#------------------------------------------------------------------------------ #$Date: 2025-01-16 02:03:11 +0200 (Thu, 16 Jan 2025) $ #$Revision: 297345 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/37/1573700.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_1573700 _journal_paper_doi 10.1039/D4DT03495C _chemical_formula_moiety 'C50 H88 Mg2 N4 Ni P2' _chemical_formula_sum 'C50 H88 Mg2 N4 Ni P2' _chemical_formula_weight 914.51 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2024-08-03 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2024-12-06 deposited with the CCDC. 2025-01-15 downloaded from the CCDC. ; _cell_angle_alpha 107.9280(10) _cell_angle_beta 93.3990(10) _cell_angle_gamma 105.3290(10) _cell_formula_units_Z 1 _cell_length_a 9.0128(4) _cell_length_b 10.6971(4) _cell_length_c 15.9172(6) _cell_measurement_reflns_used 9648 _cell_measurement_temperature 120 _cell_measurement_theta_max 27.20 _cell_measurement_theta_min 2.37 _cell_volume 1391.49(10) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 120 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _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_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_unetI/netI 0.0563 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 30580 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.502 _diffrn_reflns_theta_min 2.826 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.462 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5308 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1181 before and 0.0832 after correction. The Ratio of minimum to maximum transmission is 0.7119. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'dull light colourless' _exptl_crystal_colour_lustre dull _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.091 _exptl_crystal_description block _exptl_crystal_F_000 498 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.335 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 295 _refine_ls_number_reflns 6378 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0433 _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^)+(0.0440P)^2^+0.4568P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1064 _refine_ls_wR_factor_ref 0.1228 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4899 _reflns_number_total 6378 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4dt03495c2.cif _cod_data_source_block mo_20200605c_0ma _cod_database_code 1573700 _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 0.913 _shelx_estimated_absorpt_t_min 0.897 _olex2_refinement_description ; 1.a Ternary CH refined with riding coordinates: C21(H21), C17(H17), C8(H8), C24(H24) 1.b Aromatic/amide H refined with riding coordinates: C14(H14), C12(H12), C13(H13) 1.c Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C20(H20A,H20B,H20C), C7(H7A,H7B,H7C), C22(H22A,H22B,H22C), C6(H6A,H6B,H6C), C19(H19A,H19B,H19C), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C) ; _shelx_res_file ; TITL mo_20200605c_0ma_a.res in P-1 mo_20200605c_0ma.res created by SHELXL-2018/3 at 15:33:04 on 03-Aug-2024 REM Old TITL REM SHELXT solution in P-1: R1 0.167, Rweak 0.006, Alpha 0.040 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C50 N4 P4 Ni CELL 0.71073 9.0128 10.6971 15.9172 107.928 93.399 105.329 ZERR 1 0.0004 0.0004 0.0006 0.001 0.001 0.001 LATT 1 SFAC C H Mg N Ni P UNIT 50 88 2 4 1 2 L.S. 4 0 0 PLAN 13 SIZE 0.2 0.22 0.24 TEMP -153.15 CONF list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 0 -1 1 OMIT -1 1 0 OMIT 0 0 2 OMIT -1 0 1 OMIT 0 1 0 REM REM REM WGHT 0.044000 0.456800 FVAR 0.99234 NI1 5 0.500000 0.500000 1.000000 10.50000 0.04495 0.03644 = 0.02910 0.00682 -0.00460 0.01813 P1 6 0.359020 0.719356 0.746124 11.00000 0.04809 0.03384 = 0.04814 0.02153 0.00628 0.01276 MG1 3 0.393944 0.488850 0.857400 11.00000 0.03993 0.03086 = 0.02997 0.00873 -0.00527 0.00950 N1 4 0.241829 0.345267 0.749339 11.00000 0.03458 0.02584 = 0.02998 0.00677 -0.00141 0.00923 N2 4 0.319453 0.567090 0.766537 11.00000 0.03839 0.03062 = 0.03533 0.01307 -0.00160 0.00771 C16 1 0.179450 0.199784 0.715522 11.00000 0.03276 0.02755 = 0.03398 0.00714 -0.00434 0.00985 C15 1 0.072752 0.134284 0.760380 11.00000 0.03904 0.03095 = 0.04607 0.01297 0.00020 0.01011 C3 1 0.220542 0.441962 0.718029 11.00000 0.03469 0.03303 = 0.02719 0.00938 0.00232 0.01433 C11 1 0.239433 0.122498 0.644683 11.00000 0.04288 0.03741 = 0.03592 0.00578 -0.00380 0.01697 C5 1 -0.006737 0.517016 0.679524 11.00000 0.04643 0.05019 = 0.05303 0.01199 -0.00850 0.02313 AFIX 137 H5A 2 -0.046764 0.499293 0.731985 11.00000 -1.50000 H5B 2 -0.094111 0.500527 0.633805 11.00000 -1.50000 H5C 2 0.058463 0.612836 0.696799 11.00000 -1.50000 AFIX 0 C1 1 0.660862 0.410300 0.994590 11.00000 0.05496 0.04889 = 0.03733 0.01030 -0.00031 0.02617 C21 1 0.358475 0.838353 0.858585 11.00000 0.05094 0.03446 = 0.05326 0.01403 -0.00128 0.00909 AFIX 13 H21 2 0.428337 0.823014 0.903155 11.00000 -1.20000 AFIX 0 C20 1 0.195284 0.811376 0.883222 11.00000 0.06526 0.04441 = 0.05385 0.01367 0.01370 0.01671 AFIX 137 H20A 2 0.126138 0.828304 0.840880 11.00000 -1.50000 H20B 2 0.198204 0.872917 0.943781 11.00000 -1.50000 H20C 2 0.156378 0.715527 0.880877 11.00000 -1.50000 AFIX 0 C17 1 0.015403 0.215067 0.840849 11.00000 0.04839 0.03810 = 0.05860 0.01723 0.01776 0.01178 AFIX 13 H17 2 0.043052 0.312752 0.842432 11.00000 -1.20000 AFIX 0 C14 1 0.021922 -0.009348 0.730658 11.00000 0.05076 0.03378 = 0.06523 0.01773 0.00140 0.00665 AFIX 43 H14 2 -0.052879 -0.055092 0.759366 11.00000 -1.20000 AFIX 0 C4 1 0.091206 0.420009 0.641706 11.00000 0.04660 0.04191 = 0.03436 0.00906 -0.00850 0.01904 C8 1 0.361463 0.191817 0.598755 11.00000 0.05849 0.05431 = 0.04218 0.00854 0.01339 0.02760 AFIX 13 H8 2 0.354317 0.286987 0.609190 11.00000 -1.20000 AFIX 0 C12 1 0.185388 -0.021088 0.618877 11.00000 0.06633 0.03771 = 0.04392 -0.00067 -0.00458 0.02453 AFIX 43 H12 2 0.224308 -0.074963 0.571084 11.00000 -1.20000 AFIX 0 C2 1 0.599925 0.409437 0.905909 11.00000 0.05913 0.05111 = 0.03898 0.01342 0.00081 0.02727 C24 1 0.572396 0.752968 0.743119 11.00000 0.05480 0.04839 = 0.10096 0.04418 0.02639 0.01579 AFIX 13 H24 2 0.610680 0.845479 0.736313 11.00000 -1.20000 AFIX 0 C7 1 -0.021854 0.274349 0.605590 11.00000 0.05318 0.04815 = 0.05616 0.00303 -0.02711 0.01808 AFIX 137 H7A 2 0.033380 0.209783 0.575524 11.00000 -1.50000 H7B 2 -0.106863 0.271266 0.562928 11.00000 -1.50000 H7C 2 -0.064568 0.248604 0.655163 11.00000 -1.50000 AFIX 0 C13 1 0.077787 -0.085729 0.660865 11.00000 0.07146 0.02615 = 0.06546 0.00461 -0.00886 0.01209 AFIX 43 H13 2 0.041832 -0.183388 0.641692 11.00000 -1.20000 AFIX 0 C22 1 0.420780 0.988364 0.861620 11.00000 0.06404 0.03330 = 0.08765 0.01431 0.00411 0.00524 AFIX 137 H22A 2 0.529202 1.007183 0.851013 11.00000 -1.50000 H22B 2 0.415263 1.050465 0.920440 11.00000 -1.50000 H22C 2 0.357577 1.003035 0.815342 11.00000 -1.50000 AFIX 0 C6 1 0.164750 0.453955 0.563553 11.00000 0.08256 0.07806 = 0.03380 0.02019 -0.00231 0.03946 AFIX 137 H6A 2 0.220907 0.552393 0.582588 11.00000 -1.50000 H6B 2 0.082745 0.430629 0.513182 11.00000 -1.50000 H6C 2 0.237439 0.400464 0.545109 11.00000 -1.50000 AFIX 0 C19 1 0.097608 0.213994 0.926856 11.00000 0.08685 0.07487 = 0.05335 0.02038 0.02198 0.02454 AFIX 137 H19A 2 0.067851 0.120115 0.928917 11.00000 -1.50000 H19B 2 0.067353 0.274861 0.978274 11.00000 -1.50000 H19C 2 0.210545 0.246313 0.928748 11.00000 -1.50000 AFIX 0 C9 1 0.524270 0.205011 0.641266 11.00000 0.05254 0.11216 = 0.06043 0.01401 0.01121 0.02644 AFIX 137 H9A 2 0.540826 0.258748 0.705033 11.00000 -1.50000 H9B 2 0.602628 0.251569 0.611965 11.00000 -1.50000 H9C 2 0.533549 0.113161 0.634005 11.00000 -1.50000 AFIX 0 C18 1 -0.161252 0.164082 0.836050 11.00000 0.05392 0.07629 = 0.11408 0.02404 0.03106 0.02512 AFIX 137 H18A 2 -0.212380 0.162026 0.779352 11.00000 -1.50000 H18B 2 -0.193497 0.226308 0.885838 11.00000 -1.50000 H18C 2 -0.191074 0.071242 0.839886 11.00000 -1.50000 AFIX 0 C10 1 0.337774 0.119439 0.498252 11.00000 0.10013 0.09183 = 0.04252 0.01461 0.01713 0.04523 AFIX 137 H10A 2 0.346831 0.026388 0.485883 11.00000 -1.50000 H10B 2 0.417119 0.171395 0.472138 11.00000 -1.50000 H10C 2 0.234111 0.113902 0.471985 11.00000 -1.50000 AFIX 0 C23 1 0.674032 0.758106 0.825188 11.00000 0.04350 0.09623 = 0.15126 0.08188 0.00855 0.01172 AFIX 137 H23A 2 0.665019 0.831744 0.877602 11.00000 -1.50000 H23B 2 0.782805 0.776110 0.815265 11.00000 -1.50000 H23C 2 0.639441 0.669758 0.835322 11.00000 -1.50000 AFIX 0 C25 1 0.596142 0.649274 0.658662 11.00000 0.08857 0.07555 = 0.14460 0.04905 0.06818 0.03318 AFIX 137 H25A 2 0.567902 0.557527 0.664263 11.00000 -1.50000 H25B 2 0.705586 0.675769 0.650480 11.00000 -1.50000 H25C 2 0.530201 0.647880 0.606962 11.00000 -1.50000 AFIX 0 H1A 2 0.641480 0.318564 1.000948 11.00000 0.04740 H2A 2 0.543015 0.319554 0.862662 11.00000 0.05977 H2B 2 0.673337 0.464234 0.880581 11.00000 0.06329 H1B 2 0.768745 0.462635 1.016497 11.00000 0.05875 HKLF 4 REM mo_20200605c_0ma_a.res in P-1 REM wR2 = 0.1228, GooF = S = 1.061, Restrained GooF = 1.061 for all data REM R1 = 0.0433 for 4899 Fo > 4sig(Fo) and 0.0648 for all 6378 data REM 295 parameters refined using 0 restraints END WGHT 0.0440 0.4568 REM Highest difference peak 0.335, deepest hole -0.325, 1-sigma level 0.048 Q1 1 0.5679 0.5939 1.0787 11.00000 0.05 0.34 Q2 1 0.4911 0.5746 0.9404 11.00000 0.05 0.31 Q3 1 0.5622 0.6362 1.0571 11.00000 0.05 0.31 Q4 1 0.5297 0.4626 0.9154 11.00000 0.05 0.30 Q5 1 0.3980 0.5626 0.7939 11.00000 0.05 0.30 Q6 1 0.2673 0.3812 0.7987 11.00000 0.05 0.29 Q7 1 0.5824 0.4214 0.9623 11.00000 0.05 0.28 Q8 1 0.2597 0.7150 0.6054 11.00000 0.05 0.27 Q9 1 0.1614 0.4261 0.6774 11.00000 0.05 0.26 Q10 1 0.6267 0.4726 1.0241 11.00000 0.05 0.26 Q11 1 0.0542 0.4724 0.6624 11.00000 0.05 0.23 Q12 1 0.6190 0.5774 0.9596 11.00000 0.05 0.22 Q13 1 0.3151 0.6168 0.7754 11.00000 0.05 0.21 ; _shelx_res_checksum 43408 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.500000 1.000000 0.03707(12) Uani 1 2 d S . P . . P1 P 0.35902(7) 0.71936(5) 0.74612(4) 0.04143(15) Uani 1 1 d . . . . . Mg1 Mg 0.39394(8) 0.48885(6) 0.85740(4) 0.03462(16) Uani 1 1 d . . . . . N1 N 0.24183(18) 0.34527(15) 0.74934(10) 0.0310(3) Uani 1 1 d . . . . . N2 N 0.31945(19) 0.56709(16) 0.76654(10) 0.0351(4) Uani 1 1 d . . . . . C16 C 0.1794(2) 0.19978(18) 0.71552(12) 0.0324(4) Uani 1 1 d . . . . . C15 C 0.0728(2) 0.1343(2) 0.76038(14) 0.0390(4) Uani 1 1 d . . . . . C3 C 0.2205(2) 0.44196(19) 0.71803(12) 0.0311(4) Uani 1 1 d . . . . . C11 C 0.2394(2) 0.1225(2) 0.64468(13) 0.0397(5) Uani 1 1 d . . . . . C5 C -0.0067(3) 0.5170(2) 0.67952(16) 0.0501(6) Uani 1 1 d . . . . . H5A H -0.046764 0.499293 0.731985 0.075 Uiso 1 1 calc R U . . . H5B H -0.094111 0.500527 0.633805 0.075 Uiso 1 1 calc R U . . . H5C H 0.058463 0.612836 0.696799 0.075 Uiso 1 1 calc R U . . . C1 C 0.6609(3) 0.4103(3) 0.99459(14) 0.0462(5) Uani 1 1 d . . . . . C21 C 0.3585(3) 0.8384(2) 0.85858(15) 0.0475(5) Uani 1 1 d . . . . . H21 H 0.428337 0.823014 0.903155 0.057 Uiso 1 1 calc R U . . . C20 C 0.1953(3) 0.8114(2) 0.88322(16) 0.0549(6) Uani 1 1 d . . . . . H20A H 0.126138 0.828304 0.840880 0.082 Uiso 1 1 calc R U . . . H20B H 0.198204 0.872917 0.943781 0.082 Uiso 1 1 calc R U . . . H20C H 0.156378 0.715527 0.880877 0.082 Uiso 1 1 calc R U . . . C17 C 0.0154(3) 0.2151(2) 0.84085(16) 0.0479(5) Uani 1 1 d . . . . . H17 H 0.043052 0.312752 0.842432 0.058 Uiso 1 1 calc R U . . . C14 C 0.0219(3) -0.0093(2) 0.73066(17) 0.0512(6) Uani 1 1 d . . . . . H14 H -0.052879 -0.055092 0.759366 0.061 Uiso 1 1 calc R U . . . C4 C 0.0912(2) 0.4200(2) 0.64171(13) 0.0413(5) Uani 1 1 d . . . . . C8 C 0.3615(3) 0.1918(3) 0.59875(15) 0.0511(6) Uani 1 1 d . . . . . H8 H 0.354317 0.286987 0.609190 0.061 Uiso 1 1 calc R U . . . C12 C 0.1854(3) -0.0211(2) 0.61888(15) 0.0515(6) Uani 1 1 d . . . . . H12 H 0.224308 -0.074963 0.571084 0.062 Uiso 1 1 calc R U . . . C2 C 0.5999(3) 0.4094(3) 0.90591(15) 0.0482(5) Uani 1 1 d . . . . . C24 C 0.5724(3) 0.7530(3) 0.7431(2) 0.0627(7) Uani 1 1 d . . . . . H24 H 0.610680 0.845479 0.736313 0.075 Uiso 1 1 calc R U . . . C7 C -0.0219(3) 0.2743(2) 0.60559(16) 0.0569(6) Uani 1 1 d . . . . . H7A H 0.033380 0.209783 0.575524 0.085 Uiso 1 1 calc R U . . . H7B H -0.106863 0.271266 0.562928 0.085 Uiso 1 1 calc R U . . . H7C H -0.064568 0.248604 0.655163 0.085 Uiso 1 1 calc R U . . . C13 C 0.0778(3) -0.0857(2) 0.66087(18) 0.0583(7) Uani 1 1 d . . . . . H13 H 0.041832 -0.183388 0.641692 0.070 Uiso 1 1 calc R U . . . C22 C 0.4208(3) 0.9884(2) 0.8616(2) 0.0653(7) Uani 1 1 d . . . . . H22A H 0.529202 1.007183 0.851013 0.098 Uiso 1 1 calc R U . . . H22B H 0.415263 1.050465 0.920440 0.098 Uiso 1 1 calc R U . . . H22C H 0.357577 1.003035 0.815342 0.098 Uiso 1 1 calc R U . . . C6 C 0.1647(3) 0.4540(3) 0.56355(15) 0.0618(7) Uani 1 1 d . . . . . H6A H 0.220907 0.552393 0.582588 0.093 Uiso 1 1 calc R U . . . H6B H 0.082745 0.430629 0.513182 0.093 Uiso 1 1 calc R U . . . H6C H 0.237439 0.400464 0.545109 0.093 Uiso 1 1 calc R U . . . C19 C 0.0976(4) 0.2140(3) 0.92686(17) 0.0714(8) Uani 1 1 d . . . . . H19A H 0.067851 0.120115 0.928917 0.107 Uiso 1 1 calc R U . . . H19B H 0.067353 0.274861 0.978274 0.107 Uiso 1 1 calc R U . . . H19C H 0.210545 0.246313 0.928748 0.107 Uiso 1 1 calc R U . . . C9 C 0.5243(3) 0.2050(4) 0.64127(19) 0.0781(9) Uani 1 1 d . . . . . H9A H 0.540826 0.258748 0.705033 0.117 Uiso 1 1 calc R U . . . H9B H 0.602628 0.251569 0.611965 0.117 Uiso 1 1 calc R U . . . H9C H 0.533549 0.113161 0.634005 0.117 Uiso 1 1 calc R U . . . C18 C -0.1613(3) 0.1641(3) 0.8361(2) 0.0814(9) Uani 1 1 d . . . . . H18A H -0.212380 0.162026 0.779352 0.122 Uiso 1 1 calc R U . . . H18B H -0.193497 0.226308 0.885838 0.122 Uiso 1 1 calc R U . . . H18C H -0.191074 0.071242 0.839886 0.122 Uiso 1 1 calc R U . . . C10 C 0.3378(4) 0.1194(3) 0.49825(17) 0.0764(9) Uani 1 1 d . . . . . H10A H 0.346831 0.026388 0.485883 0.115 Uiso 1 1 calc R U . . . H10B H 0.417119 0.171395 0.472138 0.115 Uiso 1 1 calc R U . . . H10C H 0.234111 0.113902 0.471985 0.115 Uiso 1 1 calc R U . . . C23 C 0.6740(3) 0.7581(4) 0.8252(3) 0.0894(11) Uani 1 1 d . . . . . H23A H 0.665019 0.831744 0.877602 0.134 Uiso 1 1 calc R U . . . H23B H 0.782805 0.776110 0.815265 0.134 Uiso 1 1 calc R U . . . H23C H 0.639441 0.669758 0.835322 0.134 Uiso 1 1 calc R U . . . C25 C 0.5961(4) 0.6493(3) 0.6587(3) 0.0960(12) Uani 1 1 d . . . . . H25A H 0.567902 0.557527 0.664263 0.144 Uiso 1 1 calc R U . . . H25B H 0.705586 0.675769 0.650480 0.144 Uiso 1 1 calc R U . . . H25C H 0.530201 0.647880 0.606962 0.144 Uiso 1 1 calc R U . . . H1A H 0.641(3) 0.319(2) 1.0009(15) 0.047(6) Uiso 1 1 d . . . . . H2A H 0.543(3) 0.320(3) 0.8627(17) 0.060(7) Uiso 1 1 d . . . . . H2B H 0.673(3) 0.464(3) 0.8806(17) 0.063(8) Uiso 1 1 d . . . . . H1B H 0.769(3) 0.463(3) 1.0165(17) 0.059(7) Uiso 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 Ni1 0.0450(2) 0.0364(2) 0.02910(19) 0.00682(15) -0.00460(15) 0.01813(17) P1 0.0481(3) 0.0338(3) 0.0481(3) 0.0215(2) 0.0063(2) 0.0128(2) Mg1 0.0399(4) 0.0309(3) 0.0300(3) 0.0087(3) -0.0053(3) 0.0095(3) N1 0.0346(8) 0.0258(7) 0.0300(8) 0.0068(6) -0.0014(6) 0.0092(6) N2 0.0384(9) 0.0306(8) 0.0353(8) 0.0131(7) -0.0016(7) 0.0077(7) C16 0.0328(10) 0.0275(9) 0.0340(9) 0.0071(7) -0.0043(8) 0.0099(8) C15 0.0390(11) 0.0310(10) 0.0461(11) 0.0130(9) 0.0002(9) 0.0101(8) C3 0.0347(10) 0.0330(9) 0.0272(9) 0.0094(7) 0.0023(7) 0.0143(8) C11 0.0429(11) 0.0374(11) 0.0359(10) 0.0058(8) -0.0038(9) 0.0170(9) C5 0.0464(13) 0.0502(13) 0.0530(13) 0.0120(11) -0.0085(10) 0.0231(11) C1 0.0550(14) 0.0489(13) 0.0373(11) 0.0103(10) -0.0003(10) 0.0262(12) C21 0.0509(13) 0.0345(11) 0.0533(13) 0.0140(10) -0.0013(10) 0.0091(10) C20 0.0653(16) 0.0444(13) 0.0539(14) 0.0137(11) 0.0137(12) 0.0167(12) C17 0.0484(13) 0.0381(11) 0.0586(14) 0.0172(10) 0.0178(11) 0.0118(10) C14 0.0508(13) 0.0338(11) 0.0652(15) 0.0177(11) 0.0014(11) 0.0066(10) C4 0.0466(12) 0.0419(11) 0.0344(10) 0.0091(9) -0.0085(9) 0.0190(9) C8 0.0585(14) 0.0543(14) 0.0422(12) 0.0085(10) 0.0134(11) 0.0276(12) C12 0.0663(15) 0.0377(12) 0.0439(12) -0.0007(10) -0.0046(11) 0.0245(11) C2 0.0591(15) 0.0511(14) 0.0390(11) 0.0134(11) 0.0008(11) 0.0273(12) C24 0.0548(15) 0.0484(14) 0.101(2) 0.0442(15) 0.0264(15) 0.0158(12) C7 0.0532(14) 0.0481(13) 0.0562(14) 0.0030(11) -0.0271(11) 0.0181(11) C13 0.0715(17) 0.0261(11) 0.0655(15) 0.0046(10) -0.0089(13) 0.0121(11) C22 0.0640(16) 0.0333(12) 0.088(2) 0.0143(13) 0.0041(14) 0.0052(11) C6 0.0826(19) 0.0781(18) 0.0338(11) 0.0202(12) -0.0023(12) 0.0395(15) C19 0.087(2) 0.0749(19) 0.0533(15) 0.0204(14) 0.0220(14) 0.0245(16) C9 0.0525(16) 0.112(3) 0.0604(17) 0.0140(17) 0.0112(13) 0.0264(17) C18 0.0539(16) 0.076(2) 0.114(3) 0.0240(19) 0.0311(17) 0.0251(15) C10 0.100(2) 0.092(2) 0.0425(14) 0.0146(14) 0.0171(14) 0.0452(19) C23 0.0435(15) 0.096(2) 0.151(3) 0.082(2) 0.0086(18) 0.0117(15) C25 0.089(2) 0.076(2) 0.145(3) 0.049(2) 0.068(2) 0.0332(18) 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' Mg Mg 0.0486 0.0363 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 180.00(3) . 2_667 ? C1 Ni1 Mg1 67.39(7) 2_667 . ? C1 Ni1 Mg1 112.61(7) 2_667 2_667 ? C1 Ni1 Mg1 67.39(7) . 2_667 ? C1 Ni1 Mg1 112.61(7) . . ? C1 Ni1 C1 180.0 2_667 . ? C2 Ni1 Mg1 112.45(7) 2_667 . ? C2 Ni1 Mg1 112.45(7) . 2_667 ? C2 Ni1 Mg1 67.55(7) . . ? C2 Ni1 Mg1 67.55(7) 2_667 2_667 ? C2 Ni1 C1 45.10(9) . . ? C2 Ni1 C1 45.10(9) 2_667 2_667 ? C2 Ni1 C1 134.90(9) 2_667 . ? C2 Ni1 C1 134.90(9) . 2_667 ? C2 Ni1 C2 180.00(16) . 2_667 ? N2 P1 C21 100.27(9) . . ? N2 P1 C24 99.44(9) . . ? C21 P1 C24 101.14(12) . . ? Ni1 Mg1 C3 164.98(5) . . ? Ni1 Mg1 C1 47.68(5) . 2_667 ? Ni1 Mg1 C2 47.58(6) . . ? N1 Mg1 Ni1 137.21(5) . . ? N1 Mg1 C3 32.52(6) . . ? N1 Mg1 C1 127.73(8) . 2_667 ? N1 Mg1 C2 113.34(8) . . ? N2 Mg1 Ni1 154.90(5) . . ? N2 Mg1 N1 65.56(6) . . ? N2 Mg1 C3 33.23(6) . . ? N2 Mg1 C1 113.30(8) . 2_667 ? N2 Mg1 C2 144.66(8) . . ? C1 Mg1 C3 124.35(7) 2_667 . ? C1 Mg1 C2 95.24(8) 2_667 . ? C2 Mg1 C3 138.06(7) . . ? C16 N1 Mg1 136.82(12) . . ? C3 N1 Mg1 91.70(11) . . ? C3 N1 C16 131.47(15) . . ? P1 N2 Mg1 138.94(9) . . ? C3 N2 P1 129.93(13) . . ? C3 N2 Mg1 91.05(11) . . ? C15 C16 N1 119.11(17) . . ? C15 C16 C11 120.65(18) . . ? C11 C16 N1 119.76(17) . . ? C16 C15 C17 121.67(17) . . ? C14 C15 C16 118.5(2) . . ? C14 C15 C17 119.8(2) . . ? N1 C3 Mg1 55.78(9) . . ? N1 C3 N2 111.09(15) . . ? N1 C3 C4 125.49(17) . . ? N2 C3 Mg1 55.73(9) . . ? N2 C3 C4 123.22(16) . . ? C4 C3 Mg1 169.86(13) . . ? C16 C11 C8 121.34(18) . . ? C12 C11 C16 118.0(2) . . ? C12 C11 C8 120.6(2) . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? Ni1 C1 Mg1 64.92(7) . 2_667 ? Ni1 C1 H1A 121.8(13) . . ? Ni1 C1 H1B 121.3(15) . . ? Mg1 C1 H1A 92.6(13) 2_667 . ? Mg1 C1 H1B 87.7(15) 2_667 . ? C2 C1 Ni1 67.37(13) . . ? C2 C1 Mg1 132.21(16) . 2_667 ? C2 C1 H1A 115.0(13) . . ? C2 C1 H1B 115.3(15) . . ? H1A C1 H1B 110(2) . . ? P1 C21 H21 108.6 . . ? C20 C21 P1 110.76(16) . . ? C20 C21 H21 108.6 . . ? C20 C21 C22 110.0(2) . . ? C22 C21 P1 110.07(17) . . ? C22 C21 H21 108.6 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 C17 H17 107.5 . . ? C15 C17 C19 110.75(19) . . ? C15 C17 C18 112.8(2) . . ? C19 C17 H17 107.5 . . ? C19 C17 C18 110.5(2) . . ? C18 C17 H17 107.5 . . ? C15 C14 H14 119.3 . . ? C13 C14 C15 121.3(2) . . ? C13 C14 H14 119.3 . . ? C5 C4 C3 107.74(16) . . ? C7 C4 C3 114.21(16) . . ? C7 C4 C5 106.47(19) . . ? C7 C4 C6 108.3(2) . . ? C6 C4 C3 109.96(18) . . ? C6 C4 C5 110.02(18) . . ? C11 C8 H8 107.6 . . ? C11 C8 C9 110.0(2) . . ? C11 C8 C10 113.4(2) . . ? C9 C8 H8 107.6 . . ? C10 C8 H8 107.6 . . ? C10 C8 C9 110.6(2) . . ? C11 C12 H12 119.2 . . ? C13 C12 C11 121.5(2) . . ? C13 C12 H12 119.2 . . ? Ni1 C2 Mg1 64.87(7) . . ? Ni1 C2 H2A 120.0(15) . . ? Ni1 C2 H2B 118.9(16) . . ? Mg1 C2 H2A 86.0(15) . . ? Mg1 C2 H2B 91.2(16) . . ? C1 C2 Ni1 67.53(13) . . ? C1 C2 Mg1 132.32(16) . . ? C1 C2 H2A 116.1(15) . . ? C1 C2 H2B 114.3(16) . . ? H2A C2 H2B 113(2) . . ? P1 C24 H24 106.4 . . ? C23 C24 P1 117.4(2) . . ? C23 C24 H24 106.4 . . ? C25 C24 P1 108.6(2) . . ? C25 C24 H24 106.4 . . ? C25 C24 C23 110.9(3) . . ? 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 . . ? C14 C13 H13 120.0 . . ? C12 C13 C14 119.9(2) . . ? C12 C13 H13 120.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? 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 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? 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 2.3655(6) 2_667 ? Ni1 Mg1 2.3655(6) . ? Ni1 C1 1.931(2) . ? Ni1 C1 1.931(2) 2_667 ? Ni1 C2 1.929(2) . ? Ni1 C2 1.929(2) 2_667 ? P1 N2 1.7083(16) . ? P1 C21 1.851(2) . ? P1 C24 1.867(3) . ? Mg1 N1 2.0440(16) . ? Mg1 N2 2.0421(16) . ? Mg1 C3 2.4708(18) . ? Mg1 C1 2.411(2) 2_667 ? Mg1 C2 2.415(2) . ? N1 C16 1.419(2) . ? N1 C3 1.329(2) . ? N2 C3 1.354(2) . ? C16 C15 1.400(3) . ? C16 C11 1.408(3) . ? C15 C17 1.513(3) . ? C15 C14 1.396(3) . ? C3 C4 1.550(3) . ? C11 C8 1.514(3) . ? C11 C12 1.399(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5 C4 1.543(3) . ? C1 C2 1.480(3) . ? C1 H1A 0.99(2) . ? C1 H1B 0.97(3) . ? C21 H21 1.0000 . ? C21 C20 1.521(3) . ? C21 C22 1.538(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C17 H17 1.0000 . ? C17 C19 1.522(4) . ? C17 C18 1.529(3) . ? C14 H14 0.9500 . ? C14 C13 1.371(3) . ? C4 C7 1.528(3) . ? C4 C6 1.539(3) . ? C8 H8 1.0000 . ? C8 C9 1.531(4) . ? C8 C10 1.521(3) . ? C12 H12 0.9500 . ? C12 C13 1.368(4) . ? C2 H2A 0.98(3) . ? C2 H2B 0.96(3) . ? C24 H24 1.0000 . ? C24 C23 1.528(4) . ? C24 C25 1.525(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C13 H13 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 C1 C2 Mg1 -3.5(2) . . . . ? P1 N2 C3 Mg1 177.14(19) . . . . ? P1 N2 C3 N1 169.95(14) . . . . ? P1 N2 C3 C4 -15.0(3) . . . . ? Mg1 N1 C16 C15 70.7(2) . . . . ? Mg1 N1 C16 C11 -101.4(2) . . . . ? Mg1 N1 C3 N2 7.18(16) . . . . ? Mg1 N1 C3 C4 -167.74(17) . . . . ? Mg1 N2 C3 N1 -7.19(16) . . . . ? Mg1 N2 C3 C4 167.87(16) . . . . ? Mg1 C3 C4 C5 27.5(8) . . . . ? Mg1 C3 C4 C7 -90.6(8) . . . . ? Mg1 C3 C4 C6 147.4(7) . . . . ? Mg1 C1 C2 Ni1 -3.5(2) 2_667 . . . ? Mg1 C1 C2 Mg1 -7.0(4) 2_667 . . . ? N1 C16 C15 C17 3.5(3) . . . . ? N1 C16 C15 C14 -174.90(18) . . . . ? N1 C16 C11 C8 -4.6(3) . . . . ? N1 C16 C11 C12 174.02(18) . . . . ? N1 C3 C4 C5 121.1(2) . . . . ? N1 C3 C4 C7 3.1(3) . . . . ? N1 C3 C4 C6 -119.0(2) . . . . ? N2 P1 C21 C20 -68.20(17) . . . . ? N2 P1 C21 C22 169.89(17) . . . . ? N2 P1 C24 C23 -56.4(2) . . . . ? N2 P1 C24 C25 70.3(2) . . . . ? N2 C3 C4 C5 -53.2(3) . . . . ? N2 C3 C4 C7 -171.25(19) . . . . ? N2 C3 C4 C6 66.7(2) . . . . ? C16 N1 C3 Mg1 -179.3(2) . . . . ? C16 N1 C3 N2 -172.08(18) . . . . ? C16 N1 C3 C4 13.0(3) . . . . ? C16 C15 C17 C19 -102.1(2) . . . . ? C16 C15 C17 C18 133.5(2) . . . . ? C16 C15 C14 C13 1.9(3) . . . . ? C16 C11 C8 C9 94.3(2) . . . . ? C16 C11 C8 C10 -141.4(2) . . . . ? C16 C11 C12 C13 -0.2(3) . . . . ? C15 C16 C11 C8 -176.63(19) . . . . ? C15 C16 C11 C12 2.0(3) . . . . ? C15 C14 C13 C12 -0.1(4) . . . . ? C3 N1 C16 C15 -110.4(2) . . . . ? C3 N1 C16 C11 77.5(3) . . . . ? C11 C16 C15 C17 175.55(18) . . . . ? C11 C16 C15 C14 -2.9(3) . . . . ? C11 C12 C13 C14 -0.8(4) . . . . ? C21 P1 N2 Mg1 -48.30(17) . . . . ? C21 P1 N2 C3 136.06(18) . . . . ? C21 P1 C24 C23 46.1(2) . . . . ? C21 P1 C24 C25 172.82(18) . . . . ? C17 C15 C14 C13 -176.6(2) . . . . ? C14 C15 C17 C19 76.3(3) . . . . ? C14 C15 C17 C18 -48.1(3) . . . . ? C8 C11 C12 C13 178.5(2) . . . . ? C12 C11 C8 C9 -84.4(3) . . . . ? C12 C11 C8 C10 40.0(3) . . . . ? C24 P1 N2 Mg1 54.95(18) . . . . ? C24 P1 N2 C3 -120.69(19) . . . . ? C24 P1 C21 C20 -170.06(16) . . . . ? C24 P1 C21 C22 68.03(19) . . . . ?