#------------------------------------------------------------------------------ #$Date: 2024-07-19 01:10:40 +0300 (Fri, 19 Jul 2024) $ #$Revision: 293460 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572147.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_1572147 loop_ _publ_author_name 'Kreimer, Lisa N.' 'Hadlington, Terrance' _publ_section_title ; Macrocyclic bis-diphosphenes demonstrating bimetallic exo- and endo-cyclic binding modes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03516J _journal_year 2024 _chemical_formula_moiety 'C66 H88 N8 Ni2 O2 P4' _chemical_formula_sum 'C66 H88 N8 Ni2 O2 P4' _chemical_formula_weight 1266.74 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-05-23 deposited with the CCDC. 2024-07-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.10(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.890(2) _cell_length_b 21.590(4) _cell_length_c 15.520(3) _cell_measurement_reflns_used 2000 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 32.50 _cell_measurement_theta_min 1.92 _cell_volume 3309.1(11) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 150(2) _diffrn_detector Pilatus300K _diffrn_detector_area_resol_mean 5.81 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'STOE StadiVari' _diffrn_measurement_method '\w scans' _diffrn_radiation_collimation '0.6 mm diameter' _diffrn_radiation_monochromator 'Graded multilayer mirror' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_unetI/netI 0.1324 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 31963 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_min 2.299 _diffrn_source 'Genix 3D HF Mo' _diffrn_source_current 1.000 _diffrn_source_power 0.050 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'STOE X-AREA 1.76' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.271 _exptl_crystal_description block _exptl_crystal_F_000 1344 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.386 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.077 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 384 _refine_ls_number_reflns 6499 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.923 _refine_ls_R_factor_all 0.1306 _refine_ls_R_factor_gt 0.0518 _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^)+(0.0408P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.1020 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3564 _reflns_number_total 6499 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03516j2.cif _cod_data_source_block 2a _cod_original_cell_volume 3309.1(12) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1572147 _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_res_file ; TITL P21n in P2(1)/n C:\XRay\TH126_~1\P21n.res created by SHELXL-2018/3 at 11:40:27 on 16-May-2024 CELL 0.71073 9.8900 21.5900 15.5200 90.000 93.100 90.000 ZERR 2.0000 0.0020 0.0043 0.0031 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O P NI UNIT 132 176 16 4 8 4 MERG 2 OMIT -2 52 FMAP 2 GRID PLAN 20 TEMP -123 L.S. 20 ACTA WGHT 0.040800 FVAR 0.11021 NI1 6 0.194813 0.142850 0.601230 11.00000 0.02154 0.01891 = 0.01898 -0.00163 0.00020 -0.00177 P2 5 -0.027769 0.137684 0.563156 11.00000 0.02359 0.02353 = 0.02311 0.00092 0.00145 -0.00299 P1 5 0.102249 0.066632 0.517470 11.00000 0.02943 0.02072 = 0.01933 -0.00184 0.00191 -0.00422 N2 3 0.485023 0.139739 0.570933 11.00000 0.02324 0.03643 = 0.03164 0.00017 0.00615 0.00121 O1 4 -0.064839 0.002892 0.646689 11.00000 0.04302 0.02155 = 0.02458 -0.00492 0.01074 -0.00726 N3 3 0.189932 0.274902 0.659741 11.00000 0.03263 0.01709 = 0.02159 -0.00398 -0.00076 -0.00257 C25 1 0.217243 0.213827 0.676146 11.00000 0.02118 0.01894 = 0.02347 0.00193 0.00323 -0.00156 N4 3 0.279663 0.215183 0.757641 11.00000 0.03046 0.02662 = 0.02061 -0.00388 -0.00256 0.00070 N1 3 0.426109 0.057240 0.635685 11.00000 0.02931 0.03251 = 0.03068 0.00476 0.00084 0.00979 C28 1 0.119321 0.297934 0.580499 11.00000 0.03592 0.01816 = 0.02174 -0.00141 -0.00737 -0.00548 AFIX 13 H28 2 0.100545 0.261810 0.541334 11.00000 -1.20000 AFIX 0 C16 1 0.374141 0.111292 0.602519 11.00000 0.03123 0.02471 = 0.01754 -0.00602 0.00079 -0.00003 C2 1 -0.075079 0.111286 0.671629 11.00000 0.01853 0.02906 = 0.02075 -0.00026 0.00027 -0.00263 C1 1 -0.087614 0.050470 0.703831 11.00000 0.02145 0.02350 = 0.02460 -0.00595 -0.00122 -0.00276 C7 1 -0.110068 -0.028482 0.822452 11.00000 0.03151 0.02548 = 0.02082 -0.00068 0.00262 -0.00351 C6 1 -0.120727 0.037880 0.788635 11.00000 0.02260 0.03092 = 0.01825 -0.00060 0.00111 -0.00231 C27 1 0.235552 0.312619 0.727969 11.00000 0.05460 0.02160 = 0.03065 -0.00737 0.00100 0.00089 C5 1 -0.150268 0.087315 0.841019 11.00000 0.03836 0.03758 = 0.02107 -0.00255 0.00857 -0.00120 AFIX 43 H5 2 -0.174351 0.079847 0.898534 11.00000 -1.20000 AFIX 0 C15 1 -0.204120 -0.039657 0.896611 11.00000 0.09362 0.03382 = 0.02679 -0.00383 0.02265 -0.01293 AFIX 137 H15A 2 -0.298088 -0.031785 0.876280 11.00000 -1.50000 H15B 2 -0.179117 -0.011643 0.944541 11.00000 -1.50000 H15C 2 -0.195104 -0.082665 0.916282 11.00000 -1.50000 AFIX 0 C4 1 -0.145212 0.147747 0.810701 11.00000 0.04518 0.02768 = 0.03464 -0.00658 0.01166 0.00180 AFIX 43 H4 2 -0.168957 0.181257 0.846564 11.00000 -1.20000 AFIX 0 C3 1 -0.105704 0.158838 0.728587 11.00000 0.03662 0.01964 = 0.03419 0.00055 0.00714 0.00368 AFIX 43 H3 2 -0.098909 0.200527 0.709723 11.00000 -1.20000 AFIX 0 C31 1 0.325350 0.159978 0.805004 11.00000 0.03459 0.02790 = 0.02674 0.00261 -0.00366 0.00400 AFIX 13 H31 2 0.308408 0.123558 0.766098 11.00000 -1.20000 AFIX 0 C22 1 0.481891 0.201633 0.531722 11.00000 0.02901 0.03300 = 0.03490 0.00012 0.00866 -0.00209 AFIX 13 H22 2 0.385525 0.215844 0.527529 11.00000 -1.20000 AFIX 0 C19 1 0.344781 0.009590 0.677104 11.00000 0.04065 0.02978 = 0.03663 0.00305 0.00018 0.00301 AFIX 13 H19 2 0.253679 0.027812 0.686156 11.00000 -1.20000 AFIX 0 C26 1 0.291441 0.275277 0.789123 11.00000 0.04493 0.02391 = 0.02609 -0.00689 0.00088 -0.00056 C18 1 0.600652 0.103453 0.584429 11.00000 0.02426 0.05916 = 0.03788 0.00356 0.00487 0.00816 C17 1 0.563964 0.052214 0.624048 11.00000 0.03248 0.04802 = 0.04131 0.01119 0.00800 0.01430 C13 1 -0.111403 -0.056322 0.664000 11.00000 0.02597 0.01930 = 0.02175 0.00201 0.00173 -0.00270 C8 1 -0.138795 -0.073629 0.748196 11.00000 0.02402 0.02605 = 0.01928 0.00095 0.00221 0.00030 C9 1 -0.182200 -0.134094 0.761472 11.00000 0.04306 0.03200 = 0.02222 0.00173 0.00474 -0.00301 AFIX 43 H9 2 -0.203604 -0.147019 0.817638 11.00000 -1.20000 AFIX 0 C30 1 -0.015374 0.326862 0.600582 11.00000 0.03879 0.03597 = 0.05216 0.00907 -0.00158 0.00577 AFIX 137 H30A 2 -0.072565 0.295637 0.626470 11.00000 -1.50000 H30B 2 -0.060763 0.342342 0.547159 11.00000 -1.50000 H30C 2 0.000294 0.361273 0.641075 11.00000 -1.50000 AFIX 0 C10 1 -0.194366 -0.175536 0.693249 11.00000 0.05784 0.02643 = 0.02917 0.00405 0.00330 -0.01602 AFIX 43 H10 2 -0.222950 -0.216860 0.702819 11.00000 -1.20000 AFIX 0 C32 1 0.477043 0.163609 0.825942 11.00000 0.04093 0.04678 = 0.04631 0.00314 -0.01093 0.00680 AFIX 137 H32A 2 0.524407 0.166641 0.772247 11.00000 -1.50000 H32B 2 0.507074 0.126302 0.857451 11.00000 -1.50000 H32C 2 0.497464 0.200224 0.861629 11.00000 -1.50000 AFIX 0 C20 1 0.408577 -0.007730 0.765174 11.00000 0.06098 0.04015 = 0.03991 0.01103 -0.00103 0.00827 AFIX 137 H20A 2 0.492083 -0.031124 0.757821 11.00000 -1.50000 H20B 2 0.345140 -0.033239 0.796132 11.00000 -1.50000 H20C 2 0.429617 0.030014 0.798321 11.00000 -1.50000 AFIX 0 C33 1 0.243876 0.150102 0.884741 11.00000 0.05134 0.05449 = 0.03821 0.01639 0.00440 0.00585 AFIX 137 H33A 2 0.261984 0.184106 0.925575 11.00000 -1.50000 H33B 2 0.270315 0.110735 0.912204 11.00000 -1.50000 H33C 2 0.147068 0.149131 0.867593 11.00000 -1.50000 AFIX 0 C29 1 0.208872 0.343499 0.534194 11.00000 0.04534 0.03993 = 0.03577 0.00817 0.00172 -0.00796 AFIX 137 H29A 2 0.217725 0.381929 0.567627 11.00000 -1.50000 H29B 2 0.167655 0.352575 0.476738 11.00000 -1.50000 H29C 2 0.298639 0.325200 0.528536 11.00000 -1.50000 AFIX 0 C14 1 0.037110 -0.039064 0.857049 11.00000 0.05947 0.03445 = 0.05411 0.00313 -0.02752 -0.00016 AFIX 137 H14A 2 0.047424 -0.081776 0.877747 11.00000 -1.50000 H14B 2 0.058810 -0.010343 0.904704 11.00000 -1.50000 H14C 2 0.098693 -0.031803 0.810698 11.00000 -1.50000 AFIX 0 C24 1 0.562564 0.247714 0.588135 11.00000 0.04952 0.05336 = 0.05649 -0.00579 -0.00024 -0.01608 AFIX 137 H24A 2 0.523245 0.250475 0.644629 11.00000 -1.50000 H24B 2 0.559593 0.288530 0.560470 11.00000 -1.50000 H24C 2 0.656788 0.233802 0.595622 11.00000 -1.50000 AFIX 0 C23 1 0.531839 0.199189 0.440303 11.00000 0.04992 0.03661 = 0.04588 0.00990 0.01639 0.00307 AFIX 137 H23A 2 0.627091 0.186475 0.442659 11.00000 -1.50000 H23B 2 0.522952 0.240266 0.413729 11.00000 -1.50000 H23C 2 0.477503 0.169260 0.405899 11.00000 -1.50000 AFIX 0 C21 1 0.323993 -0.046646 0.619309 11.00000 0.09276 0.03177 = 0.04948 0.00056 -0.00741 0.00526 AFIX 137 H21A 2 0.282298 -0.033777 0.563441 11.00000 -1.50000 H21B 2 0.264600 -0.076306 0.646529 11.00000 -1.50000 H21C 2 0.411650 -0.066188 0.610619 11.00000 -1.50000 AFIX 0 C12 1 -0.123868 -0.096680 0.593295 11.00000 0.02465 0.02087 = 0.02308 -0.00239 0.00126 -0.00213 C11 1 -0.164878 -0.156645 0.611420 11.00000 0.05048 0.02679 = 0.02430 -0.00269 0.00294 -0.00754 AFIX 43 H11 2 -0.172936 -0.185816 0.565603 11.00000 -1.20000 AFIX 3 H26 2 0.337012 0.285175 0.849290 11.00000 0.07632 AFIX 3 H27 2 0.219112 0.356575 0.714980 11.00000 0.05670 AFIX 3 H17 2 0.616212 0.011475 0.638180 11.00000 0.05106 AFIX 3 H18 2 0.690312 0.115675 0.559290 11.00000 0.04180 AFIX 0 HKLF 4 REM P21n in P2(1)/n REM wR2 = 0.1020, GooF = S = 0.923, Restrained GooF = 0.923 for all data REM R1 = 0.0518 for 3564 Fo > 4sig(Fo) and 0.1306 for all 6499 data REM 384 parameters refined using 0 restraints END WGHT 0.0404 0.0000 REM Highest difference peak 0.386, deepest hole -0.298, 1-sigma level 0.077 Q1 1 0.1303 0.1039 0.5630 11.00000 0.05 0.39 Q2 1 0.3327 0.1468 0.6339 11.00000 0.05 0.37 Q3 1 0.1808 0.1030 0.6479 11.00000 0.05 0.36 Q4 1 0.2530 0.1705 0.5652 11.00000 0.05 0.36 Q5 1 0.1797 0.1789 0.6374 11.00000 0.05 0.34 Q6 1 -0.0916 0.1472 0.5046 11.00000 0.05 0.32 Q7 1 0.6002 0.0336 0.7787 11.00000 0.05 0.31 Q8 1 0.0687 0.1703 0.5784 11.00000 0.05 0.30 Q9 1 0.2838 0.1362 0.5606 11.00000 0.05 0.30 Q10 1 0.0784 0.1258 0.5910 11.00000 0.05 0.29 Q11 1 -0.1307 -0.0902 0.5389 11.00000 0.05 0.29 Q12 1 0.5695 0.1567 0.7775 11.00000 0.05 0.29 Q13 1 -0.3600 0.0090 0.9965 11.00000 0.05 0.29 Q14 1 -0.0978 0.2969 0.6618 11.00000 0.05 0.28 Q15 1 0.2179 0.2832 0.7661 11.00000 0.05 0.28 Q16 1 -0.0833 0.1810 0.5264 11.00000 0.05 0.28 Q17 1 -0.1709 -0.0566 0.7245 11.00000 0.05 0.28 Q18 1 0.5042 0.1700 0.5420 11.00000 0.05 0.28 Q19 1 0.0138 0.1545 0.4938 11.00000 0.05 0.27 Q20 1 -0.0612 0.0760 0.6376 11.00000 0.05 0.27 ; _shelx_res_checksum 45563 _shelx_hkl_file ; -5 12 -5 2.21 6.27 -5 25 0 9.76 14.04 -4 11 0 2.65 7.92 -2 3 -13 -2.93 5.88 -2 5 1 32.28 5.31 -2 13 6 10.21 8.57 -1 21 9 -6.68 14.34 -1 22 9 6.26 13.48 -1 23 9 1.50 13.79 -1 24 9 5.35 14.71 1 8 8 3.03 6.95 1 21 11 10.43 12.41 1 22 11 2.57 13.24 3 -3 1 27.50 3.95 3 9 10 3.70 6.97 4 -5 -1 29.79 5.94 5 18 13 -2.56 13.91 6 -4 2 10.18 5.51 6 4 9 9.17 3.78 6 16 13 12.10 12.19 9 0 6 2.30 7.01 -6 21 -7 3.12 13.11 -6 22 -8 8.62 12.08 -6 22 -7 9.72 12.68 -4 14 2 71.47 9.89 -4 22 4 -4.02 14.34 -4 23 4 4.97 15.22 -3 20 6 22.95 14.84 -3 22 6 4.03 14.23 -3 23 6 2.46 13.75 -3 24 6 11.76 14.23 -3 25 6 -2.81 14.89 -2 16 7 7.12 10.89 -1 9 6 32.44 7.34 -1 14 8 6.08 9.50 -1 19 9 37.21 14.35 -1 20 9 8.52 12.72 0 13 9 28.80 10.14 1 3 5 15.26 4.59 1 6 7 13.60 6.01 1 19 11 5.97 12.15 2 -2 1 222.16 4.70 2 8 9 22.63 6.96 2 14 11 -0.88 9.02 3 -5 -3 1.42 5.13 3 3 7 51.97 3.83 3 16 12 13.03 12.26 4 10 11 4.45 8.99 5 9 11 8.99 7.94 5 12 12 -0.25 9.53 5 17 13 0.61 13.78 -6 20 -8 7.47 10.92 -6 21 -9 2.03 11.42 -6 21 -8 -3.65 11.48 -6 22 -6 4.32 13.05 -6 22 -5 -0.23 14.53 -6 23 -6 0.79 13.42 -6 23 -5 2.06 14.24 -5 11 -7 27.37 7.04 -5 12 -4 2.14 7.21 -5 20 1 -5.78 13.24 -5 22 1 5.13 13.32 -4 16 3 4.90 10.28 -4 20 4 -1.51 12.31 -4 21 4 8.99 13.31 -4 24 4 3.95 13.69 -3 9 2 10.61 6.89 -2 10 5 40.63 7.79 -2 12 6 1.53 8.62 -2 21 8 -6.47 14.63 -2 22 8 27.15 13.66 -2 23 8 9.76 14.04 -2 24 8 5.43 15.93 -2 25 8 6.30 15.06 -1 0 -11 11.68 6.27 0 -2 -10 2.58 4.84 0 -2 -5 0.80 3.83 0 8 7 16.34 6.78 1 -2 -1 218.72 5.01 2 -4 -3 1.81 4.59 2 19 12 7.95 13.46 2 20 12 6.64 14.45 3 15 12 7.31 11.66 4 2 7 7.76 2.49 4 13 12 9.55 10.59 4 19 13 -3.60 15.22 6 0 6 2.90 3.51 6 11 12 5.45 8.91 6 15 13 11.15 11.11 7 -4 2 0.64 7.14 -6 19 -8 10.11 10.19 -6 19 -7 3.54 11.00 -6 20 -9 -1.43 10.04 -6 20 -5 -2.36 10.67 -6 21 -5 -1.17 13.08 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-7 -7 4 31.59 2.63 -6 -15 0 6.44 3.45 -4 -26 -2 -4.18 4.70 -4 -9 -1 31.18 3.00 -3 -25 -3 3.11 4.54 -3 -14 -3 16.62 3.61 -3 -9 -2 4.51 2.38 -3 5 7 26.35 1.33 -2 -23 -4 4.83 4.52 -2 -16 -4 42.19 3.84 -2 -10 -3 15.29 2.54 -2 6 7 74.69 2.17 -1 -5 -2 1.23 1.50 0 -24 -5 3.57 3.47 0 -16 -5 0.34 2.81 0 4 3 1.39 1.28 1 -26 -5 1.56 4.42 1 -3 -2 56.23 1.30 3 5 3 9.14 2.16 7 -19 -5 0.15 2.48 7 -18 -5 1.08 2.33 7 -4 -2 9.92 1.72 7 -2 -1 5.14 2.05 -9 -8 9 4.17 2.92 -8 -13 4 1.76 3.31 -8 -10 5 8.29 2.87 -8 -5 8 2.54 2.51 -7 -13 2 1.33 2.84 -7 -4 6 4.27 1.77 -6 -23 0 0.24 4.21 -6 -22 0 8.28 4.50 -6 -16 0 13.90 3.98 -6 -11 1 33.25 3.47 -6 -4 4 3.45 1.75 -5 -25 -1 0.03 4.17 -4 -25 -2 -2.23 4.64 -3 -24 -3 1.56 4.50 -3 -4 0 63.64 2.13 -2 -22 -4 0.03 3.83 -2 -21 -4 1.24 3.84 -2 -20 -4 2.96 4.16 -2 -19 -4 43.13 4.73 -2 -18 -4 20.55 4.34 -2 -17 -4 46.14 3.99 -1 -8 -3 25.11 2.40 0 -22 -5 -0.55 3.85 0 -10 -4 49.94 2.98 0 6 5 -0.41 1.82 1 -25 -5 1.70 4.22 6 -14 -5 9.44 1.96 6 -3 -2 0.18 1.20 9 -7 -2 39.25 2.35 -9 -16 6 10.59 3.97 -9 -15 6 2.07 3.69 -9 -12 7 2.32 3.32 -9 -7 10 -2.08 2.61 -9 -6 11 3.07 2.53 -8 -8 6 0.21 2.54 -7 -14 2 4.16 3.59 -7 -1 9 8.49 1.68 -6 -21 0 -4.65 4.12 -6 -20 0 -5.10 3.94 -6 -19 0 12.54 4.48 -6 -18 0 26.66 4.46 -5 -24 -1 4.36 4.27 -5 -23 -1 -0.19 4.53 -5 -15 -1 -1.15 3.56 -5 -10 0 0.33 2.41 -5 -7 1 13.93 2.28 -4 -24 -2 2.57 4.33 -3 -23 -3 5.38 4.13 -3 -16 -3 0.15 3.96 -3 -15 -3 15.84 3.52 -2 -7 -2 13.53 2.21 1 -24 -5 6.50 3.57 2 -26 -5 -0.83 4.22 2 5 3 20.34 1.80 2 6 4 14.16 1.95 4 4 2 117.27 3.27 6 -1 -1 9.41 1.56 8 -3 -1 35.07 2.48 -9 -18 6 0.56 4.48 -9 -17 6 0.55 3.97 -9 -10 8 -0.30 3.04 -8 -14 4 -1.31 3.16 -7 -23 2 -4.38 4.38 -7 -15 2 1.43 4.05 -7 -8 4 0.02 2.58 -7 -6 5 7.97 2.28 -7 -3 7 24.24 2.12 -6 -12 1 -0.66 3.15 -5 -22 -1 12.15 4.70 -5 -21 -1 -5.19 4.63 -5 -20 -1 7.82 4.76 -5 -17 -1 -1.53 4.38 -5 -16 -1 -0.67 3.67 -5 -5 2 3.09 2.10 -4 -23 -2 -3.02 3.99 -4 -22 -2 29.51 4.94 -4 -16 -2 7.85 4.20 -4 -10 -1 6.81 2.71 -4 7 13 5.77 2.15 -3 -22 -3 27.17 4.62 -3 -20 -3 5.27 4.40 -3 -18 -3 9.48 4.42 -3 -17 -3 -1.69 3.60 -3 -10 -2 3.48 2.34 -3 7 10 105.87 3.07 -2 -11 -3 2.54 2.31 -2 8 10 22.24 2.65 -1 -3 -1 7.12 1.62 0 -4 -2 172.71 2.41 0 7 6 1.97 1.98 1 -9 -4 154.34 3.41 2 -25 -5 -3.58 3.96 2 -8 -4 -0.40 1.75 3 -26 -5 -0.82 4.45 3 -12 -5 1.33 1.63 4 -12 -5 70.65 2.31 6 -23 -5 0.22 3.07 7 0 0 -0.57 1.98 8 -5 -2 4.56 1.74 -8 -16 4 1.65 3.96 -7 -22 2 0.34 4.09 -7 -20 2 -2.33 4.19 -7 -18 2 15.84 4.49 -7 -16 2 2.54 3.82 -5 -19 -1 2.18 4.07 -5 -18 -1 -0.50 4.35 -5 -11 0 37.46 3.47 -4 -21 -2 4.10 4.32 -4 -20 -2 14.76 4.56 -4 -18 -2 38.74 4.31 -4 -17 -2 -0.07 3.64 -4 -7 0 23.04 2.46 -3 -27 -2 2.38 4.41 -3 -7 -1 1.03 2.30 -2 -26 -3 1.32 4.53 -1 -14 -4 16.62 2.71 0 -27 -4 14.70 4.26 1 -22 -5 17.78 3.71 2 -24 -5 2.97 3.86 2 -5 -3 5.76 1.01 2 4 2 4.43 1.45 3 -25 -5 8.31 4.43 3 3 1 27.20 1.89 4 -25 -5 2.06 3.82 4 3 1 26.67 2.27 5 -13 -5 9.53 2.12 6 -15 -5 32.15 2.37 -9 -14 7 1.61 3.72 -9 -11 8 7.88 3.39 -9 -9 9 2.82 2.90 -8 -17 4 1.18 3.97 -8 -12 5 -2.30 2.73 -8 -9 6 0.33 2.73 -8 -7 7 0.81 2.46 -7 -19 2 10.21 3.84 -6 -24 1 3.37 4.64 -6 -13 1 -0.80 3.09 -6 -9 2 15.16 2.51 -6 -3 5 90.48 2.57 -3 -26 -2 0.21 4.47 -3 -11 -2 25.32 2.73 -2 -25 -3 0.86 4.17 -2 -12 -3 1.07 2.32 -2 7 8 0.24 1.66 -1 -22 -4 10.80 4.05 -1 -15 -4 5.49 3.02 -1 -9 -3 2.50 2.58 0 -26 -4 -0.88 4.26 0 -7 -3 11.79 1.78 0 3 2 82.38 1.60 1 -21 -5 5.64 2.97 1 -20 -5 0.40 3.13 1 -19 -5 20.19 3.45 1 -18 -5 35.83 3.52 2 -23 -5 5.26 3.66 2 -14 -5 0.55 2.32 6 -22 -5 11.70 3.07 6 1 0 6.10 1.82 9 -4 -1 5.37 2.42 -9 -16 7 -6.52 3.86 -9 -15 7 -1.55 3.66 -9 -8 10 4.87 2.77 -7 -9 4 5.18 2.49 -6 -23 1 0.17 4.12 -6 -14 1 3.64 3.20 -5 -25 0 8.74 4.31 -5 -12 0 -0.97 2.69 -5 -8 1 14.69 2.31 -4 -26 -1 -3.83 4.19 -4 -11 -1 51.99 3.17 -3 6 8 33.74 1.72 -2 -24 -3 2.66 4.30 -2 -8 -2 18.86 2.50 -2 -5 -1 9.22 1.91 -1 -21 -4 20.10 4.02 -1 -19 -4 1.17 3.80 -1 -17 -4 10.12 3.50 -1 -16 -4 3.89 2.88 -1 8 8 2.61 1.74 0 -25 -4 -1.82 3.60 1 -27 -4 1.87 4.71 1 6 4 77.25 2.47 1 7 5 186.76 3.93 2 -22 -5 6.26 3.71 3 -24 -5 2.35 4.02 3 -13 -5 1.08 1.95 4 -24 -5 1.64 3.91 4 -13 -5 4.49 1.83 4 0 -1 -0.68 1.13 5 -23 -5 1.39 3.24 5 3 1 1.89 2.09 6 -21 -5 -0.05 2.80 6 -20 -5 6.95 2.92 6 -16 -5 9.11 2.22 -9 -12 8 -3.61 3.49 -9 -10 9 2.96 3.31 -9 -7 11 2.63 2.46 -8 -13 5 26.71 3.55 -8 -10 6 38.68 3.41 -8 -6 8 -0.26 2.52 -7 -5 6 3.25 1.84 -6 -20 1 -4.35 4.51 -6 -15 1 3.60 3.44 -6 -10 2 10.09 2.94 -5 -13 0 -0.01 3.46 -4 -25 -1 0.94 4.28 -4 -12 -1 2.05 2.83 -4 -5 1 25.25 2.55 -3 -25 -2 3.59 4.10 -3 -12 -2 12.39 2.65 -2 -23 -3 -0.66 4.45 -2 -13 -3 18.11 2.61 -1 -18 -4 44.25 3.82 0 -24 -4 -0.32 4.30 0 -12 -4 1.39 2.22 1 -6 -3 1.42 1.36 1 5 3 50.48 1.94 2 -21 -5 5.34 2.96 2 -15 -5 1.24 2.23 3 -23 -5 -1.85 3.41 3 0 -1 917.05 4.18 4 -23 -5 -0.04 3.75 5 -22 -5 -2.82 3.27 -9 -13 8 8.63 3.40 -8 -14 5 8.35 3.32 -8 -8 7 -0.33 2.57 -7 -23 3 -1.81 4.19 -7 -7 5 0.86 2.25 -6 -19 1 4.28 3.98 -6 -17 1 57.22 4.77 -5 -23 0 3.93 4.19 -5 -22 0 8.11 4.65 -5 -6 2 40.27 2.68 -4 -24 -1 4.52 4.24 -4 -8 0 18.85 2.46 -4 -3 2 4.65 1.79 -3 -24 -2 5.18 4.06 -3 -23 -2 9.90 4.58 -3 -8 -1 14.08 2.87 -3 -5 0 5.96 1.94 -2 -22 -3 5.38 3.96 -2 -14 -3 2.96 2.70 -1 -6 -2 8.88 1.65 1 -26 -4 9.42 4.86 2 -27 -4 -5.04 4.29 2 -20 -5 44.95 3.47 2 -19 -5 3.25 2.68 2 -18 -5 10.22 2.86 2 -17 -5 2.35 2.51 2 -16 -5 30.94 2.78 2 3 1 0.79 1.37 3 -22 -5 -3.77 3.42 3 -14 -5 45.19 2.62 4 -22 -5 10.30 3.73 -9 -14 8 -0.74 3.62 -8 -20 5 6.90 4.42 -8 -19 5 2.84 4.27 -8 -18 5 4.72 3.84 -8 -17 5 6.45 3.70 -8 -15 5 2.74 2.98 -8 -11 6 11.92 2.78 -7 -21 3 2.12 3.93 -7 -20 3 2.61 4.07 -7 -16 3 5.97 4.00 -7 -15 3 4.57 3.67 -6 -11 2 1.70 2.85 -5 -21 0 32.77 4.77 -5 -14 0 1.75 3.30 -4 -23 -1 4.96 4.13 -4 -22 -1 11.84 4.66 -4 -13 -1 1.35 2.62 -3 -22 -2 7.48 4.41 -3 -13 -2 2.61 2.39 -2 -27 -2 -0.10 4.36 -2 -21 -3 1.40 3.95 -2 -20 -3 31.87 4.47 -2 -19 -3 -4.21 4.12 -2 -16 -3 0.31 3.46 -2 -15 -3 -3.58 2.72 -1 -10 -3 24.37 2.57 0 -13 -4 40.98 2.87 1 -25 -4 4.73 3.56 3 -21 -5 10.76 3.15 4 2 0 280.21 3.73 -7 -19 3 8.80 3.93 -7 -18 3 6.71 3.77 -7 -17 3 6.49 3.80 -6 -24 2 6.89 4.12 -5 -20 0 2.72 4.28 -5 -19 0 3.94 4.30 -5 -18 0 1.13 4.18 -5 -16 0 3.35 3.52 -4 -21 -1 28.17 4.76 -4 -14 -1 -0.61 3.07 -3 -27 -1 -1.14 4.10 -3 -21 -2 10.38 4.32 -3 -14 -2 7.55 2.61 -2 -18 -3 23.90 3.91 -2 -17 -3 1.16 3.58 -2 -9 -2 5.67 2.39 3 6 3 12.96 2.07 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 88537 loop_ _space_group_symop_operation_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_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 0.19481(4) 0.14285(2) 0.60123(3) 0.01984(13) Uani 1 1 d . . . . . P2 P -0.02777(8) 0.13768(5) 0.56316(6) 0.0234(2) Uani 1 1 d . . . . . P1 P 0.10225(9) 0.06663(5) 0.51747(6) 0.0231(2) Uani 1 1 d . . . . . N2 N 0.4850(3) 0.13974(16) 0.5709(2) 0.0303(8) Uani 1 1 d . . . . . O1 O -0.0648(2) 0.00289(12) 0.64669(16) 0.0294(6) Uani 1 1 d . . . . . N3 N 0.1899(3) 0.27490(14) 0.65974(19) 0.0239(7) Uani 1 1 d . . . . . C25 C 0.2172(3) 0.21383(17) 0.6761(2) 0.0211(8) Uani 1 1 d . . . . . N4 N 0.2797(3) 0.21518(15) 0.75764(19) 0.0260(8) Uani 1 1 d . . . . . N1 N 0.4261(3) 0.05724(15) 0.6357(2) 0.0309(8) Uani 1 1 d . . . . . C28 C 0.1193(3) 0.29793(17) 0.5805(2) 0.0256(9) Uani 1 1 d . . . . . H28 H 0.100545 0.261810 0.541334 0.031 Uiso 1 1 calc R U . . . C16 C 0.3741(3) 0.11129(18) 0.6025(2) 0.0245(9) Uani 1 1 d . . . . . C2 C -0.0751(3) 0.11129(18) 0.6716(2) 0.0228(9) Uani 1 1 d . . . . . C1 C -0.0876(3) 0.05047(18) 0.7038(2) 0.0233(9) Uani 1 1 d . . . . . C7 C -0.1101(3) -0.02848(18) 0.8225(2) 0.0259(9) Uani 1 1 d . . . . . C6 C -0.1207(3) 0.03788(18) 0.7886(2) 0.0239(9) Uani 1 1 d . . . . . C27 C 0.2356(4) 0.3126(2) 0.7280(3) 0.0357(10) Uani 1 1 d . . . . . C5 C -0.1503(4) 0.0873(2) 0.8410(3) 0.0321(10) Uani 1 1 d . . . . . H5 H -0.174351 0.079847 0.898534 0.039 Uiso 1 1 calc R U . . . C15 C -0.2041(5) -0.0397(2) 0.8966(3) 0.0507(12) Uani 1 1 d . . . . . H15A H -0.298088 -0.031785 0.876280 0.076 Uiso 1 1 calc R U . . . H15B H -0.179117 -0.011643 0.944541 0.076 Uiso 1 1 calc R U . . . H15C H -0.195104 -0.082665 0.916282 0.076 Uiso 1 1 calc R U . . . C4 C -0.1452(4) 0.1477(2) 0.8107(3) 0.0355(10) Uani 1 1 d . . . . . H4 H -0.168957 0.181257 0.846564 0.043 Uiso 1 1 calc R U . . . C3 C -0.1057(3) 0.15884(18) 0.7286(3) 0.0300(10) Uani 1 1 d . . . . . H3 H -0.098909 0.200527 0.709723 0.036 Uiso 1 1 calc R U . . . C31 C 0.3253(3) 0.15998(18) 0.8050(2) 0.0299(10) Uani 1 1 d . . . . . H31 H 0.308408 0.123558 0.766098 0.036 Uiso 1 1 calc R U . . . C22 C 0.4819(4) 0.20163(19) 0.5317(3) 0.0321(10) Uani 1 1 d . . . . . H22 H 0.385525 0.215844 0.527529 0.038 Uiso 1 1 calc R U . . . C19 C 0.3448(4) 0.0096(2) 0.6771(3) 0.0358(10) Uani 1 1 d . . . . . H19 H 0.253679 0.027812 0.686156 0.043 Uiso 1 1 calc R U . . . C26 C 0.2914(4) 0.27528(19) 0.7891(3) 0.0317(10) Uani 1 1 d . . . . . C18 C 0.6007(4) 0.1035(2) 0.5844(3) 0.0403(11) Uani 1 1 d . . . . . C17 C 0.5640(4) 0.0522(2) 0.6240(3) 0.0404(12) Uani 1 1 d . . . . . C13 C -0.1114(3) -0.05632(17) 0.6640(2) 0.0223(9) Uani 1 1 d . . . . . C8 C -0.1388(3) -0.07363(18) 0.7482(2) 0.0231(9) Uani 1 1 d . . . . . C9 C -0.1822(4) -0.13409(19) 0.7615(2) 0.0323(10) Uani 1 1 d . . . . . H9 H -0.203604 -0.147019 0.817638 0.039 Uiso 1 1 calc R U . . . C30 C -0.0154(4) 0.3269(2) 0.6006(3) 0.0425(12) Uani 1 1 d . . . . . H30A H -0.072565 0.295637 0.626470 0.064 Uiso 1 1 calc R U . . . H30B H -0.060763 0.342342 0.547159 0.064 Uiso 1 1 calc R U . . . H30C H 0.000294 0.361273 0.641075 0.064 Uiso 1 1 calc R U . . . C10 C -0.1944(4) -0.1755(2) 0.6932(3) 0.0378(11) Uani 1 1 d . . . . . H10 H -0.222950 -0.216860 0.702819 0.045 Uiso 1 1 calc R U . . . C32 C 0.4770(4) 0.1636(2) 0.8259(3) 0.0452(12) Uani 1 1 d . . . . . H32A H 0.524407 0.166641 0.772247 0.068 Uiso 1 1 calc R U . . . H32B H 0.507074 0.126302 0.857451 0.068 Uiso 1 1 calc R U . . . H32C H 0.497464 0.200224 0.861629 0.068 Uiso 1 1 calc R U . . . C20 C 0.4086(4) -0.0077(2) 0.7652(3) 0.0471(12) Uani 1 1 d . . . . . H20A H 0.492083 -0.031124 0.757821 0.071 Uiso 1 1 calc R U . . . H20B H 0.345140 -0.033239 0.796132 0.071 Uiso 1 1 calc R U . . . H20C H 0.429617 0.030014 0.798321 0.071 Uiso 1 1 calc R U . . . C33 C 0.2439(4) 0.1501(2) 0.8847(3) 0.0479(12) Uani 1 1 d . . . . . H33A H 0.261984 0.184106 0.925575 0.072 Uiso 1 1 calc R U . . . H33B H 0.270315 0.110735 0.912204 0.072 Uiso 1 1 calc R U . . . H33C H 0.147068 0.149131 0.867593 0.072 Uiso 1 1 calc R U . . . C29 C 0.2089(4) 0.34350(19) 0.5342(3) 0.0404(11) Uani 1 1 d . . . . . H29A H 0.217725 0.381929 0.567627 0.061 Uiso 1 1 calc R U . . . H29B H 0.167655 0.352575 0.476738 0.061 Uiso 1 1 calc R U . . . H29C H 0.298639 0.325200 0.528536 0.061 Uiso 1 1 calc R U . . . C14 C 0.0371(4) -0.0391(2) 0.8570(3) 0.0504(13) Uani 1 1 d . . . . . H14A H 0.047424 -0.081776 0.877747 0.076 Uiso 1 1 calc R U . . . H14B H 0.058810 -0.010343 0.904704 0.076 Uiso 1 1 calc R U . . . H14C H 0.098693 -0.031803 0.810698 0.076 Uiso 1 1 calc R U . . . C24 C 0.5626(4) 0.2477(2) 0.5881(3) 0.0532(13) Uani 1 1 d . . . . . H24A H 0.523245 0.250475 0.644629 0.080 Uiso 1 1 calc R U . . . H24B H 0.559593 0.288530 0.560470 0.080 Uiso 1 1 calc R U . . . H24C H 0.656788 0.233802 0.595622 0.080 Uiso 1 1 calc R U . . . C23 C 0.5318(4) 0.1992(2) 0.4403(3) 0.0436(12) Uani 1 1 d . . . . . H23A H 0.627091 0.186475 0.442659 0.065 Uiso 1 1 calc R U . . . H23B H 0.522952 0.240266 0.413729 0.065 Uiso 1 1 calc R U . . . H23C H 0.477503 0.169260 0.405899 0.065 Uiso 1 1 calc R U . . . C21 C 0.3240(5) -0.0466(2) 0.6193(3) 0.0584(14) Uani 1 1 d . . . . . H21A H 0.282298 -0.033777 0.563441 0.088 Uiso 1 1 calc R U . . . H21B H 0.264600 -0.076306 0.646529 0.088 Uiso 1 1 calc R U . . . H21C H 0.411650 -0.066188 0.610619 0.088 Uiso 1 1 calc R U . . . C12 C -0.1239(3) -0.09668(17) 0.5933(2) 0.0229(9) Uani 1 1 d . . . . . C11 C -0.1649(4) -0.15664(18) 0.6114(2) 0.0338(10) Uani 1 1 d . . . . . H11 H -0.172936 -0.185816 0.565603 0.041 Uiso 1 1 calc R U . . . H26 H 0.337012 0.285175 0.849290 0.076(16) Uiso 1 1 d R . . . . H27 H 0.219112 0.356575 0.714980 0.057(14) Uiso 1 1 d R . . . . H17 H 0.616212 0.011475 0.638180 0.051(13) Uiso 1 1 d R . . . . H18 H 0.690312 0.115675 0.559290 0.042(11) Uiso 1 1 d 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 Ni1 0.0215(2) 0.0189(3) 0.0190(3) -0.0016(2) 0.00020(18) -0.0018(2) P2 0.0236(5) 0.0235(6) 0.0231(5) 0.0009(5) 0.0015(4) -0.0030(5) P1 0.0294(5) 0.0207(6) 0.0193(5) -0.0018(4) 0.0019(4) -0.0042(4) N2 0.0232(15) 0.036(2) 0.0316(19) 0.0002(17) 0.0061(14) 0.0012(16) O1 0.0430(15) 0.0216(17) 0.0246(16) -0.0049(12) 0.0107(13) -0.0073(12) N3 0.0326(17) 0.017(2) 0.0216(18) -0.0040(14) -0.0008(14) -0.0026(14) C25 0.0212(18) 0.019(2) 0.023(2) 0.0019(17) 0.0032(16) -0.0016(16) N4 0.0305(17) 0.027(2) 0.0206(18) -0.0039(15) -0.0026(14) 0.0007(15) N1 0.0293(17) 0.033(2) 0.031(2) 0.0048(16) 0.0008(15) 0.0098(16) C28 0.036(2) 0.018(2) 0.022(2) -0.0014(17) -0.0074(18) -0.0055(17) C16 0.031(2) 0.025(3) 0.018(2) -0.0060(17) 0.0008(17) 0.0000(18) C2 0.0185(18) 0.029(3) 0.021(2) -0.0003(18) 0.0003(16) -0.0026(16) C1 0.0215(19) 0.023(2) 0.025(2) -0.0059(18) -0.0012(16) -0.0028(16) C7 0.032(2) 0.025(3) 0.021(2) -0.0007(18) 0.0026(17) -0.0035(18) C6 0.0226(19) 0.031(3) 0.018(2) -0.0006(18) 0.0011(16) -0.0023(17) C27 0.055(3) 0.022(3) 0.031(3) -0.007(2) 0.001(2) 0.001(2) C5 0.038(2) 0.038(3) 0.021(2) -0.003(2) 0.0086(18) -0.0012(19) C15 0.094(3) 0.034(3) 0.027(3) -0.004(2) 0.023(2) -0.013(3) C4 0.045(2) 0.028(3) 0.035(2) -0.007(2) 0.0117(19) 0.002(2) C3 0.037(2) 0.020(3) 0.034(2) 0.0006(18) 0.0071(19) 0.0037(17) C31 0.035(2) 0.028(3) 0.027(2) 0.0026(18) -0.0037(18) 0.0040(18) C22 0.029(2) 0.033(3) 0.035(3) 0.000(2) 0.0087(19) -0.0021(18) C19 0.041(2) 0.030(3) 0.037(3) 0.003(2) 0.000(2) 0.003(2) C26 0.045(2) 0.024(3) 0.026(2) -0.0069(19) 0.001(2) -0.0006(19) C18 0.024(2) 0.059(3) 0.038(3) 0.004(2) 0.005(2) 0.008(2) C17 0.032(2) 0.048(3) 0.041(3) 0.011(2) 0.008(2) 0.014(2) C13 0.0260(18) 0.019(2) 0.022(2) 0.0020(17) 0.0017(16) -0.0027(16) C8 0.0240(19) 0.026(3) 0.019(2) 0.0009(18) 0.0022(16) 0.0003(17) C9 0.043(2) 0.032(3) 0.022(2) 0.0017(19) 0.0047(18) -0.003(2) C30 0.039(2) 0.036(3) 0.052(3) 0.009(2) -0.002(2) 0.006(2) C10 0.058(3) 0.026(3) 0.029(3) 0.004(2) 0.003(2) -0.016(2) C32 0.041(2) 0.047(3) 0.046(3) 0.003(2) -0.011(2) 0.007(2) C20 0.061(3) 0.040(3) 0.040(3) 0.011(2) -0.001(2) 0.008(2) C33 0.051(2) 0.054(3) 0.038(3) 0.016(2) 0.004(2) 0.006(2) C29 0.045(2) 0.040(3) 0.036(3) 0.008(2) 0.002(2) -0.008(2) C14 0.059(3) 0.034(3) 0.054(3) 0.003(2) -0.028(2) 0.000(2) C24 0.050(3) 0.053(4) 0.056(3) -0.006(3) 0.000(2) -0.016(2) C23 0.050(3) 0.037(3) 0.046(3) 0.010(2) 0.016(2) 0.003(2) C21 0.093(4) 0.032(3) 0.049(3) 0.001(2) -0.007(3) 0.005(3) C12 0.0246(19) 0.021(2) 0.023(2) -0.0024(17) 0.0013(17) -0.0021(16) C11 0.050(2) 0.027(3) 0.024(2) -0.0027(18) 0.0029(19) -0.0075(19) 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' P P 0.1023 0.0942 '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' 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 C16 Ni1 C25 101.64(15) . . ? C16 Ni1 P2 152.19(12) . . ? C25 Ni1 P2 106.05(10) . . ? C16 Ni1 P1 95.39(12) . . ? C25 Ni1 P1 162.73(10) . . ? P2 Ni1 P1 56.83(4) . . ? C2 P2 P1 105.33(13) . . ? C2 P2 Ni1 93.89(11) . . ? P1 P2 Ni1 61.79(4) . . ? C12 P1 P2 99.02(12) 3_556 . ? C12 P1 Ni1 102.38(12) 3_556 . ? P2 P1 Ni1 61.37(4) . . ? C16 N2 C18 111.1(3) . . ? C16 N2 C22 123.8(3) . . ? C18 N2 C22 125.0(3) . . ? C1 O1 C13 119.5(3) . . ? C25 N3 C27 111.7(3) . . ? C25 N3 C28 124.3(3) . . ? C27 N3 C28 124.0(3) . . ? N3 C25 N4 103.0(3) . . ? N3 C25 Ni1 129.7(3) . . ? N4 C25 Ni1 127.0(3) . . ? C25 N4 C26 111.6(3) . . ? C25 N4 C31 123.8(3) . . ? C26 N4 C31 124.6(3) . . ? C16 N1 C17 111.7(3) . . ? C16 N1 C19 123.9(3) . . ? C17 N1 C19 124.4(3) . . ? N3 C28 C30 110.5(3) . . ? N3 C28 C29 110.5(3) . . ? C30 C28 C29 111.6(3) . . ? N1 C16 N2 103.1(3) . . ? N1 C16 Ni1 130.0(3) . . ? N2 C16 Ni1 126.9(3) . . ? C3 C2 C1 115.6(3) . . ? C3 C2 P2 114.9(3) . . ? C1 C2 P2 129.5(3) . . ? O1 C1 C6 120.9(3) . . ? O1 C1 C2 116.3(3) . . ? C6 C1 C2 122.9(3) . . ? C8 C7 C6 109.5(3) . . ? C8 C7 C15 111.7(3) . . ? C6 C7 C15 111.8(3) . . ? C8 C7 C14 107.6(3) . . ? C6 C7 C14 107.8(3) . . ? C15 C7 C14 108.3(3) . . ? C5 C6 C1 118.1(4) . . ? C5 C6 C7 122.3(4) . . ? C1 C6 C7 119.3(3) . . ? C26 C27 N3 106.9(4) . . ? C6 C5 C4 120.9(4) . . ? C3 C4 C5 119.7(4) . . ? C4 C3 C2 122.7(4) . . ? N4 C31 C32 109.9(3) . . ? N4 C31 C33 111.1(3) . . ? C32 C31 C33 113.1(3) . . ? N2 C22 C24 111.0(4) . . ? N2 C22 C23 110.7(3) . . ? C24 C22 C23 111.8(3) . . ? N1 C19 C21 111.1(4) . . ? N1 C19 C20 110.7(3) . . ? C21 C19 C20 111.8(4) . . ? C27 C26 N4 106.8(4) . . ? C17 C18 N2 107.2(3) . . ? C18 C17 N1 106.9(4) . . ? O1 C13 C8 120.6(3) . . ? O1 C13 C12 115.9(3) . . ? C8 C13 C12 123.5(3) . . ? C9 C8 C13 117.7(3) . . ? C9 C8 C7 122.3(3) . . ? C13 C8 C7 119.8(3) . . ? C10 C9 C8 120.4(4) . . ? C11 C10 C9 119.9(4) . . ? C11 C12 C13 115.8(3) . . ? C11 C12 P1 124.1(3) . 3_556 ? C13 C12 P1 119.8(3) . 3_556 ? C10 C11 C12 122.7(4) . . ? 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 C16 1.899(4) . ? Ni1 C25 1.929(4) . ? Ni1 P2 2.2510(11) . ? Ni1 P1 2.2599(11) . ? P2 C2 1.861(4) . ? P2 P1 2.1466(14) . ? P1 C12 1.861(4) 3_556 ? N2 C16 1.370(4) . ? N2 C18 1.393(5) . ? N2 C22 1.468(5) . ? O1 C1 1.383(4) . ? O1 C13 1.390(4) . ? N3 C25 1.367(4) . ? N3 C27 1.391(5) . ? N3 C28 1.468(4) . ? C25 N4 1.377(4) . ? N4 C26 1.389(5) . ? N4 C31 1.459(5) . ? N1 C16 1.365(5) . ? N1 C17 1.389(4) . ? N1 C19 1.475(5) . ? C28 C30 1.519(5) . ? C28 C29 1.529(5) . ? C2 C3 1.399(5) . ? C2 C1 1.413(5) . ? C1 C6 1.400(5) . ? C7 C8 1.524(5) . ? C7 C6 1.528(5) . ? C7 C15 1.538(5) . ? C7 C14 1.541(5) . ? C6 C5 1.382(5) . ? C27 C26 1.341(5) . ? C5 C4 1.389(5) . ? C4 C3 1.374(5) . ? C31 C32 1.520(5) . ? C31 C33 1.528(5) . ? C22 C24 1.522(5) . ? C22 C23 1.528(5) . ? C19 C21 1.517(6) . ? C19 C20 1.521(5) . ? C18 C17 1.326(6) . ? C13 C8 1.400(5) . ? C13 C12 1.401(5) . ? C8 C9 1.393(5) . ? C9 C10 1.386(5) . ? C10 C11 1.380(5) . ? C12 C11 1.390(5) . ?