#------------------------------------------------------------------------------ #$Date: 2024-07-26 01:55:02 +0300 (Fri, 26 Jul 2024) $ #$Revision: 293547 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/67/7716734.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_7716734 loop_ _publ_author_name 'Mani, Ganesan' 'Mondal, Munmun' _publ_section_title ; Copper(I) Complexes Bearing the Pyrrole-Bridged S,N and N-Donor Ligands as Catalysts for the Tandem Hydroamination-Alkynylation: Effect of Anions on Product Formation ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D4DT01937G _journal_year 2024 _chemical_formula_sum 'C47 H40 Cl2 N2 Ni P2' _chemical_formula_weight 824.36 _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_block_doi 10.5517/ccdc.csd.cc2h3pq1 _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-09-26 deposited with the CCDC. 2024-07-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.2620(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.4431(7) _cell_length_b 15.2942(6) _cell_length_c 17.7753(7) _cell_measurement_reflns_used 83247 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.087 _cell_measurement_theta_min 1.904 _cell_volume 4068.9(3) _computing_molecular_graphics ortep _computing_publication_material ciftab _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker-D8 Venture APEX3' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_unetI/netI 0.0422 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 83247 _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 27.087 _diffrn_reflns_theta_min 1.904 _diffrn_source 'Fine focused sealed tube' _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.346 _exptl_crystal_description prism _exptl_crystal_F_000 1712 _exptl_crystal_size_max 0.239 _exptl_crystal_size_mid 0.141 _exptl_crystal_size_min 0.076 _exptl_transmission_factor_max 0.7455 _exptl_transmission_factor_min 0.6896 _refine_diff_density_max 0.385 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.067 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 495 _refine_ls_number_reflns 8944 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0405 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+1.8519P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.0989 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6557 _reflns_number_total 8944 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4dt01937g2.cif _cod_data_source_block L1NiCl2 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7716734 _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 gm_rg_197_0m P -1 R = 0.05 New:P21/n shelx.res created by SHELXL-2018/3 at 10:44:07 on 12-Jun-2023 CELL 0.71073 15.4431 15.2942 17.7753 90.000 104.262 90.000 ZERR 4.00 0.0007 0.0006 0.0007 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H CL N NI P UNIT 188 160 8 8 4 8 MERG 2 OMIT 1 0 1 OMIT -9 1 2 HTAB N1 Cl1 HTAB N2 Cl2 HTAB C23 Cl2 HTAB N1 Cl1 HTAB N2 Cl2 FMAP 2 PLAN 20 ACTA HTAB 2.00000 BOND $H CONF L.S. 20 TEMP 23.00 WGHT 0.036500 1.851900 FVAR 0.33403 C1 1 -0.964745 0.144343 1.054985 11.00000 0.04066 0.04841 = 0.05690 0.00724 0.02156 0.00493 AFIX 23 H01C 2 -0.938652 0.108078 1.099576 11.00000 -1.20000 H01D 2 -1.029042 0.143591 1.048036 11.00000 -1.20000 AFIX 0 C2 1 -0.943107 0.105489 0.984815 11.00000 0.03693 0.03773 = 0.05641 0.00312 0.01655 0.00214 C3 1 -0.995671 0.086580 0.913348 11.00000 0.03180 0.05919 = 0.06180 0.00146 0.00544 0.00227 AFIX 43 H018 2 -1.057299 0.093815 0.897733 11.00000 -1.20000 AFIX 0 C4 1 -0.940770 0.054089 0.866867 11.00000 0.03945 0.05144 = 0.04485 -0.00162 0.00346 -0.00060 AFIX 43 H00U 2 -0.959778 0.036525 0.815335 11.00000 -1.20000 AFIX 0 C5 1 -0.854566 0.053027 0.911127 11.00000 0.03643 0.03624 = 0.04153 -0.00068 0.00886 -0.00074 C6 1 -0.769282 0.016678 0.894333 11.00000 0.03420 0.03808 = 0.03940 -0.00431 0.00804 -0.00048 C7 1 -0.752211 -0.078301 0.925350 11.00000 0.03524 0.03588 = 0.04711 -0.00653 0.00456 -0.00236 C8 1 -0.785278 -0.108917 0.986117 11.00000 0.05302 0.04869 = 0.05612 0.00540 0.01694 0.00793 AFIX 43 H01G 2 -0.818554 -0.071620 1.009367 11.00000 -1.20000 AFIX 0 C9 1 -0.769786 -0.194157 1.013066 11.00000 0.07165 0.05594 = 0.07647 0.01806 0.01828 0.00456 AFIX 43 H01W 2 -0.792735 -0.213397 1.053870 11.00000 -1.20000 AFIX 0 C10 1 -0.720648 -0.250002 0.979533 11.00000 0.06199 0.04319 = 0.09940 0.00968 0.00602 0.00666 AFIX 43 H027 2 -0.710657 -0.307308 0.997014 11.00000 -1.20000 AFIX 0 C11 1 -0.686510 -0.220457 0.920095 11.00000 0.06207 0.04602 = 0.10001 -0.01115 0.02380 0.00478 AFIX 43 H029 2 -0.652715 -0.257850 0.897454 11.00000 -1.20000 AFIX 0 C12 1 -0.701738 -0.135713 0.893417 11.00000 0.05609 0.04130 = 0.07427 -0.00816 0.02629 0.00189 AFIX 43 H01F 2 -0.677627 -0.116778 0.853194 11.00000 -1.20000 AFIX 0 C13 1 -0.780142 0.017886 0.805288 11.00000 0.03953 0.04822 = 0.03907 -0.00804 0.00649 0.00271 C14 1 -0.837120 -0.040906 0.757602 11.00000 0.05735 0.07706 = 0.04971 -0.01862 0.01033 -0.01665 AFIX 43 H01Y 2 -0.869733 -0.080504 0.779300 11.00000 -1.20000 AFIX 0 C15 1 -0.845880 -0.041164 0.677939 11.00000 0.06580 0.10503 = 0.05282 -0.03089 0.00270 -0.01083 AFIX 43 H02D 2 -0.885281 -0.080132 0.646867 11.00000 -1.20000 AFIX 0 C16 1 -0.797654 0.014774 0.644644 11.00000 0.08158 0.10004 = 0.03879 -0.00852 0.00638 0.01049 AFIX 43 H02C 2 -0.802649 0.013015 0.591446 11.00000 -1.20000 AFIX 0 C17 1 -0.741799 0.073554 0.690432 11.00000 0.08436 0.07553 = 0.04475 0.00574 0.01949 0.00501 AFIX 43 H01S 2 -0.709460 0.112798 0.668101 11.00000 -1.20000 AFIX 0 C18 1 -0.733003 0.075055 0.770313 11.00000 0.05779 0.05124 = 0.04167 -0.00203 0.01037 0.00088 AFIX 43 H017 2 -0.694619 0.115366 0.800660 11.00000 -1.20000 AFIX 0 C19 1 -0.688806 0.071391 0.933777 11.00000 0.03888 0.03438 = 0.03717 -0.00505 0.00883 0.00016 C20 1 -0.600153 0.050473 0.953488 11.00000 0.04108 0.03972 = 0.05254 -0.00667 0.00505 0.00426 AFIX 43 H00X 2 -0.576209 -0.004841 0.950503 11.00000 -1.20000 AFIX 0 C21 1 -0.551033 0.127378 0.979213 11.00000 0.03301 0.04756 = 0.04662 -0.00750 0.00555 0.00060 AFIX 43 H00K 2 -0.489195 0.131464 0.996171 11.00000 -1.20000 AFIX 0 C22 1 -0.609703 0.194062 0.974864 11.00000 0.03633 0.03997 = 0.03101 -0.00318 0.00970 -0.00250 C23 1 -0.595204 0.285408 1.005028 11.00000 0.04157 0.03932 = 0.03607 -0.00091 0.01088 -0.00562 AFIX 23 H01A 2 -0.629093 0.326000 0.967053 11.00000 -1.20000 H01B 2 -0.532426 0.300531 1.014668 11.00000 -1.20000 AFIX 0 C24 1 -0.545660 0.231929 1.164481 11.00000 0.04436 0.04399 = 0.03186 0.00030 0.00835 0.00714 C25 1 -0.548135 0.140957 1.164367 11.00000 0.05058 0.04793 = 0.04869 0.00379 0.01427 0.00633 AFIX 43 H01E 2 -0.594616 0.111470 1.130714 11.00000 -1.20000 AFIX 0 C26 1 -0.480741 0.094318 1.214839 11.00000 0.06887 0.05533 = 0.06159 0.01462 0.02453 0.02054 AFIX 43 H01M 2 -0.482078 0.033525 1.214399 11.00000 -1.20000 AFIX 0 C27 1 -0.412247 0.137273 1.265314 11.00000 0.06061 0.09114 = 0.04959 0.01076 0.00456 0.03164 AFIX 43 H01V 2 -0.367879 0.105688 1.299369 11.00000 -1.20000 AFIX 0 C28 1 -0.409548 0.227164 1.265285 11.00000 0.05502 0.08518 = 0.05385 -0.00871 -0.00775 0.01501 AFIX 43 H023 2 -0.363151 0.256250 1.299398 11.00000 -1.20000 AFIX 0 C29 1 -0.475065 0.274410 1.215100 11.00000 0.05223 0.05739 = 0.04822 -0.00747 -0.00018 0.00754 AFIX 43 H01L 2 -0.472109 0.335144 1.215037 11.00000 -1.20000 AFIX 0 C30 1 -0.618396 0.405923 1.128405 11.00000 0.04324 0.03692 = 0.04866 -0.00886 -0.00463 0.00464 C31 1 -0.591019 0.472183 1.087477 11.00000 0.06236 0.04058 = 0.08605 -0.00336 0.00577 -0.00444 AFIX 43 H01R 2 -0.572919 0.459902 1.042428 11.00000 -1.20000 AFIX 0 C32 1 -0.590583 0.558503 1.114173 11.00000 0.07501 0.03801 = 0.13918 -0.00380 -0.00712 -0.00571 AFIX 43 H02A 2 -0.572413 0.603662 1.086542 11.00000 -1.20000 AFIX 0 C33 1 -0.616950 0.576773 1.181165 11.00000 0.07502 0.05501 = 0.13959 -0.04958 -0.02318 0.01866 AFIX 43 H02E 2 -0.616922 0.634130 1.198543 11.00000 -1.20000 AFIX 0 C34 1 -0.642878 0.510900 1.221543 11.00000 0.07963 0.07551 = 0.08931 -0.04637 -0.01547 0.02737 AFIX 43 H02M 2 -0.660124 0.523442 1.266944 11.00000 -1.20000 AFIX 0 C35 1 -0.644127 0.425786 1.196528 11.00000 0.06683 0.05899 = 0.05877 -0.02251 -0.00081 0.01033 AFIX 43 H01U 2 -0.662129 0.381317 1.224980 11.00000 -1.20000 AFIX 0 C36 1 -0.947080 0.281250 1.168863 11.00000 0.07470 0.07644 = 0.04134 0.00235 0.02329 0.03168 C37 1 -0.890142 0.334016 1.219323 11.00000 0.09030 0.15037 = 0.06986 -0.04406 0.01130 0.03710 AFIX 43 H02R 2 -0.839574 0.355981 1.206330 11.00000 -1.20000 AFIX 0 C38 1 -0.907226 0.355609 1.291077 11.00000 0.16112 0.23808 = 0.06918 -0.05303 0.00865 0.09512 AFIX 43 H02Y 2 -0.868162 0.391437 1.325992 11.00000 -1.20000 AFIX 0 C39 1 -0.981777 0.323274 1.308612 11.00000 0.23635 0.18202 = 0.06219 0.01303 0.06768 0.12962 AFIX 43 H02W 2 -0.993124 0.336830 1.356284 11.00000 -1.20000 AFIX 0 C40 1 -1.040155 0.271576 1.258101 11.00000 0.20607 0.11867 = 0.11837 0.04512 0.12386 0.08029 AFIX 43 H030 2 -1.091331 0.251034 1.270982 11.00000 -1.20000 AFIX 0 C41 1 -1.023625 0.249616 1.187973 11.00000 0.11855 0.08014 = 0.08733 0.02230 0.07273 0.03923 AFIX 43 H02J 2 -1.063257 0.213866 1.153461 11.00000 -1.20000 AFIX 0 C42 1 -1.005696 0.324159 1.008059 11.00000 0.03922 0.04780 = 0.05555 0.01195 0.01349 0.00838 C43 1 -1.051772 0.390429 1.034813 11.00000 0.07380 0.05630 = 0.09020 0.01452 0.03114 0.02542 AFIX 43 H02H 2 -1.039917 0.403111 1.087536 11.00000 -1.20000 AFIX 0 C44 1 -1.115948 0.437604 0.981607 11.00000 0.08481 0.08232 = 0.15635 0.04676 0.04948 0.04794 AFIX 43 H02U 2 -1.147724 0.481537 0.999150 11.00000 -1.20000 AFIX 0 C45 1 -1.132825 0.420390 0.904437 11.00000 0.05574 0.12161 = 0.13594 0.07735 0.01176 0.02351 AFIX 43 H02P 2 -1.175989 0.452626 0.869761 11.00000 -1.20000 AFIX 0 C46 1 -1.086987 0.356095 0.877127 11.00000 0.06515 0.11009 = 0.07717 0.04109 -0.00484 -0.00178 AFIX 43 H02K 2 -1.099080 0.344187 0.824253 11.00000 -1.20000 AFIX 0 C47 1 -1.022556 0.309140 0.929101 11.00000 0.05915 0.06948 = 0.05667 0.01752 0.00755 0.00758 AFIX 43 H01X 2 -0.989927 0.266660 0.910656 11.00000 -1.20000 AFIX 0 CL1 3 -0.756744 0.169627 1.171992 11.00000 0.05085 0.08388 = 0.05942 0.03722 0.01450 0.00988 CL2 3 -0.801623 0.344887 0.976974 11.00000 0.05021 0.05404 = 0.04670 0.01704 0.01014 0.01031 N1 4 -0.856963 0.084719 0.982827 11.00000 0.03258 0.04165 = 0.04124 -0.00211 0.00545 0.00344 N2 4 -0.693728 0.160003 0.946307 11.00000 0.03239 0.03765 = 0.03786 -0.00425 0.00792 0.00294 NI1 5 -0.778312 0.265541 1.080338 11.00000 0.03908 0.03697 = 0.03102 0.00227 0.00831 0.00484 P1 6 -0.924458 0.257140 1.075528 11.00000 0.04152 0.04481 = 0.03679 0.00380 0.01499 0.01037 P2 6 -0.632030 0.292655 1.095964 11.00000 0.04067 0.03223 = 0.03152 -0.00243 0.00534 0.00122 H1 2 -0.816477 0.091154 1.018706 11.00000 0.03384 H2 2 -0.738609 0.186241 0.939264 11.00000 0.02925 HKLF 4 1.0 0.00 -1.00 0.00 1.00 0.00 0.00 0.00 0.00 1.00 REM gm_rg_197_0m P -1 R = 0.05 New:P21/n REM wR2 = 0.0989, GooF = S = 1.019, Restrained GooF = 1.019 for all data REM R1 = 0.0405 for 6557 Fo > 4sig(Fo) and 0.0647 for all 8944 data REM 495 parameters refined using 0 restraints END WGHT 0.0359 1.8044 REM Instructions for potential hydrogen bonds HTAB C23 Cl2 HTAB N1 Cl1 HTAB N2 Cl2 REM Highest difference peak 0.385, deepest hole -0.327, 1-sigma level 0.067 Q1 1 -0.9356 0.3810 1.3284 11.00000 0.05 0.39 Q2 1 -0.9146 0.3342 1.2962 11.00000 0.05 0.33 Q3 1 -0.9856 0.2816 1.2209 11.00000 0.05 0.33 Q4 1 -0.8577 0.2728 1.0805 11.00000 0.05 0.28 Q5 1 -1.0622 0.2621 1.2490 11.00000 0.05 0.27 Q6 1 -0.8604 0.3785 1.2110 11.00000 0.05 0.27 Q7 1 -0.7976 -0.2053 0.9749 11.00000 0.05 0.26 Q8 1 -0.8998 0.3256 1.2381 11.00000 0.05 0.25 Q9 1 -0.7030 0.2653 1.0846 11.00000 0.05 0.25 Q10 1 -1.0423 0.3506 1.0202 11.00000 0.05 0.24 Q11 1 -0.6754 -0.2411 0.9626 11.00000 0.05 0.24 Q12 1 -0.9221 0.2841 1.1183 11.00000 0.05 0.23 Q13 1 -0.8187 -0.2594 1.0176 11.00000 0.05 0.23 Q14 1 -0.8087 0.0397 0.9021 11.00000 0.05 0.22 Q15 1 -0.7253 -0.2141 1.0200 11.00000 0.05 0.22 Q16 1 -0.9224 0.4007 1.3866 11.00000 0.05 0.22 Q17 1 -0.8790 0.4147 1.2715 11.00000 0.05 0.22 Q18 1 -0.9930 0.2878 1.0372 11.00000 0.05 0.22 Q19 1 -0.8628 0.2981 1.2270 11.00000 0.05 0.22 Q20 1 -1.1001 0.2220 1.0639 11.00000 0.05 0.22 ; _shelx_res_checksum 43664 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 C1 C -0.96474(16) 0.14434(16) 1.05498(15) 0.0470(6) Uani 1 1 d . . . . . H01C H -0.938652 0.108078 1.099576 0.056 Uiso 1 1 calc R U . . . H01D H -1.029042 0.143591 1.048036 0.056 Uiso 1 1 calc R U . . . C2 C -0.94311(15) 0.10549(15) 0.98482(15) 0.0428(5) Uani 1 1 d . . . . . C3 C -0.99567(16) 0.08658(18) 0.91335(16) 0.0520(6) Uani 1 1 d . . . . . H018 H -1.057299 0.093815 0.897733 0.062 Uiso 1 1 calc R U . . . C4 C -0.94077(16) 0.05409(17) 0.86687(15) 0.0465(6) Uani 1 1 d . . . . . H00U H -0.959778 0.036525 0.815335 0.056 Uiso 1 1 calc R U . . . C5 C -0.85457(15) 0.05303(15) 0.91113(13) 0.0382(5) Uani 1 1 d . . . . . C6 C -0.76928(14) 0.01668(15) 0.89433(13) 0.0374(5) Uani 1 1 d . . . . . C7 C -0.75221(15) -0.07830(15) 0.92535(14) 0.0404(5) Uani 1 1 d . . . . . C8 C -0.78528(18) -0.10892(17) 0.98612(16) 0.0520(6) Uani 1 1 d . . . . . H01G H -0.818554 -0.071620 1.009367 0.062 Uiso 1 1 calc R U . . . C9 C -0.7698(2) -0.1942(2) 1.01307(19) 0.0680(8) Uani 1 1 d . . . . . H01W H -0.792735 -0.213397 1.053870 0.082 Uiso 1 1 calc R U . . . C10 C -0.7206(2) -0.25000(19) 0.9795(2) 0.0706(9) Uani 1 1 d . . . . . H027 H -0.710657 -0.307308 0.997014 0.085 Uiso 1 1 calc R U . . . C11 C -0.6865(2) -0.22046(19) 0.9201(2) 0.0687(9) Uani 1 1 d . . . . . H029 H -0.652715 -0.257850 0.897454 0.082 Uiso 1 1 calc R U . . . C12 C -0.70174(18) -0.13571(17) 0.89342(18) 0.0554(7) Uani 1 1 d . . . . . H01F H -0.677627 -0.116778 0.853194 0.067 Uiso 1 1 calc R U . . . C13 C -0.78014(16) 0.01789(16) 0.80529(14) 0.0428(6) Uani 1 1 d . . . . . C14 C -0.83712(19) -0.0409(2) 0.75760(16) 0.0619(8) Uani 1 1 d . . . . . H01Y H -0.869733 -0.080504 0.779300 0.074 Uiso 1 1 calc R U . . . C15 C -0.8459(2) -0.0412(3) 0.67794(18) 0.0766(10) Uani 1 1 d . . . . . H02D H -0.885281 -0.080132 0.646867 0.092 Uiso 1 1 calc R U . . . C16 C -0.7977(2) 0.0148(2) 0.64464(17) 0.0749(9) Uani 1 1 d . . . . . H02C H -0.802649 0.013015 0.591446 0.090 Uiso 1 1 calc R U . . . C17 C -0.7418(2) 0.0736(2) 0.69043(16) 0.0676(8) Uani 1 1 d . . . . . H01S H -0.709460 0.112798 0.668101 0.081 Uiso 1 1 calc R U . . . C18 C -0.73300(18) 0.07506(18) 0.77031(14) 0.0506(6) Uani 1 1 d . . . . . H017 H -0.694619 0.115366 0.800660 0.061 Uiso 1 1 calc R U . . . C19 C -0.68881(15) 0.07139(15) 0.93378(13) 0.0369(5) Uani 1 1 d . . . . . C20 C -0.60015(16) 0.05047(16) 0.95349(14) 0.0456(6) Uani 1 1 d . . . . . H00X H -0.576209 -0.004841 0.950503 0.055 Uiso 1 1 calc R U . . . C21 C -0.55103(15) 0.12738(16) 0.97921(14) 0.0431(6) Uani 1 1 d . . . . . H00K H -0.489195 0.131464 0.996171 0.052 Uiso 1 1 calc R U . . . C22 C -0.60970(14) 0.19406(15) 0.97486(12) 0.0355(5) Uani 1 1 d . . . . . C23 C -0.59520(16) 0.28541(15) 1.00503(13) 0.0388(5) Uani 1 1 d . . . . . H01A H -0.629093 0.326000 0.967053 0.047 Uiso 1 1 calc R U . . . H01B H -0.532426 0.300531 1.014668 0.047 Uiso 1 1 calc R U . . . C24 C -0.54566(16) 0.23193(16) 1.16448(13) 0.0403(5) Uani 1 1 d . . . . . C25 C -0.54814(17) 0.14096(17) 1.16437(15) 0.0487(6) Uani 1 1 d . . . . . H01E H -0.594616 0.111470 1.130714 0.058 Uiso 1 1 calc R U . . . C26 C -0.4807(2) 0.0943(2) 1.21484(17) 0.0604(7) Uani 1 1 d . . . . . H01M H -0.482078 0.033525 1.214399 0.073 Uiso 1 1 calc R U . . . C27 C -0.4122(2) 0.1373(2) 1.26531(17) 0.0687(9) Uani 1 1 d . . . . . H01V H -0.367879 0.105688 1.299369 0.082 Uiso 1 1 calc R U . . . C28 C -0.4095(2) 0.2272(2) 1.26528(17) 0.0684(9) Uani 1 1 d . . . . . H023 H -0.363151 0.256250 1.299398 0.082 Uiso 1 1 calc R U . . . C29 C -0.47506(18) 0.27441(19) 1.21510(15) 0.0548(7) Uani 1 1 d . . . . . H01L H -0.472109 0.335144 1.215037 0.066 Uiso 1 1 calc R U . . . C30 C -0.61840(16) 0.40592(16) 1.12840(14) 0.0457(6) Uani 1 1 d . . . . . C31 C -0.5910(2) 0.47218(18) 1.0875(2) 0.0652(8) Uani 1 1 d . . . . . H01R H -0.572919 0.459902 1.042428 0.078 Uiso 1 1 calc R U . . . C32 C -0.5906(2) 0.5585(2) 1.1142(3) 0.0899(12) Uani 1 1 d . . . . . H02A H -0.572413 0.603662 1.086542 0.108 Uiso 1 1 calc R U . . . C33 C -0.6170(3) 0.5768(3) 1.1812(3) 0.0986(15) Uani 1 1 d . . . . . H02E H -0.616922 0.634130 1.198543 0.118 Uiso 1 1 calc R U . . . C34 C -0.6429(2) 0.5109(3) 1.2215(2) 0.0878(12) Uani 1 1 d . . . . . H02M H -0.660124 0.523442 1.266944 0.105 Uiso 1 1 calc R U . . . C35 C -0.6441(2) 0.4258(2) 1.19653(17) 0.0644(8) Uani 1 1 d . . . . . H01U H -0.662129 0.381317 1.224980 0.077 Uiso 1 1 calc R U . . . C36 C -0.9471(2) 0.2812(2) 1.16886(16) 0.0626(8) Uani 1 1 d . . . . . C37 C -0.8901(3) 0.3340(3) 1.2193(2) 0.1050(15) Uani 1 1 d . . . . . H02R H -0.839574 0.355981 1.206330 0.126 Uiso 1 1 calc R U . . . C38 C -0.9072(4) 0.3556(4) 1.2911(3) 0.160(3) Uani 1 1 d . . . . . H02Y H -0.868162 0.391437 1.325992 0.191 Uiso 1 1 calc R U . . . C39 C -0.9818(6) 0.3233(5) 1.3086(3) 0.155(3) Uani 1 1 d . . . . . H02W H -0.993124 0.336830 1.356284 0.186 Uiso 1 1 calc R U . . . C40 C -1.0402(4) 0.2716(3) 1.2581(3) 0.133(2) Uani 1 1 d . . . . . H030 H -1.091331 0.251034 1.270982 0.160 Uiso 1 1 calc R U . . . C41 C -1.0236(3) 0.2496(2) 1.1880(2) 0.0871(12) Uani 1 1 d . . . . . H02J H -1.063257 0.213866 1.153461 0.104 Uiso 1 1 calc R U . . . C42 C -1.00570(16) 0.32416(17) 1.00806(15) 0.0472(6) Uani 1 1 d . . . . . C43 C -1.0518(2) 0.3904(2) 1.0348(2) 0.0715(9) Uani 1 1 d . . . . . H02H H -1.039917 0.403111 1.087536 0.086 Uiso 1 1 calc R U . . . C44 C -1.1159(3) 0.4376(3) 0.9816(3) 0.1044(15) Uani 1 1 d . . . . . H02U H -1.147724 0.481537 0.999150 0.125 Uiso 1 1 calc R U . . . C45 C -1.1328(2) 0.4204(3) 0.9044(3) 0.1065(16) Uani 1 1 d . . . . . H02P H -1.175989 0.452626 0.869761 0.128 Uiso 1 1 calc R U . . . C46 C -1.0870(2) 0.3561(3) 0.8771(2) 0.0881(12) Uani 1 1 d . . . . . H02K H -1.099080 0.344187 0.824253 0.106 Uiso 1 1 calc R U . . . C47 C -1.02256(19) 0.3091(2) 0.92910(17) 0.0629(8) Uani 1 1 d . . . . . H01X H -0.989927 0.266660 0.910656 0.076 Uiso 1 1 calc R U . . . Cl1 Cl -0.75674(5) 0.16963(5) 1.17199(4) 0.0646(2) Uani 1 1 d . . . . . Cl2 Cl -0.80162(4) 0.34489(4) 0.97697(4) 0.05063(16) Uani 1 1 d . . . . . N1 N -0.85696(13) 0.08472(13) 0.98283(12) 0.0391(4) Uani 1 1 d . . . . . N2 N -0.69373(13) 0.16000(13) 0.94631(11) 0.0361(4) Uani 1 1 d . . . . . Ni1 Ni -0.77831(2) 0.26554(2) 1.08034(2) 0.03575(9) Uani 1 1 d . . . . . P1 P -0.92446(4) 0.25714(4) 1.07553(4) 0.04011(15) Uani 1 1 d . . . . . P2 P -0.63203(4) 0.29265(4) 1.09596(3) 0.03543(14) Uani 1 1 d . . . . . H1 H -0.8165(16) 0.0912(15) 1.0187(14) 0.034(7) Uiso 1 1 d . . . . . H2 H -0.7386(15) 0.1862(15) 0.9393(13) 0.029(6) 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 C1 0.0407(13) 0.0484(15) 0.0569(15) 0.0072(12) 0.0216(12) 0.0049(11) C2 0.0369(13) 0.0377(13) 0.0564(15) 0.0031(11) 0.0166(11) 0.0021(10) C3 0.0318(13) 0.0592(17) 0.0618(17) 0.0015(13) 0.0054(12) 0.0023(11) C4 0.0395(13) 0.0514(15) 0.0448(14) -0.0016(11) 0.0035(11) -0.0006(11) C5 0.0364(12) 0.0362(12) 0.0415(13) -0.0007(10) 0.0089(10) -0.0007(10) C6 0.0342(12) 0.0381(12) 0.0394(12) -0.0043(10) 0.0080(10) -0.0005(9) C7 0.0352(12) 0.0359(13) 0.0471(14) -0.0065(10) 0.0046(10) -0.0024(10) C8 0.0530(16) 0.0487(15) 0.0561(16) 0.0054(12) 0.0169(13) 0.0079(12) C9 0.072(2) 0.0559(18) 0.076(2) 0.0181(16) 0.0183(16) 0.0046(15) C10 0.0620(19) 0.0432(17) 0.099(3) 0.0097(16) 0.0060(18) 0.0067(14) C11 0.0621(19) 0.0460(17) 0.100(3) -0.0111(16) 0.0238(17) 0.0048(14) C12 0.0561(16) 0.0413(15) 0.0743(19) -0.0082(13) 0.0263(14) 0.0019(12) C13 0.0395(13) 0.0482(14) 0.0391(13) -0.0080(10) 0.0065(10) 0.0027(11) C14 0.0574(17) 0.077(2) 0.0497(16) -0.0186(14) 0.0103(13) -0.0166(15) C15 0.066(2) 0.105(3) 0.0528(18) -0.0309(18) 0.0027(15) -0.0108(19) C16 0.082(2) 0.100(3) 0.0388(16) -0.0085(17) 0.0064(15) 0.010(2) C17 0.084(2) 0.076(2) 0.0448(16) 0.0057(15) 0.0195(15) 0.0050(17) C18 0.0578(16) 0.0512(15) 0.0417(14) -0.0020(11) 0.0104(12) 0.0009(12) C19 0.0389(12) 0.0344(12) 0.0372(12) -0.0050(9) 0.0088(10) 0.0002(10) C20 0.0411(13) 0.0397(13) 0.0525(15) -0.0067(11) 0.0051(11) 0.0043(10) C21 0.0330(12) 0.0476(14) 0.0466(14) -0.0075(11) 0.0055(10) 0.0006(10) C22 0.0363(12) 0.0400(13) 0.0310(11) -0.0032(9) 0.0097(9) -0.0025(10) C23 0.0416(13) 0.0393(13) 0.0361(12) -0.0009(10) 0.0109(10) -0.0056(10) C24 0.0444(13) 0.0440(13) 0.0319(12) 0.0003(10) 0.0083(10) 0.0071(10) C25 0.0506(15) 0.0479(15) 0.0487(15) 0.0038(12) 0.0143(12) 0.0063(12) C26 0.0689(19) 0.0553(17) 0.0616(18) 0.0146(14) 0.0245(15) 0.0205(15) C27 0.0606(19) 0.091(3) 0.0496(17) 0.0108(16) 0.0046(14) 0.0316(17) C28 0.0550(18) 0.085(2) 0.0539(18) -0.0087(16) -0.0078(14) 0.0150(16) C29 0.0522(16) 0.0574(17) 0.0482(15) -0.0075(13) -0.0002(12) 0.0075(13) C30 0.0432(14) 0.0369(13) 0.0487(14) -0.0089(11) -0.0046(11) 0.0046(10) C31 0.0624(18) 0.0406(16) 0.086(2) -0.0034(14) 0.0058(16) -0.0044(13) C32 0.075(2) 0.0380(17) 0.139(4) -0.004(2) -0.007(2) -0.0057(16) C33 0.075(2) 0.055(2) 0.140(4) -0.050(3) -0.023(2) 0.0187(19) C34 0.080(2) 0.076(3) 0.089(3) -0.046(2) -0.0155(19) 0.027(2) C35 0.0668(19) 0.0590(18) 0.0588(18) -0.0225(14) -0.0008(14) 0.0103(15) C36 0.075(2) 0.076(2) 0.0413(15) 0.0024(14) 0.0233(14) 0.0317(16) C37 0.090(3) 0.150(4) 0.070(2) -0.044(3) 0.011(2) 0.037(3) C38 0.161(5) 0.238(7) 0.069(3) -0.053(4) 0.009(3) 0.095(5) C39 0.236(8) 0.182(6) 0.062(3) 0.013(3) 0.068(4) 0.130(6) C40 0.206(6) 0.119(4) 0.118(4) 0.045(3) 0.124(4) 0.080(4) C41 0.119(3) 0.080(2) 0.087(2) 0.0223(19) 0.073(2) 0.039(2) C42 0.0392(13) 0.0478(15) 0.0556(15) 0.0119(12) 0.0135(11) 0.0084(11) C43 0.074(2) 0.0563(18) 0.090(2) 0.0145(16) 0.0311(18) 0.0254(16) C44 0.085(3) 0.082(3) 0.156(4) 0.047(3) 0.049(3) 0.048(2) C45 0.056(2) 0.122(4) 0.136(4) 0.077(3) 0.012(2) 0.024(2) C46 0.065(2) 0.110(3) 0.077(2) 0.041(2) -0.0048(18) -0.002(2) C47 0.0592(17) 0.069(2) 0.0567(17) 0.0175(15) 0.0076(14) 0.0076(15) Cl1 0.0508(4) 0.0839(5) 0.0594(4) 0.0372(4) 0.0145(3) 0.0099(4) Cl2 0.0502(4) 0.0540(4) 0.0467(3) 0.0170(3) 0.0101(3) 0.0103(3) N1 0.0326(11) 0.0416(11) 0.0412(11) -0.0021(9) 0.0055(9) 0.0034(9) N2 0.0324(10) 0.0376(11) 0.0379(10) -0.0043(8) 0.0079(8) 0.0029(9) Ni1 0.03908(17) 0.03697(16) 0.03102(15) 0.00227(12) 0.00831(12) 0.00484(12) P1 0.0415(3) 0.0448(4) 0.0368(3) 0.0038(3) 0.0150(3) 0.0104(3) P2 0.0407(3) 0.0322(3) 0.0315(3) -0.0024(2) 0.0053(2) 0.0012(2) 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' Cl Cl 0.1484 0.1585 '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_ _citation_id _citation_doi _citation_year 1 10.1039/D3DT03163B 2023 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 C2 C1 P1 113.89(17) . . ? C2 C1 H01C 108.8 . . ? P1 C1 H01C 108.8 . . ? C2 C1 H01D 108.8 . . ? P1 C1 H01D 108.8 . . ? H01C C1 H01D 107.7 . . ? C3 C2 N1 106.6(2) . . ? C3 C2 C1 131.4(2) . . ? N1 C2 C1 122.0(2) . . ? C2 C3 C4 108.4(2) . . ? C2 C3 H018 125.8 . . ? C4 C3 H018 125.8 . . ? C5 C4 C3 107.9(2) . . ? C5 C4 H00U 126.1 . . ? C3 C4 H00U 126.1 . . ? C4 C5 N1 106.5(2) . . ? C4 C5 C6 131.0(2) . . ? N1 C5 C6 122.18(19) . . ? C19 C6 C5 110.89(18) . . ? C19 C6 C13 109.58(18) . . ? C5 C6 C13 108.30(18) . . ? C19 C6 C7 107.66(18) . . ? C5 C6 C7 110.53(18) . . ? C13 C6 C7 109.87(19) . . ? C12 C7 C8 117.3(2) . . ? C12 C7 C6 120.7(2) . . ? C8 C7 C6 122.0(2) . . ? C7 C8 C9 121.4(3) . . ? C7 C8 H01G 119.3 . . ? C9 C8 H01G 119.3 . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H01W 120.0 . . ? C8 C9 H01W 120.0 . . ? C11 C10 C9 119.3(3) . . ? C11 C10 H027 120.4 . . ? C9 C10 H027 120.4 . . ? C10 C11 C12 120.7(3) . . ? C10 C11 H029 119.7 . . ? C12 C11 H029 119.7 . . ? C11 C12 C7 121.3(3) . . ? C11 C12 H01F 119.3 . . ? C7 C12 H01F 119.3 . . ? C18 C13 C14 117.4(2) . . ? C18 C13 C6 122.1(2) . . ? C14 C13 C6 120.5(2) . . ? C15 C14 C13 120.8(3) . . ? C15 C14 H01Y 119.6 . . ? C13 C14 H01Y 119.6 . . ? C16 C15 C14 121.0(3) . . ? C16 C15 H02D 119.5 . . ? C14 C15 H02D 119.5 . . ? C15 C16 C17 119.1(3) . . ? C15 C16 H02C 120.4 . . ? C17 C16 H02C 120.4 . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H01S 119.8 . . ? C18 C17 H01S 119.8 . . ? C13 C18 C17 121.3(3) . . ? C13 C18 H017 119.4 . . ? C17 C18 H017 119.4 . . ? C20 C19 N2 106.3(2) . . ? C20 C19 C6 130.1(2) . . ? N2 C19 C6 123.0(2) . . ? C19 C20 C21 108.2(2) . . ? C19 C20 H00X 125.9 . . ? C21 C20 H00X 125.9 . . ? C22 C21 C20 108.1(2) . . ? C22 C21 H00K 126.0 . . ? C20 C21 H00K 126.0 . . ? C21 C22 N2 107.1(2) . . ? C21 C22 C23 130.2(2) . . ? N2 C22 C23 122.1(2) . . ? C22 C23 P2 108.64(15) . . ? C22 C23 H01A 110.0 . . ? P2 C23 H01A 110.0 . . ? C22 C23 H01B 110.0 . . ? P2 C23 H01B 110.0 . . ? H01A C23 H01B 108.3 . . ? C29 C24 C25 119.0(2) . . ? C29 C24 P2 121.44(19) . . ? C25 C24 P2 119.53(19) . . ? C26 C25 C24 119.7(3) . . ? C26 C25 H01E 120.1 . . ? C24 C25 H01E 120.1 . . ? C27 C26 C25 120.6(3) . . ? C27 C26 H01M 119.7 . . ? C25 C26 H01M 119.7 . . ? C26 C27 C28 119.7(3) . . ? C26 C27 H01V 120.1 . . ? C28 C27 H01V 120.1 . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H023 119.8 . . ? C29 C28 H023 119.8 . . ? C28 C29 C24 120.5(3) . . ? C28 C29 H01L 119.8 . . ? C24 C29 H01L 119.8 . . ? C31 C30 C35 119.3(3) . . ? C31 C30 P2 124.1(2) . . ? C35 C30 P2 116.5(2) . . ? C30 C31 C32 119.5(3) . . ? C30 C31 H01R 120.3 . . ? C32 C31 H01R 120.3 . . ? C33 C32 C31 120.3(4) . . ? C33 C32 H02A 119.8 . . ? C31 C32 H02A 119.8 . . ? C34 C33 C32 119.7(3) . . ? C34 C33 H02E 120.1 . . ? C32 C33 H02E 120.1 . . ? C33 C34 C35 121.1(4) . . ? C33 C34 H02M 119.5 . . ? C35 C34 H02M 119.5 . . ? C34 C35 C30 120.1(3) . . ? C34 C35 H01U 119.9 . . ? C30 C35 H01U 119.9 . . ? C37 C36 C41 119.7(3) . . ? C37 C36 P1 119.1(3) . . ? C41 C36 P1 121.2(3) . . ? C36 C37 C38 120.3(5) . . ? C36 C37 H02R 119.9 . . ? C38 C37 H02R 119.9 . . ? C39 C38 C37 118.9(6) . . ? C39 C38 H02Y 120.6 . . ? C37 C38 H02Y 120.6 . . ? C38 C39 C40 121.5(4) . . ? C38 C39 H02W 119.3 . . ? C40 C39 H02W 119.3 . . ? C39 C40 C41 120.0(5) . . ? C39 C40 H030 120.0 . . ? C41 C40 H030 120.0 . . ? C40 C41 C36 119.6(5) . . ? C40 C41 H02J 120.2 . . ? C36 C41 H02J 120.2 . . ? C47 C42 C43 119.0(3) . . ? C47 C42 P1 120.1(2) . . ? C43 C42 P1 120.9(2) . . ? C42 C43 C44 119.0(4) . . ? C42 C43 H02H 120.5 . . ? C44 C43 H02H 120.5 . . ? C45 C44 C43 120.9(4) . . ? C45 C44 H02U 119.5 . . ? C43 C44 H02U 119.5 . . ? C44 C45 C46 120.7(3) . . ? C44 C45 H02P 119.7 . . ? C46 C45 H02P 119.7 . . ? C45 C46 C47 119.1(4) . . ? C45 C46 H02K 120.4 . . ? C47 C46 H02K 120.4 . . ? C46 C47 C42 121.2(3) . . ? C46 C47 H01X 119.4 . . ? C42 C47 H01X 119.4 . . ? C5 N1 C2 110.6(2) . . ? C5 N1 H1 127.1(17) . . ? C2 N1 H1 122.3(17) . . ? C22 N2 C19 110.35(19) . . ? C22 N2 H2 125.6(17) . . ? C19 N2 H2 124.0(17) . . ? Cl1 Ni1 Cl2 171.36(3) . . ? Cl1 Ni1 P1 87.51(3) . . ? Cl2 Ni1 P1 92.56(3) . . ? Cl1 Ni1 P2 93.94(3) . . ? Cl2 Ni1 P2 87.32(3) . . ? P1 Ni1 P2 171.19(3) . . ? C36 P1 C42 103.35(12) . . ? C36 P1 C1 103.89(14) . . ? C42 P1 C1 104.62(12) . . ? C36 P1 Ni1 111.85(11) . . ? C42 P1 Ni1 121.09(8) . . ? C1 P1 Ni1 110.46(8) . . ? C30 P2 C24 105.34(11) . . ? C30 P2 C23 107.34(12) . . ? C24 P2 C23 102.83(11) . . ? C30 P2 Ni1 104.42(8) . . ? C24 P2 Ni1 122.45(8) . . ? C23 P2 Ni1 113.48(8) . . ? 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 C1 C2 1.492(3) . ? C1 P1 1.840(3) . ? C1 H01C 0.9700 . ? C1 H01D 0.9700 . ? C2 C3 1.360(4) . ? C2 N1 1.377(3) . ? C3 C4 1.412(4) . ? C3 H018 0.9300 . ? C4 C5 1.369(3) . ? C4 H00U 0.9300 . ? C5 N1 1.373(3) . ? C5 C6 1.525(3) . ? C6 C19 1.519(3) . ? C6 C13 1.550(3) . ? C6 C7 1.553(3) . ? C7 C12 1.385(3) . ? C7 C8 1.385(3) . ? C8 C9 1.389(4) . ? C8 H01G 0.9300 . ? C9 C10 1.372(4) . ? C9 H01W 0.9300 . ? C10 C11 1.369(5) . ? C10 H027 0.9300 . ? C11 C12 1.380(4) . ? C11 H029 0.9300 . ? C12 H01F 0.9300 . ? C13 C18 1.380(4) . ? C13 C14 1.391(3) . ? C14 C15 1.389(4) . ? C14 H01Y 0.9300 . ? C15 C16 1.362(5) . ? C15 H02D 0.9300 . ? C16 C17 1.367(4) . ? C16 H02C 0.9300 . ? C17 C18 1.393(4) . ? C17 H01S 0.9300 . ? C18 H017 0.9300 . ? C19 C20 1.365(3) . ? C19 N2 1.379(3) . ? C20 C21 1.413(3) . ? C20 H00X 0.9300 . ? C21 C22 1.354(3) . ? C21 H00K 0.9300 . ? C22 N2 1.374(3) . ? C22 C23 1.493(3) . ? C23 P2 1.844(2) . ? C23 H01A 0.9700 . ? C23 H01B 0.9700 . ? C24 C29 1.392(3) . ? C24 C25 1.392(3) . ? C24 P2 1.823(2) . ? C25 C26 1.392(4) . ? C25 H01E 0.9300 . ? C26 C27 1.374(4) . ? C26 H01M 0.9300 . ? C27 C28 1.375(4) . ? C27 H01V 0.9300 . ? C28 C29 1.377(4) . ? C28 H023 0.9300 . ? C29 H01L 0.9300 . ? C30 C31 1.374(4) . ? C30 C35 1.398(4) . ? C30 P2 1.822(2) . ? C31 C32 1.402(4) . ? C31 H01R 0.9300 . ? C32 C33 1.379(6) . ? C32 H02A 0.9300 . ? C33 C34 1.354(6) . ? C33 H02E 0.9300 . ? C34 C35 1.374(4) . ? C34 H02M 0.9300 . ? C35 H01U 0.9300 . ? C36 C37 1.357(5) . ? C36 C41 1.395(5) . ? C36 P1 1.816(3) . ? C37 C38 1.404(6) . ? C37 H02R 0.9300 . ? C38 C39 1.358(9) . ? C38 H02Y 0.9300 . ? C39 C40 1.358(9) . ? C39 H02W 0.9300 . ? C40 C41 1.374(5) . ? C40 H030 0.9300 . ? C41 H02J 0.9300 . ? C42 C47 1.382(4) . ? C42 C43 1.388(4) . ? C42 P1 1.823(2) . ? C43 C44 1.391(5) . ? C43 H02H 0.9300 . ? C44 C45 1.357(6) . ? C44 H02U 0.9300 . ? C45 C46 1.369(6) . ? C45 H02P 0.9300 . ? C46 C47 1.381(4) . ? C46 H02K 0.9300 . ? C47 H01X 0.9300 . ? Cl1 Ni1 2.1563(7) . ? Cl2 Ni1 2.1569(6) . ? N1 H1 0.78(2) . ? N2 H2 0.78(2) . ? Ni1 P1 2.2411(7) . ? Ni1 P2 2.2457(7) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1 Cl1 0.78(2) 2.91(2) 3.581(2) 145(2) . yes N2 H2 Cl2 0.78(2) 2.76(2) 3.394(2) 140(2) . yes C23 H01A Cl2 0.97 2.73 3.233(2) 113.0 . yes N1 H1 Cl1 0.78(2) 2.91(2) 3.581(2) 145(2) . yes N2 H2 Cl2 0.78(2) 2.76(2) 3.394(2) 140(2) . yes 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 P1 C1 C2 C3 -108.0(3) . . . . ? P1 C1 C2 N1 69.2(3) . . . . ? N1 C2 C3 C4 -0.2(3) . . . . ? C1 C2 C3 C4 177.3(2) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? C3 C4 C5 N1 -0.4(3) . . . . ? C3 C4 C5 C6 173.3(2) . . . . ? C4 C5 C6 C19 147.4(3) . . . . ? N1 C5 C6 C19 -39.9(3) . . . . ? C4 C5 C6 C13 27.1(3) . . . . ? N1 C5 C6 C13 -160.1(2) . . . . ? C4 C5 C6 C7 -93.3(3) . . . . ? N1 C5 C6 C7 79.5(3) . . . . ? C19 C6 C7 C12 -83.3(3) . . . . ? C5 C6 C7 C12 155.4(2) . . . . ? C13 C6 C7 C12 36.0(3) . . . . ? C19 C6 C7 C8 95.9(3) . . . . ? C5 C6 C7 C8 -25.4(3) . . . . ? C13 C6 C7 C8 -144.9(2) . . . . ? C12 C7 C8 C9 -1.1(4) . . . . ? C6 C7 C8 C9 179.7(2) . . . . ? C7 C8 C9 C10 0.1(5) . . . . ? C8 C9 C10 C11 0.7(5) . . . . ? C9 C10 C11 C12 -0.6(5) . . . . ? C10 C11 C12 C7 -0.4(5) . . . . ? C8 C7 C12 C11 1.2(4) . . . . ? C6 C7 C12 C11 -179.6(2) . . . . ? C19 C6 C13 C18 -11.7(3) . . . . ? C5 C6 C13 C18 109.4(3) . . . . ? C7 C6 C13 C18 -129.8(2) . . . . ? C19 C6 C13 C14 166.8(2) . . . . ? C5 C6 C13 C14 -72.1(3) . . . . ? C7 C6 C13 C14 48.7(3) . . . . ? C18 C13 C14 C15 -0.2(4) . . . . ? C6 C13 C14 C15 -178.8(3) . . . . ? C13 C14 C15 C16 1.4(5) . . . . ? C14 C15 C16 C17 -1.9(5) . . . . ? C15 C16 C17 C18 1.3(5) . . . . ? C14 C13 C18 C17 -0.4(4) . . . . ? C6 C13 C18 C17 178.2(2) . . . . ? C16 C17 C18 C13 -0.1(5) . . . . ? C5 C6 C19 C20 158.6(2) . . . . ? C13 C6 C19 C20 -81.9(3) . . . . ? C7 C6 C19 C20 37.6(3) . . . . ? C5 C6 C19 N2 -31.4(3) . . . . ? C13 C6 C19 N2 88.1(2) . . . . ? C7 C6 C19 N2 -152.4(2) . . . . ? N2 C19 C20 C21 0.8(3) . . . . ? C6 C19 C20 C21 172.1(2) . . . . ? C19 C20 C21 C22 -0.1(3) . . . . ? C20 C21 C22 N2 -0.6(3) . . . . ? C20 C21 C22 C23 170.2(2) . . . . ? C21 C22 C23 P2 -100.8(3) . . . . ? N2 C22 C23 P2 68.8(2) . . . . ? C29 C24 C25 C26 0.4(4) . . . . ? P2 C24 C25 C26 177.92(19) . . . . ? C24 C25 C26 C27 0.6(4) . . . . ? C25 C26 C27 C28 -0.9(5) . . . . ? C26 C27 C28 C29 0.1(5) . . . . ? C27 C28 C29 C24 0.9(5) . . . . ? C25 C24 C29 C28 -1.2(4) . . . . ? P2 C24 C29 C28 -178.7(2) . . . . ? C35 C30 C31 C32 -0.9(4) . . . . ? P2 C30 C31 C32 174.2(2) . . . . ? C30 C31 C32 C33 0.3(5) . . . . ? C31 C32 C33 C34 0.4(5) . . . . ? C32 C33 C34 C35 -0.6(5) . . . . ? C33 C34 C35 C30 0.0(5) . . . . ? C31 C30 C35 C34 0.7(4) . . . . ? P2 C30 C35 C34 -174.7(2) . . . . ? C41 C36 C37 C38 1.1(6) . . . . ? P1 C36 C37 C38 178.3(4) . . . . ? C36 C37 C38 C39 -0.4(8) . . . . ? C37 C38 C39 C40 -0.7(9) . . . . ? C38 C39 C40 C41 1.2(8) . . . . ? C39 C40 C41 C36 -0.5(6) . . . . ? C37 C36 C41 C40 -0.6(5) . . . . ? P1 C36 C41 C40 -177.8(3) . . . . ? C47 C42 C43 C44 2.4(5) . . . . ? P1 C42 C43 C44 -177.3(3) . . . . ? C42 C43 C44 C45 -0.9(6) . . . . ? C43 C44 C45 C46 0.0(7) . . . . ? C44 C45 C46 C47 -0.5(6) . . . . ? C45 C46 C47 C42 2.0(5) . . . . ? C43 C42 C47 C46 -3.0(5) . . . . ? P1 C42 C47 C46 176.7(3) . . . . ? C4 C5 N1 C2 0.2(3) . . . . ? C6 C5 N1 C2 -174.1(2) . . . . ? C3 C2 N1 C5 0.0(3) . . . . ? C1 C2 N1 C5 -177.8(2) . . . . ? C21 C22 N2 C19 1.1(3) . . . . ? C23 C22 N2 C19 -170.61(19) . . . . ? C20 C19 N2 C22 -1.1(3) . . . . ? C6 C19 N2 C22 -173.2(2) . . . . ? C37 C36 P1 C42 -104.8(3) . . . . ? C41 C36 P1 C42 72.4(3) . . . . ? C37 C36 P1 C1 146.2(3) . . . . ? C41 C36 P1 C1 -36.6(3) . . . . ? C37 C36 P1 Ni1 27.0(3) . . . . ? C41 C36 P1 Ni1 -155.8(2) . . . . ? C47 C42 P1 C36 -165.6(2) . . . . ? C43 C42 P1 C36 14.0(3) . . . . ? C47 C42 P1 C1 -57.2(2) . . . . ? C43 C42 P1 C1 122.5(2) . . . . ? C47 C42 P1 Ni1 68.2(2) . . . . ? C43 C42 P1 Ni1 -112.1(2) . . . . ? C2 C1 P1 C36 -172.92(19) . . . . ? C2 C1 P1 C42 79.0(2) . . . . ? C2 C1 P1 Ni1 -52.8(2) . . . . ? C31 C30 P2 C24 112.9(2) . . . . ? C35 C30 P2 C24 -71.9(2) . . . . ? C31 C30 P2 C23 3.9(3) . . . . ? C35 C30 P2 C23 179.04(19) . . . . ? C31 C30 P2 Ni1 -116.9(2) . . . . ? C35 C30 P2 Ni1 58.3(2) . . . . ? C29 C24 P2 C30 -14.2(2) . . . . ? C25 C24 P2 C30 168.3(2) . . . . ? C29 C24 P2 C23 98.1(2) . . . . ? C25 C24 P2 C23 -79.4(2) . . . . ? C29 C24 P2 Ni1 -132.91(19) . . . . ? C25 C24 P2 Ni1 49.6(2) . . . . ? C22 C23 P2 C30 -177.31(15) . . . . ? C22 C23 P2 C24 71.88(18) . . . . ? C22 C23 P2 Ni1 -62.46(17) . . . . ?