#------------------------------------------------------------------------------ #$Date: 2025-01-16 02:03:11 +0200 (Thu, 16 Jan 2025) $ #$Revision: 297345 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/36/1573699.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_1573699 _journal_paper_doi 10.1039/D4DT03495C _chemical_formula_moiety 'C96 H116 Mg2 N4 Ni P2, 4(C6 H6)' _chemical_formula_sum 'C120 H140 Mg2 N4 Ni P2' _chemical_formula_weight 1807.62 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yc' _space_group_name_H-M_alt 'P 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2024-11-20 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-12-06 deposited with the CCDC. 2025-01-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.001(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 18.2558(11) _cell_length_b 15.2714(9) _cell_length_c 18.9886(12) _cell_measurement_reflns_used 9983 _cell_measurement_temperature 150.00 _cell_measurement_theta_max 60.599 _cell_measurement_theta_min 3.324 _cell_volume 5136.6(5) _computing_cell_refinement 'SAINT V8.40B (2016)' _computing_data_reduction 'SAINT V8.40B (2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 150.00 _diffrn_measured_fraction_theta_full 0.958 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.1040 _diffrn_reflns_av_unetI/netI 0.0451 _diffrn_reflns_Laue_measured_fraction_full 0.958 _diffrn_reflns_Laue_measured_fraction_max 0.963 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 113318 _diffrn_reflns_point_group_measured_fraction_full 0.958 _diffrn_reflns_point_group_measured_fraction_max 0.963 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 56.965 _diffrn_reflns_theta_min 3.635 _diffrn_source_current 3.57 _diffrn_source_power 0.24947159999999996 _diffrn_source_voltage 69.88 _exptl_absorpt_coefficient_mu 1.543 _exptl_absorpt_correction_T_max 0.7518 _exptl_absorpt_correction_T_min 0.5860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1367 before and 0.0867 after correction. The Ratio of minimum to maximum transmission is 0.7795. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear whiteish white' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier whiteish _exptl_crystal_colour_primary white _exptl_crystal_density_diffrn 1.169 _exptl_crystal_description block _exptl_crystal_F_000 1940 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.838 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 648 _refine_ls_number_reflns 10130 _refine_ls_number_restraints 232 _refine_ls_restrained_S_all 1.104 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0549 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+1.1484P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1504 _refine_ls_wR_factor_ref 0.1551 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8774 _reflns_number_total 10130 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4dt03495c2.cif _cod_data_source_block ga20240829xa_0ma_a _cod_database_code 1573699 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_max 0.802 _shelx_estimated_absorpt_t_min 0.748 _olex2_refinement_description ; 1. Restrained distances C60-C59 = C63-C62 = C62-C61 1.37 with sigma of 0.02 C60-C61 1.38 with sigma of 0.02 C59-C58 = C58-C63 1.36 with sigma of 0.02 C53-C54 = C56-C57 = C57-C52 1.37 with sigma of 0.02 C53-C52 1.38 with sigma of 0.02 C54-C55 = C55-C56 1.36 with sigma of 0.02 C60-C58 = C58-C62 = C63-C61 2.37 with sigma of 0.04 C60-C62 2.38 with sigma of 0.04 C59-C63 2.36 with sigma of 0.04 C53-C55 = C55-C57 = C56-C52 2.37 with sigma of 0.04 C53-C57 2.38 with sigma of 0.04 C54-C56 2.36 with sigma of 0.04 C60-C59 \\sim C59-C58 \\sim C58-C63 \\sim C63-C62 \\sim C62-C61 \\sim C61-C60 with sigma of 0.02 C60-C62 \\sim C60-C58 \\sim C62-C58 \\sim C63-C59 \\sim C63-C61 \\sim C61-C59 with sigma of 0.04 C53-C54 \\sim C54-C55 \\sim C55-C56 \\sim C56-C57 \\sim C57-C52 \\sim C52-C53 with sigma of 0.02 C53-C57 \\sim C53-C55 \\sim C57-C55 \\sim C56-C54 \\sim C56-C52 \\sim C52-C54 with sigma of 0.04 2. Restrained planarity C60, C59, C58, C63, C62, C61 with sigma of 0.1 C53, C54, C55, C56, C57, C52 with sigma of 0.1 3. Uiso/Uaniso restraints and constraints C60 \\sim C59 \\sim C58 \\sim C63 \\sim C62 \\sim C61: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C52: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 4. Rigid body (RIGU) restrains C60, C59, C58, C63, C62, C61 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C53, C54, C55, C56, C57, C52 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Fixed Sof: C46B(0.5) H46B(0.5) C47B(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C46A(0.5) H46A(0.5) C47A(0.5) H47D(0.5) H47E(0.5) H47F(0.5) C48B(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C48A(0.5) H48D(0.5) H48E(0.5) H48F(0.5) C60(0.5) H60(0.5) C59(0.5) H59(0.5) C58(0.5) H58(0.5) C63(0.5) H63(0.5) C62(0.5) H62(0.5) C61(0.5) H61(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5) C55(0.5) H55(0.5) C56(0.5) H56(0.5) C57(0.5) H57(0.5) C52(0.5) H52(0.5) 6.a Ternary CH refined with riding coordinates: C20(H20), C33(H33), C11(H11), C46B(H46B), C8(H8), C46A(H46A) 6.b Aromatic/amide H refined with riding coordinates: C18(H18), C41(H41), C16(H16), C22(H22), C35(H35), C26(H26), C32(H32), C36(H36), C23(H23), C45(H45), C37(H37), C39(H39), C42(H42), C31(H31), C25(H25), C28(H28), C24(H24), C44(H44), C38(H38), C49(H49), C29(H29), C50(H50), C30(H30), C64(H64), C51(H51), C43(H43), C65(H65), C66(H66), C60(H60), C59(H59), C58(H58), C63(H63), C62(H62), C61(H61), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C52(H52) 6.c Fitted hexagon refined as free rotating group: C60(C59,C58,C63,C62,C61) 6.d Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C47B(H47A,H47B, H47C), C47A(H47D,H47E,H47F), C48B(H48A,H48B,H48C), C48A(H48D,H48E,H48F) ; _shelx_res_file ; TITL Ga20240829xa_0ma_a.res in P2/c ga20240829xa_0ma_a.res created by SHELXL-2018/3 at 15:45:25 on 19-Nov-2024 REM Old TITL __TMP__ in P2/c REM SHELXT solution in P2/c: R1 0.183, Rweak 0.015, Alpha 0.061 REM 0.664 for 413 systematic absences, Orientation as input REM Formula found by SHELXT: C98 N20 Ni P4 CELL 1.34139 18.2558 15.2714 18.9886 90 104.001 90 ZERR 2 0.0011 0.0009 0.0012 0 0.002 0 LATT 1 SYMM -X,+Y,0.5-Z SFAC C H Mg N Ni P DISP C 0.0137 0.0067 57.1 DISP H 0 0 0.6 DISP Mg 0.1421 0.1346 1045 DISP N 0.0241 0.0134 109.9 DISP Ni -1.3357 3.2904 25038 DISP P 0.2543 0.3332 2560.5 UNIT 240 280 4 8 2 4 DFIX 1.37 C60 C59 C63 C62 C62 C61 DANG 2.37 C60 C58 C58 C62 C63 C61 DFIX 1.38 C60 C61 DANG 2.38 C60 C62 DFIX 1.36 C59 C58 C58 C63 DANG 2.36 C59 C63 SADI C60 C59 C59 C58 C58 C63 C63 C62 C62 C61 C61 C60 SADI 0.04 C60 C62 C60 C58 C62 C58 C63 C59 C63 C61 C61 C59 FLAT C60 C59 C58 C63 C62 C61 SIMU C60 C59 C58 C63 C62 C61 RIGU C60 C59 C58 C63 C62 C61 DFIX 1.37 C53 C54 C56 C57 C57 C52 DANG 2.37 C53 C55 C55 C57 C56 C52 DFIX 1.38 C53 C52 DANG 2.38 C53 C57 DFIX 1.36 C54 C55 C55 C56 DANG 2.36 C54 C56 SADI C53 C54 C54 C55 C55 C56 C56 C57 C57 C52 C52 C53 SADI 0.04 C53 C57 C53 C55 C57 C55 C56 C54 C56 C52 C52 C54 FLAT C53 C54 C55 C56 C57 C52 SIMU C53 C54 C55 C56 C57 C52 RIGU C53 C54 C55 C56 C57 C52 L.S. 20 PLAN 13 SIZE 0.2 0.2 0.15 TEMP -123.15 CONF LIST 6 MORE -1 BOND $H fmap 2 acta SHEL 999 0.8 OMIT -7 3 8 OMIT -5 2 17 OMIT -4 2 16 OMIT -3 3 5 OMIT -1 2 3 OMIT 0 1 0 OMIT 0 1 2 OMIT 0 2 2 OMIT 0 3 3 OMIT 0 5 5 OMIT 1 0 0 OMIT 1 1 0 OMIT 1 1 3 OMIT 1 10 2 OMIT 2 3 5 OMIT 3 0 4 OMIT 6 4 3 OMIT 14 0 2 REM REM REM WGHT 0.092600 1.148400 FVAR 0.94070 NI1 5 0.500000 0.887830 0.250000 10.50000 0.02132 0.03086 = 0.03384 0.00000 0.00931 0.00000 P1 6 0.221118 1.029900 0.222123 11.00000 0.03175 0.02668 = 0.04545 0.00429 0.01044 0.00618 MG1 3 0.371394 0.879184 0.261347 11.00000 0.02173 0.02789 = 0.03916 0.00123 0.01000 -0.00010 N2 4 0.285623 0.788655 0.261627 11.00000 0.02332 0.02327 = 0.03027 0.00114 0.00746 0.00062 N1 4 0.264629 0.931259 0.247561 11.00000 0.02416 0.02635 = 0.04131 0.00273 0.00908 0.00255 C15 1 0.291701 0.636692 0.222704 11.00000 0.02550 0.02628 = 0.03271 -0.00211 0.00733 -0.00153 C14 1 0.280232 0.697628 0.274786 11.00000 0.02174 0.02300 = 0.03211 0.00093 0.00603 -0.00066 C20 1 0.263899 0.733586 0.400682 11.00000 0.03059 0.02909 = 0.03067 0.00116 0.00906 -0.00021 AFIX 13 H20 2 0.233102 0.782475 0.373467 11.00000 -1.20000 AFIX 0 C3 1 0.232874 0.851242 0.247018 11.00000 0.02350 0.02858 = 0.02915 0.00088 0.00745 0.00177 C18 1 0.276263 0.577220 0.356906 11.00000 0.03424 0.03140 = 0.03480 0.00418 0.01150 -0.00074 AFIX 43 H18 2 0.269860 0.556931 0.402332 11.00000 -1.20000 AFIX 0 C19 1 0.273509 0.666966 0.343293 11.00000 0.02446 0.02753 = 0.03107 0.00150 0.00676 -0.00032 C21 1 0.219258 0.698873 0.453528 11.00000 0.03748 0.02761 = 0.03624 -0.00197 0.01433 -0.00355 C40 1 0.228683 0.667767 0.088737 11.00000 0.03720 0.03257 = 0.03285 -0.00171 0.01091 0.00298 C41 1 0.173240 0.603344 0.082544 11.00000 0.04049 0.03863 = 0.04312 0.00077 0.00677 -0.00275 AFIX 43 H41 2 0.178072 0.559833 0.119138 11.00000 -1.20000 AFIX 0 C16 1 0.296079 0.547813 0.240059 11.00000 0.03514 0.02743 = 0.03776 -0.00406 0.01064 -0.00040 AFIX 43 H16 2 0.304914 0.507311 0.205046 11.00000 -1.20000 AFIX 0 C34 1 0.365561 0.620654 0.127088 11.00000 0.03592 0.03242 = 0.03360 -0.00035 0.01375 -0.00082 C4 1 0.146200 0.837478 0.229802 11.00000 0.02240 0.03326 = 0.03904 0.00128 0.00629 0.00128 C5 1 0.121612 0.741709 0.233076 11.00000 0.02422 0.03793 = 0.04547 -0.00129 0.00671 -0.00358 AFIX 137 H5A 2 0.140301 0.707021 0.197657 11.00000 -1.50000 H5B 2 0.066378 0.738551 0.221749 11.00000 -1.50000 H5C 2 0.142464 0.718434 0.281913 11.00000 -1.50000 AFIX 0 C33 1 0.301134 0.668601 0.149331 11.00000 0.03302 0.02651 = 0.03392 -0.00298 0.01088 -0.00190 AFIX 13 H33 2 0.316995 0.731311 0.156322 11.00000 -1.20000 AFIX 0 C27 1 0.338711 0.774448 0.440601 11.00000 0.03472 0.03911 = 0.02741 0.00162 0.01071 -0.00560 C22 1 0.141573 0.710636 0.438284 11.00000 0.03895 0.04682 = 0.04336 0.00033 0.01696 -0.00227 AFIX 43 H22 2 0.116687 0.738900 0.394451 11.00000 -1.20000 AFIX 0 C17 1 0.288114 0.516002 0.306087 11.00000 0.04058 0.02861 = 0.04217 0.00118 0.01125 0.00048 C35 1 0.439222 0.642189 0.162141 11.00000 0.03705 0.04879 = 0.03821 -0.00621 0.00831 0.00295 AFIX 43 H35 2 0.447944 0.686986 0.197916 11.00000 -1.20000 AFIX 0 C6 1 0.113875 0.890794 0.284255 11.00000 0.02590 0.04097 = 0.05066 0.00114 0.01378 0.00339 AFIX 137 H6A 2 0.142862 0.878094 0.333754 11.00000 -1.50000 H6B 2 0.060897 0.874757 0.279341 11.00000 -1.50000 H6C 2 0.117312 0.953429 0.274294 11.00000 -1.50000 AFIX 0 C26 1 0.254000 0.657349 0.518404 11.00000 0.04771 0.03217 = 0.04025 0.00309 0.01679 -0.00017 AFIX 43 H26 2 0.307089 0.648541 0.530292 11.00000 -1.20000 AFIX 0 C32 1 0.339937 0.862786 0.459530 11.00000 0.04765 0.04430 = 0.04244 -0.00972 0.01877 -0.00995 AFIX 43 H32 2 0.295351 0.896846 0.444393 11.00000 -1.20000 AFIX 0 C7 1 0.110586 0.867642 0.151751 11.00000 0.02830 0.04818 = 0.04351 0.00604 0.00016 0.00201 AFIX 137 H7A 2 0.117922 0.930872 0.147910 11.00000 -1.50000 H7B 2 0.056446 0.854436 0.139544 11.00000 -1.50000 H7C 2 0.134694 0.836838 0.118064 11.00000 -1.50000 AFIX 0 C36 1 0.500466 0.599703 0.146078 11.00000 0.03702 0.06289 = 0.04774 -0.00354 0.01175 0.00546 AFIX 43 H36 2 0.550487 0.615546 0.170491 11.00000 -1.20000 AFIX 0 C23 1 0.099338 0.681879 0.485888 11.00000 0.04480 0.05366 = 0.06254 -0.00220 0.02960 -0.00832 AFIX 43 H23 2 0.046212 0.690340 0.474334 11.00000 -1.20000 AFIX 0 C45 1 0.218762 0.731316 0.034829 11.00000 0.05111 0.04675 = 0.04148 0.00900 0.01138 -0.00053 AFIX 43 H45 2 0.255456 0.776167 0.037873 11.00000 -1.20000 AFIX 0 C2 1 0.569907 0.889845 0.344709 11.00000 0.02880 0.04417 = 0.03785 -0.00057 0.00728 0.00183 C13 1 0.248368 0.999809 0.087470 11.00000 0.04695 0.05412 = 0.04701 0.01272 0.01492 0.00748 AFIX 137 H13A 2 0.259183 0.939419 0.104231 11.00000 -1.50000 H13B 2 0.276995 1.013866 0.051436 11.00000 -1.50000 H13C 2 0.194246 1.006050 0.065426 11.00000 -1.50000 AFIX 0 C37 1 0.488104 0.534235 0.094334 11.00000 0.04809 0.05679 = 0.06361 -0.00470 0.03065 0.00814 AFIX 43 H37 2 0.529620 0.504425 0.083295 11.00000 -1.20000 AFIX 0 C11 1 0.271238 1.062268 0.151837 11.00000 0.04615 0.03250 = 0.06035 0.01299 0.02046 0.00648 AFIX 13 H11 2 0.326907 1.057534 0.172672 11.00000 -1.20000 AFIX 0 C39 1 0.354136 0.555735 0.074840 11.00000 0.04400 0.05066 = 0.05595 -0.01966 0.02474 -0.01192 AFIX 43 H39 2 0.304233 0.540485 0.049613 11.00000 -1.20000 AFIX 0 C42 1 0.111225 0.602126 0.023625 11.00000 0.03894 0.05601 = 0.04973 -0.00164 0.00343 -0.00363 AFIX 43 H42 2 0.074438 0.557247 0.019821 11.00000 -1.20000 AFIX 0 C31 1 0.405318 0.901683 0.500149 11.00000 0.06220 0.06531 = 0.04347 -0.01856 0.01997 -0.02682 AFIX 43 H31 2 0.405280 0.961868 0.512797 11.00000 -1.20000 AFIX 0 C25 1 0.211912 0.628724 0.565833 11.00000 0.06664 0.03570 = 0.04557 0.00584 0.02592 -0.00253 AFIX 43 H25 2 0.236427 0.600340 0.609732 11.00000 -1.20000 AFIX 0 C28 1 0.404809 0.726066 0.461935 11.00000 0.03702 0.05343 = 0.03998 0.01162 0.00644 -0.00278 AFIX 43 H28 2 0.405359 0.666168 0.448567 11.00000 -1.20000 AFIX 0 C24 1 0.134868 0.641130 0.549778 11.00000 0.06549 0.03872 = 0.05616 -0.00088 0.03658 -0.00961 AFIX 43 H24 2 0.106411 0.621694 0.582579 11.00000 -1.20000 AFIX 0 C1 1 0.489705 0.888722 0.349429 11.00000 0.03080 0.05665 = 0.03801 0.00354 0.01104 0.00017 PART 2 C46B 1 0.280434 0.416671 0.314324 10.50000 0.04510 AFIX 13 H46B 2 0.315886 0.395208 0.285399 10.50000 -1.20000 AFIX 0 PART 0 C44 1 0.155819 0.729995 -0.023435 11.00000 0.05679 0.06676 = 0.04557 0.01846 0.00739 0.00604 AFIX 43 H44 2 0.149683 0.774323 -0.059492 11.00000 -1.20000 AFIX 0 C8 1 0.266926 1.100910 0.299247 11.00000 0.05432 0.02997 = 0.05793 -0.00200 0.00511 0.00536 AFIX 13 H8 2 0.258350 1.162665 0.281673 11.00000 -1.20000 AFIX 0 C38 1 0.415614 0.512433 0.058944 11.00000 0.05696 0.05530 = 0.07503 -0.03040 0.03625 -0.01169 AFIX 43 H38 2 0.407159 0.467480 0.023306 11.00000 -1.20000 AFIX 0 C49 1 0.072163 0.534231 0.241378 11.00000 0.04588 0.04700 = 0.11521 0.00474 0.02628 -0.00414 AFIX 43 H49 2 0.122147 0.534163 0.234869 11.00000 -1.20000 AFIX 0 C29 1 0.470314 0.765188 0.502901 11.00000 0.03900 0.09080 = 0.04560 0.02017 0.00113 -0.00606 AFIX 43 H29 2 0.515299 0.731775 0.517825 11.00000 -1.20000 AFIX 0 C50 1 0.060786 0.534003 0.309027 11.00000 0.05145 0.04218 = 0.10291 -0.01422 0.01240 -0.00363 AFIX 43 H50 2 0.102530 0.533465 0.350145 11.00000 -1.20000 AFIX 0 C30 1 0.469914 0.853036 0.521953 11.00000 0.05766 0.09393 = 0.03549 -0.00512 0.00608 -0.03556 AFIX 43 H30 2 0.514555 0.879429 0.550176 11.00000 -1.20000 AFIX 0 C64 1 -0.041035 1.025467 0.047589 11.00000 0.07236 0.10692 = 0.06633 0.00910 0.00785 0.03276 AFIX 43 H64 2 -0.069699 1.043303 0.080699 11.00000 -1.20000 AFIX 0 C12 1 0.251776 1.156984 0.127579 11.00000 0.11526 0.04004 = 0.08617 0.02657 0.04951 0.01785 AFIX 137 H12A 2 0.196815 1.163677 0.112341 11.00000 -1.50000 H12B 2 0.273965 1.171009 0.086829 11.00000 -1.50000 H12C 2 0.272109 1.196799 0.168065 11.00000 -1.50000 AFIX 0 C51 1 -0.012012 0.534559 0.317905 11.00000 0.06910 0.05455 = 0.09885 -0.01702 0.03300 0.00281 AFIX 43 H51 2 -0.020446 0.535169 0.365348 11.00000 -1.20000 AFIX 0 C43 1 0.102436 0.665439 -0.029504 11.00000 0.04498 0.07308 = 0.04289 0.00320 0.00052 0.00602 AFIX 43 H43 2 0.059895 0.664366 -0.069852 11.00000 -1.20000 AFIX 0 C65 1 -0.050215 0.943324 0.018447 11.00000 0.05913 0.09289 = 0.07591 0.02385 -0.00645 0.00662 AFIX 43 H65 2 -0.085085 0.904002 0.031427 11.00000 -1.20000 AFIX 0 C9 1 0.227006 1.090945 0.360803 11.00000 0.06914 0.07556 = 0.05890 -0.01976 0.01095 0.01109 AFIX 137 H9A 2 0.173884 1.107770 0.343461 11.00000 -1.50000 H9B 2 0.251362 1.128820 0.401391 11.00000 -1.50000 H9C 2 0.230156 1.029852 0.377055 11.00000 -1.50000 AFIX 0 C10 1 0.351390 1.090526 0.328469 11.00000 0.05342 0.06416 = 0.06951 -0.00319 -0.00056 -0.01094 AFIX 137 H10A 2 0.361929 1.034520 0.354118 11.00000 -1.50000 H10B 2 0.370666 1.138562 0.362069 11.00000 -1.50000 H10C 2 0.376193 1.091780 0.288117 11.00000 -1.50000 AFIX 0 C66 1 -0.009390 0.917737 -0.029231 11.00000 0.08743 0.07264 = 0.07425 -0.00122 -0.01137 0.01954 AFIX 43 H66 2 -0.015858 0.860664 -0.049702 11.00000 -1.20000 AFIX 0 PART 2 C47B 1 0.218784 0.372645 0.283088 10.50000 0.05860 AFIX 137 H47A 2 0.175985 0.395011 0.300446 10.50000 -1.50000 H47B 2 0.226176 0.310411 0.295341 10.50000 -1.50000 H47C 2 0.208488 0.379874 0.230319 10.50000 -1.50000 AFIX 0 PART 1 C46A 1 0.302281 0.419467 0.328267 10.50000 0.03824 AFIX 13 H46A 2 0.328278 0.424319 0.380898 10.50000 -1.20000 AFIX 0 C47A 1 0.226886 0.379797 0.331025 10.50000 0.10448 AFIX 137 H47D 2 0.206777 0.410363 0.367668 10.50000 -1.50000 H47E 2 0.233703 0.317639 0.343750 10.50000 -1.50000 H47F 2 0.191450 0.385751 0.283439 10.50000 -1.50000 AFIX 0 PART 2 C48B 1 0.322463 0.387104 0.390739 10.50000 0.07668 AFIX 137 H48A 2 0.371712 0.416213 0.404402 10.50000 -1.50000 H48B 2 0.329753 0.323514 0.391067 10.50000 -1.50000 H48C 2 0.292739 0.402720 0.425503 10.50000 -1.50000 AFIX 0 PART 1 C48A 1 0.355189 0.371031 0.300398 10.50000 0.08028 AFIX 137 H48D 2 0.333400 0.357169 0.249219 10.50000 -1.50000 H48E 2 0.367604 0.316582 0.328023 10.50000 -1.50000 H48F 2 0.401157 0.405838 0.304676 10.50000 -1.50000 AFIX 66 PART -1 C60 1 0.524584 1.215958 0.288128 10.50000 0.08715 0.11178 = 0.08250 0.02876 0.02286 0.00457 AFIX 43 H60 2 0.555694 1.174685 0.319007 10.50000 -1.20000 AFIX 65 C59 1 0.479045 1.189149 0.221958 10.50000 0.07354 0.11085 = 0.09286 -0.00653 0.05048 0.00311 AFIX 43 H59 2 0.479030 1.129552 0.207612 10.50000 -1.20000 AFIX 65 C58 1 0.433527 1.249538 0.176776 10.50000 0.07049 0.13284 = 0.07471 -0.00908 0.03172 -0.00169 AFIX 43 H58 2 0.402402 1.231214 0.131552 10.50000 -1.20000 AFIX 65 C63 1 0.433548 1.336737 0.197766 10.50000 0.08828 0.13808 = 0.06746 0.01673 0.04462 0.03685 AFIX 43 H63 2 0.402438 1.378010 0.166886 10.50000 -1.20000 AFIX 65 C62 1 0.479087 1.363548 0.263936 10.50000 0.10801 0.09994 = 0.10133 -0.01280 0.05700 -0.00113 AFIX 43 H62 2 0.479101 1.423146 0.278281 10.50000 -1.20000 AFIX 65 C61 1 0.524605 1.303160 0.309118 10.50000 0.11156 0.14139 = 0.04578 -0.01406 0.02007 -0.02205 AFIX 43 H61 2 0.555729 1.321484 0.354342 10.50000 -1.20000 AFIX 0 PART 0 H2A 2 0.595319 0.943449 0.362051 11.00000 0.04872 H2B 2 0.600404 0.837215 0.366030 11.00000 0.04671 H1A 2 0.473620 0.942051 0.371848 11.00000 0.05335 H1B 2 0.474577 0.836201 0.373314 11.00000 0.06375 PART -1 C53 1 0.019318 1.129773 0.233844 10.50000 0.06238 0.03601 = 0.08657 0.00188 0.01662 0.00459 AFIX 43 H53 2 0.030700 1.071467 0.222658 10.50000 -1.20000 AFIX 0 C54 1 -0.032988 1.145246 0.273610 10.50000 0.04561 0.03945 = 0.07477 0.00565 0.00832 -0.01077 AFIX 43 H54 2 -0.056928 1.097943 0.291642 10.50000 -1.20000 AFIX 0 C55 1 -0.050082 1.230447 0.286857 10.50000 0.06574 0.04469 = 0.07582 -0.00311 0.02761 0.00771 AFIX 43 H55 2 -0.086347 1.242039 0.314081 10.50000 -1.20000 AFIX 0 C56 1 -0.015558 1.298417 0.261347 10.50000 0.09300 0.03141 = 0.07225 0.00112 0.03496 0.01028 AFIX 43 H56 2 -0.028619 1.356877 0.270310 10.50000 -1.20000 AFIX 0 C57 1 0.037492 1.283462 0.223126 10.50000 0.06605 0.04047 = 0.05824 0.00427 0.01551 -0.00617 AFIX 43 H57 2 0.061688 1.331051 0.205761 10.50000 -1.20000 AFIX 0 C52 1 0.055316 1.199569 0.210185 10.50000 0.05371 0.04705 = 0.08274 0.00168 0.02183 0.01270 AFIX 43 H52 2 0.093057 1.188700 0.184509 10.50000 -1.20000 AFIX 0 HKLF 4 REM Ga20240829xa_0ma_a.res in P2/c REM wR2 = 0.1551, GooF = S = 1.113, Restrained GooF = 1.104 for all data REM R1 = 0.0549 for 8774 Fo > 4sig(Fo) and 0.0621 for all 10130 data REM 648 parameters refined using 232 restraints END WGHT 0.0926 1.1484 REM Highest difference peak 0.838, deepest hole -0.485, 1-sigma level 0.046 Q1 1 0.3529 0.3794 0.3651 11.00000 0.05 0.84 Q2 1 0.2441 0.3647 0.2587 11.00000 0.05 0.75 Q3 1 0.2984 0.3948 0.4022 11.00000 0.05 0.61 Q4 1 0.2100 0.3760 0.3016 11.00000 0.05 0.51 Q5 1 0.4436 0.8912 0.2480 11.00000 0.05 0.44 Q6 1 0.2365 0.3840 0.3688 11.00000 0.05 0.44 Q7 1 0.2682 0.4252 0.3412 11.00000 0.05 0.43 Q8 1 0.2968 0.4110 0.2990 11.00000 0.05 0.35 Q9 1 0.5175 0.8861 0.3242 11.00000 0.05 0.30 Q10 1 0.1674 1.0337 0.2211 11.00000 0.05 0.28 Q11 1 0.4710 1.3768 0.2207 11.00000 0.05 0.27 Q12 1 -0.1089 1.0434 0.2970 11.00000 0.05 0.27 Q13 1 0.2603 0.5325 0.3208 11.00000 0.05 0.21 ; _shelx_res_checksum 61076 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, 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_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 Ni1 Ni 0.500000 0.88783(2) 0.250000 0.02822(12) Uani 1 2 d S T P . . P1 P 0.22112(3) 1.02990(3) 0.22212(3) 0.03444(14) Uani 1 1 d . . . . . Mg1 Mg 0.37139(3) 0.87918(4) 0.26135(3) 0.02914(16) Uani 1 1 d . . . . . N2 N 0.28562(8) 0.78866(9) 0.26163(8) 0.0255(3) Uani 1 1 d . . . . . N1 N 0.26463(8) 0.93126(10) 0.24756(9) 0.0304(3) Uani 1 1 d . . . . . C15 C 0.29170(10) 0.63669(12) 0.22270(10) 0.0281(4) Uani 1 1 d . . . . . C14 C 0.28023(9) 0.69763(11) 0.27479(9) 0.0257(3) Uani 1 1 d . . . . . C20 C 0.26390(10) 0.73359(12) 0.40068(10) 0.0298(4) Uani 1 1 d . . . . . H20 H 0.233102 0.782475 0.373467 0.036 Uiso 1 1 calc R U . . . C3 C 0.23287(9) 0.85124(12) 0.24702(9) 0.0269(4) Uani 1 1 d . . . . . C18 C 0.27626(11) 0.57722(12) 0.35691(10) 0.0329(4) Uani 1 1 d . . . . . H18 H 0.269860 0.556931 0.402332 0.040 Uiso 1 1 calc R U . . . C19 C 0.27351(10) 0.66697(11) 0.34329(9) 0.0277(4) Uani 1 1 d . . . . . C21 C 0.21926(11) 0.69887(12) 0.45353(10) 0.0328(4) Uani 1 1 d . . . . . C40 C 0.22868(11) 0.66777(13) 0.08874(10) 0.0338(4) Uani 1 1 d . . . . . C41 C 0.17324(12) 0.60334(14) 0.08254(12) 0.0413(5) Uani 1 1 d . . . . . H41 H 0.178072 0.559833 0.119138 0.050 Uiso 1 1 calc R U . . . C16 C 0.29608(11) 0.54781(12) 0.24006(11) 0.0331(4) Uani 1 1 d . . . . . H16 H 0.304914 0.507311 0.205046 0.040 Uiso 1 1 calc R U . . . C34 C 0.36556(11) 0.62065(12) 0.12709(11) 0.0331(4) Uani 1 1 d . . . . . C4 C 0.14620(10) 0.83748(12) 0.22980(10) 0.0318(4) Uani 1 1 d . . . . . C5 C 0.12161(10) 0.74171(13) 0.23308(11) 0.0362(4) Uani 1 1 d . . . . . H5A H 0.140301 0.707021 0.197657 0.054 Uiso 1 1 calc R U . . . H5B H 0.066378 0.738551 0.221749 0.054 Uiso 1 1 calc R U . . . H5C H 0.142464 0.718434 0.281913 0.054 Uiso 1 1 calc R U . . . C33 C 0.30113(10) 0.66860(12) 0.14933(10) 0.0307(4) Uani 1 1 d . . . . . H33 H 0.316995 0.731311 0.156322 0.037 Uiso 1 1 calc R U . . . C27 C 0.33871(11) 0.77445(13) 0.44060(10) 0.0332(4) Uani 1 1 d . . . . . C22 C 0.14157(12) 0.71064(15) 0.43828(12) 0.0418(5) Uani 1 1 d . . . . . H22 H 0.116687 0.738900 0.394451 0.050 Uiso 1 1 calc R U . . . C17 C 0.28811(11) 0.51600(13) 0.30609(11) 0.0369(4) Uani 1 1 d . . . . . C35 C 0.43922(12) 0.64219(15) 0.16214(12) 0.0415(5) Uani 1 1 d . . . . . H35 H 0.447944 0.686986 0.197916 0.050 Uiso 1 1 calc R U . . . C6 C 0.11387(11) 0.89079(13) 0.28426(12) 0.0384(5) Uani 1 1 d . . . . . H6A H 0.142862 0.878094 0.333754 0.058 Uiso 1 1 calc R U . . . H6B H 0.060897 0.874757 0.279341 0.058 Uiso 1 1 calc R U . . . H6C H 0.117312 0.953429 0.274294 0.058 Uiso 1 1 calc R U . . . C26 C 0.25400(13) 0.65735(13) 0.51840(11) 0.0390(4) Uani 1 1 d . . . . . H26 H 0.307089 0.648541 0.530292 0.047 Uiso 1 1 calc R U . . . C32 C 0.33994(13) 0.86279(15) 0.45953(12) 0.0434(5) Uani 1 1 d . . . . . H32 H 0.295351 0.896846 0.444393 0.052 Uiso 1 1 calc R U . . . C7 C 0.11059(12) 0.86764(15) 0.15175(12) 0.0415(5) Uani 1 1 d . . . . . H7A H 0.117922 0.930872 0.147910 0.062 Uiso 1 1 calc R U . . . H7B H 0.056446 0.854436 0.139544 0.062 Uiso 1 1 calc R U . . . H7C H 0.134694 0.836838 0.118064 0.062 Uiso 1 1 calc R U . . . C36 C 0.50047(13) 0.59970(17) 0.14608(13) 0.0490(5) Uani 1 1 d . . . . . H36 H 0.550487 0.615546 0.170491 0.059 Uiso 1 1 calc R U . . . C23 C 0.09934(14) 0.68188(16) 0.48589(14) 0.0508(6) Uani 1 1 d . . . . . H23 H 0.046212 0.690340 0.474334 0.061 Uiso 1 1 calc R U . . . C45 C 0.21876(14) 0.73132(16) 0.03483(12) 0.0464(5) Uani 1 1 d . . . . . H45 H 0.255456 0.776167 0.037873 0.056 Uiso 1 1 calc R U . . . C2 C 0.56991(12) 0.88984(15) 0.34471(12) 0.0371(4) Uani 1 1 d . . . . . C13 C 0.24837(13) 0.99981(16) 0.08747(13) 0.0487(5) Uani 1 1 d . . . . . H13A H 0.259183 0.939419 0.104231 0.073 Uiso 1 1 calc R U . . . H13B H 0.276995 1.013866 0.051436 0.073 Uiso 1 1 calc R U . . . H13C H 0.194246 1.006050 0.065426 0.073 Uiso 1 1 calc R U . . . C37 C 0.48810(14) 0.53424(17) 0.09433(14) 0.0532(6) Uani 1 1 d . . . . . H37 H 0.529620 0.504425 0.083295 0.064 Uiso 1 1 calc R U . . . C11 C 0.27124(13) 1.06227(14) 0.15184(13) 0.0450(5) Uani 1 1 d . . . . . H11 H 0.326907 1.057534 0.172672 0.054 Uiso 1 1 calc R U . . . C39 C 0.35414(13) 0.55574(16) 0.07484(13) 0.0480(5) Uani 1 1 d . . . . . H39 H 0.304233 0.540485 0.049613 0.058 Uiso 1 1 calc R U . . . C42 C 0.11123(13) 0.60213(16) 0.02363(13) 0.0495(6) Uani 1 1 d . . . . . H42 H 0.074438 0.557247 0.019821 0.059 Uiso 1 1 calc R U . . . C31 C 0.40532(16) 0.90168(19) 0.50015(13) 0.0558(7) Uani 1 1 d . . . . . H31 H 0.405280 0.961868 0.512797 0.067 Uiso 1 1 calc R U . . . C25 C 0.21191(15) 0.62872(14) 0.56583(13) 0.0472(5) Uani 1 1 d . . . . . H25 H 0.236427 0.600340 0.609732 0.057 Uiso 1 1 calc R U . . . C28 C 0.40481(12) 0.72607(16) 0.46193(12) 0.0440(5) Uani 1 1 d . . . . . H28 H 0.405359 0.666168 0.448567 0.053 Uiso 1 1 calc R U . . . C24 C 0.13487(15) 0.64113(15) 0.54978(14) 0.0497(6) Uani 1 1 d . . . . . H24 H 0.106411 0.621694 0.582579 0.060 Uiso 1 1 calc R U . . . C1 C 0.48971(12) 0.88872(16) 0.34943(12) 0.0414(5) Uani 1 1 d . . . . . C46B C 0.2804(4) 0.4167(4) 0.3143(3) 0.0451(15) Uiso 0.5 1 d . . P A 2 H46B H 0.315886 0.395208 0.285399 0.054 Uiso 0.5 1 calc R U P A 2 C44 C 0.15582(15) 0.72999(19) -0.02343(14) 0.0572(6) Uani 1 1 d . . . . . H44 H 0.149683 0.774323 -0.059492 0.069 Uiso 1 1 calc R U . . . C8 C 0.26693(14) 1.10091(14) 0.29925(14) 0.0489(6) Uani 1 1 d . . . . . H8 H 0.258350 1.162665 0.281673 0.059 Uiso 1 1 calc R U . . . C38 C 0.41561(15) 0.51243(17) 0.05894(16) 0.0590(7) Uani 1 1 d . . . . . H38 H 0.407159 0.467480 0.023306 0.071 Uiso 1 1 calc R U . . . C49 C 0.07216(16) 0.53423(18) 0.2414(2) 0.0682(8) Uani 1 1 d . . . . . H49 H 0.122147 0.534163 0.234869 0.082 Uiso 1 1 calc R U . . . C29 C 0.47031(14) 0.7652(2) 0.50290(14) 0.0600(7) Uani 1 1 d . . . . . H29 H 0.515299 0.731775 0.517825 0.072 Uiso 1 1 calc R U . . . C50 C 0.06079(16) 0.53400(17) 0.3090(2) 0.0666(8) Uani 1 1 d . . . . . H50 H 0.102530 0.533465 0.350145 0.080 Uiso 1 1 calc R U . . . C30 C 0.46991(16) 0.8530(2) 0.52195(13) 0.0632(8) Uani 1 1 d . . . . . H30 H 0.514555 0.879429 0.550176 0.076 Uiso 1 1 calc R U . . . C64 C -0.0410(2) 1.0255(3) 0.04759(19) 0.0834(10) Uani 1 1 d . . . . . H64 H -0.069699 1.043303 0.080699 0.100 Uiso 1 1 calc R U . . . C12 C 0.2518(2) 1.15698(18) 0.12758(19) 0.0762(9) Uani 1 1 d . . . . . H12A H 0.196815 1.163677 0.112341 0.114 Uiso 1 1 calc R U . . . H12B H 0.273965 1.171009 0.086829 0.114 Uiso 1 1 calc R U . . . H12C H 0.272109 1.196799 0.168065 0.114 Uiso 1 1 calc R U . . . C51 C -0.01201(18) 0.53456(19) 0.3179(2) 0.0720(8) Uani 1 1 d . . . . . H51 H -0.020446 0.535169 0.365348 0.086 Uiso 1 1 calc R U . . . C43 C 0.10244(14) 0.66544(19) -0.02950(13) 0.0554(6) Uani 1 1 d . . . . . H43 H 0.059895 0.664366 -0.069852 0.066 Uiso 1 1 calc R U . . . C65 C -0.05021(19) 0.9433(3) 0.01845(19) 0.0799(10) Uani 1 1 d . . . . . H65 H -0.085085 0.904002 0.031427 0.096 Uiso 1 1 calc R U . . . C9 C 0.22701(18) 1.0909(2) 0.36080(16) 0.0686(8) Uani 1 1 d . . . . . H9A H 0.173884 1.107770 0.343461 0.103 Uiso 1 1 calc R U . . . H9B H 0.251362 1.128820 0.401391 0.103 Uiso 1 1 calc R U . . . H9C H 0.230156 1.029852 0.377055 0.103 Uiso 1 1 calc R U . . . C10 C 0.35139(16) 1.0905(2) 0.32847(17) 0.0650(7) Uani 1 1 d . . . . . H10A H 0.361929 1.034520 0.354118 0.098 Uiso 1 1 calc R U . . . H10B H 0.370666 1.138562 0.362069 0.098 Uiso 1 1 calc R U . . . H10C H 0.376193 1.091780 0.288117 0.098 Uiso 1 1 calc R U . . . C66 C -0.0094(2) 0.9177(3) -0.0292(2) 0.0834(10) Uani 1 1 d . . . . . H66 H -0.015858 0.860664 -0.049702 0.100 Uiso 1 1 calc R U . . . C47B C 0.2188(3) 0.3726(4) 0.2831(3) 0.0586(13) Uiso 0.5 1 d . . P A 2 H47A H 0.175985 0.395011 0.300446 0.088 Uiso 0.5 1 calc R U P A 2 H47B H 0.226176 0.310411 0.295341 0.088 Uiso 0.5 1 calc R U P A 2 H47C H 0.208488 0.379874 0.230319 0.088 Uiso 0.5 1 calc R U P A 2 C46A C 0.3023(3) 0.4195(3) 0.3283(3) 0.0382(12) Uiso 0.5 1 d . . P A 1 H46A H 0.328278 0.424319 0.380898 0.046 Uiso 0.5 1 calc R U P A 1 C47A C 0.2269(6) 0.3798(6) 0.3310(6) 0.104(3) Uiso 0.5 1 d . . P A 1 H47D H 0.206777 0.410363 0.367668 0.157 Uiso 0.5 1 calc R U P A 1 H47E H 0.233703 0.317639 0.343750 0.157 Uiso 0.5 1 calc R U P A 1 H47F H 0.191450 0.385751 0.283439 0.157 Uiso 0.5 1 calc R U P A 1 C48B C 0.3225(4) 0.3871(4) 0.3907(4) 0.0767(17) Uiso 0.5 1 d . . P A 2 H48A H 0.371712 0.416213 0.404402 0.115 Uiso 0.5 1 calc R U P A 2 H48B H 0.329753 0.323514 0.391067 0.115 Uiso 0.5 1 calc R U P A 2 H48C H 0.292739 0.402720 0.425503 0.115 Uiso 0.5 1 calc R U P A 2 C48A C 0.3552(4) 0.3710(5) 0.3004(4) 0.0803(18) Uiso 0.5 1 d . . P A 1 H48D H 0.333400 0.357169 0.249219 0.120 Uiso 0.5 1 calc R U P A 1 H48E H 0.367604 0.316582 0.328023 0.120 Uiso 0.5 1 calc R U P A 1 H48F H 0.401157 0.405838 0.304676 0.120 Uiso 0.5 1 calc R U P A 1 C60 C 0.5246(5) 1.2160(4) 0.2881(4) 0.093(3) Uani 0.5 1 d DG U P B -1 H60 H 0.555694 1.174685 0.319007 0.112 Uiso 0.5 1 calc R U P B -1 C59 C 0.4790(5) 1.1891(3) 0.2220(4) 0.087(3) Uani 0.5 1 d DG U P B -1 H59 H 0.479030 1.129552 0.207612 0.105 Uiso 0.5 1 calc R U P B -1 C58 C 0.4335(3) 1.2495(4) 0.1768(3) 0.090(2) Uani 0.5 1 d DG U P B -1 H58 H 0.402402 1.231214 0.131552 0.108 Uiso 0.5 1 calc R U P B -1 C63 C 0.4335(3) 1.3367(4) 0.1978(3) 0.094(2) Uani 0.5 1 d DG U P B -1 H63 H 0.402438 1.378010 0.166886 0.112 Uiso 0.5 1 calc R U P B -1 C62 C 0.4791(3) 1.3635(3) 0.2639(3) 0.098(2) Uani 0.5 1 d DG U P B -1 H62 H 0.479101 1.423146 0.278281 0.117 Uiso 0.5 1 calc R U P B -1 C61 C 0.5246(4) 1.3032(4) 0.3091(3) 0.099(2) Uani 0.5 1 d DG U P B -1 H61 H 0.555729 1.321484 0.354342 0.119 Uiso 0.5 1 calc R U P B -1 H2A H 0.5953(15) 0.9434(18) 0.3621(14) 0.049(7) Uiso 1 1 d . . . . . H2B H 0.6004(14) 0.8372(17) 0.3660(13) 0.047(6) Uiso 1 1 d . . . . . H1A H 0.4736(15) 0.9421(18) 0.3718(14) 0.053(7) Uiso 1 1 d . . . . . H1B H 0.4746(16) 0.836(2) 0.3733(16) 0.064(8) Uiso 1 1 d . . . . . C53 C 0.0193(12) 1.1298(7) 0.2338(15) 0.062(3) Uani 0.5 1 d D U P C -1 H53 H 0.030700 1.071467 0.222658 0.074 Uiso 0.5 1 calc R U P C -1 C54 C -0.0330(11) 1.1452(6) 0.2736(12) 0.054(2) Uani 0.5 1 d D U P C -1 H54 H -0.056928 1.097943 0.291642 0.065 Uiso 0.5 1 calc R U P C -1 C55 C -0.0501(7) 1.2304(6) 0.2869(7) 0.060(2) Uani 0.5 1 d D U P C -1 H55 H -0.086347 1.242039 0.314081 0.072 Uiso 0.5 1 calc R U P C -1 C56 C -0.0156(6) 1.2984(5) 0.2613(6) 0.063(3) Uani 0.5 1 d D U P C -1 H56 H -0.028619 1.356877 0.270310 0.076 Uiso 0.5 1 calc R U P C -1 C57 C 0.0375(6) 1.2835(5) 0.2231(6) 0.055(2) Uani 0.5 1 d D U P C -1 H57 H 0.061688 1.331051 0.205761 0.066 Uiso 0.5 1 calc R U P C -1 C52 C 0.0553(8) 1.1996(6) 0.2102(9) 0.060(2) Uani 0.5 1 d D U P C -1 H52 H 0.093057 1.188700 0.184509 0.072 Uiso 0.5 1 calc R U P C -1 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 Ni1 0.02132(19) 0.0309(2) 0.0338(2) 0.000 0.00931(14) 0.000 P1 0.0318(3) 0.0267(2) 0.0454(3) 0.00429(19) 0.0104(2) 0.00618(18) Mg1 0.0217(3) 0.0279(3) 0.0392(3) 0.0012(2) 0.0100(2) -0.0001(2) N2 0.0233(7) 0.0233(7) 0.0303(7) 0.0011(5) 0.0075(6) 0.0006(5) N1 0.0242(7) 0.0264(8) 0.0413(9) 0.0027(6) 0.0091(6) 0.0025(6) C15 0.0255(8) 0.0263(8) 0.0327(9) -0.0021(7) 0.0073(7) -0.0015(7) C14 0.0217(8) 0.0230(8) 0.0321(9) 0.0009(6) 0.0060(6) -0.0007(6) C20 0.0306(9) 0.0291(9) 0.0307(9) 0.0012(7) 0.0091(7) -0.0002(7) C3 0.0235(8) 0.0286(9) 0.0291(9) 0.0009(7) 0.0074(6) 0.0018(7) C18 0.0342(10) 0.0314(9) 0.0348(9) 0.0042(7) 0.0115(7) -0.0007(7) C19 0.0245(8) 0.0275(9) 0.0311(9) 0.0015(7) 0.0068(7) -0.0003(7) C21 0.0375(10) 0.0276(9) 0.0362(10) -0.0020(7) 0.0143(8) -0.0036(7) C40 0.0372(10) 0.0326(9) 0.0328(9) -0.0017(7) 0.0109(8) 0.0030(8) C41 0.0405(11) 0.0386(11) 0.0431(11) 0.0008(8) 0.0068(9) -0.0027(8) C16 0.0351(10) 0.0274(9) 0.0378(10) -0.0041(7) 0.0106(8) -0.0004(7) C34 0.0359(10) 0.0324(9) 0.0336(10) -0.0003(7) 0.0137(8) -0.0008(7) C4 0.0224(8) 0.0333(9) 0.0390(10) 0.0013(8) 0.0063(7) 0.0013(7) C5 0.0242(9) 0.0379(10) 0.0455(11) -0.0013(8) 0.0067(8) -0.0036(7) C33 0.0330(9) 0.0265(9) 0.0339(9) -0.0030(7) 0.0109(7) -0.0019(7) C27 0.0347(10) 0.0391(10) 0.0274(9) 0.0016(7) 0.0107(7) -0.0056(8) C22 0.0390(11) 0.0468(12) 0.0434(11) 0.0003(9) 0.0170(9) -0.0023(9) C17 0.0406(11) 0.0286(9) 0.0422(11) 0.0012(8) 0.0113(8) 0.0005(8) C35 0.0370(11) 0.0488(12) 0.0382(11) -0.0062(9) 0.0083(8) 0.0030(9) C6 0.0259(9) 0.0410(11) 0.0507(12) 0.0011(8) 0.0138(8) 0.0034(8) C26 0.0477(12) 0.0322(10) 0.0403(11) 0.0031(8) 0.0168(9) -0.0002(8) C32 0.0477(12) 0.0443(12) 0.0424(11) -0.0097(9) 0.0188(9) -0.0100(9) C7 0.0283(10) 0.0482(12) 0.0435(11) 0.0060(9) 0.0002(8) 0.0020(8) C36 0.0370(12) 0.0629(15) 0.0477(13) -0.0035(10) 0.0117(10) 0.0055(10) C23 0.0448(12) 0.0537(14) 0.0625(15) -0.0022(11) 0.0296(11) -0.0083(10) C45 0.0511(13) 0.0468(12) 0.0415(11) 0.0090(9) 0.0114(10) -0.0005(10) C2 0.0288(10) 0.0442(12) 0.0378(11) -0.0006(8) 0.0073(8) 0.0018(8) C13 0.0470(12) 0.0541(13) 0.0470(12) 0.0127(10) 0.0149(10) 0.0075(10) C37 0.0481(13) 0.0568(14) 0.0636(15) -0.0047(11) 0.0307(11) 0.0081(11) C11 0.0462(12) 0.0325(11) 0.0604(14) 0.0130(9) 0.0205(10) 0.0065(9) C39 0.0440(12) 0.0507(13) 0.0560(13) -0.0197(10) 0.0247(10) -0.0119(10) C42 0.0389(12) 0.0560(14) 0.0497(13) -0.0016(10) 0.0034(10) -0.0036(10) C31 0.0622(16) 0.0653(16) 0.0435(12) -0.0186(11) 0.0200(11) -0.0268(13) C25 0.0666(16) 0.0357(11) 0.0456(12) 0.0058(9) 0.0259(11) -0.0025(10) C28 0.0370(11) 0.0534(13) 0.0400(11) 0.0116(9) 0.0064(9) -0.0028(9) C24 0.0655(15) 0.0387(11) 0.0562(14) -0.0009(10) 0.0366(12) -0.0096(10) C1 0.0308(10) 0.0566(14) 0.0380(11) 0.0035(9) 0.0110(8) 0.0002(9) C44 0.0568(15) 0.0668(16) 0.0456(13) 0.0185(11) 0.0074(11) 0.0060(12) C8 0.0543(14) 0.0300(10) 0.0579(14) -0.0020(9) 0.0051(11) 0.0054(9) C38 0.0570(15) 0.0553(14) 0.0750(17) -0.0304(13) 0.0363(13) -0.0117(12) C49 0.0459(14) 0.0470(14) 0.115(3) 0.0047(15) 0.0263(16) -0.0041(11) C29 0.0390(12) 0.091(2) 0.0456(13) 0.0202(13) 0.0011(10) -0.0061(12) C50 0.0515(15) 0.0422(13) 0.103(2) -0.0142(14) 0.0124(15) -0.0036(11) C30 0.0577(16) 0.094(2) 0.0355(12) -0.0051(12) 0.0061(11) -0.0356(15) C64 0.072(2) 0.107(3) 0.0663(19) 0.0091(19) 0.0078(16) 0.033(2) C12 0.115(3) 0.0400(14) 0.086(2) 0.0266(14) 0.0495(19) 0.0178(15) C51 0.0691(19) 0.0546(16) 0.099(2) -0.0170(15) 0.0330(17) 0.0028(14) C43 0.0450(13) 0.0731(17) 0.0429(12) 0.0032(11) 0.0005(10) 0.0060(12) C65 0.0591(18) 0.093(3) 0.076(2) 0.0238(19) -0.0065(15) 0.0066(16) C9 0.0691(18) 0.0756(19) 0.0589(16) -0.0198(14) 0.0110(13) 0.0111(15) C10 0.0534(15) 0.0642(16) 0.0695(17) -0.0032(14) -0.0006(13) -0.0109(13) C66 0.087(2) 0.073(2) 0.074(2) -0.0012(17) -0.0114(18) 0.0195(19) C60 0.087(7) 0.112(5) 0.083(5) 0.029(5) 0.023(4) 0.005(6) C59 0.074(6) 0.111(5) 0.093(5) -0.007(4) 0.050(4) 0.003(4) C58 0.070(4) 0.133(6) 0.075(4) -0.009(4) 0.032(3) -0.002(4) C63 0.088(5) 0.138(6) 0.067(4) 0.017(4) 0.045(3) 0.037(5) C62 0.108(6) 0.100(5) 0.101(5) -0.013(4) 0.057(4) -0.001(4) C61 0.112(6) 0.141(6) 0.046(3) -0.014(4) 0.020(4) -0.022(5) C53 0.062(10) 0.036(3) 0.087(7) 0.002(4) 0.017(5) 0.005(4) C54 0.046(6) 0.039(5) 0.075(6) 0.006(5) 0.008(4) -0.011(5) C55 0.066(6) 0.045(5) 0.076(5) -0.003(6) 0.028(4) 0.008(6) C56 0.093(11) 0.031(3) 0.072(9) 0.001(3) 0.035(4) 0.010(4) C57 0.066(6) 0.040(4) 0.058(6) 0.004(4) 0.016(4) -0.006(4) C52 0.054(4) 0.047(5) 0.083(5) 0.002(5) 0.022(3) 0.013(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 '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' Mg Mg 0.1421 0.1346 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -1.3357 3.2904 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2543 0.3332 '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 _geom_angle_publ_flag Mg1 Ni1 Mg1 173.73(3) 2_655 . ? C2 Ni1 Mg1 69.33(6) 2_655 . ? C2 Ni1 Mg1 69.33(6) . 2_655 ? C2 Ni1 Mg1 110.77(6) . . ? C2 Ni1 Mg1 110.77(6) 2_655 2_655 ? C2 Ni1 C2 178.18(13) . 2_655 ? C2 Ni1 C1 45.12(9) 2_655 2_655 ? C2 Ni1 C1 45.12(9) . . ? C2 Ni1 C1 134.86(9) . 2_655 ? C2 Ni1 C1 134.86(9) 2_655 . ? C1 Ni1 Mg1 114.35(6) 2_655 . ? C1 Ni1 Mg1 65.69(6) 2_655 2_655 ? C1 Ni1 Mg1 114.35(6) . 2_655 ? C1 Ni1 Mg1 65.70(6) . . ? C1 Ni1 C1 179.20(15) 2_655 . ? N1 P1 C11 99.25(9) . . ? N1 P1 C8 101.64(9) . . ? C8 P1 C11 101.87(12) . . ? Ni1 Mg1 C3 167.14(5) . . ? Ni1 Mg1 C2 46.36(5) . 2_655 ? N2 Mg1 Ni1 141.48(5) . . ? N2 Mg1 C3 32.13(6) . . ? N2 Mg1 C2 120.77(7) . 2_655 ? N2 Mg1 C1 126.03(7) . . ? N1 Mg1 Ni1 151.38(5) . . ? N1 Mg1 N2 64.51(6) . . ? N1 Mg1 C3 32.49(6) . . ? N1 Mg1 C2 116.61(7) . 2_655 ? N1 Mg1 C1 136.90(8) . . ? C2 Mg1 C3 122.61(7) 2_655 . ? C1 Mg1 Ni1 47.65(5) . . ? C1 Mg1 C3 143.10(7) . . ? C1 Mg1 C2 93.93(7) . 2_655 ? C14 N2 Mg1 137.05(11) . . ? C3 N2 Mg1 91.66(11) . . ? C3 N2 C14 131.23(14) . . ? P1 N1 Mg1 137.12(9) . . ? C3 N1 P1 128.52(13) . . ? C3 N1 Mg1 92.45(11) . . ? C14 C15 C33 119.92(15) . . ? C16 C15 C14 119.10(16) . . ? C16 C15 C33 120.96(16) . . ? C15 C14 N2 119.62(15) . . ? C15 C14 C19 119.13(16) . . ? C19 C14 N2 120.71(15) . . ? C19 C20 H20 106.0 . . ? C19 C20 C21 114.00(15) . . ? C21 C20 H20 106.0 . . ? C27 C20 H20 106.0 . . ? C27 C20 C19 112.47(15) . . ? C27 C20 C21 111.72(15) . . ? N2 C3 Mg1 56.21(9) . . ? N2 C3 N1 111.01(15) . . ? N2 C3 C4 126.42(16) . . ? N1 C3 Mg1 55.06(9) . . ? N1 C3 C4 122.56(15) . . ? C4 C3 Mg1 173.94(13) . . ? C19 C18 H18 118.8 . . ? C19 C18 C17 122.32(17) . . ? C17 C18 H18 118.8 . . ? C14 C19 C20 118.98(15) . . ? C18 C19 C14 119.25(16) . . ? C18 C19 C20 121.77(16) . . ? C22 C21 C20 119.79(17) . . ? C22 C21 C26 117.79(18) . . ? C26 C21 C20 122.39(17) . . ? C41 C40 C33 123.16(18) . . ? C45 C40 C41 117.9(2) . . ? C45 C40 C33 118.90(18) . . ? C40 C41 H41 119.6 . . ? C42 C41 C40 120.8(2) . . ? C42 C41 H41 119.6 . . ? C15 C16 H16 118.6 . . ? C17 C16 C15 122.88(17) . . ? C17 C16 H16 118.6 . . ? C35 C34 C33 118.35(17) . . ? C39 C34 C33 123.31(18) . . ? C39 C34 C35 118.33(19) . . ? C5 C4 C3 114.45(15) . . ? C5 C4 C6 108.23(16) . . ? C5 C4 C7 105.35(16) . . ? C6 C4 C3 108.89(15) . . ? C7 C4 C3 109.54(15) . . ? C7 C4 C6 110.31(16) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C15 C33 C40 114.63(15) . . ? C15 C33 C34 111.34(15) . . ? C15 C33 H33 106.1 . . ? C40 C33 C34 111.80(15) . . ? C40 C33 H33 106.1 . . ? C34 C33 H33 106.1 . . ? C32 C27 C20 118.70(18) . . ? C28 C27 C20 122.50(19) . . ? C28 C27 C32 118.7(2) . . ? C21 C22 H22 119.3 . . ? C21 C22 C23 121.4(2) . . ? C23 C22 H22 119.3 . . ? C18 C17 C46B 123.9(3) . . ? C18 C17 C46A 119.7(2) . . ? C16 C17 C18 117.27(17) . . ? C16 C17 C46B 118.1(3) . . ? C16 C17 C46A 122.5(2) . . ? C34 C35 H35 119.3 . . ? C34 C35 C36 121.5(2) . . ? C36 C35 H35 119.3 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C21 C26 H26 119.6 . . ? C25 C26 C21 120.8(2) . . ? C25 C26 H26 119.6 . . ? C27 C32 H32 119.5 . . ? C31 C32 C27 121.0(2) . . ? C31 C32 H32 119.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C35 C36 H36 120.2 . . ? C37 C36 C35 119.5(2) . . ? C37 C36 H36 120.2 . . ? C22 C23 H23 120.1 . . ? C24 C23 C22 119.8(2) . . ? C24 C23 H23 120.1 . . ? C40 C45 H45 119.6 . . ? C44 C45 C40 120.8(2) . . ? C44 C45 H45 119.6 . . ? Ni1 C2 Mg1 64.31(6) . 2_655 ? Ni1 C2 H2A 119.2(15) . . ? Ni1 C2 H2B 122.5(14) . . ? Mg1 C2 H2A 93.8(16) 2_655 . ? Mg1 C2 H2B 88.2(14) 2_655 . ? C1 C2 Ni1 67.61(12) . . ? C1 C2 Mg1 131.76(15) . 2_655 ? C1 C2 H2A 113.0(16) . . ? C1 C2 H2B 115.1(15) . . ? H2A C2 H2B 112(2) . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? C36 C37 H37 120.1 . . ? C38 C37 C36 119.7(2) . . ? C38 C37 H37 120.1 . . ? P1 C11 H11 109.1 . . ? C13 C11 P1 108.78(15) . . ? C13 C11 H11 109.1 . . ? C13 C11 C12 110.5(2) . . ? C12 C11 P1 110.37(17) . . ? C12 C11 H11 109.1 . . ? C34 C39 H39 119.8 . . ? C34 C39 C38 120.3(2) . . ? C38 C39 H39 119.8 . . ? C41 C42 H42 119.7 . . ? C43 C42 C41 120.6(2) . . ? C43 C42 H42 119.7 . . ? C32 C31 H31 120.1 . . ? C30 C31 C32 119.8(3) . . ? C30 C31 H31 120.1 . . ? C26 C25 H25 119.7 . . ? C24 C25 C26 120.6(2) . . ? C24 C25 H25 119.7 . . ? C27 C28 H28 119.9 . . ? C27 C28 C29 120.2(2) . . ? C29 C28 H28 119.9 . . ? C23 C24 C25 119.6(2) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? Ni1 C1 Mg1 66.65(7) . . ? Ni1 C1 H1A 122.0(15) . . ? Ni1 C1 H1B 122.8(17) . . ? Mg1 C1 H1A 92.2(15) . . ? Mg1 C1 H1B 88.1(17) . . ? C2 C1 Ni1 67.27(12) . . ? C2 C1 Mg1 133.84(15) . . ? C2 C1 H1A 114.4(16) . . ? C2 C1 H1B 115.0(17) . . ? H1A C1 H1B 109(2) . . ? C17 C46B H46B 100.4 . . ? C17 C46B C48B 110.5(5) . . ? C47B C46B C17 123.1(5) . . ? C47B C46B H46B 100.4 . . ? C47B C46B C48B 116.8(5) . . ? C48B C46B H46B 100.4 . . ? C45 C44 H44 119.6 . . ? C43 C44 C45 120.8(2) . . ? C43 C44 H44 119.6 . . ? P1 C8 H8 106.5 . . ? C9 C8 P1 109.83(19) . . ? C9 C8 H8 106.5 . . ? C10 C8 P1 116.95(18) . . ? C10 C8 H8 106.5 . . ? C10 C8 C9 109.9(2) . . ? C37 C38 C39 120.6(2) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C50 C49 H49 119.8 . . ? C50 C49 C51 120.3(3) . 2 ? C51 C49 H49 119.8 2 . ? C28 C29 H29 120.0 . . ? C30 C29 C28 120.1(3) . . ? C30 C29 H29 120.0 . . ? C49 C50 H50 120.3 . . ? C49 C50 C51 119.4(3) . . ? C51 C50 H50 120.3 . . ? C31 C30 C29 120.2(2) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C65 C64 H64 119.9 . . ? C65 C64 C66 120.2(4) . 3_575 ? C66 C64 H64 119.9 3_575 . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C49 C51 C50 120.3(3) 2 . ? C49 C51 H51 119.9 2 . ? C50 C51 H51 119.9 . . ? C42 C43 H43 120.4 . . ? C44 C43 C42 119.2(2) . . ? C44 C43 H43 120.4 . . ? C64 C65 H65 120.0 . . ? C66 C65 C64 120.0(4) . . ? C66 C65 H65 120.0 . . ? 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 . . ? C64 C66 H66 120.1 3_575 . ? C65 C66 C64 119.8(4) . 3_575 ? C65 C66 H66 120.1 . . ? C46B C47B H47A 109.5 . . ? C46B C47B H47B 109.5 . . ? C46B C47B H47C 109.5 . . ? H47A C47B H47B 109.5 . . ? H47A C47B H47C 109.5 . . ? H47B C47B H47C 109.5 . . ? C17 C46A H46A 102.1 . . ? C47A C46A C17 107.4(5) . . ? C47A C46A H46A 102.1 . . ? C48A C46A C17 118.9(5) . . ? C48A C46A H46A 102.1 . . ? C48A C46A C47A 120.7(6) . . ? C46A C47A H47D 109.5 . . ? C46A C47A H47E 109.5 . . ? C46A C47A H47F 109.5 . . ? H47D C47A H47E 109.5 . . ? H47D C47A H47F 109.5 . . ? H47E C47A H47F 109.5 . . ? C46B C48B H48A 109.5 . . ? C46B C48B H48B 109.5 . . ? C46B C48B H48C 109.5 . . ? H48A C48B H48B 109.5 . . ? H48A C48B H48C 109.5 . . ? H48B C48B H48C 109.5 . . ? C46A C48A H48D 109.5 . . ? C46A C48A H48E 109.5 . . ? C46A C48A H48F 109.5 . . ? H48D C48A H48E 109.5 . . ? H48D C48A H48F 109.5 . . ? H48E C48A H48F 109.5 . . ? C59 C60 H60 120.0 . . ? C59 C60 C61 120.0 . . ? C61 C60 H60 120.0 . . ? C60 C59 H59 120.0 . . ? C60 C59 C58 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C58 H58 120.0 . . ? C63 C58 C59 120.0 . . ? C63 C58 H58 120.0 . . ? C58 C63 H63 120.0 . . ? C62 C63 C58 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C62 H62 120.0 . . ? C63 C62 C61 120.0 . . ? C61 C62 H62 120.0 . . ? C60 C61 H61 120.0 . . ? C62 C61 C60 120.0 . . ? C62 C61 H61 120.0 . . ? C54 C53 H53 120.2 . . ? C54 C53 C52 119.6(12) . . ? C52 C53 H53 120.2 . . ? C53 C54 H54 120.6 . . ? C53 C54 C55 118.8(11) . . ? C55 C54 H54 120.6 . . ? C54 C55 H55 119.6 . . ? C56 C55 C54 120.7(7) . . ? C56 C55 H55 119.6 . . ? C55 C56 H56 119.6 . . ? C55 C56 C57 120.7(8) . . ? C57 C56 H56 119.6 . . ? C56 C57 H57 120.4 . . ? C52 C57 C56 119.1(9) . . ? C52 C57 H57 120.4 . . ? C53 C52 H52 119.5 . . ? C57 C52 C53 121.0(8) . . ? C57 C52 H52 119.5 . . ? 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 Ni1 Mg1 2.4126(6) . ? Ni1 Mg1 2.4126(6) 2_655 ? Ni1 C2 1.937(2) . ? Ni1 C2 1.937(2) 2_655 ? Ni1 C1 1.942(2) . ? Ni1 C1 1.942(2) 2_655 ? P1 N1 1.7169(15) . ? P1 C11 1.858(2) . ? P1 C8 1.851(2) . ? Mg1 N2 2.0898(15) . ? Mg1 N1 2.0623(16) . ? Mg1 C3 2.5136(18) . ? Mg1 C2 2.505(2) 2_655 ? Mg1 C1 2.395(2) . ? N2 C14 1.420(2) . ? N2 C3 1.337(2) . ? N1 C3 1.351(2) . ? C15 C14 1.410(2) . ? C15 C16 1.394(3) . ? C15 C33 1.525(3) . ? C14 C19 1.416(2) . ? C20 H20 1.0000 . ? C20 C19 1.532(2) . ? C20 C21 1.532(2) . ? C20 C27 1.526(3) . ? C3 C4 1.551(2) . ? C18 H18 0.9500 . ? C18 C19 1.393(3) . ? C18 C17 1.398(3) . ? C21 C22 1.389(3) . ? C21 C26 1.394(3) . ? C40 C41 1.396(3) . ? C40 C33 1.529(3) . ? C40 C45 1.390(3) . ? C41 H41 0.9500 . ? C41 C42 1.386(3) . ? C16 H16 0.9500 . ? C16 C17 1.385(3) . ? C34 C33 1.529(3) . ? C34 C35 1.388(3) . ? C34 C39 1.382(3) . ? C4 C5 1.536(3) . ? C4 C6 1.541(3) . ? C4 C7 1.538(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C33 H33 1.0000 . ? C27 C32 1.395(3) . ? C27 C28 1.389(3) . ? C22 H22 0.9500 . ? C22 C23 1.393(3) . ? C17 C46B 1.535(6) . ? C17 C46A 1.538(5) . ? C35 H35 0.9500 . ? C35 C36 1.389(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C26 H26 0.9500 . ? C26 C25 1.388(3) . ? C32 H32 0.9500 . ? C32 C31 1.388(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C36 H36 0.9500 . ? C36 C37 1.382(4) . ? C23 H23 0.9500 . ? C23 C24 1.378(4) . ? C45 H45 0.9500 . ? C45 C44 1.389(3) . ? C2 C1 1.488(3) . ? C2 H2A 0.96(3) . ? C2 H2B 1.01(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13 C11 1.527(3) . ? C37 H37 0.9500 . ? C37 C38 1.372(4) . ? C11 H11 1.0000 . ? C11 C12 1.533(3) . ? C39 H39 0.9500 . ? C39 C38 1.397(3) . ? C42 H42 0.9500 . ? C42 C43 1.378(4) . ? C31 H31 0.9500 . ? C31 C30 1.370(4) . ? C25 H25 0.9500 . ? C25 C24 1.378(4) . ? C28 H28 0.9500 . ? C28 C29 1.394(3) . ? C24 H24 0.9500 . ? C1 H1A 1.00(3) . ? C1 H1B 0.99(3) . ? C46B H46B 1.0000 . ? C46B C47B 1.322(9) . ? C46B C48B 1.536(9) . ? C44 H44 0.9500 . ? C44 C43 1.371(4) . ? C8 H8 1.0000 . ? C8 C9 1.527(4) . ? C8 C10 1.515(4) . ? C38 H38 0.9500 . ? C49 H49 0.9500 . ? C49 C50 1.350(5) . ? C49 C51 1.369(5) 2 ? C29 H29 0.9500 . ? C29 C30 1.390(5) . ? C50 H50 0.9500 . ? C50 C51 1.380(4) . ? C30 H30 0.9500 . ? C64 H64 0.9500 . ? C64 C65 1.365(5) . ? C64 C66 1.370(6) 3_575 ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C51 H51 0.9500 . ? C43 H43 0.9500 . ? C65 H65 0.9500 . ? C65 C66 1.362(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C66 H66 0.9500 . ? C47B H47A 0.9800 . ? C47B H47B 0.9800 . ? C47B H47C 0.9800 . ? C46A H46A 1.0000 . ? C46A C47A 1.516(11) . ? C46A C48A 1.417(9) . ? C47A H47D 0.9800 . ? C47A H47E 0.9800 . ? C47A H47F 0.9800 . ? C48B H48A 0.9800 . ? C48B H48B 0.9800 . ? C48B H48C 0.9800 . ? C48A H48D 0.9800 . ? C48A H48E 0.9800 . ? C48A H48F 0.9800 . ? C60 H60 0.9500 . ? C60 C59 1.3900 . ? C60 C61 1.3900 . ? C59 H59 0.9500 . ? C59 C58 1.3900 . ? C58 H58 0.9500 . ? C58 C63 1.3900 . ? C63 H63 0.9500 . ? C63 C62 1.3900 . ? C62 H62 0.9500 . ? C62 C61 1.3900 . ? C61 H61 0.9500 . ? C53 H53 0.9500 . ? C53 C54 1.374(8) . ? C53 C52 1.383(9) . ? C54 H54 0.9500 . ? C54 C55 1.375(8) . ? C55 H55 0.9500 . ? C55 C56 1.363(8) . ? C56 H56 0.9500 . ? C56 C57 1.363(8) . ? C57 H57 0.9500 . ? C57 C52 1.359(7) . ? C52 H52 0.9500 . ? 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 Ni1 C2 C1 Mg1 3.49(18) . . . . ? P1 N1 C3 Mg1 166.28(18) . . . . ? P1 N1 C3 N2 171.84(13) . . . . ? P1 N1 C3 C4 -7.0(3) . . . . ? Mg1 N2 C14 C15 -73.8(2) . . . . ? Mg1 N2 C14 C19 97.8(2) . . . . ? Mg1 N2 C3 N1 -5.48(15) . . . . ? Mg1 N2 C3 C4 173.32(16) . . . . ? Mg1 N1 C3 N2 5.55(15) . . . . ? Mg1 N1 C3 C4 -173.30(15) . . . . ? Mg1 C2 C1 Ni1 -4.88(17) 2_655 . . . ? Mg1 C2 C1 Mg1 -1.4(3) 2_655 . . . ? N2 C14 C19 C20 6.3(2) . . . . ? N2 C14 C19 C18 -173.35(15) . . . . ? N2 C3 C4 C5 2.2(3) . . . . ? N2 C3 C4 C6 123.44(19) . . . . ? N2 C3 C4 C7 -115.9(2) . . . . ? N1 P1 C11 C13 67.58(16) . . . . ? N1 P1 C11 C12 -171.0(2) . . . . ? N1 P1 C8 C9 -83.94(18) . . . . ? N1 P1 C8 C10 42.2(2) . . . . ? N1 C3 C4 C5 -179.15(17) . . . . ? N1 C3 C4 C6 -57.9(2) . . . . ? N1 C3 C4 C7 62.8(2) . . . . ? C15 C14 C19 C20 177.83(15) . . . . ? C15 C14 C19 C18 -1.8(2) . . . . ? C15 C16 C17 C18 -0.9(3) . . . . ? C15 C16 C17 C46B 169.7(3) . . . . ? C15 C16 C17 C46A -172.6(3) . . . . ? C14 N2 C3 Mg1 177.5(2) . . . . ? C14 N2 C3 N1 172.04(17) . . . . ? C14 N2 C3 C4 -9.2(3) . . . . ? C14 C15 C16 C17 1.4(3) . . . . ? C14 C15 C33 C40 -95.6(2) . . . . ? C14 C15 C33 C34 136.23(17) . . . . ? C20 C21 C22 C23 -178.4(2) . . . . ? C20 C21 C26 C25 178.35(19) . . . . ? C20 C27 C32 C31 175.59(19) . . . . ? C20 C27 C28 C29 -175.28(19) . . . . ? C3 N2 C14 C15 109.9(2) . . . . ? C3 N2 C14 C19 -78.6(2) . . . . ? C18 C17 C46B C47B 97.3(6) . . . . ? C18 C17 C46B C48B -47.5(6) . . . . ? C18 C17 C46A C47A 76.2(6) . . . . ? C18 C17 C46A C48A -142.2(5) . . . . ? C19 C20 C21 C22 -91.6(2) . . . . ? C19 C20 C21 C26 90.2(2) . . . . ? C19 C20 C27 C32 142.70(18) . . . . ? C19 C20 C27 C28 -40.5(2) . . . . ? C19 C18 C17 C16 -1.0(3) . . . . ? C19 C18 C17 C46B -171.0(3) . . . . ? C19 C18 C17 C46A 171.0(3) . . . . ? C21 C20 C19 C14 150.76(16) . . . . ? C21 C20 C19 C18 -29.6(2) . . . . ? C21 C20 C27 C32 -87.6(2) . . . . ? C21 C20 C27 C28 89.1(2) . . . . ? C21 C22 C23 C24 0.3(4) . . . . ? C21 C26 C25 C24 -0.2(3) . . . . ? C40 C41 C42 C43 -1.1(4) . . . . ? C40 C45 C44 C43 -0.7(4) . . . . ? C41 C40 C33 C15 -35.9(3) . . . . ? C41 C40 C33 C34 92.0(2) . . . . ? C41 C40 C45 C44 -0.4(3) . . . . ? C41 C42 C43 C44 -0.1(4) . . . . ? C16 C15 C14 N2 171.70(16) . . . . ? C16 C15 C14 C19 0.0(2) . . . . ? C16 C15 C33 C40 86.0(2) . . . . ? C16 C15 C33 C34 -42.2(2) . . . . ? C16 C17 C46B C47B -72.6(6) . . . . ? C16 C17 C46B C48B 142.5(4) . . . . ? C16 C17 C46A C47A -112.4(5) . . . . ? C16 C17 C46A C48A 29.3(7) . . . . ? C34 C35 C36 C37 -0.3(4) . . . . ? C34 C39 C38 C37 -0.7(4) . . . . ? C33 C15 C14 N2 -6.7(2) . . . . ? C33 C15 C14 C19 -178.40(15) . . . . ? C33 C15 C16 C17 179.77(18) . . . . ? C33 C40 C41 C42 -175.3(2) . . . . ? C33 C40 C45 C44 176.3(2) . . . . ? C33 C34 C35 C36 178.3(2) . . . . ? C33 C34 C39 C38 -177.7(2) . . . . ? C27 C20 C19 C14 -80.7(2) . . . . ? C27 C20 C19 C18 98.9(2) . . . . ? C27 C20 C21 C22 139.48(19) . . . . ? C27 C20 C21 C26 -38.7(2) . . . . ? C27 C32 C31 C30 0.2(4) . . . . ? C27 C28 C29 C30 -0.6(3) . . . . ? C22 C21 C26 C25 0.1(3) . . . . ? C22 C23 C24 C25 -0.4(4) . . . . ? C17 C18 C19 C14 2.3(3) . . . . ? C17 C18 C19 C20 -177.31(18) . . . . ? C35 C34 C33 C15 -74.1(2) . . . . ? C35 C34 C33 C40 156.26(18) . . . . ? C35 C34 C39 C38 0.9(4) . . . . ? C35 C36 C37 C38 0.6(4) . . . . ? C26 C21 C22 C23 -0.2(3) . . . . ? C26 C25 C24 C23 0.4(4) . . . . ? C32 C27 C28 C29 1.5(3) . . . . ? C32 C31 C30 C29 0.6(4) . . . . ? C36 C37 C38 C39 -0.1(4) . . . . ? C45 C40 C41 C42 1.3(3) . . . . ? C45 C40 C33 C15 147.50(18) . . . . ? C45 C40 C33 C34 -84.6(2) . . . . ? C45 C44 C43 C42 1.0(4) . . . . ? C11 P1 N1 Mg1 36.70(16) . . . . ? C11 P1 N1 C3 -122.92(17) . . . . ? C11 P1 C8 C9 173.88(18) . . . . ? C11 P1 C8 C10 -60.0(2) . . . . ? C39 C34 C33 C15 104.6(2) . . . . ? C39 C34 C33 C40 -25.1(3) . . . . ? C39 C34 C35 C36 -0.5(3) . . . . ? C28 C27 C32 C31 -1.3(3) . . . . ? C28 C29 C30 C31 -0.4(4) . . . . ? C8 P1 N1 Mg1 -67.55(16) . . . . ? C8 P1 N1 C3 132.82(18) . . . . ? C8 P1 C11 C13 171.65(15) . . . . ? C8 P1 C11 C12 -67.0(2) . . . . ? C49 C50 C51 C49 0.8(4) . . . 2 ? C64 C65 C66 C64 0.2(5) . . . 3_575 ? C51 C49 C50 C51 -0.3(4) 2 . . . ? C66 C64 C65 C66 -0.2(5) 3_575 . . . ? C60 C59 C58 C63 0.0 . . . . ? C59 C60 C61 C62 0.0 . . . . ? C59 C58 C63 C62 0.0 . . . . ? C58 C63 C62 C61 0.0 . . . . ? C63 C62 C61 C60 0.0 . . . . ? C61 C60 C59 C58 0.0 . . . . ? C53 C54 C55 C56 -0.3(14) . . . . ? C54 C53 C52 C57 -3(2) . . . . ? C54 C55 C56 C57 -1.0(17) . . . . ? C55 C56 C57 C52 0.5(12) . . . . ? C56 C57 C52 C53 1(2) . . . . ? C52 C53 C54 C55 2.1(10) . . . . ?