#------------------------------------------------------------------------------ #$Date: 2019-12-11 12:32:21 +0200 (Wed, 11 Dec 2019) $ #$Revision: 244995 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/65/1556509.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1556509 loop_ _publ_author_name 'Vindus, D.' 'Niemeyer, M.' _publ_section_title ; Hetero- and Homoleptic Magnesium Triazenides ; _journal_name_full Inorganics _journal_page_first 33 _journal_paper_doi 10.3390/inorganics5020033 _journal_volume 5 _journal_year 2017 _chemical_formula_sum 'C49 H62 I Mg N3 O' _chemical_formula_weight 860.23 _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.8180(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.9827(2) _cell_length_b 23.6098(6) _cell_length_c 22.1855(5) _cell_measurement_reflns_used 9911 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 29.1 _cell_measurement_theta_min 2.5 _cell_volume 4704.62(19) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker Smart Apex II' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0512 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 67161 _diffrn_reflns_theta_full 29.30 _diffrn_reflns_theta_max 29.30 _diffrn_reflns_theta_min 1.84 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_T_max 0.451 _exptl_absorpt_correction_T_min 0.381 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour rod _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_description yellow _exptl_crystal_F_000 1800 _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _refine_diff_density_max 0.708 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 521 _refine_ls_number_reflns 12780 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.934 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0363 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.0938 _reflns_number_gt 7680 _reflns_number_total 12780 _reflns_threshold_expression >2sigma(I) _cod_data_source_file Inorganics-2017-5-33.cif _cod_data_source_block 2a _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 1556509 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg Mg -0.05675(7) 0.74167(3) 0.36005(3) 0.03197(15) Uani 1 1 d . . . I I 0.203374(15) 0.737680(8) 0.417163(7) 0.05164(7) Uani 1 1 d . . . N1 N -0.04935(16) 0.71030(7) 0.27084(7) 0.0281(3) Uani 1 1 d . . . N2 N -0.10953(16) 0.75632(6) 0.24741(7) 0.0257(3) Uani 1 1 d . . . N3 N -0.13900(15) 0.79253(6) 0.29016(6) 0.0264(3) Uani 1 1 d . . . O53 O -0.20856(16) 0.72048(7) 0.42217(7) 0.0517(4) Uani 1 1 d . . . C11 C 0.00596(19) 0.67197(8) 0.22698(8) 0.0308(4) Uani 1 1 d . . . C12 C -0.0017(2) 0.61415(9) 0.23986(9) 0.0379(5) Uani 1 1 d . . . C13 C 0.0540(3) 0.57509(10) 0.19851(11) 0.0515(6) Uani 1 1 d . . . H13A H 0.0487 0.5357 0.2072 0.0515(18) Uiso 1 1 calc R . . C14 C 0.1163(3) 0.59271(11) 0.14560(11) 0.0590(7) Uani 1 1 d . . . H14A H 0.1527 0.5658 0.1176 0.0515(18) Uiso 1 1 calc R . . C15 C 0.1255(3) 0.65025(10) 0.13350(10) 0.0481(6) Uani 1 1 d . . . H15A H 0.1694 0.6623 0.0970 0.0515(18) Uiso 1 1 calc R . . C16 C 0.0727(2) 0.69072(9) 0.17295(9) 0.0351(5) Uani 1 1 d . . . C21 C -0.0714(3) 0.59165(8) 0.29599(9) 0.0393(5) Uani 1 1 d . . . C22 C 0.0189(3) 0.57412(9) 0.34442(11) 0.0505(6) Uani 1 1 d . . . C23 C -0.0501(4) 0.54819(11) 0.39325(11) 0.0673(8) Uani 1 1 d . . . H23A H 0.0100 0.5366 0.4266 0.0515(18) Uiso 1 1 calc R . . C24 C -0.2010(4) 0.53862(11) 0.39521(12) 0.0709(8) Uani 1 1 d . . . C25 C -0.2870(3) 0.55696(10) 0.34712(12) 0.0596(7) Uani 1 1 d . . . H25A H -0.3917 0.5514 0.3481 0.0515(18) Uiso 1 1 calc R . . C26 C -0.2258(3) 0.58321(9) 0.29731(10) 0.0439(5) Uani 1 1 d . . . C31 C -0.21486(18) 0.84173(8) 0.26897(8) 0.0253(4) Uani 1 1 d . . . C32 C -0.21552(18) 0.89018(8) 0.30530(8) 0.0267(4) Uani 1 1 d . . . C33 C -0.2909(2) 0.93791(8) 0.28369(9) 0.0343(5) Uani 1 1 d . . . H33A H -0.2935 0.9710 0.3080 0.0515(18) Uiso 1 1 calc R . . C34 C -0.3617(2) 0.93857(9) 0.22806(9) 0.0385(5) Uani 1 1 d . . . H34A H -0.4117 0.9717 0.2144 0.0515(18) Uiso 1 1 calc R . . C35 C -0.3591(2) 0.89057(9) 0.19248(9) 0.0373(5) Uani 1 1 d . . . H35A H -0.4066 0.8908 0.1539 0.0515(18) Uiso 1 1 calc R . . C36 C -0.2875(2) 0.84204(9) 0.21282(9) 0.0331(4) Uani 1 1 d . . . H36A H -0.2878 0.8089 0.1885 0.0515(18) Uiso 1 1 calc R . . C41 C -0.13645(19) 0.89197(8) 0.36530(8) 0.0272(4) Uani 1 1 d . . . C42 C 0.0203(2) 0.89704(9) 0.36810(9) 0.0342(5) Uani 1 1 d . . . C43 C 0.0900(2) 0.89796(10) 0.42436(10) 0.0464(6) Uani 1 1 d . . . H43A H 0.1954 0.9012 0.4262 0.0515(18) Uiso 1 1 calc R . . C44 C 0.0130(2) 0.89435(11) 0.47825(10) 0.0461(6) Uani 1 1 d . B . C45 C -0.1411(2) 0.89169(9) 0.47407(9) 0.0373(5) Uani 1 1 d . . . H45A H -0.1967 0.8905 0.5102 0.0515(18) Uiso 1 1 calc R . . C46 C -0.21719(19) 0.89065(8) 0.41913(8) 0.0282(4) Uani 1 1 d . . . C51 C -0.4074(2) 0.71409(13) 0.34898(12) 0.0604(7) Uani 1 1 d . . . H51A H -0.5030 0.6958 0.3397 0.103(4) Uiso 1 1 calc R . . H51B H -0.3345 0.7033 0.3186 0.103(4) Uiso 1 1 calc R . . H51C H -0.4202 0.7553 0.3487 0.103(4) Uiso 1 1 calc R . . C52 C -0.3534(3) 0.69564(11) 0.40953(12) 0.0549(7) Uani 1 1 d . . . H52A H -0.4249 0.7077 0.4406 0.079(4) Uiso 1 1 calc R . . H52B H -0.3460 0.6538 0.4107 0.079(4) Uiso 1 1 calc R . . C54 C -0.1675(3) 0.72205(14) 0.48891(13) 0.0728(8) Uani 1 1 d . . . H54A H -0.0883 0.7505 0.4963 0.079(4) Uiso 1 1 calc R . . H54B H -0.2555 0.7328 0.5127 0.079(4) Uiso 1 1 calc R . . C55 C -0.1152(4) 0.66581(16) 0.50696(16) 0.1021(12) Uani 1 1 d . . . H55A H -0.0800 0.6670 0.5490 0.103(4) Uiso 1 1 calc R . . H55B H -0.0334 0.6542 0.4809 0.103(4) Uiso 1 1 calc R . . H55C H -0.1971 0.6386 0.5031 0.103(4) Uiso 1 1 calc R . . C61 C 0.0961(2) 0.75140(9) 0.15744(9) 0.0355(5) Uani 1 1 d . . . C62 C 0.2201(2) 0.78004(10) 0.18112(9) 0.0426(5) Uani 1 1 d . . . C63 C 0.2406(3) 0.83667(11) 0.16553(11) 0.0567(7) Uani 1 1 d . . . H63A H 0.3249 0.8561 0.1815 0.0515(18) Uiso 1 1 calc R . . C64 C 0.1439(4) 0.86552(11) 0.12798(12) 0.0645(8) Uani 1 1 d . . . C65 C 0.0256(3) 0.83594(12) 0.10383(11) 0.0599(7) Uani 1 1 d . . . H65A H -0.0405 0.8548 0.0767 0.0515(18) Uiso 1 1 calc R . . C66 C -0.0012(2) 0.77935(10) 0.11754(9) 0.0440(5) Uani 1 1 d . . . C221 C 0.1857(3) 0.58148(12) 0.34345(13) 0.0724(8) Uani 1 1 d . . . H22A H 0.2271 0.5751 0.3840 0.108(3) Uiso 1 1 calc R . . H22B H 0.2096 0.6200 0.3303 0.108(3) Uiso 1 1 calc R . . H22C H 0.2286 0.5541 0.3154 0.108(3) Uiso 1 1 calc R . . C241 C -0.2683(4) 0.50732(15) 0.44799(14) 0.1136(14) Uani 1 1 d . . . H24A H -0.2011 0.5100 0.4831 0.108(3) Uiso 1 1 calc R . . H24B H -0.2829 0.4674 0.4372 0.108(3) Uiso 1 1 calc R . . H24C H -0.3645 0.5244 0.4578 0.108(3) Uiso 1 1 calc R . . C261 C -0.3238(3) 0.59972(11) 0.24438(11) 0.0563(6) Uani 1 1 d . . . H26A H -0.3065 0.6396 0.2343 0.108(3) Uiso 1 1 calc R . . H26B H -0.4285 0.5944 0.2549 0.108(3) Uiso 1 1 calc R . . H26C H -0.3001 0.5759 0.2096 0.108(3) Uiso 1 1 calc R . . C421 C 0.1107(2) 0.90474(10) 0.31084(10) 0.0445(6) Uani 1 1 d . . . H42A H 0.0666 0.8797 0.2789 0.034(4) Uiso 1 1 calc R . . C422 C 0.2747(2) 0.88904(13) 0.31859(11) 0.0628(8) Uani 1 1 d . . . H42B H 0.2829 0.8508 0.3354 0.072(2) Uiso 1 1 calc R . . H42C H 0.3234 0.9160 0.3460 0.072(2) Uiso 1 1 calc R . . H42D H 0.3232 0.8902 0.2793 0.072(2) Uiso 1 1 calc R . . C423 C 0.1000(3) 0.96579(12) 0.28882(13) 0.0728(8) Uani 1 1 d . . . H42E H -0.0042 0.9750 0.2794 0.072(2) Uiso 1 1 calc R . . H42F H 0.1597 0.9703 0.2525 0.072(2) Uiso 1 1 calc R . . H42G H 0.1375 0.9913 0.3204 0.072(2) Uiso 1 1 calc R . . C441 C 0.0965(3) 0.89483(15) 0.53852(11) 0.0721(9) Uani 1 1 d D . . H44J H 0.2055 0.8901 0.5315 0.108 Uiso 0.67 1 calc PR A 1 H44K H 0.1825 0.8720 0.5239 0.108 Uiso 0.33 1 calc PR A 2 C442 C 0.0464(4) 0.85169(14) 0.58172(15) 0.1086(13) Uani 1 1 d . B . H44A H 0.0367 0.8151 0.5612 0.163 Uiso 1 1 calc R . . H44B H -0.0502 0.8628 0.5979 0.163 Uiso 1 1 calc R . . H44C H 0.1195 0.8485 0.6148 0.163 Uiso 1 1 calc R . . C443 C 0.0682(6) 0.95299(17) 0.56964(19) 0.0955(19) Uani 0.67 1 d PD B 1 H44D H 0.0920 0.9837 0.5417 0.143 Uiso 0.67 1 calc PR B 1 H44E H 0.1315 0.9561 0.6058 0.143 Uiso 0.67 1 calc PR B 1 H44F H -0.0366 0.9557 0.5810 0.143 Uiso 0.67 1 calc PR B 1 C444 C 0.1889(11) 0.9457(4) 0.5550(6) 0.096(4) Uiso 0.33 1 d PD B 2 H44G H 0.2504 0.9565 0.5207 0.144 Uiso 0.33 1 calc PR B 2 H44H H 0.2534 0.9366 0.5896 0.144 Uiso 0.33 1 calc PR B 2 H44I H 0.1233 0.9773 0.5653 0.144 Uiso 0.33 1 calc PR B 2 C461 C -0.38712(19) 0.89129(8) 0.41906(9) 0.0329(5) Uani 1 1 d . . . H46A H -0.4226 0.8836 0.3769 0.034(4) Uiso 1 1 calc R . . C462 C -0.4540(2) 0.84631(10) 0.45987(10) 0.0489(6) Uani 1 1 d . . . H46B H -0.4058 0.8098 0.4524 0.072(2) Uiso 1 1 calc R . . H46C H -0.5610 0.8431 0.4514 0.072(2) Uiso 1 1 calc R . . H46D H -0.4381 0.8571 0.5021 0.072(2) Uiso 1 1 calc R . . C463 C -0.4434(2) 0.94954(10) 0.43685(12) 0.0554(6) Uani 1 1 d . . . H46E H -0.4042 0.9780 0.4091 0.072(2) Uiso 1 1 calc R . . H46F H -0.4099 0.9583 0.4780 0.072(2) Uiso 1 1 calc R . . H46G H -0.5525 0.9499 0.4349 0.072(2) Uiso 1 1 calc R . . C621 C 0.3276(3) 0.75090(12) 0.22322(12) 0.0608(7) Uani 1 1 d . . . H62B H 0.2770 0.7412 0.2607 0.108(3) Uiso 1 1 calc R . . H62C H 0.4114 0.7762 0.2323 0.108(3) Uiso 1 1 calc R . . H62D H 0.3646 0.7163 0.2042 0.108(3) Uiso 1 1 calc R . . C641 C 0.1666(5) 0.92763(12) 0.11399(15) 0.1051(13) Uani 1 1 d . . . H64B H 0.1333 0.9354 0.0725 0.108(3) Uiso 1 1 calc R . . H64C H 0.2724 0.9371 0.1184 0.108(3) Uiso 1 1 calc R . . H64D H 0.1087 0.9507 0.1420 0.108(3) Uiso 1 1 calc R . . C661 C -0.1342(3) 0.74871(11) 0.09149(12) 0.0601(7) Uani 1 1 d . . . H66B H -0.2015 0.7761 0.0721 0.108(3) Uiso 1 1 calc R . . H66C H -0.1866 0.7291 0.1238 0.108(3) Uiso 1 1 calc R . . H66D H -0.1011 0.7210 0.0616 0.108(3) Uiso 1 1 calc R . . 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 Mg 0.0292(3) 0.0429(4) 0.0238(3) 0.0022(3) 0.0002(3) 0.0028(3) I 0.03368(8) 0.07649(14) 0.04449(10) -0.00778(8) -0.00897(6) 0.00349(7) N1 0.0299(8) 0.0278(9) 0.0267(8) -0.0015(7) 0.0008(6) -0.0010(7) N2 0.0264(7) 0.0270(9) 0.0237(8) -0.0020(7) -0.0014(6) -0.0016(6) N3 0.0278(7) 0.0261(9) 0.0253(8) -0.0021(7) -0.0010(6) -0.0003(6) O53 0.0395(8) 0.0756(12) 0.0402(9) 0.0126(8) 0.0082(7) 0.0010(8) C11 0.0323(9) 0.0310(12) 0.0290(10) -0.0045(9) -0.0020(8) 0.0022(8) C12 0.0464(11) 0.0307(12) 0.0368(12) -0.0046(10) 0.0025(9) 0.0013(9) C13 0.0695(15) 0.0314(13) 0.0541(15) -0.0051(11) 0.0137(12) 0.0039(11) C14 0.0764(17) 0.0471(16) 0.0543(16) -0.0189(13) 0.0260(13) 0.0043(13) C15 0.0588(14) 0.0479(15) 0.0379(12) -0.0079(11) 0.0150(11) -0.0028(11) C16 0.0370(10) 0.0368(12) 0.0316(11) -0.0044(9) 0.0013(8) -0.0008(9) C21 0.0601(13) 0.0223(11) 0.0354(12) -0.0054(9) 0.0020(10) 0.0012(10) C22 0.0787(17) 0.0260(13) 0.0464(14) -0.0049(11) -0.0092(12) 0.0038(11) C23 0.128(3) 0.0386(15) 0.0352(14) 0.0013(12) -0.0147(16) 0.0037(16) C24 0.129(3) 0.0441(16) 0.0400(15) -0.0021(13) 0.0190(17) -0.0124(17) C25 0.0807(18) 0.0451(15) 0.0537(16) -0.0064(13) 0.0223(14) -0.0125(13) C26 0.0607(14) 0.0306(13) 0.0406(13) -0.0052(10) 0.0076(11) -0.0022(10) C31 0.0237(8) 0.0266(11) 0.0256(9) 0.0014(8) 0.0003(7) -0.0022(7) C32 0.0242(8) 0.0293(11) 0.0265(10) 0.0002(8) 0.0016(7) -0.0034(7) C33 0.0395(10) 0.0285(11) 0.0348(11) -0.0010(9) -0.0011(9) 0.0008(9) C34 0.0416(11) 0.0336(12) 0.0401(12) 0.0079(10) -0.0031(9) 0.0045(9) C35 0.0382(11) 0.0436(14) 0.0300(11) 0.0060(10) -0.0063(9) 0.0021(9) C36 0.0337(10) 0.0366(12) 0.0289(10) -0.0027(9) -0.0024(8) -0.0002(9) C41 0.0297(9) 0.0237(11) 0.0280(10) -0.0036(8) -0.0010(8) -0.0003(7) C42 0.0298(9) 0.0419(13) 0.0311(11) -0.0059(9) 0.0013(8) -0.0042(8) C43 0.0257(10) 0.0751(17) 0.0384(13) -0.0092(12) -0.0024(9) -0.0053(10) C44 0.0333(11) 0.0722(17) 0.0327(12) -0.0067(11) -0.0049(9) -0.0041(10) C45 0.0335(10) 0.0513(14) 0.0272(10) -0.0051(10) 0.0022(8) -0.0029(9) C46 0.0284(9) 0.0290(11) 0.0274(10) -0.0042(8) 0.0006(7) -0.0008(8) C51 0.0366(12) 0.087(2) 0.0580(16) -0.0131(15) 0.0062(11) -0.0120(13) C52 0.0456(12) 0.0506(16) 0.0692(18) -0.0080(13) 0.0213(12) -0.0123(11) C54 0.0575(17) 0.096(2) 0.0650(19) 0.0184(17) 0.0115(14) 0.0068(16) C55 0.113(3) 0.111(3) 0.083(2) 0.020(2) 0.029(2) 0.001(2) C61 0.0406(11) 0.0415(13) 0.0245(10) -0.0014(9) 0.0071(8) -0.0012(9) C62 0.0439(12) 0.0514(15) 0.0327(12) -0.0050(10) 0.0079(9) -0.0101(10) C63 0.0690(16) 0.0537(17) 0.0479(15) -0.0066(13) 0.0193(13) -0.0232(14) C64 0.099(2) 0.0460(17) 0.0498(16) 0.0020(13) 0.0333(16) -0.0082(16) C65 0.0831(19) 0.0588(18) 0.0383(14) 0.0152(13) 0.0158(13) 0.0220(15) C66 0.0518(13) 0.0526(16) 0.0278(11) 0.0010(10) 0.0061(10) 0.0082(11) C221 0.086(2) 0.0542(18) 0.076(2) -0.0081(15) -0.0282(16) 0.0119(15) C241 0.196(4) 0.089(3) 0.056(2) 0.0141(19) 0.035(2) -0.024(3) C261 0.0567(14) 0.0582(17) 0.0540(16) -0.0092(13) 0.0031(12) -0.0035(12) C421 0.0313(10) 0.0672(17) 0.0351(12) -0.0073(11) 0.0055(9) -0.0127(10) C422 0.0329(11) 0.108(2) 0.0479(15) -0.0111(15) 0.0071(10) -0.0067(13) C423 0.0667(17) 0.085(2) 0.0669(19) 0.0132(16) 0.0181(14) -0.0208(15) C441 0.0465(14) 0.136(3) 0.0338(14) -0.0094(16) -0.0066(11) -0.0136(16) C442 0.168(4) 0.078(2) 0.078(2) 0.0156(19) -0.073(2) -0.014(2) C443 0.170(5) 0.063(3) 0.052(3) 0.006(2) -0.067(3) -0.048(3) C461 0.0267(9) 0.0412(13) 0.0308(11) -0.0056(9) 0.0003(8) -0.0005(8) C462 0.0374(11) 0.0585(16) 0.0509(14) 0.0028(12) 0.0055(10) -0.0085(11) C463 0.0401(12) 0.0562(16) 0.0700(17) -0.0134(13) 0.0051(12) 0.0098(11) C621 0.0472(14) 0.082(2) 0.0534(16) -0.0003(14) -0.0061(12) -0.0137(12) C641 0.176(4) 0.052(2) 0.089(3) 0.0097(18) 0.047(3) -0.008(2) C661 0.0565(15) 0.081(2) 0.0424(14) -0.0048(13) -0.0119(12) 0.0098(13) 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' 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' Mg Mg 0.0486 0.0363 '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' 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 O53 Mg N3 114.51(6) . . O53 Mg N1 125.70(7) . . N3 Mg N1 61.45(6) . . O53 Mg N2 125.68(6) . . N3 Mg N2 30.55(5) . . N1 Mg N2 30.89(5) . . O53 Mg I 105.39(5) . . N3 Mg I 132.64(5) . . N1 Mg I 113.36(5) . . N2 Mg I 128.51(4) . . N2 N1 C11 113.57(15) . . N2 N1 Mg 93.57(10) . . C11 N1 Mg 151.42(13) . . N3 N2 N1 109.84(14) . . N3 N2 Mg 54.31(9) . . N1 N2 Mg 55.53(9) . . N2 N3 C31 113.28(14) . . N2 N3 Mg 95.14(11) . . C31 N3 Mg 151.33(12) . . C52 O53 C54 113.72(18) . . C52 O53 Mg 125.57(14) . . C54 O53 Mg 120.17(14) . . C12 C11 C16 120.04(17) . . C12 C11 N1 117.56(16) . . C16 C11 N1 122.35(17) . . C11 C12 C13 119.41(19) . . C11 C12 C21 122.60(17) . . C13 C12 C21 117.97(19) . . C14 C13 C12 121.0(2) . . C13 C14 C15 119.2(2) . . C16 C15 C14 122.1(2) . . C15 C16 C11 118.13(19) . . C15 C16 C61 117.86(18) . . C11 C16 C61 123.93(17) . . C22 C21 C26 120.3(2) . . C22 C21 C12 119.8(2) . . C26 C21 C12 119.5(2) . . C23 C22 C21 117.8(3) . . C23 C22 C221 120.9(2) . . C21 C22 C221 121.3(2) . . C24 C23 C22 123.0(3) . . C23 C24 C25 117.8(2) . . C23 C24 C241 120.5(3) . . C25 C24 C241 121.7(3) . . C24 C25 C26 122.2(3) . . C25 C26 C21 118.9(2) . . C25 C26 C261 120.1(2) . . C21 C26 C261 120.9(2) . . C36 C31 C32 120.21(17) . . C36 C31 N3 120.92(17) . . C32 C31 N3 118.87(16) . . C33 C32 C31 117.92(17) . . C33 C32 C41 120.20(17) . . C31 C32 C41 121.88(16) . . C34 C33 C32 122.07(19) . . C33 C34 C35 119.38(19) . . C34 C35 C36 120.22(19) . . C35 C36 C31 120.19(19) . . C46 C41 C42 119.33(17) . . C46 C41 C32 120.63(15) . . C42 C41 C32 120.00(16) . . C43 C42 C41 118.49(18) . . C43 C42 C421 120.48(17) . . C41 C42 C421 120.95(18) . . C42 C43 C44 123.20(18) . . C45 C44 C43 116.93(19) . . C45 C44 C441 122.49(19) . . C43 C44 C441 120.56(19) . . C44 C45 C46 122.51(18) . . C45 C46 C41 119.43(16) . . C45 C46 C461 118.71(16) . . C41 C46 C461 121.78(16) . . O53 C52 C51 109.64(18) . . C55 C54 O53 108.5(3) . . C62 C61 C66 119.7(2) . . C62 C61 C16 119.5(2) . . C66 C61 C16 120.7(2) . . C63 C62 C61 118.6(2) . . C63 C62 C621 120.5(2) . . C61 C62 C621 120.9(2) . . C64 C63 C62 122.7(2) . . C65 C64 C63 117.6(2) . . C65 C64 C641 121.2(3) . . C63 C64 C641 121.2(3) . . C64 C65 C66 122.5(3) . . C65 C66 C61 118.8(2) . . C65 C66 C661 121.1(2) . . C61 C66 C661 120.1(2) . . C423 C421 C422 108.8(2) . . C423 C421 C42 110.31(19) . . C422 C421 C42 113.63(19) . . C442 C441 C444 124.6(5) . . C442 C441 C44 114.5(2) . . C444 C441 C44 118.8(5) . . C442 C441 C443 105.5(3) . . C444 C441 C443 44.1(4) . . C44 C441 C443 108.3(3) . . C463 C461 C462 109.93(17) . . C463 C461 C46 110.20(16) . . C462 C461 C46 113.26(17) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mg O53 2.0157(15) . Mg N3 2.0880(16) . Mg N1 2.1151(16) . Mg N2 2.5605(16) . Mg I 2.6438(7) . N1 N2 1.317(2) . N1 C11 1.424(2) . N2 N3 1.307(2) . N3 C31 1.423(2) . O53 C52 1.451(3) . O53 C54 1.521(3) . C11 C12 1.397(3) . C11 C16 1.419(3) . C12 C13 1.399(3) . C12 C21 1.499(3) . C13 C14 1.372(3) . C14 C15 1.388(3) . C15 C16 1.384(3) . C16 C61 1.489(3) . C21 C22 1.400(3) . C21 C26 1.401(3) . C22 C23 1.397(4) . C22 C221 1.508(4) . C23 C24 1.376(4) . C24 C25 1.378(4) . C24 C241 1.518(4) . C25 C26 1.387(3) . C26 C261 1.509(3) . C31 C36 1.398(3) . C31 C32 1.400(3) . C32 C33 1.396(3) . C32 C41 1.500(3) . C33 C34 1.380(3) . C34 C35 1.381(3) . C35 C36 1.386(3) . C41 C46 1.406(2) . C41 C42 1.414(2) . C42 C43 1.389(3) . C42 C421 1.528(3) . C43 C44 1.392(3) . C44 C45 1.387(3) . C44 C441 1.524(3) . C45 C46 1.389(3) . C46 C461 1.526(2) . C51 C52 1.487(4) . C54 C55 1.462(4) . C61 C62 1.399(3) . C61 C66 1.400(3) . C62 C63 1.394(3) . C62 C621 1.501(3) . C63 C64 1.376(4) . C64 C65 1.374(4) . C64 C641 1.513(4) . C65 C66 1.392(3) . C66 C661 1.504(4) . C421 C423 1.524(4) . C421 C422 1.527(3) . C441 C442 1.473(4) . C441 C444 1.503(6) . C441 C443 1.560(5) . C461 C463 1.519(3) . C461 C462 1.524(3) . loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 2 0 0 21982.11 22559.97 315.88 o 4 0 0 728.48 752.19 25.96 o 6 0 0 1.59 5.30 12.82 o 8 0 0 1695.19 1858.94 52.91 o 10 0 0 2804.73 2654.71 232.37 o 12 0 0 1621.11 1991.35 247.95 o 1 1 0 1069.71 1015.90 37.51 o 2 1 0 20533.67 21139.36 205.22 o 3 1 0 1081.12 1084.33 18.25 o 4 1 0 7162.88 6376.61 48.80 o 5 1 0 299.00 242.86 14.04 o 6 1 0 5821.90 5789.06 60.53 o 7 1 0 314.16 279.87 18.29 o 8 1 0 3278.25 3316.12 47.81 o 9 1 0 93.41 71.13 15.94 o 10 1 0 60.70 61.79 30.54 o 11 1 0 25.78 38.84 68.34 o 12 1 0 613.13 969.71 199.91 o 2 2 0 10276.95 11447.51 159.20 o 3 2 0 848.94 828.63 17.60 o 4 2 0 1074.66 877.62 20.81 o 5 2 0 1098.47 1303.55 26.19 o 6 2 0 172.17 187.98 14.19 o 7 2 0 30.43 6.59 11.98 o 8 2 0 3160.04 3132.63 48.47 o 9 2 0 3.81 -7.04 17.82 o 10 2 0 1383.77 1560.86 72.65 o 11 2 0 92.70 81.81 70.61 o 12 2 0 737.46 823.02 188.23 o 1 3 0 7.95 32.09 6.48 o 2 3 0 27806.46 28458.07 272.88 o 3 3 0 157.63 129.80 9.92 o 4 3 0 25416.37 25283.99 277.76 o 5 3 0 234.28 218.87 12.96 o 6 3 0 8729.96 8133.04 65.20 o 7 3 0 757.09 738.78 26.71 o 8 3 0 4944.07 4652.36 76.93 o 9 3 0 2.01 -0.25 23.93 o 10 3 0 102.89 118.35 35.58 o 11 3 0 25.87 46.10 35.02 o 12 3 0 0.63 40.24 110.34 o 0 4 0 934.59 599.51 398.53 o 1 4 0 1470.88 1456.84 26.73 o 2 4 0 16334.72 15477.15 143.94 o 3 4 0 1443.59 1327.11 26.60 o 4 4 0 885.73 747.90 20.58 o 6 4 0 9.83 15.31 10.45 o 7 4 0 0.66 -3.08 13.13 o 8 4 0 5595.66 5407.69 71.78 o 9 4 0 523.80 498.73 45.22 o 10 4 0 759.90 849.29 71.62 o 11 4 0 200.72 202.14 47.70 o 12 4 0 360.90 337.52 144.09 o 1 5 0 1499.28 1630.08 31.45 o 2 5 0 2676.95 2727.64 41.78 o 3 5 0 1881.44 2078.14 36.25 o 4 5 0 18998.26 19143.70 135.19 o 5 5 0 3042.69 3248.42 42.18 o 6 5 0 5711.12 5605.33 57.77 o 7 5 0 2031.34 2074.01 43.79 o 8 5 0 4251.67 4200.37 80.38 o 9 5 0 4.05 26.55 19.87 o 10 5 0 123.89 98.98 43.09 o 11 5 0 23.67 59.71 41.74 o 12 5 0 67.67 48.68 41.84 o 0 6 0 181298.89 134861.42 20856.90 o 1 6 0 1671.19 1840.54 33.37 o 2 6 0 13541.58 13425.50 216.83 o 3 6 0 469.91 408.56 17.08 o 4 6 0 28.02 38.68 10.34 o 5 6 0 5.65 6.09 10.28 o 6 6 0 11.61 11.46 10.78 o 7 6 0 325.15 309.93 25.00 o 8 6 0 1711.74 1763.37 50.00 o 9 6 0 329.97 341.88 27.30 o 10 6 0 1450.80 1543.02 94.94 o 11 6 0 116.30 207.86 52.72 o 12 6 0 540.96 585.54 70.52 o 1 7 0 4134.09 4319.34 77.66 o 2 7 0 8.10 14.93 9.41 o 3 7 0 1346.36 1471.36 25.35 o 4 7 0 6271.33 6088.27 64.34 o 5 7 0 5682.81 5713.66 58.98 o 6 7 0 1333.19 1332.08 32.75 o 7 7 0 3914.46 3848.90 70.62 o 8 7 0 1424.18 1570.31 50.30 o 9 7 0 32.20 3.78 22.59 o 10 7 0 25.39 35.07 35.94 o 11 7 0 27.18 37.11 44.16 o 12 7 0 619.55 747.52 80.01 o 0 8 0 24266.38 21915.24 1464.83 o 1 8 0 3445.51 3338.11 71.94 o 2 8 0 8836.29 8950.30 149.96 o 3 8 0 1815.75 1805.80 29.40 o 4 8 0 35.31 21.92 9.69 o 5 8 0 2313.58 2280.34 43.27 o 6 8 0 8.98 2.82 13.17 o 7 8 0 11.45 1.29 17.43 o 8 8 0 527.54 558.69 42.77 o 9 8 0 71.23 61.25 26.58 o 10 8 0 1101.15 1038.35 77.53 o 11 8 0 193.26 147.95 54.06 o 1 9 0 3532.09 3624.63 58.14 o 2 9 0 12.63 5.17 9.64 o 3 9 0 2116.98 2067.07 39.83 o 4 9 0 5440.60 5282.51 88.40 o 5 9 0 3051.44 3017.91 44.77 o 6 9 0 2492.84 2483.27 48.00 o 7 9 0 2504.79 2361.41 63.59 o 8 9 0 1107.76 1136.49 58.49 o 9 9 0 16.77 -1.32 23.43 o 10 9 0 120.57 91.15 29.56 o 11 9 0 8.60 -3.35 42.98 o 0 10 0 8909.63 8198.13 266.66 o 1 10 0 1761.00 1838.07 31.19 o 2 10 0 3198.47 3342.54 50.07 o 3 10 0 3565.95 3778.02 60.05 o 4 10 0 1937.32 1948.05 34.82 o 5 10 0 728.38 798.25 28.30 o 6 10 0 49.67 62.03 20.73 o 7 10 0 1.59 -16.78 22.77 o 8 10 0 2143.25 2094.81 83.25 o 9 10 0 268.01 254.63 36.99 o 10 10 0 277.04 241.38 37.20 o 11 10 0 308.40 372.35 69.31 o 1 11 0 1055.71 970.20 26.09 o 2 11 0 1404.41 1531.05 37.09 o 3 11 0 4195.95 4167.37 77.86 o 4 11 0 9330.92 9295.70 153.79 o 5 11 0 5173.64 5186.84 127.25 o 6 11 0 4776.52 4968.72 114.78 o 7 11 0 1658.29 1798.39 70.90 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