.00871 0.00430 -0.01095 N1 5 0.390459 0.621575 0.435880 11.00000 0.02234 0.02341 = 0.01960 -0.00368 0.00013 -0.00679 N2 5 0.315418 0.448449 0.417112 11.00000 0.02382 0.02240 = 0.02051 -0.00449 0.00061 -0.00801 C1 1 0.630735 0.662578 0.291729 11.00000 0.02191 0.02169 = 0.02418 -0.00121 -0.00341 -0.00655 C2 1 0.742525 0.695931 0.228856 11.00000 0.02277 0.02518 = 0.02186 -0.00070 -0.00098 -0.00752 C3 1 0.794607 0.773261 0.258928 11.00000 0.02219 0.02580 = 0.02942 -0.00012 -0.00076 -0.00965 AFIX 43 H3 2 0.873677 0.791398 0.218688 11.00000 -1.20000 AFIX 0 C4 1 0.739793 0.827458 0.344600 11.00000 0.02493 0.02456 = 0.02884 -0.00120 -0.00707 -0.00908 C5 1 0.627968 0.798588 0.402363 11.00000 0.02699 0.02396 = 0.02358 -0.00505 -0.00247 -0.00872 AFIX 43 H5 2 0.586729 0.834057 0.460324 11.00000 -1.20000 AFIX 0 C6 1 0.571992 0.716825 0.377769 11.00000 0.02340 0.02080 = 0.02242 -0.00211 -0.00204 -0.00511 C7 1 0.458197 0.692471 0.444000 11.00000 0.02446 0.02121 = 0.02107 -0.00475 -0.00194 -0.00499 AFIX 43 H7 2 0.428055 0.732015 0.500317 11.00000 -1.20000 AFIX 0 C8 1 0.799459 0.650288 0.130006 11.00000 0.02647 0.02765 = 0.02367 -0.00286 0.00306 -0.00854 C9 1 0.670550 0.675045 0.076272 11.00000 0.03670 0.03984 = 0.02615 -0.00484 -0.00229 -0.01302 AFIX 137 H9A 2 0.594755 0.644987 0.112475 11.00000 -1.50000 H9B 2 0.705867 0.640565 0.015196 11.00000 -1.50000 H9C 2 0.628692 0.755396 0.066825 11.00000 -1.50000 AFIX 0 C10 1 0.876956 0.525176 0.134988 11.00000 0.03916 0.03015 = 0.02876 -0.00488 0.00743 -0.00603 AFIX 137 H10A 2 0.966586 0.510543 0.161941 11.00000 -1.50000 H10B 2 0.902923 0.496461 0.071681 11.00000 -1.50000 H10C 2 0.810958 0.488452 0.174531 11.00000 -1.50000 AFIX 0 C11 1 0.910162 0.704278 0.072521 11.00000 0.03999 0.04160 = 0.02857 -0.00290 0.00651 -0.01968 AFIX 137 H11A 2 0.863921 0.784711 0.068003 11.00000 -1.50000 H11B 2 0.941024 0.674852 0.009408 11.00000 -1.50000 H11C 2 0.996320 0.687790 0.103401 11.00000 -1.50000 AFIX 0 C12 1 0.805583 0.912390 0.370838 11.00000 0.03036 0.02805 = 0.03414 -0.00420 -0.00380 -0.01479 C13 1 0.934552 0.852765 0.421136 11.00000 0.04351 0.04630 = 0.04748 -0.00310 -0.01507 -0.02431 AFIX 137 H13A 2 0.899944 0.814463 0.478269 11.00000 -1.50000 H13B 2 0.977292 0.906850 0.437820 11.00000 -1.50000 H13C 2 1.009435 0.798603 0.379696 11.00000 -1.50000 AFIX 0 C14 1 0.859038 0.974734 0.283720 11.00000 0.10200 0.05776 = 0.04839 0.01519 -0.02447 -0.05923 AFIX 137 H14A 2 0.942133 0.923354 0.244770 11.00000 -1.50000 H14B 2 0.890584 1.034015 0.302612 11.00000 -1.50000 H14C 2 0.778779 1.006931 0.247744 11.00000 -1.50000 AFIX 0 C15 1 0.691399 0.997847 0.435900 11.00000 0.04427 0.04325 = 0.10066 -0.03743 0.00094 -0.01816 AFIX 137 H15A 2 0.606583 1.035550 0.404924 11.00000 -1.50000 H15B 2 0.735308 1.052376 0.450256 11.00000 -1.50000 H15C 2 0.659104 0.960401 0.494232 11.00000 -1.50000 AFIX 0 C16 1 0.276471 0.604452 0.506542 11.00000 0.02233 0.02804 = 0.01846 -0.00154 -0.00219 -0.00761 C17 1 0.202665 0.673387 0.580545 11.00000 0.03109 0.03053 = 0.02839 -0.00707 0.00017 -0.01135 AFIX 43 H17 2 0.227841 0.738167 0.586912 11.00000 -1.20000 AFIX 0 C18 1 0.092790 0.647883 0.644841 11.00000 0.02610 0.04114 = 0.02289 -0.01055 0.00343 -0.00664 AFIX 43 H18 2 0.042198 0.695390 0.695267 11.00000 -1.20000 AFIX 0 C19 1 0.055817 0.553261 0.636243 11.00000 0.02506 0.04030 = 0.02065 0.00002 0.00174 -0.01091 AFIX 43 H19 2 -0.019438 0.535943 0.681103 11.00000 -1.20000 AFIX 0 C20 1 0.127532 0.484314 0.563093 11.00000 0.02593 0.02964 = 0.02421 -0.00055 -0.00347 -0.00974 AFIX 43 H20 2 0.102300 0.419274 0.557805 11.00000 -1.20000 AFIX 0 C21 1 0.236920 0.509837 0.496921 11.00000 0.02228 0.02386 = 0.01998 -0.00185 -0.00253 -0.00465 C22 1 0.294649 0.357280 0.399086 11.00000 0.02425 0.02570 = 0.02360 -0.00130 -0.00146 -0.00948 AFIX 43 H22 2 0.226155 0.331369 0.443360 11.00000 -1.20000 AFIX 0 C23 1 0.365442 0.292941 0.318927 11.00000 0.02368 0.02332 = 0.02379 -0.00358 -0.00184 -0.00814 C24 1 0.316097 0.202771 0.307314 11.00000 0.02589 0.02513 = 0.03060 -0.00196 -0.00199 -0.01010 AFIX 43 H24 2 0.240424 0.187881 0.353399 11.00000 -1.20000 AFIX 0 C25 1 0.373566 0.136375 0.232079 11.00000 0.02514 0.02181 = 0.03335 -0.00369 -0.00670 -0.00670 C26 1 0.487999 0.161723 0.166965 11.00000 0.02642 0.02428 = 0.02740 -0.00694 -0.00279 -0.00660 AFIX 43 H26 2 0.528727 0.117030 0.113749 11.00000 -1.20000 AFIX 0 C27 1 0.544947 0.245852 0.174558 11.00000 0.02217 0.02458 = 0.02388 -0.00114 -0.00277 -0.00580 C28 1 0.480342 0.315799 0.252537 11.00000 0.02063 0.01967 = 0.02535 -0.00335 -0.00244 -0.00525 C29 1 0.671344 0.265566 0.100899 11.00000 0.02748 0.02625 = 0.02521 -0.00588 0.00273 -0.01007 C30 1 0.723200 0.181489 0.023477 11.00000 0.04709 0.04389 = 0.03623 -0.01468 0.01257 -0.01963 AFIX 137 H30A 2 0.754965 0.106355 0.051420 11.00000 -1.50000 H30B 2 0.805817 0.195514 -0.020563 11.00000 -1.50000 H30C 2 0.642059 0.188701 -0.010056 11.00000 -1.50000 AFIX 0 C31 1 0.802599 0.253791 0.149354 11.00000 0.02202 0.03111 = 0.03775 0.00133 0.00094 -0.00787 AFIX 137 H31A 2 0.772751 0.307422 0.199039 11.00000 -1.50000 H31B 2 0.883075 0.267905 0.103234 11.00000 -1.50000 H31C 2 0.835913 0.178515 0.176778 11.00000 -1.50000 AFIX 0 C32 1 0.620721 0.381349 0.054079 11.00000 0.03951 0.03724 = 0.02975 0.00234 -0.00566 -0.01449 AFIX 137 H32A 2 0.536032 0.387779 0.024185 11.00000 -1.50000 H32B 2 0.701362 0.392795 0.006530 11.00000 -1.50000 H32C 2 0.592412 0.437474 0.101598 11.00000 -1.50000 AFIX 0 C33 1 0.315989 0.043155 0.214083 11.00000 0.02759 0.02475 = 0.03919 -0.00702 -0.00547 -0.01073 C34 1 0.216380 0.083726 0.141783 11.00000 0.07279 0.04757 = 0.10726 0.00487 -0.06023 -0.02540 AFIX 137 H34A 2 0.135483 0.149477 0.164219 11.00000 -1.50000 H34B 2 0.176204 0.025279 0.131400 11.00000 -1.50000 H34C 2 0.272696 0.102798 0.082727 11.00000 -1.50000 AFIX 0 C35 1 0.229868 0.006229 0.303816 11.00000 0.10754 0.07610 = 0.06361 -0.02888 0.02827 -0.07420 AFIX 137 H35A 2 0.292489 -0.016583 0.352207 11.00000 -1.50000 H35B 2 0.199393 -0.056317 0.290790 11.00000 -1.50000 H35C 2 0.142532 0.067925 0.325954 11.00000 -1.50000 AFIX 0 C36 1 0.441299 -0.058506 0.180105 11.00000 0.04339 0.02588 = 0.09686 -0.01526 -0.00820 -0.01146 AFIX 137 H36A 2 0.493840 -0.041106 0.118954 11.00000 -1.50000 H36B 2 0.401876 -0.118834 0.174008 11.00000 -1.50000 H36C 2 0.509316 -0.081398 0.225354 11.00000 -1.50000 AFIX 0 HKLF 4 REM megm_lamgabra_0m_a.res in P-1 REM wR2 = 0.094260, GooF = S = 1.04699, Restrained GooF = 1.04699 for all data REM R1 = 0.039124 for 6089 Fo > 4sig(Fo) and 0.063990 for all 7986 data REM 391 parameters refined using 0 restraints END WGHT 0.0327 1.4751 REM Highest difference peak 0.562, deepest hole -0.624, 1-sigma level 0.070 Q1 1 0.2800 0.6768 0.2177 11.00000 0.05 0.56 Q2 1 0.3545 0.5026 0.3661 11.00000 0.05 0.49 Q3 1 0.2327 0.6153 0.2975 11.00000 0.05 0.40 Q4 1 0.4950 0.5613 0.2815 11.00000 0.05 0.39 Q5 1 0.4985 0.4162 0.3150 11.00000 0.05 0.39 Q6 1 0.2712 0.6804 0.2701 11.00000 0.05 0.37 Q7 1 0.6233 0.6841 0.3441 11.00000 0.05 0.35 Q8 1 0.5019 0.3585 0.2651 11.00000 0.05 0.35 ; _shelx_res_checksum 60681 _shelx_hkl_file ; -2 0 0 1121.21 32.21 -2 0 0 1033.24 31.56 -2 0 0 937.46 32.22 -2 0 0 1029.69 32.28 -2 0 0 1000.51 31.50 -2 0 0 1078.67 31.59 -2 0 0 1082.39 32.67 -2 0 0 1054.93 31.55 -2 0 0 1060.33 32.61 -2 0 0 1048.53 33.48 2 0 0 1097.99 32.18 2 0 0 965.72 31.35 2 0 0 1054.88 32.64 2 0 0 1016.18 32.56 2 0 0 965.91 31.36 2 0 0 1055.17 33.45 2 0 0 1097.07 32.73 -3 0 0 86.68 6.18 -3 0 0 81.24 5.51 -3 0 0 84.09 4.85 -3 0 0 82.09 4.76 -3 0 0 83.84 5.94 -3 0 0 78.91 4.74 -3 0 0 81.54 5.48 -3 0 0 74.64 6.16 -3 0 0 77.82 4.71 -3 0 0 90.01 5.48 3 0 0 82.45 4.65 3 0 0 84.86 5.97 3 0 0 84.50 6.12 3 0 0 79.97 4.48 3 0 0 101.11 6.31 3 0 0 85.26 5.40 3 0 0 88.93 6.27 3 0 0 73.47 4.46 -4 0 0 114.51 6.86 -4 0 0 114.88 6.84 -4 0 0 117.46 7.05 -4 0 0 119.19 8.96 -4 0 0 132.10 7.22 -4 0 0 119.52 8.31 -4 0 0 122.60 7.80 -4 0 0 116.39 8.72 4 0 0 119.29 6.69 4 0 0 109.30 6.40 4 0 0 108.79 8.79 4 0 0 130.38 7.75 4 0 0 112.60 8.39 4 0 0 121.92 8.74 4 0 0 133.27 9.07 4 0 0 123.13 6.68 -5 0 0 193.66 9.86 -5 0 0 196.07 9.64 -5 0 0 159.37 12.04 -5 0 0 189.59 9.81 -5 0 0 191.95 9.56 -5 0 0 161.71 9.71 -5 0 0 188.18 10.67 -5 0 0 179.92 11.53 -5 0 0 203.54 11.59 5 0 0 171.01 9.06 5 0 0 187.50 17.45 5 0 0 186.66 12.04 5 0 0 178.38 9.11 5 0 0 194.38 12.24 5 0 0 186.03 10.45 5 0 0 209.09 12.15 5 0 0 194.43 9.21 -6 0 0 594.60 22.15 -6 0 0 526.93 32.32 -6 0 0 601.35 22.29 -6 0 0 598.99 24.42 -6 0 0 638.98 23.71 -6 0 0 569.97 21.88 -6 0 0 554.86 24.31 -6 0 0 586.83 21.90 6 0 0 630.38 25.66 6 0 0 601.17 25.24 6 0 0 575.72 23.04 6 0 0 594.88 21.39 6 0 0 607.02 25.25 6 0 0 599.07 21.39 6 0 0 598.31 26.14 6 0 0 597.00 21.51 6 0 0 620.98 21.54 -7 0 0 -1.00 4.89 -7 0 0 -2.27 4.00 -7 0 0 -3.13 5.20 -7 0 0 0.04 4.85 -7 0 0 3.25 4.43 -7 0 0 -0.37 5.09 -7 0 0 -4.39 5.83 -7 0 0 -0.91 4.82 7 0 0 -7.15 6.16 7 0 0 4.29 4.08 7 0 0 0.13 4.39 7 0 0 -0.79 3.87 7 0 0 -3.93 4.47 7 0 0 1.70 3.93 7 0 0 -1.38 6.11 -8 0 0 6.03 6.63 -8 0 0 9.93 6.76 -8 0 0 7.89 6.10 -8 0 0 3.56 7.83 -8 0 0 13.08 6.03 -8 0 0 7.51 6.71 -8 0 0 21.60 8.67 -8 0 0 12.49 5.41 8 0 0 7.08 8.64 8 0 0 11.65 5.62 8 0 0 10.37 5.42 8 0 0 9.74 5.33 8 0 0 14.45 6.57 8 0 0 5.19 7.41 8 0 0 20.65 6.75 8 0 0 16.05 5.25 -9 0 0 97.91 10.81 -9 0 0 110.15 17.15 -9 0 0 95.16 11.56 -9 0 0 81.37 10.69 -9 0 0 79.59 9.96 -9 0 0 84.70 12.98 -9 0 0 88.10 11.04 9 0 0 103.20 9.65 9 0 0 102.76 12.16 9 0 0 78.17 10.15 9 0 0 102.27 15.55 9 0 0 101.30 9.49 9 0 0 112.87 9.84 9 0 0 87.24 13.22 -10 0 0 -1.90 6.42 -10 0 0 6.98 8.39 -10 0 0 -4.33 6.96 -10 0 0 5.08 6.50 -10 0 0 0.35 8.31 -10 0 0 7.99 7.88 10 0 0 0.88 5.97 10 0 0 2.87 7.17 10 0 0 10.73 11.03 10 0 0 9.15 6.25 10 0 0 8.97 6.00 10 0 0 -2.41 9.08 -11 0 0 14.36 8.28 -11 0 0 18.84 11.69 -11 0 0 -4.45 7.44 -11 0 0 17.85 8.20 -11 0 0 29.19 11.64 -11 0 0 17.89 7.95 -11 0 0 7.21 11.60 11 0 0 20.19 12.15 11 0 0 21.18 6.73 11 0 0 16.02 12.89 11 -1 0 23.25 12.34 11 -1 0 56.87 9.57 11 -1 0 65.32 15.06 11 -1 0 35.84 14.99 -11 1 0 41.57 12.91 -11 1 0 36.46 9.57 -11 1 0 30.04 10.04 -11 1 0 27.96 9.56 -11 1 0 35.93 12.94 -11 1 0 31.21 11.08 -11 1 0 35.04 9.57 10 -1 0 -11.95 8.28 10 -1 0 5.61 6.83 10 -1 0 9.24 6.82 10 -1 0 1.92 7.67 10 -1 0 -14.65 12.63 -10 1 0 11.55 8.86 -10 1 0 7.98 8.63 -10 1 0 5.48 9.85 -10 1 0 3.63 7.15 -10 1 0 -0.77 7.03 -10 1 0 3.36 6.99 -10 1 0 9.91 11.19 9 -1 0 78.96 9.66 9 -1 0 53.57 12.74 9 -1 0 70.52 10.90 9 -1 0 51.44 11.61 9 -1 0 89.92 10.92 9 -1 0 79.86 10.88 9 -1 0 50.46 8.52 -9 1 0 70.14 14.81 -9 1 0 70.18 10.03 -9 1 0 67.49 10.00 -9 1 0 47.53 11.15 -9 1 0 86.71 12.10 -9 1 0 63.77 9.92 -9 1 0 74.37 11.10 8 -1 0 18.14 6.28 8 -1 0 9.15 7.16 8 -1 0 21.15 9.32 8 -1 0 26.65 9.48 8 -1 0 9.91 5.92 8 -1 0 11.17 6.37 8 -1 0 7.60 8.95 8 -1 0 12.88 6.09 8 -1 0 9.12 6.13 -8 1 0 5.83 7.35 -8 1 0 13.72 7.62 -8 1 0 2.84 6.80 -8 1 0 7.76 6.29 -8 1 0 12.07 6.38 -8 1 0 11.47 8.49 -8 1 0 17.67 8.61 -8 1 0 17.20 6.71 7 -1 0 13.51 7.52 7 -1 0 7.89 5.06 7 -1 0 4.36 7.63 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1995.75 60.14 2 3 0 2070.81 61.95 2 3 0 2051.26 60.65 2 3 0 2037.02 62.06 2 3 0 2049.47 60.49 -3 -3 0 48.81 5.62 -3 -3 0 44.42 4.14 -3 -3 0 48.52 3.16 -3 -3 0 47.13 3.21 -3 -3 0 50.14 3.17 -3 -3 0 52.15 4.12 -3 -3 0 46.40 4.42 -3 -3 0 46.61 4.18 -3 -3 0 54.09 3.27 3 3 0 47.30 2.72 3 3 0 47.62 2.71 3 3 0 48.29 5.03 3 3 0 48.10 2.91 3 3 0 51.34 3.04 3 3 0 53.65 4.52 3 3 0 43.13 4.16 3 3 0 53.17 4.17 3 3 0 59.22 6.07 -4 -3 0 15.67 2.38 -4 -3 0 23.38 4.24 -4 -3 0 16.39 2.49 -4 -3 0 15.00 2.83 -4 -3 0 20.31 4.28 -4 -3 0 19.35 4.80 -4 -3 0 13.72 2.44 -4 -3 0 12.52 3.88 -4 -3 0 10.82 2.51 4 3 0 17.67 2.04 4 3 0 11.26 4.38 4 3 0 10.94 4.16 4 3 0 17.63 3.26 4 3 0 17.10 1.90 4 3 0 13.48 4.45 4 3 0 14.58 4.06 -5 -3 0 354.51 12.35 -5 -3 0 363.32 12.44 -5 -3 0 377.56 16.90 -5 -3 0 359.51 14.14 -5 -3 0 349.59 15.43 -5 -3 0 369.29 12.81 -5 -3 0 371.04 12.89 -5 -3 0 377.42 16.98 5 3 0 332.47 11.26 5 3 0 364.71 15.80 5 3 0 351.19 11.58 5 3 0 345.80 11.49 5 3 0 360.43 14.14 5 3 0 366.92 16.59 -6 -3 0 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54.07 12.84 8 -4 0 66.84 13.61 8 -4 0 66.82 13.42 -8 4 0 73.99 12.91 -8 4 0 62.10 17.44 -8 4 0 52.52 11.01 -8 4 0 54.95 18.05 -8 4 0 54.47 12.26 -8 4 0 62.02 11.98 -8 4 0 58.47 13.06 7 -4 0 148.99 18.48 7 -4 0 158.08 14.21 7 -4 0 170.26 14.17 7 -4 0 185.51 23.11 7 -4 0 172.52 17.00 7 -4 0 159.02 13.54 7 -4 0 160.10 17.88 7 -4 0 163.97 15.19 -7 4 0 189.50 15.94 -7 4 0 144.60 15.69 -7 4 0 188.56 14.76 -7 4 0 161.26 16.33 -7 4 0 172.09 20.81 -7 4 0 162.36 14.83 6 -4 0 2.51 6.68 6 -4 0 -1.95 5.87 6 -4 0 -3.42 6.37 6 -4 0 0.50 5.72 6 -4 0 -5.16 6.54 6 -4 0 -2.40 5.76 6 -4 0 -1.02 6.72 6 -4 0 5.07 5.28 6 -4 0 -1.13 6.42 -6 4 0 -0.10 7.02 -6 4 0 7.67 7.05 -6 4 0 0.72 6.55 -6 4 0 9.83 8.43 -6 4 0 0.92 7.04 -6 4 0 -5.79 6.44 5 -4 0 20.45 5.93 5 -4 0 23.88 6.77 5 -4 0 30.85 7.95 5 -4 0 30.46 7.12 5 -4 0 14.61 10.47 5 -4 0 33.16 8.38 5 -4 0 24.77 6.50 5 -4 0 27.24 6.83 5 -4 0 16.51 7.07 -5 4 0 29.09 7.34 -5 4 0 18.68 7.14 -5 4 0 27.45 7.17 -5 4 0 23.61 8.12 -5 4 0 23.85 6.74 -5 4 0 22.70 6.51 4 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5.65 -3 -4 0 115.83 5.53 -3 -4 0 107.45 6.01 -3 -4 0 112.59 5.55 -3 -4 0 106.10 6.82 -3 -4 0 111.93 5.77 -3 -4 0 113.33 5.62 3 4 0 111.67 5.15 3 4 0 116.79 7.72 3 4 0 103.59 5.10 3 4 0 110.48 5.59 3 4 0 106.50 6.55 3 4 0 107.98 6.18 3 4 0 123.37 7.35 3 4 0 107.86 6.84 3 4 0 111.09 5.66 -4 -4 0 105.86 7.07 -4 -4 0 116.99 5.79 -4 -4 0 125.14 5.83 -4 -4 0 120.67 5.92 -4 -4 0 121.34 7.50 -4 -4 0 116.33 9.49 -4 -4 0 122.02 5.79 4 4 0 104.10 8.53 4 4 0 118.34 8.23 4 4 0 105.46 4.83 4 4 0 119.18 5.34 4 4 0 109.30 6.92 4 4 0 103.02 7.70 4 4 0 107.41 7.23 4 4 0 114.01 5.16 4 4 0 113.55 4.81 -5 -4 0 90.73 9.17 -5 -4 0 76.76 4.98 -5 -4 0 82.27 5.47 -5 -4 0 97.48 5.09 -5 -4 0 87.10 5.22 -5 -4 0 86.65 7.40 5 4 0 100.92 8.48 5 4 0 83.85 3.15 5 4 0 77.88 8.33 5 4 0 84.70 6.04 5 4 0 83.30 3.71 5 4 0 82.38 3.25 5 4 0 92.89 7.76 5 4 0 84.34 3.54 -6 -4 0 41.58 4.05 -6 -4 0 49.92 7.70 -6 -4 0 43.22 6.64 -6 -4 0 44.21 4.78 -6 -4 0 48.04 8.25 -6 -4 0 40.45 4.28 -6 -4 0 47.99 4.11 6 4 0 53.71 8.33 6 4 0 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22.90 10.37 -7 7 0 3.40 9.22 -7 7 0 9.98 9.40 -7 7 0 -8.01 9.61 6 -7 0 23.95 9.10 6 -7 0 20.06 9.78 6 -7 0 24.37 10.31 6 -7 0 29.97 10.08 6 -7 0 33.64 9.18 6 -7 0 19.17 10.55 6 -7 0 22.00 9.88 6 -7 0 21.31 10.52 6 -7 0 28.21 11.82 -6 7 0 34.63 11.19 -6 7 0 36.05 10.71 -6 7 0 32.73 14.73 -6 7 0 29.71 10.29 -6 7 0 24.97 10.87 -6 7 0 33.78 10.81 5 -7 0 148.90 14.84 5 -7 0 131.00 14.32 5 -7 0 127.69 13.87 5 -7 0 120.28 14.37 5 -7 0 133.09 15.28 5 -7 0 134.59 15.34 5 -7 0 127.76 15.14 5 -7 0 125.06 12.50 5 -7 0 131.19 21.30 -5 7 0 124.17 15.09 -5 7 0 123.73 14.84 -5 7 0 140.48 14.31 -5 7 0 123.15 14.57 -5 7 0 141.40 21.92 -5 7 0 107.00 13.83 -5 7 0 131.19 15.32 4 -7 0 16.88 6.37 4 -7 0 23.90 7.21 4 -7 0 28.97 8.53 4 -7 0 24.69 9.37 4 -7 0 40.99 8.99 4 -7 0 40.28 9.58 4 -7 0 47.00 9.05 4 -7 0 20.96 8.71 4 -7 0 30.77 11.91 -4 7 0 25.41 8.50 -4 7 0 32.77 7.50 -4 7 0 30.18 9.24 -4 7 0 32.27 10.34 -4 7 0 25.50 8.48 -4 7 0 26.32 9.04 -4 7 0 25.13 7.80 -4 7 0 27.12 9.23 3 -7 0 79.88 10.29 3 -7 0 80.37 10.29 3 -7 0 80.03 14.67 3 -7 0 70.39 9.86 3 -7 0 85.23 10.56 3 -7 0 59.69 8.74 3 -7 0 62.08 7.41 3 -7 0 59.35 9.01 3 -7 0 90.17 11.01 -3 7 0 111.46 23.31 -3 7 0 75.12 10.32 -3 7 0 72.71 10.77 -3 7 0 50.48 9.38 -3 7 0 70.00 10.24 -3 7 0 83.40 11.55 -3 7 0 87.51 9.75 -3 7 0 85.41 8.84 2 -7 0 382.90 18.25 2 -7 0 384.14 18.74 2 -7 0 356.13 16.72 2 -7 0 397.56 24.77 2 -7 0 356.66 18.07 2 -7 0 366.65 18.05 -2 7 0 355.33 17.94 -2 7 0 345.76 14.31 -2 7 0 380.90 24.10 -2 7 0 368.38 16.00 -2 7 0 366.17 18.84 -2 7 0 355.78 18.68 -2 7 0 333.59 17.65 1 -7 0 81.84 9.21 1 -7 0 69.26 9.22 1 -7 0 75.08 10.12 1 -7 0 58.86 6.68 1 -7 0 116.38 20.23 1 -7 0 59.18 8.51 1 -7 0 79.20 9.23 -1 7 0 71.83 11.28 -1 7 0 55.64 4.69 -1 7 0 64.20 9.09 -1 7 0 75.20 8.94 -1 7 0 62.42 7.32 -1 7 0 62.51 8.64 -1 7 0 73.40 12.79 -1 7 0 60.51 6.69 -1 7 0 57.58 9.04 0 -7 0 178.75 10.95 0 -7 0 166.06 14.51 0 -7 0 155.99 12.38 0 -7 0 149.65 10.85 0 -7 0 145.02 10.43 0 -7 0 157.81 10.69 0 -7 0 152.24 8.34 0 7 0 181.49 10.03 0 7 0 162.53 14.22 0 7 0 154.94 10.39 0 7 0 151.99 7.96 0 7 0 150.50 6.08 0 7 0 152.38 10.52 0 7 0 159.44 11.29 0 7 0 140.66 11.43 0 7 0 147.57 11.02 -1 -7 0 378.43 16.93 -1 -7 0 399.03 17.45 -1 -7 0 382.59 21.38 -1 -7 0 393.12 16.85 -1 -7 0 375.40 17.25 -1 -7 0 376.72 16.73 1 7 0 380.26 13.23 1 7 0 366.24 21.04 1 7 0 388.96 16.64 1 7 0 384.41 17.37 1 7 0 405.05 16.80 1 7 0 382.36 16.47 1 7 0 394.50 17.36 -2 -7 0 254.50 12.52 -2 -7 0 236.81 12.28 -2 -7 0 237.79 13.05 -2 -7 0 236.14 12.06 -2 -7 0 260.75 16.41 -2 -7 0 248.61 12.49 2 7 0 242.51 11.81 2 7 0 234.53 12.38 2 7 0 229.49 13.48 2 7 0 239.86 8.09 2 7 0 269.07 12.06 2 7 0 244.62 12.53 2 7 0 235.63 14.38 -3 -7 0 459.68 16.48 -3 -7 0 523.61 19.65 -3 -7 0 505.14 19.89 -3 -7 0 521.37 20.03 -3 -7 0 502.69 16.94 -3 -7 0 532.58 19.81 3 7 0 531.01 23.80 3 7 0 554.06 21.97 3 7 0 530.12 19.39 3 7 0 543.77 20.90 3 7 0 521.95 17.34 3 7 0 523.18 19.31 3 7 0 512.56 20.00 -4 -7 0 559.00 20.44 -4 -7 0 558.76 18.18 -4 -7 0 532.55 18.78 -4 -7 0 573.07 20.42 4 7 0 529.39 20.28 4 7 0 563.82 22.35 4 7 0 550.70 23.96 4 7 0 527.12 24.07 4 7 0 563.74 19.74 4 7 0 515.52 22.98 4 7 0 595.02 19.85 4 7 0 545.87 20.44 -5 -7 0 -7.46 5.20 -5 -7 0 1.08 3.16 -5 -7 0 -2.88 3.30 -5 -7 0 1.97 3.41 -5 -7 0 1.65 3.20 -5 -7 0 3.02 3.15 5 7 0 -5.16 5.31 5 7 0 1.48 3.13 5 7 0 -4.93 3.51 5 7 0 -0.28 3.17 5 7 0 -0.72 4.94 5 7 0 2.70 2.60 5 7 0 2.02 2.96 5 7 0 -1.42 2.80 5 7 0 3.17 3.24 -6 -7 0 20.02 8.33 -6 -7 0 32.34 4.74 -6 -7 0 28.62 5.44 -6 -7 0 28.18 4.71 -6 -7 0 22.52 4.46 -6 -7 0 38.44 4.75 6 7 0 26.65 3.69 6 7 0 27.60 3.51 6 7 0 23.82 7.10 6 7 0 34.50 6.97 6 7 0 35.08 6.08 6 7 0 25.90 5.19 6 7 0 37.76 8.78 6 7 0 30.39 3.23 -7 -7 0 18.71 3.80 -7 -7 0 16.70 5.89 -7 -7 0 17.38 4.03 -7 -7 0 31.99 9.11 -7 -7 0 21.28 6.11 -7 -7 0 16.44 4.02 7 7 0 20.53 8.74 7 7 0 16.19 7.16 7 7 0 25.65 7.97 -8 -7 0 43.07 4.35 -8 -7 0 40.89 4.61 -8 -7 0 40.80 10.32 -8 -7 0 46.72 4.80 -8 -7 0 35.48 8.10 8 7 0 41.97 10.03 8 7 0 41.25 10.23 -9 -7 0 354.45 23.11 -9 -7 0 367.79 11.99 -9 -7 0 346.34 12.47 -9 -7 0 346.78 11.82 -9 -7 0 358.92 19.44 -9 -7 0 358.82 22.33 -9 -7 0 361.71 12.62 9 7 0 390.92 22.43 9 7 0 368.43 22.56 -10 -7 0 25.71 10.39 -10 -7 0 49.59 10.90 -10 -7 0 28.37 10.49 10 7 0 43.77 12.97 10 7 0 29.31 11.43 -11 -7 0 23.98 10.67 -11 -7 0 18.85 11.34 11 7 0 32.15 12.87 -12 -7 0 72.64 14.07 -12 -7 0 50.64 12.54 -12 -7 0 83.26 15.46 12 7 0 47.97 14.99 8 -8 0 62.63 13.58 8 -8 0 39.35 10.82 8 -8 0 31.75 12.76 8 -8 0 43.03 13.73 8 -8 0 40.13 13.07 -8 8 0 34.28 14.12 -8 8 0 18.76 12.07 -8 8 0 33.57 9.30 -8 8 0 62.27 14.96 -8 8 0 35.35 19.81 -8 8 0 41.18 13.12 -8 8 0 84.10 17.15 7 -8 0 33.74 12.14 7 -8 0 59.40 13.39 7 -8 0 50.57 11.05 7 -8 0 39.95 12.17 7 -8 0 54.28 16.97 7 -8 0 51.30 14.11 -7 8 0 42.19 12.68 -7 8 0 73.53 13.20 -7 8 0 32.62 12.11 -7 8 0 54.66 10.06 -7 8 0 63.38 14.49 -7 8 0 104.85 24.80 -7 8 0 60.57 14.35 -7 8 0 28.58 12.12 6 -8 0 26.01 10.40 6 -8 0 24.69 21.21 6 -8 0 18.14 9.68 6 -8 0 19.16 9.14 6 -8 0 26.05 12.08 6 -8 0 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9.43 2 1 19 35.63 9.13 2 1 19 32.54 13.82 -3 -1 -19 19.02 16.32 -3 -1 -19 33.19 13.80 -3 -1 -19 31.76 13.48 -3 -1 -19 19.21 12.93 3 1 19 4.79 5.02 3 1 19 16.14 11.90 3 1 19 14.44 5.80 3 1 19 28.26 14.58 -2 -2 -19 15.17 12.87 -2 -2 -19 45.94 15.15 -2 -2 -19 58.70 14.49 -2 -2 -19 19.64 14.08 2 2 19 17.54 12.21 2 2 19 2.59 11.76 2 2 19 3.70 5.50 2 2 19 5.98 5.80 -3 -2 -19 57.79 15.43 -3 -2 -19 67.90 19.81 -3 -2 -19 48.27 13.45 -3 -2 -19 31.21 15.31 -3 -2 -19 35.63 14.20 3 2 19 -11.66 16.21 3 2 19 46.26 13.53 3 2 19 45.89 15.47 -2 -3 -19 21.50 14.52 -2 -3 -19 1.38 20.21 -2 -3 -19 -12.62 13.68 2 3 19 -0.45 11.64 2 3 19 5.49 10.96 -3 -3 -19 22.49 14.93 -3 -3 -19 51.74 17.44 -3 -3 -19 66.85 15.95 -3 -3 -19 53.81 15.65 -3 -3 -19 71.16 14.31 3 3 19 52.70 13.44 3 3 19 58.64 14.40 3 3 19 37.58 13.93 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6848 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71079 9.728 12.746 14.533 84.453 78.987 71.350 ) _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 72817 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_megm_lamgail_a_0m _database_code_depnum_ccdc_archive 'CCDC 2177923' loop_ _audit_author_name _audit_author_address 'Lucia Alvarez Miguel' ;Universidad de Alcala Spain ; _audit_update_record ; 2022-06-08 deposited with the CCDC. 2023-02-22 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT213_megm_lamgail_a_0m ; PROBLEM: Atom C28 has ADP max/min Ratio ..... 4.4 prolat RESPONSE: Disorder in both carbons of one tert-butyl group ; _vrf_PLAT220_megm_lamgail_a_0m ; PROBLEM: NonSolvent Resd 1 C Ueq(max)/Ueq(min) Range 7.4 Ratio RESPONSE: Presence of strongly vibrating terminal phenyl and tert-butyl groups ; _vrf_PLAT242_megm_lamgail_a_0m ; PROBLEM: Low 'MainMol' Ueq as Compared to Neighbors of C26 Check RESPONSE: We observed deviations of expected thermal parameters which are in agreement with a slight rotational disorder of the tert-butyl groups ; # Added during the CSD deposition process: Wednesday 08 June 2022 05:35 PM # end Validation Reply Form _audit_creation_date 2022-06-08 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _shelxl_version_number 2013-3 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H46 Ga I N2 O2' _chemical_formula_sum 'C36 H46 Ga I N2 O2' _chemical_formula_weight 735.37 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.6466(3) _cell_length_b 18.2837(7) _cell_length_c 25.0241(11) _cell_angle_alpha 90 _cell_angle_beta 96.779(2) _cell_angle_gamma 90 _cell_volume 3474.1(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9507 _cell_measurement_temperature 200.0 _cell_measurement_theta_max 26.82 _cell_measurement_theta_min 2.70 _shelx_estimated_absorpt_T_max 0.858 _shelx_estimated_absorpt_T_min 0.637 _exptl_absorpt_coefficient_mu 1.713 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.6780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0915 before and 0.0638 after correction. The Ratio of minimum to maximum transmission is 0.9086. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear brown' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1504 _exptl_crystal_size_max 0.289 _exptl_crystal_size_mid 0.232 _exptl_crystal_size_min 0.092 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_unetI/netI 0.0405 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 142440 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.564 _diffrn_reflns_theta_min 2.374 _diffrn_ambient_temperature 200.0 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.4074 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_collimation 'focusing mirrors' _diffrn_radiation_monochromator 'multilayer mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus sealed tube' _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_type 'INCOATEC I\ms 3.0' _diffrn_source_voltage 50 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8570 _reflns_number_total 11584 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.40B (Bruker, 2019)' _computing_data_collection 'Apex3 v2019.11-0 (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40B (Bruker, 2019)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL 2013/3 (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.440 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.084 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 391 _refine_ls_number_reflns 11584 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0396 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+2.6355P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.0908 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C7(H7), C13(H13), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C30(H30) 2.b Idealised Me refined as rotating group: C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A, H10B,H10C), C11(H11A,H11B,H11C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B, H35C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.01932(2) 0.70697(2) 0.47092(2) 0.03515(5) Uani 1 1 d . . . . . Ga1 Ga 0.31152(3) 0.64628(2) 0.50504(2) 0.02100(6) Uani 1 1 d . . . . . O1 O 0.3136(2) 0.64240(8) 0.58014(6) 0.0281(3) Uani 1 1 d . . . . . O2 O 0.4828(2) 0.71957(8) 0.51526(6) 0.0270(3) Uani 1 1 d . . . . . N1 N 0.2725(2) 0.53680(10) 0.50050(7) 0.0216(4) Uani 1 1 d . . . . . N2 N 0.3999(2) 0.62291(10) 0.43273(7) 0.0233(4) Uani 1 1 d . . . . . C1 C 0.2650(3) 0.59141(12) 0.61241(9) 0.0228(4) Uani 1 1 d . . . . . C2 C 0.2541(3) 0.60806(12) 0.66766(9) 0.0241(4) Uani 1 1 d . . . . . C3 C 0.2824(3) 0.68645(13) 0.68891(9) 0.0282(5) Uani 1 1 d . . . . . C4 C 0.1454(4) 0.73728(14) 0.65832(12) 0.0402(6) Uani 1 1 d . . . . . H4A H 0.1510 0.7326 0.6195 0.060 Uiso 1 1 calc R U . . . H4B H 0.1702 0.7880 0.6694 0.060 Uiso 1 1 calc R U . . . H4C H 0.0274 0.7237 0.6665 0.060 Uiso 1 1 calc R U . . . C5 C 0.4681(4) 0.71314(14) 0.68160(11) 0.0362(6) Uani 1 1 d . . . . . H5A H 0.5553 0.6825 0.7030 0.054 Uiso 1 1 calc R U . . . H5B H 0.4818 0.7641 0.6936 0.054 Uiso 1 1 calc R U . . . H5C H 0.4858 0.7099 0.6435 0.054 Uiso 1 1 calc R U . . . C6 C 0.2597(4) 0.69241(15) 0.74870(11) 0.0420(7) Uani 1 1 d . . . . . H6A H 0.1415 0.6758 0.7544 0.063 Uiso 1 1 calc R U . . . H6B H 0.2752 0.7434 0.7603 0.063 Uiso 1 1 calc R U . . . H6C H 0.3479 0.6618 0.7697 0.063 Uiso 1 1 calc R U . . . C7 C 0.2163(3) 0.55110(13) 0.70063(9) 0.0279(5) Uani 1 1 d . . . . . H7 H 0.2128 0.5618 0.7376 0.034 Uiso 1 1 calc R U . . . C8 C 0.1534(4) 0.41868(13) 0.72517(10) 0.0345(6) Uani 1 1 d . . . . . C9 C 0.0264(5) 0.44372(16) 0.76361(12) 0.0515(8) Uani 1 1 d . . . . . H9A H 0.0785 0.4846 0.7853 0.077 Uiso 1 1 calc R U . . . H9B H 0.0029 0.4031 0.7873 0.077 Uiso 1 1 calc R U . . . H9C H -0.0841 0.4596 0.7431 0.077 Uiso 1 1 calc R U . . . C10 C 0.3300(5) 0.4001(2) 0.75641(16) 0.0753(13) Uani 1 1 d . . . . . H10A H 0.4093 0.3812 0.7317 0.113 Uiso 1 1 calc R U . . . H10B H 0.3135 0.3630 0.7836 0.113 Uiso 1 1 calc R U . . . H10C H 0.3812 0.4442 0.7742 0.113 Uiso 1 1 calc R U . . . C11 C 0.0740(7) 0.34958(17) 0.69724(14) 0.0726(13) Uani 1 1 d . . . . . H11A H -0.0360 0.3621 0.6750 0.109 Uiso 1 1 calc R U . . . H11B H 0.0500 0.3136 0.7245 0.109 Uiso 1 1 calc R U . . . H11C H 0.1574 0.3289 0.6745 0.109 Uiso 1 1 calc R U . . . C12 C 0.1824(3) 0.47813(12) 0.68373(9) 0.0276(5) Uani 1 1 d . . . . . C13 C 0.1846(3) 0.46395(12) 0.63029(9) 0.0266(5) Uani 1 1 d . . . . . H13 H 0.1574 0.4161 0.6171 0.032 Uiso 1 1 calc R U . . . C14 C 0.2264(3) 0.51894(11) 0.59403(9) 0.0232(4) Uani 1 1 d . . . . . C15 C 0.2342(3) 0.49615(12) 0.54043(9) 0.0239(4) Uani 1 1 d . . . . . H15 H 0.2090 0.4461 0.5326 0.029 Uiso 1 1 calc R U . . . C16 C 0.2776(3) 0.50712(12) 0.44842(9) 0.0228(4) Uani 1 1 d . . . . . C17 C 0.2211(3) 0.43684(12) 0.43205(10) 0.0291(5) Uani 1 1 d . . . . . H17 H 0.1748 0.4046 0.4566 0.035 Uiso 1 1 calc R U . . . C18 C 0.2333(3) 0.41505(13) 0.38004(10) 0.0334(5) Uani 1 1 d . . . . . H18 H 0.1963 0.3672 0.3690 0.040 Uiso 1 1 calc R U . . . C19 C 0.2983(3) 0.46137(14) 0.34371(10) 0.0330(5) Uani 1 1 d . . . . . H19 H 0.3055 0.4453 0.3079 0.040 Uiso 1 1 calc R U . . . C20 C 0.3530(3) 0.53091(13) 0.35905(9) 0.0289(5) Uani 1 1 d . . . . . H20 H 0.3968 0.5629 0.3338 0.035 Uiso 1 1 calc R U . . . C21 C 0.3441(3) 0.55420(12) 0.41153(9) 0.0231(4) Uani 1 1 d . . . . . C22 C 0.4783(3) 0.67101(13) 0.40566(9) 0.0256(4) Uani 1 1 d . . . . . H22 H 0.4956 0.6584 0.3698 0.031 Uiso 1 1 calc R U . . . C23 C 0.5404(3) 0.74055(12) 0.42453(9) 0.0249(4) Uani 1 1 d . . . . . C24 C 0.6173(3) 0.78520(12) 0.38746(9) 0.0282(5) Uani 1 1 d . . . . . H24 H 0.6176 0.7689 0.3514 0.034 Uiso 1 1 calc R U . . . C25 C 0.6911(3) 0.85128(13) 0.40230(10) 0.0304(5) Uani 1 1 d . . . . . C26 C 0.7840(4) 0.89989(14) 0.36434(11) 0.0381(6) Uani 1 1 d . . . . . C27 C 0.8088(6) 0.86215(19) 0.31275(14) 0.0677(12) Uani 1 1 d . . . . . H27A H 0.8776 0.8174 0.3205 0.102 Uiso 1 1 calc R U . . . H27B H 0.8715 0.8947 0.2904 0.102 Uiso 1 1 calc R U . . . H27C H 0.6936 0.8497 0.2935 0.102 Uiso 1 1 calc R U . . . C28 C 0.6755(10) 0.9664(2) 0.3505(3) 0.155(3) Uani 1 1 d . . . . . H28A H 0.5556 0.9517 0.3364 0.232 Uiso 1 1 calc R U . . . H28B H 0.7277 0.9948 0.3232 0.232 Uiso 1 1 calc R U . . . H28C H 0.6718 0.9963 0.3829 0.232 Uiso 1 1 calc R U . . . C29 C 0.9629(8) 0.9204(4) 0.39042(18) 0.169(4) Uani 1 1 d . . . . . H29A H 0.9516 0.9518 0.4216 0.253 Uiso 1 1 calc R U . . . H29B H 1.0261 0.9468 0.3645 0.253 Uiso 1 1 calc R U . . . H29C H 1.0283 0.8761 0.4023 0.253 Uiso 1 1 calc R U . . . C30 C 0.6828(4) 0.87321(13) 0.45576(10) 0.0326(5) Uani 1 1 d . . . . . H30 H 0.7288 0.9200 0.4662 0.039 Uiso 1 1 calc R U . . . C31 C 0.6128(3) 0.83204(12) 0.49426(9) 0.0268(5) Uani 1 1 d . . . . . C32 C 0.6187(4) 0.85896(13) 0.55264(10) 0.0327(5) Uani 1 1 d . . . . . C33 C 0.6949(5) 0.93644(16) 0.55997(12) 0.0516(8) Uani 1 1 d . . . . . H33A H 0.8147 0.9371 0.5498 0.077 Uiso 1 1 calc R U . . . H33B H 0.6977 0.9511 0.5977 0.077 Uiso 1 1 calc R U . . . H33C H 0.6209 0.9706 0.5371 0.077 Uiso 1 1 calc R U . . . C34 C 0.7407(4) 0.80775(15) 0.58896(10) 0.0389(6) Uani 1 1 d . . . . . H34A H 0.6948 0.7577 0.5857 0.058 Uiso 1 1 calc R U . . . H34B H 0.7455 0.8239 0.6264 0.058 Uiso 1 1 calc R U . . . H34C H 0.8593 0.8090 0.5778 0.058 Uiso 1 1 calc R U . . . C35 C 0.4337(4) 0.86008(16) 0.56980(11) 0.0427(7) Uani 1 1 d . . . . . H35A H 0.3582 0.8923 0.5457 0.064 Uiso 1 1 calc R U . . . H35B H 0.4391 0.8782 0.6068 0.064 Uiso 1 1 calc R U . . . H35C H 0.3850 0.8104 0.5679 0.064 Uiso 1 1 calc R U . . . C36 C 0.5411(3) 0.76258(12) 0.47880(9) 0.0234(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.02954(9) 0.03432(9) 0.04129(10) -0.00002(7) 0.00288(7) 0.00583(7) Ga1 0.02456(12) 0.01991(11) 0.01898(11) -0.00114(9) 0.00450(9) -0.00211(9) O1 0.0410(10) 0.0228(7) 0.0208(7) -0.0004(6) 0.0055(7) -0.0076(7) O2 0.0352(9) 0.0271(8) 0.0190(7) -0.0001(6) 0.0045(6) -0.0090(7) N1 0.0225(9) 0.0218(8) 0.0204(9) -0.0010(7) 0.0024(7) -0.0006(7) N2 0.0264(9) 0.0228(9) 0.0213(9) -0.0038(7) 0.0054(7) -0.0029(7) C1 0.0222(10) 0.0238(10) 0.0224(10) 0.0018(8) 0.0030(8) 0.0005(8) C2 0.0269(11) 0.0243(10) 0.0212(10) 0.0006(8) 0.0038(8) 0.0014(8) C3 0.0362(13) 0.0252(10) 0.0240(11) -0.0023(9) 0.0064(9) -0.0004(9) C4 0.0489(16) 0.0271(12) 0.0442(16) -0.0025(11) 0.0043(13) 0.0062(11) C5 0.0418(15) 0.0331(13) 0.0340(13) -0.0098(10) 0.0059(11) -0.0088(11) C6 0.0612(19) 0.0347(13) 0.0320(13) -0.0078(11) 0.0135(13) -0.0024(13) C7 0.0332(12) 0.0283(11) 0.0229(11) 0.0017(9) 0.0060(9) 0.0015(9) C8 0.0493(16) 0.0258(11) 0.0317(12) 0.0076(9) 0.0189(11) 0.0078(11) C9 0.076(2) 0.0387(15) 0.0467(17) 0.0108(13) 0.0365(16) 0.0086(15) C10 0.066(2) 0.092(3) 0.071(2) 0.056(2) 0.0191(19) 0.028(2) C11 0.139(4) 0.0314(15) 0.057(2) 0.0027(14) 0.049(2) -0.0148(19) C12 0.0331(12) 0.0235(10) 0.0281(11) 0.0042(9) 0.0111(9) 0.0034(9) C13 0.0315(12) 0.0212(10) 0.0281(11) 0.0019(8) 0.0070(9) 0.0026(9) C14 0.0262(11) 0.0216(10) 0.0221(10) 0.0013(8) 0.0041(8) 0.0004(8) C15 0.0252(11) 0.0211(9) 0.0253(11) 0.0013(8) 0.0023(8) 0.0003(8) C16 0.0228(10) 0.0230(10) 0.0229(10) -0.0021(8) 0.0040(8) 0.0023(8) C17 0.0341(12) 0.0241(10) 0.0296(12) -0.0032(9) 0.0059(10) -0.0019(9) C18 0.0389(14) 0.0250(11) 0.0367(13) -0.0096(10) 0.0058(11) -0.0021(10) C19 0.0373(14) 0.0330(12) 0.0286(12) -0.0110(10) 0.0039(10) 0.0022(10) C20 0.0317(12) 0.0310(11) 0.0248(11) -0.0043(9) 0.0065(9) -0.0021(10) C21 0.0228(10) 0.0227(10) 0.0239(10) -0.0048(8) 0.0033(8) -0.0007(8) C22 0.0262(11) 0.0301(11) 0.0211(10) -0.0034(9) 0.0052(8) -0.0044(9) C23 0.0271(11) 0.0250(10) 0.0233(10) -0.0017(8) 0.0051(9) -0.0030(9) C24 0.0330(12) 0.0292(11) 0.0230(11) -0.0010(9) 0.0063(9) -0.0029(9) C25 0.0374(13) 0.0261(11) 0.0286(12) 0.0041(9) 0.0074(10) -0.0029(10) C26 0.0543(17) 0.0293(12) 0.0326(13) 0.0037(10) 0.0131(12) -0.0111(11) C27 0.103(3) 0.0508(19) 0.060(2) -0.0068(16) 0.055(2) -0.0290(19) C28 0.253(8) 0.065(3) 0.182(6) 0.084(3) 0.173(6) 0.082(4) C29 0.159(5) 0.286(9) 0.055(3) 0.048(4) -0.016(3) -0.186(6) C30 0.0443(15) 0.0223(10) 0.0315(12) -0.0012(9) 0.0063(11) -0.0072(10) C31 0.0305(12) 0.0258(11) 0.0241(11) -0.0012(9) 0.0030(9) -0.0025(9) C32 0.0449(15) 0.0283(11) 0.0259(12) -0.0061(9) 0.0081(10) -0.0084(10) C33 0.083(2) 0.0361(14) 0.0370(15) -0.0132(12) 0.0146(15) -0.0205(15) C34 0.0461(16) 0.0445(15) 0.0254(12) -0.0023(11) 0.0009(11) -0.0043(12) C35 0.0550(18) 0.0403(14) 0.0349(14) -0.0076(11) 0.0145(13) 0.0043(13) C36 0.0224(11) 0.0249(10) 0.0226(10) 0.0008(8) 0.0019(8) -0.0017(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ga1 2.5499(3) . ? Ga1 O1 1.8791(15) . ? Ga1 O2 1.8701(16) . ? Ga1 N1 2.0250(18) . ? Ga1 N2 2.0500(17) . ? O1 C1 1.315(3) . ? O2 C36 1.322(3) . ? N1 C15 1.306(3) . ? N1 C16 1.417(3) . ? N2 C21 1.410(3) . ? N2 C22 1.299(3) . ? C1 C2 1.428(3) . ? C1 C14 1.422(3) . ? C2 C3 1.535(3) . ? C2 C7 1.380(3) . ? C3 C4 1.536(4) . ? C3 C5 1.532(4) . ? C3 C6 1.530(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7 0.9500 . ? C7 C12 1.414(3) . ? C8 C9 1.516(4) . ? C8 C10 1.517(5) . ? C8 C11 1.534(4) . ? C8 C12 1.536(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.364(3) . ? C13 H13 0.9500 . ? C13 C14 1.416(3) . ? C14 C15 1.412(3) . ? C15 H15 0.9500 . ? C16 C17 1.401(3) . ? C16 C21 1.401(3) . ? C17 H17 0.9500 . ? C17 C18 1.375(3) . ? C18 H18 0.9500 . ? C18 C19 1.377(4) . ? C19 H19 0.9500 . ? C19 C20 1.379(3) . ? C20 H20 0.9500 . ? C20 C21 1.390(3) . ? C22 H22 0.9500 . ? C22 C23 1.418(3) . ? C23 C24 1.415(3) . ? C23 C36 1.416(3) . ? C24 H24 0.9500 . ? C24 C25 1.366(3) . ? C25 C26 1.535(3) . ? C25 C30 1.405(3) . ? C26 C27 1.495(4) . ? C26 C28 1.489(5) . ? C26 C29 1.492(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30 0.9500 . ? C30 C31 1.380(3) . ? C31 C32 1.537(3) . ? C31 C36 1.419(3) . ? C32 C33 1.534(4) . ? C32 C34 1.540(4) . ? C32 C35 1.527(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 I1 104.77(5) . . ? O1 Ga1 N1 90.15(7) . . ? O1 Ga1 N2 155.55(8) . . ? O2 Ga1 I1 107.80(5) . . ? O2 Ga1 O1 88.11(7) . . ? O2 Ga1 N1 144.32(8) . . ? O2 Ga1 N2 88.37(7) . . ? N1 Ga1 I1 107.09(5) . . ? N1 Ga1 N2 78.83(7) . . ? N2 Ga1 I1 99.35(6) . . ? C1 O1 Ga1 132.15(14) . . ? C36 O2 Ga1 128.32(14) . . ? C15 N1 Ga1 124.37(15) . . ? C15 N1 C16 121.26(19) . . ? C16 N1 Ga1 114.23(13) . . ? C21 N2 Ga1 113.64(13) . . ? C22 N2 Ga1 122.66(15) . . ? C22 N2 C21 123.01(18) . . ? O1 C1 C2 119.77(19) . . ? O1 C1 C14 121.65(19) . . ? C14 C1 C2 118.56(19) . . ? C1 C2 C3 120.82(19) . . ? C7 C2 C1 117.3(2) . . ? C7 C2 C3 121.9(2) . . ? C2 C3 C4 109.4(2) . . ? C5 C3 C2 110.55(19) . . ? C5 C3 C4 109.6(2) . . ? C6 C3 C2 112.17(19) . . ? C6 C3 C4 107.1(2) . . ? C6 C3 C5 107.9(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7 117.4 . . ? C2 C7 C12 125.2(2) . . ? C12 C7 H7 117.4 . . ? C9 C8 C10 109.8(3) . . ? C9 C8 C11 106.8(3) . . ? C9 C8 C12 111.7(2) . . ? C10 C8 C11 109.3(3) . . ? C10 C8 C12 108.4(2) . . ? C11 C8 C12 110.9(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 C8 120.1(2) . . ? C13 C12 C7 116.7(2) . . ? C13 C12 C8 123.1(2) . . ? C12 C13 H13 119.2 . . ? C12 C13 C14 121.5(2) . . ? C14 C13 H13 119.2 . . ? C13 C14 C1 120.6(2) . . ? C15 C14 C1 123.49(19) . . ? C15 C14 C13 115.9(2) . . ? N1 C15 C14 126.6(2) . . ? N1 C15 H15 116.7 . . ? C14 C15 H15 116.7 . . ? C17 C16 N1 125.4(2) . . ? C21 C16 N1 114.99(19) . . ? C21 C16 C17 119.6(2) . . ? C16 C17 H17 120.4 . . ? C18 C17 C16 119.3(2) . . ? C18 C17 H17 120.4 . . ? C17 C18 H18 119.4 . . ? C17 C18 C19 121.1(2) . . ? C19 C18 H18 119.4 . . ? C18 C19 H19 119.9 . . ? C18 C19 C20 120.3(2) . . ? C20 C19 H19 119.9 . . ? C19 C20 H20 120.1 . . ? C19 C20 C21 119.9(2) . . ? C21 C20 H20 120.1 . . ? C16 C21 N2 114.63(18) . . ? C20 C21 N2 125.6(2) . . ? C20 C21 C16 119.8(2) . . ? N2 C22 H22 116.9 . . ? N2 C22 C23 126.2(2) . . ? C23 C22 H22 116.9 . . ? C24 C23 C22 116.6(2) . . ? C24 C23 C36 120.6(2) . . ? C36 C23 C22 122.5(2) . . ? C23 C24 H24 119.3 . . ? C25 C24 C23 121.5(2) . . ? C25 C24 H24 119.3 . . ? C24 C25 C26 123.4(2) . . ? C24 C25 C30 116.6(2) . . ? C30 C25 C26 120.0(2) . . ? C27 C26 C25 112.5(2) . . ? C28 C26 C25 109.3(3) . . ? C28 C26 C27 107.5(3) . . ? C29 C26 C25 110.0(3) . . ? C29 C26 C27 106.9(4) . . ? C29 C26 C28 110.7(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30 117.5 . . ? C31 C30 C25 125.0(2) . . ? C31 C30 H30 117.5 . . ? C30 C31 C32 121.2(2) . . ? C30 C31 C36 117.8(2) . . ? C36 C31 C32 120.9(2) . . ? C31 C32 C34 108.3(2) . . ? C33 C32 C31 112.2(2) . . ? C33 C32 C34 107.2(2) . . ? C35 C32 C31 110.3(2) . . ? C35 C32 C33 107.8(2) . . ? C35 C32 C34 111.0(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O2 C36 C23 122.0(2) . . ? O2 C36 C31 119.68(19) . . ? C23 C36 C31 118.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I1 Ga1 O1 C1 93.4(2) . . . . ? I1 Ga1 O2 C36 -64.16(19) . . . . ? Ga1 O1 C1 C2 -169.54(16) . . . . ? Ga1 O1 C1 C14 11.9(3) . . . . ? Ga1 O2 C36 C23 -28.1(3) . . . . ? Ga1 O2 C36 C31 154.14(17) . . . . ? Ga1 N1 C15 C14 -5.2(3) . . . . ? Ga1 N1 C16 C17 -166.67(19) . . . . ? Ga1 N1 C16 C21 12.7(2) . . . . ? Ga1 N2 C21 C16 -15.1(2) . . . . ? Ga1 N2 C21 C20 165.92(19) . . . . ? Ga1 N2 C22 C23 11.1(3) . . . . ? O1 Ga1 O2 C36 -169.07(19) . . . . ? O1 C1 C2 C3 5.4(3) . . . . ? O1 C1 C2 C7 -174.9(2) . . . . ? O1 C1 C14 C13 176.2(2) . . . . ? O1 C1 C14 C15 -1.0(3) . . . . ? O2 Ga1 O1 C1 -158.6(2) . . . . ? N1 Ga1 O1 C1 -14.3(2) . . . . ? N1 Ga1 O2 C36 103.3(2) . . . . ? N1 C16 C17 C18 179.9(2) . . . . ? N1 C16 C21 N2 1.7(3) . . . . ? N1 C16 C21 C20 -179.2(2) . . . . ? N2 Ga1 O1 C1 -76.8(3) . . . . ? N2 Ga1 O2 C36 35.14(19) . . . . ? N2 C22 C23 C24 -178.1(2) . . . . ? N2 C22 C23 C36 7.4(4) . . . . ? C1 C2 C3 C4 59.6(3) . . . . ? C1 C2 C3 C5 -61.1(3) . . . . ? C1 C2 C3 C6 178.4(2) . . . . ? C1 C2 C7 C12 -2.0(4) . . . . ? C1 C14 C15 N1 -1.7(4) . . . . ? C2 C1 C14 C13 -2.3(3) . . . . ? C2 C1 C14 C15 -179.5(2) . . . . ? C2 C7 C12 C8 176.2(2) . . . . ? C2 C7 C12 C13 -1.2(4) . . . . ? C3 C2 C7 C12 177.7(2) . . . . ? C7 C2 C3 C4 -120.0(2) . . . . ? C7 C2 C3 C5 119.2(3) . . . . ? C7 C2 C3 C6 -1.3(3) . . . . ? C7 C12 C13 C14 2.7(4) . . . . ? C8 C12 C13 C14 -174.6(2) . . . . ? C9 C8 C12 C7 46.7(4) . . . . ? C9 C8 C12 C13 -136.1(3) . . . . ? C10 C8 C12 C7 -74.3(3) . . . . ? C10 C8 C12 C13 102.9(3) . . . . ? C11 C8 C12 C7 165.7(3) . . . . ? C11 C8 C12 C13 -17.1(4) . . . . ? C12 C13 C14 C1 -1.0(4) . . . . ? C12 C13 C14 C15 176.4(2) . . . . ? C13 C14 C15 N1 -179.0(2) . . . . ? C14 C1 C2 C3 -176.0(2) . . . . ? C14 C1 C2 C7 3.7(3) . . . . ? C15 N1 C16 C17 9.2(3) . . . . ? C15 N1 C16 C21 -171.5(2) . . . . ? C16 N1 C15 C14 179.4(2) . . . . ? C16 C17 C18 C19 -0.7(4) . . . . ? C17 C16 C21 N2 -178.9(2) . . . . ? C17 C16 C21 C20 0.1(3) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? C18 C19 C20 C21 0.6(4) . . . . ? C19 C20 C21 N2 178.2(2) . . . . ? C19 C20 C21 C16 -0.7(4) . . . . ? C21 N2 C22 C23 -179.0(2) . . . . ? C21 C16 C17 C18 0.6(3) . . . . ? C22 N2 C21 C16 174.1(2) . . . . ? C22 N2 C21 C20 -4.8(4) . . . . ? C22 C23 C24 C25 -175.9(2) . . . . ? C22 C23 C36 O2 -0.4(4) . . . . ? C22 C23 C36 C31 177.4(2) . . . . ? C23 C24 C25 C26 176.9(2) . . . . ? C23 C24 C25 C30 -1.5(4) . . . . ? C24 C23 C36 O2 -174.6(2) . . . . ? C24 C23 C36 C31 3.2(3) . . . . ? C24 C25 C26 C27 -8.8(4) . . . . ? C24 C25 C26 C28 110.5(4) . . . . ? C24 C25 C26 C29 -127.8(4) . . . . ? C24 C25 C30 C31 2.8(4) . . . . ? C25 C30 C31 C32 176.6(2) . . . . ? C25 C30 C31 C36 -1.0(4) . . . . ? C26 C25 C30 C31 -175.7(3) . . . . ? C30 C25 C26 C27 169.6(3) . . . . ? C30 C25 C26 C28 -71.2(5) . . . . ? C30 C25 C26 C29 50.5(5) . . . . ? C30 C31 C32 C33 4.7(4) . . . . ? C30 C31 C32 C34 -113.5(3) . . . . ? C30 C31 C32 C35 124.8(3) . . . . ? C30 C31 C36 O2 175.8(2) . . . . ? C30 C31 C36 C23 -2.0(3) . . . . ? C32 C31 C36 O2 -1.7(3) . . . . ? C32 C31 C36 C23 -179.6(2) . . . . ? C36 C23 C24 C25 -1.4(4) . . . . ? C36 C31 C32 C33 -177.9(2) . . . . ? C36 C31 C32 C34 64.0(3) . . . . ? C36 C31 C32 C35 -57.7(3) . . . . ? _shelx_res_file ; TITL megm_lamgail_a_0m_a.res in P2(1)/c REM Old TITL MEGM_LAMGaIl_a_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.091, Rweak 0.009, Alpha 0.028, Orientation as input REM Formula found by SHELXT: C36 N2 O2 Ga I CELL 0.71073 7.6466 18.2837 25.0241 90 96.779 90 ZERR 4 0.0003 0.0007 0.0011 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Ga I N O UNIT 144 184 4 4 8 8 L.S. 4 0 0 PLAN 11 SIZE 0.092 0.232 0.289 TEMP -73.15 CONF list 4 fmap 2 53 MORE -1 BOND $H ACTA OMIT 0 1 2 OMIT -1 1 2 REM REM REM WGHT 0.039000 2.635500 FVAR 0.30158 I1 4 0.019325 0.706975 0.470922 11.00000 0.02954 0.03432 = 0.04129 -0.00002 0.00288 0.00583 GA1 3 0.311519 0.646277 0.505035 11.00000 0.02456 0.01991 = 0.01898 -0.00114 0.00450 -0.00211 O1 6 0.313586 0.642400 0.580144 11.00000 0.04102 0.02282 = 0.02077 -0.00043 0.00549 -0.00763 O2 6 0.482773 0.719575 0.515264 11.00000 0.03517 0.02714 = 0.01903 -0.00006 0.00447 -0.00904 N1 5 0.272476 0.536800 0.500498 11.00000 0.02254 0.02181 = 0.02044 -0.00098 0.00242 -0.00058 N2 5 0.399933 0.622911 0.432727 11.00000 0.02644 0.02283 = 0.02125 -0.00383 0.00540 -0.00290 C1 1 0.265005 0.591415 0.612406 11.00000 0.02221 0.02378 = 0.02239 0.00179 0.00298 0.00049 C2 1 0.254059 0.608058 0.667657 11.00000 0.02687 0.02434 = 0.02121 0.00058 0.00376 0.00144 C3 1 0.282447 0.686454 0.688914 11.00000 0.03618 0.02517 = 0.02398 -0.00232 0.00636 -0.00044 C4 1 0.145398 0.737284 0.658319 11.00000 0.04891 0.02705 = 0.04425 -0.00249 0.00431 0.00622 AFIX 137 H4A 2 0.151047 0.732593 0.619548 11.00000 -1.50000 H4B 2 0.170249 0.787998 0.669405 11.00000 -1.50000 H4C 2 0.027445 0.723697 0.666480 11.00000 -1.50000 AFIX 0 C5 1 0.468067 0.713138 0.681605 11.00000 0.04182 0.03311 = 0.03396 -0.00977 0.00589 -0.00879 AFIX 137 H5A 2 0.555297 0.682540 0.703008 11.00000 -1.50000 H5B 2 0.481820 0.764054 0.693604 11.00000 -1.50000 H5C 2 0.485815 0.709888 0.643528 11.00000 -1.50000 AFIX 0 C6 1 0.259722 0.692410 0.748705 11.00000 0.06125 0.03469 = 0.03198 -0.00783 0.01349 -0.00236 AFIX 137 H6A 2 0.141480 0.675806 0.754401 11.00000 -1.50000 H6B 2 0.275228 0.743435 0.760294 11.00000 -1.50000 H6C 2 0.347907 0.661804 0.769707 11.00000 -1.50000 AFIX 0 C7 1 0.216291 0.551097 0.700630 11.00000 0.03325 0.02833 = 0.02291 0.00169 0.00602 0.00155 AFIX 43 H7 2 0.212774 0.561762 0.737643 11.00000 -1.20000 AFIX 0 C8 1 0.153351 0.418684 0.725168 11.00000 0.04932 0.02579 = 0.03172 0.00756 0.01894 0.00783 C9 1 0.026450 0.443715 0.763608 11.00000 0.07607 0.03874 = 0.04665 0.01077 0.03648 0.00863 AFIX 137 H9A 2 0.078480 0.484589 0.785298 11.00000 -1.50000 H9B 2 0.002871 0.403148 0.787333 11.00000 -1.50000 H9C 2 -0.084063 0.459595 0.743051 11.00000 -1.50000 AFIX 0 C10 1 0.329994 0.400113 0.756414 11.00000 0.06580 0.09190 = 0.07085 0.05625 0.01906 0.02809 AFIX 137 H10A 2 0.409331 0.381157 0.731666 11.00000 -1.50000 H10B 2 0.313521 0.362954 0.783597 11.00000 -1.50000 H10C 2 0.381230 0.444233 0.774163 11.00000 -1.50000 AFIX 0 C11 1 0.074004 0.349583 0.697242 11.00000 0.13873 0.03144 = 0.05652 0.00267 0.04926 -0.01478 AFIX 137 H11A 2 -0.036045 0.362118 0.674977 11.00000 -1.50000 H11B 2 0.049978 0.313575 0.724453 11.00000 -1.50000 H11C 2 0.157381 0.328906 0.674455 11.00000 -1.50000 AFIX 0 C12 1 0.182409 0.478129 0.683726 11.00000 0.03308 0.02354 = 0.02806 0.00419 0.01111 0.00343 C13 1 0.184603 0.463950 0.630287 11.00000 0.03148 0.02118 = 0.02812 0.00186 0.00701 0.00265 AFIX 43 H13 2 0.157429 0.416066 0.617092 11.00000 -1.20000 AFIX 0 C14 1 0.226441 0.518942 0.594027 11.00000 0.02619 0.02159 = 0.02209 0.00125 0.00413 0.00042 C15 1 0.234178 0.496145 0.540427 11.00000 0.02522 0.02110 = 0.02531 0.00126 0.00231 0.00032 AFIX 43 H15 2 0.208950 0.446136 0.532624 11.00000 -1.20000 AFIX 0 C16 1 0.277614 0.507115 0.448421 11.00000 0.02284 0.02300 = 0.02295 -0.00210 0.00404 0.00227 C17 1 0.221101 0.436841 0.432051 11.00000 0.03411 0.02407 = 0.02959 -0.00319 0.00589 -0.00190 AFIX 43 H17 2 0.174832 0.404596 0.456632 11.00000 -1.20000 AFIX 0 C18 1 0.233327 0.415053 0.380038 11.00000 0.03889 0.02501 = 0.03674 -0.00960 0.00579 -0.00213 AFIX 43 H18 2 0.196322 0.367242 0.368966 11.00000 -1.20000 AFIX 0 C19 1 0.298311 0.461367 0.343713 11.00000 0.03729 0.03296 = 0.02861 -0.01097 0.00393 0.00216 AFIX 43 H19 2 0.305470 0.445326 0.307927 11.00000 -1.20000 AFIX 0 C20 1 0.353023 0.530908 0.359052 11.00000 0.03172 0.03104 = 0.02480 -0.00430 0.00652 -0.00207 AFIX 43 H20 2 0.396761 0.562852 0.333790 11.00000 -1.20000 AFIX 0 C21 1 0.344088 0.554199 0.411527 11.00000 0.02282 0.02269 = 0.02387 -0.00480 0.00333 -0.00070 C22 1 0.478260 0.671008 0.405660 11.00000 0.02619 0.03012 = 0.02105 -0.00339 0.00522 -0.00445 AFIX 43 H22 2 0.495611 0.658427 0.369830 11.00000 -1.20000 AFIX 0 C23 1 0.540359 0.740548 0.424529 11.00000 0.02707 0.02498 = 0.02327 -0.00169 0.00509 -0.00298 C24 1 0.617298 0.785201 0.387456 11.00000 0.03303 0.02920 = 0.02301 -0.00102 0.00627 -0.00289 AFIX 43 H24 2 0.617623 0.768870 0.351428 11.00000 -1.20000 AFIX 0 C25 1 0.691131 0.851275 0.402303 11.00000 0.03742 0.02609 = 0.02861 0.00414 0.00737 -0.00285 C26 1 0.784040 0.899890 0.364338 11.00000 0.05429 0.02926 = 0.03263 0.00373 0.01307 -0.01113 C27 1 0.808812 0.862146 0.312752 11.00000 0.10276 0.05084 = 0.06025 -0.00678 0.05457 -0.02904 AFIX 137 H27A 2 0.877575 0.817374 0.320546 11.00000 -1.50000 H27B 2 0.871537 0.894675 0.290386 11.00000 -1.50000 H27C 2 0.693557 0.849654 0.293517 11.00000 -1.50000 AFIX 0 C28 1 0.675510 0.966352 0.350512 11.00000 0.25279 0.06481 = 0.18231 0.08418 0.17339 0.08173 AFIX 137 H28A 2 0.555629 0.951738 0.336366 11.00000 -1.50000 H28B 2 0.727689 0.994790 0.323218 11.00000 -1.50000 H28C 2 0.671784 0.996268 0.382853 11.00000 -1.50000 AFIX 0 C29 1 0.962871 0.920425 0.390421 11.00000 0.15899 0.28588 = 0.05463 0.04793 -0.01563 -0.18577 AFIX 137 H29A 2 0.951612 0.951839 0.421562 11.00000 -1.50000 H29B 2 1.026144 0.946824 0.364543 11.00000 -1.50000 H29C 2 1.028315 0.876098 0.402291 11.00000 -1.50000 AFIX 0 C30 1 0.682752 0.873207 0.455765 11.00000 0.04425 0.02231 = 0.03154 -0.00116 0.00633 -0.00719 AFIX 43 H30 2 0.728848 0.919996 0.466197 11.00000 -1.20000 AFIX 0 C31 1 0.612756 0.832037 0.494265 11.00000 0.03046 0.02578 = 0.02412 -0.00120 0.00300 -0.00249 C32 1 0.618743 0.858959 0.552643 11.00000 0.04487 0.02833 = 0.02593 -0.00606 0.00811 -0.00844 C33 1 0.694885 0.936437 0.559974 11.00000 0.08347 0.03613 = 0.03697 -0.01325 0.01459 -0.02050 AFIX 137 H33A 2 0.814716 0.937089 0.549758 11.00000 -1.50000 H33B 2 0.697697 0.951138 0.597726 11.00000 -1.50000 H33C 2 0.620876 0.970570 0.537120 11.00000 -1.50000 AFIX 0 C34 1 0.740671 0.807747 0.588962 11.00000 0.04614 0.04447 = 0.02543 -0.00235 0.00094 -0.00429 AFIX 137 H34A 2 0.694807 0.757692 0.585737 11.00000 -1.50000 H34B 2 0.745530 0.823917 0.626446 11.00000 -1.50000 H34C 2 0.859261 0.809045 0.577815 11.00000 -1.50000 AFIX 0 C35 1 0.433674 0.860081 0.569801 11.00000 0.05503 0.04030 = 0.03493 -0.00756 0.01453 0.00433 AFIX 137 H35A 2 0.358205 0.892280 0.545728 11.00000 -1.50000 H35B 2 0.439059 0.878239 0.606806 11.00000 -1.50000 H35C 2 0.384962 0.810446 0.567882 11.00000 -1.50000 AFIX 0 C36 1 0.541147 0.762579 0.478797 11.00000 0.02242 0.02488 = 0.02258 0.00078 0.00192 -0.00170 HKLF 4 REM megm_lamgail_a_0m_a.res in P2(1)/c REM R1 = 0.0396 for 8570 Fo > 4sig(Fo) and 0.0663 for all 11584 data REM 391 parameters refined using 0 restraints END WGHT 0.0306 2.7109 REM Highest difference peak 0.440, deepest hole -0.669, 1-sigma level 0.084 Q1 1 0.6313 0.9593 0.3361 11.00000 0.05 0.44 Q2 1 0.1649 0.6992 0.4796 11.00000 0.05 0.41 Q3 1 0.4261 0.6891 0.5034 11.00000 0.05 0.39 Q4 1 0.2048 0.5577 0.5989 11.00000 0.05 0.37 Q5 1 0.2211 0.5820 0.6793 11.00000 0.05 0.37 Q6 1 0.9951 0.8989 0.3855 11.00000 0.05 0.37 Q7 1 0.3368 0.5435 0.3806 11.00000 0.05 0.36 Q8 1 0.1019 0.7406 0.4821 11.00000 0.05 0.36 Q9 1 0.5008 0.7020 0.4148 11.00000 0.05 0.36 Q10 1 0.2826 0.5026 0.3572 11.00000 0.05 0.35 Q11 1 0.5778 0.7605 0.4020 11.00000 0.05 0.34 ; _shelx_res_checksum 74943 _shelx_hkl_file ; -2 0 0 1662.23 54.89 -2 0 0 1563.74 53.59 -2 0 0 1520.75 50.89 2 0 0 1620.44 49.90 2 0 0 1535.95 50.79 -2 0 0 1569.04 51.39 -2 0 0 1550.74 52.09 2 0 0 1600.64 52.29 2 0 0 1560.64 51.59 -2 0 0 1544.05 49.90 -3 0 0 5910.01 181.18 -3 0 0 5872.91 179.48 -3 0 0 5983.90 176.58 -3 0 0 5860.71 173.58 3 0 0 5710.13 176.08 -3 0 0 5802.82 175.78 3 0 0 5834.52 177.18 3 0 0 5816.32 173.08 -3 0 0 5743.73 177.18 4 0 0 3377.86 109.09 4 0 0 3499.95 112.29 -4 0 0 3579.04 114.39 -4 0 0 3502.25 117.79 -4 0 0 3571.04 110.69 4 0 0 3618.74 114.49 -4 0 0 3513.05 119.69 -4 0 0 3548.24 112.69 -4 0 0 3381.16 114.69 -4 0 0 3428.26 113.09 4 0 0 3458.45 114.79 -5 0 0 44.70 12.30 -5 0 0 27.40 8.80 -5 0 0 26.70 8.40 5 0 0 14.60 8.40 -5 0 0 42.00 10.80 -5 0 0 51.29 11.70 5 0 0 26.80 7.30 5 0 0 42.00 10.80 -5 0 0 34.80 8.90 5 0 0 29.90 10.60 -5 0 0 29.50 9.60 -6 0 0 967.50 42.50 -6 0 0 968.00 46.50 6 0 0 949.11 47.60 -6 0 0 906.41 44.70 -6 0 0 934.41 50.49 6 0 0 974.00 41.80 6 0 0 976.40 44.70 -6 0 0 972.20 48.50 -6 0 0 986.10 53.99 6 0 0 913.21 46.40 -6 0 0 922.31 45.10 7 0 0 333.07 29.10 -7 0 0 382.86 36.50 -7 0 0 362.46 25.90 -7 0 0 343.17 31.40 7 0 0 327.47 28.80 -7 0 0 311.37 27.90 7 0 0 341.07 27.10 7 0 0 337.17 27.20 8 0 0 -3.10 11.20 -8 0 0 -3.90 10.20 8 0 0 -0.20 11.30 -8 0 0 -5.60 13.80 -8 0 0 4.80 17.20 9 0 0 41.00 17.70 -9 0 0 58.49 17.60 -9 0 0 -6.20 23.50 -9 0 0 66.09 24.10 9 0 0 72.99 19.30 -10 0 0 15.20 28.90 -10 0 0 48.20 18.80 10 0 0 87.29 25.20 10 0 0 75.19 22.00 11 0 0 -19.20 23.20 11 0 0 -16.00 20.10 2 -1 0 34.70 5.10 -2 -1 0 39.90 6.00 2 -1 0 30.50 5.40 2 -1 0 31.40 5.40 2 -1 0 36.10 5.90 -2 -1 0 40.30 5.10 -2 -1 0 25.40 5.50 -2 -1 0 33.60 5.40 -2 -1 0 42.80 6.50 -2 -1 0 44.90 6.80 -2 -1 0 52.19 6.60 2 1 0 32.70 4.60 -2 1 0 31.80 5.70 -2 1 0 29.70 5.90 2 1 0 33.10 5.50 2 1 0 39.70 6.50 -2 1 0 45.80 7.50 -2 1 0 38.50 5.60 -2 1 0 28.30 6.20 -2 1 0 42.50 6.40 2 1 0 43.90 5.90 -3 -1 0 10.50 5.10 3 -1 0 0.60 5.10 -3 -1 0 6.00 4.10 3 -1 0 -0.20 4.40 -3 -1 0 4.20 4.30 3 -1 0 10.80 5.40 3 -1 0 7.40 4.30 -3 -1 0 -0.80 5.40 -3 -1 0 -0.70 4.80 -3 -1 0 5.50 5.00 -3 -1 0 6.80 5.50 -3 1 0 0.10 4.80 3 1 0 2.30 4.20 -3 1 0 3.10 4.50 -3 1 0 -0.70 5.70 -3 1 0 7.20 4.80 -3 1 0 -0.30 5.50 -3 1 0 9.00 5.20 3 1 0 5.80 5.40 3 1 0 4.60 4.80 3 1 0 8.70 4.60 -3 1 0 3.20 4.50 4 -1 0 1303.97 52.69 4 -1 0 1270.47 48.50 4 -1 0 1297.87 50.79 -4 -1 0 1321.67 50.99 -4 -1 0 1336.17 53.49 -4 -1 0 1397.66 57.59 -4 -1 0 1326.27 51.79 -4 -1 0 1371.96 49.20 4 -1 0 1334.37 52.79 -4 -1 0 1456.15 56.29 -4 1 0 1392.86 56.19 -4 1 0 1413.56 49.99 -4 1 0 1371.66 52.49 4 1 0 1380.36 53.39 4 1 0 1410.16 50.99 4 1 0 1461.25 52.89 -4 1 0 1278.87 56.39 -4 1 0 1372.56 52.59 -4 1 0 1380.96 51.49 4 1 0 1315.87 47.90 -4 1 0 1286.07 52.89 -5 -1 0 280.97 19.00 5 -1 0 279.37 21.50 -5 -1 0 290.47 21.40 5 -1 0 242.78 21.20 -5 -1 0 309.67 21.30 -5 -1 0 284.27 24.60 -5 -1 0 345.87 24.10 -5 -1 0 317.37 28.30 5 -1 0 299.97 18.60 -5 -1 0 273.67 20.20 5 1 0 286.67 22.00 -5 1 0 325.57 25.90 -5 1 0 278.57 20.70 5 1 0 320.07 20.80 -5 1 0 275.57 23.20 -5 1 0 245.28 21.10 5 1 0 309.37 22.10 -5 1 0 276.87 20.30 -5 1 0 266.57 19.80 5 1 0 233.78 16.70 -5 1 0 310.07 19.90 -6 -1 0 17.90 10.70 -6 -1 0 -4.40 8.30 6 -1 0 5.60 7.80 6 -1 0 21.60 9.80 6 -1 0 3.80 7.70 -6 -1 0 1.20 7.70 -6 -1 0 1.80 9.70 -6 -1 0 -5.00 8.80 -6 -1 0 6.00 8.10 -6 -1 0 2.10 9.30 6 -1 0 7.40 11.30 6 1 0 0.30 8.40 -6 1 0 -1.60 11.30 6 1 0 0.80 7.80 6 1 0 2.10 8.90 -6 1 0 6.10 7.00 -6 1 0 10.80 10.00 6 1 0 4.30 7.70 -6 1 0 9.80 9.30 -6 1 0 -2.20 9.20 -6 1 0 13.70 10.90 -6 1 0 7.40 8.10 -7 -1 0 565.44 41.00 -7 -1 0 584.44 33.30 7 -1 0 564.14 38.40 7 -1 0 579.04 38.90 -7 -1 0 540.15 35.10 -7 -1 0 581.74 44.40 7 -1 0 532.75 34.60 -7 -1 0 566.24 36.70 -7 1 0 580.44 38.10 -7 1 0 564.84 37.40 7 1 0 598.24 37.20 -7 1 0 650.13 37.20 7 1 0 562.74 34.40 7 1 0 642.24 33.20 -7 1 0 566.34 41.60 -7 1 0 568.64 33.80 -7 1 0 537.75 42.00 -8 -1 0 175.98 32.80 8 -1 0 201.78 25.30 -8 -1 0 170.68 32.40 -8 -1 0 212.58 32.20 8 -1 0 203.18 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