#------------------------------------------------------------------------------ #$Date: 2024-10-06 10:06:31 +0300 (Sun, 06 Oct 2024) $ #$Revision: 295190 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572145.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_1572145 loop_ _publ_author_name 'Kreimer, Lisa N.' 'Hadlington, Terrance J.' _publ_section_title ; Macrocyclic bis-diphosphenes demonstrating bimetallic exo- and endo-cyclic binding modes. ; _journal_issue 35 _journal_name_full 'Chemical science' _journal_page_first 14154 _journal_page_last 14160 _journal_paper_doi 10.1039/d4sc03516j _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C72 H108 N4 Ni2 O4 P4' _chemical_formula_sum 'C72 H108 N4 Ni2 O4 P4' _chemical_formula_weight 1334.92 _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 _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 66.91(3) _cell_angle_beta 70.89(3) _cell_angle_gamma 76.79(3) _cell_formula_units_Z 1 _cell_length_a 9.912(2) _cell_length_b 14.075(3) _cell_length_c 15.094(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 1818.2(8) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (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 0.0886 _diffrn_reflns_av_unetI/netI 0.1514 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 24420 _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 25.998 _diffrn_reflns_theta_min 2.189 _diffrn_source 'Genix 3D HF Mo' _diffrn_source_current 1.000 _diffrn_source_power 0.050 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.760 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'STOE X-AREA 1.76' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.219 _exptl_crystal_description block _exptl_crystal_F_000 716 _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.396 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.079 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 404 _refine_ls_number_reflns 7148 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.964 _refine_ls_R_factor_all 0.1592 _refine_ls_R_factor_gt 0.0644 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0595P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1155 _refine_ls_wR_factor_ref 0.1483 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3550 _reflns_number_total 7148 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03516j2.cif _cod_data_source_block 3 _cod_depositor_comments 'Adding full bibliography for 1572143--1572150.cif.' _cod_original_cell_volume 1818.3(8) _cod_database_code 1572145 _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 ; REM Old TITL P-1 in P-1 REM SHELXT solution in P-1: R1 0.188, Rweak 0.030, Alpha 0.058 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C37 N2 O P2 Ni TITL C:\XRay\LNK007\P-1_a.res in P-1 C:\XRay\LNK007\P-1_a.res created by SHELXL-2018/3 at 11:04:59 on 22-Sep-2023 CELL 0.71073 9.9124 14.0747 15.0945 66.909 70.893 76.786 ZERR 1.0000 0.0020 0.0028 0.0030 0.030 0.030 0.030 LATT 1 SFAC C H N O P NI UNIT 72 108 4 4 4 2 MERG 2 OMIT -2 52 FMAP 2 GRID PLAN 20 TEMP -123 BOND L.S. 20 ACTA WGHT 0.059500 FVAR 0.58044 NI1 6 0.885280 0.451340 0.570295 11.00000 0.03107 0.03666 = 0.03714 -0.01210 -0.01440 -0.00752 P1 5 0.894850 0.539705 0.405949 11.00000 0.03158 0.03671 = 0.03587 -0.01295 -0.01567 -0.00614 P2 5 0.914304 0.432488 0.716866 11.00000 0.03505 0.03506 = 0.03764 -0.01053 -0.01462 -0.00535 O1 4 0.777206 0.624705 0.572696 11.00000 0.04070 0.03231 = 0.03727 -0.01169 -0.02117 -0.00018 N2 3 0.733133 0.283621 0.598081 11.00000 0.03750 0.03802 = 0.04145 -0.01026 -0.01651 -0.00910 N1 3 0.582225 0.394703 0.656620 11.00000 0.03172 0.04777 = 0.03690 -0.01190 -0.01514 -0.00993 C1 1 0.777112 0.705338 0.480698 11.00000 0.03110 0.03423 = 0.04120 -0.01187 -0.02104 0.00071 C12 1 0.862581 0.567630 0.716845 11.00000 0.03188 0.04209 = 0.02950 -0.01026 -0.01464 -0.00628 O2 4 0.594889 1.244656 -0.017348 11.00000 0.07527 0.09461 = 0.05808 -0.01477 -0.02566 -0.03835 C2 1 0.827602 0.676043 0.396462 11.00000 0.03248 0.03672 = 0.04080 -0.01600 -0.01487 -0.00933 C6 1 0.728125 0.806138 0.479184 11.00000 0.03320 0.03920 = 0.03937 -0.01787 -0.01643 -0.00086 C13 1 0.799881 0.648543 0.647443 11.00000 0.03363 0.03942 = 0.03437 -0.01808 -0.01229 -0.00330 C24 1 0.724857 0.375061 0.612371 11.00000 0.03090 0.03536 = 0.02915 -0.00190 -0.01503 -0.00708 C3 1 0.822791 0.755228 0.306709 11.00000 0.03211 0.03748 = 0.03965 -0.01327 -0.01252 -0.00799 AFIX 43 H3 2 0.854674 0.738213 0.247569 11.00000 -1.20000 AFIX 0 C7 1 0.674349 0.827520 0.577928 11.00000 0.03973 0.03272 = 0.04480 -0.01530 -0.02130 0.00075 C4 1 0.773734 0.858568 0.298332 11.00000 0.03311 0.04069 = 0.03820 -0.01311 -0.01767 -0.00428 C5 1 0.727008 0.882424 0.385857 11.00000 0.04227 0.02942 = 0.04099 -0.01058 -0.01885 -0.00006 AFIX 43 H5 2 0.693510 0.952451 0.381910 11.00000 -1.20000 AFIX 0 C11 1 0.885461 0.592419 0.790723 11.00000 0.03804 0.04488 = 0.04081 -0.01233 -0.01730 -0.00304 AFIX 43 H11 2 0.926965 0.538736 0.839525 11.00000 -1.20000 AFIX 0 C10 1 0.850973 0.691955 0.797618 11.00000 0.03507 0.04232 = 0.04211 -0.02075 -0.01521 -0.00066 C27 1 0.514212 0.488540 0.680858 11.00000 0.03339 0.05281 = 0.05355 -0.02461 -0.01424 -0.00874 AFIX 13 H27 2 0.590510 0.520121 0.686345 11.00000 -1.20000 AFIX 0 C9 1 0.784878 0.769058 0.726624 11.00000 0.04075 0.03786 = 0.05141 -0.01981 -0.02179 0.00245 AFIX 43 H9 2 0.757719 0.837020 0.730091 11.00000 -1.20000 AFIX 0 C8 1 0.758194 0.748148 0.651148 11.00000 0.03353 0.04048 = 0.04250 -0.01795 -0.01386 -0.00286 C20 1 0.887269 0.715256 0.877183 11.00000 0.04803 0.05173 = 0.03793 -0.01753 -0.02132 -0.00423 C14 1 0.769750 0.946043 0.197321 11.00000 0.04527 0.03240 = 0.04111 -0.00720 -0.02038 -0.00401 C30 1 0.866009 0.227588 0.555550 11.00000 0.04081 0.04201 = 0.06290 -0.01819 -0.02072 -0.00579 AFIX 13 H30 2 0.946431 0.268764 0.538858 11.00000 -1.20000 AFIX 0 C19 1 0.691679 0.940079 0.561029 11.00000 0.05653 0.03692 = 0.04709 -0.01727 -0.02438 0.00199 AFIX 137 H19A 2 0.793224 0.951259 0.531422 11.00000 -1.50000 H19B 2 0.657845 0.951579 0.625128 11.00000 -1.50000 H19C 2 0.634968 0.988854 0.515809 11.00000 -1.50000 AFIX 0 C26 1 0.598100 0.249292 0.630843 11.00000 0.04058 0.04352 = 0.04895 -0.00631 -0.02105 -0.01655 C17 1 0.614434 0.998783 0.199966 11.00000 0.05675 0.05640 = 0.04279 -0.01631 -0.02754 0.01218 AFIX 137 H17A 2 0.578965 1.028086 0.253677 11.00000 -1.50000 H17B 2 0.552687 0.947234 0.212053 11.00000 -1.50000 H17C 2 0.613057 1.054508 0.135846 11.00000 -1.50000 AFIX 0 C18 1 0.514607 0.809551 0.625358 11.00000 0.04274 0.05436 = 0.05236 -0.02245 -0.02436 0.00586 AFIX 137 H18A 2 0.458616 0.853351 0.577814 11.00000 -1.50000 H18B 2 0.478837 0.827606 0.686126 11.00000 -1.50000 H18C 2 0.504951 0.736288 0.642246 11.00000 -1.50000 AFIX 0 C25 1 0.504901 0.317922 0.667270 11.00000 0.03449 0.05067 = 0.04506 -0.00874 -0.01613 -0.01495 C32 1 0.860469 0.220368 0.459407 11.00000 0.05007 0.06396 = 0.06946 -0.03484 -0.01849 0.00008 AFIX 137 H32A 2 0.779386 0.183345 0.472857 11.00000 -1.50000 H32B 2 0.950222 0.182568 0.432060 11.00000 -1.50000 H32C 2 0.848210 0.290516 0.411039 11.00000 -1.50000 AFIX 0 C29 1 0.453189 0.566713 0.596672 11.00000 0.06139 0.05414 = 0.09505 -0.03443 -0.05200 0.01308 AFIX 137 H29A 2 0.529609 0.581488 0.534009 11.00000 -1.50000 H29B 2 0.413625 0.631114 0.611187 11.00000 -1.50000 H29C 2 0.376843 0.538124 0.590345 11.00000 -1.50000 AFIX 0 C15 1 0.823463 0.904945 0.109874 11.00000 0.06605 0.05173 = 0.04311 -0.01167 -0.01987 0.00447 AFIX 137 H15A 2 0.822870 0.963133 0.047150 11.00000 -1.50000 H15B 2 0.760243 0.855476 0.119371 11.00000 -1.50000 H15C 2 0.921551 0.869999 0.107298 11.00000 -1.50000 AFIX 0 C23 1 0.827982 0.825439 0.878393 11.00000 0.08376 0.06647 = 0.06488 -0.03507 -0.04098 -0.00482 AFIX 137 H23A 2 0.868201 0.876267 0.813202 11.00000 -1.50000 H23B 2 0.854825 0.836457 0.930336 11.00000 -1.50000 H23C 2 0.723014 0.834044 0.892414 11.00000 -1.50000 AFIX 0 C21 1 1.050618 0.703533 0.857044 11.00000 0.05928 0.08043 = 0.08080 -0.04217 -0.03714 -0.00042 AFIX 137 H21A 2 1.090111 0.632404 0.859167 11.00000 -1.50000 H21B 2 1.074957 0.717976 0.908098 11.00000 -1.50000 H21C 2 1.091517 0.752703 0.790957 11.00000 -1.50000 AFIX 0 C31 1 0.895980 0.122195 0.632220 11.00000 0.05894 0.05109 = 0.08157 -0.01421 -0.04032 0.00139 AFIX 137 H31A 2 0.908035 0.131841 0.689949 11.00000 -1.50000 H31B 2 0.984027 0.084834 0.602319 11.00000 -1.50000 H31C 2 0.815224 0.081882 0.653882 11.00000 -1.50000 AFIX 0 C16 1 0.864886 1.027015 0.177548 11.00000 0.09029 0.06016 = 0.05249 0.00581 -0.03236 -0.03804 AFIX 137 H16A 2 0.860470 1.083380 0.114286 11.00000 -1.50000 H16B 2 0.964302 0.994572 0.173623 11.00000 -1.50000 H16C 2 0.831131 1.055218 0.232005 11.00000 -1.50000 AFIX 0 C28 1 0.401290 0.462438 0.781220 11.00000 0.06230 0.09945 = 0.07398 -0.05205 0.00896 -0.02638 AFIX 137 H28A 2 0.319443 0.439222 0.775586 11.00000 -1.50000 H28B 2 0.368622 0.524398 0.800631 11.00000 -1.50000 H28C 2 0.443218 0.406917 0.831959 11.00000 -1.50000 AFIX 0 C35 1 0.656139 1.325678 -0.016520 11.00000 0.07374 0.10127 = 0.07234 -0.02946 -0.02874 -0.02557 AFIX 23 H35A 2 0.651981 1.387272 -0.077333 11.00000 -1.20000 H35B 2 0.758259 1.302911 -0.016352 11.00000 -1.20000 AFIX 0 C22 1 0.823079 0.639143 0.981091 11.00000 0.11030 0.07686 = 0.04423 -0.01741 -0.03029 -0.03133 AFIX 137 H22A 2 0.717968 0.650044 0.995906 11.00000 -1.50000 H22B 2 0.853041 0.651131 1.031256 11.00000 -1.50000 H22C 2 0.857217 0.567625 0.982498 11.00000 -1.50000 AFIX 0 C34 1 0.673689 1.205692 -0.095516 11.00000 0.07115 0.08655 = 0.06462 -0.01757 -0.02464 -0.01800 AFIX 23 H34A 2 0.771380 1.175704 -0.087522 11.00000 -1.20000 H34B 2 0.683101 1.263018 -0.160735 11.00000 -1.20000 AFIX 0 C36 1 0.576352 1.353467 0.073439 11.00000 0.11275 0.15334 = 0.07459 -0.05366 -0.01249 -0.05610 AFIX 137 H36A 2 0.474941 1.374542 0.073715 11.00000 -1.50000 H36B 2 0.617107 1.411097 0.072654 11.00000 -1.50000 H36C 2 0.584225 1.293145 0.133462 11.00000 -1.50000 AFIX 0 C33 1 0.597681 1.124144 -0.092842 11.00000 0.10273 0.09809 = 0.07283 -0.01330 -0.04406 -0.03666 AFIX 137 H33A 2 0.596724 1.064643 -0.030838 11.00000 -1.50000 H33B 2 0.647694 1.101473 -0.150194 11.00000 -1.50000 H33C 2 0.498695 1.152749 -0.095738 11.00000 -1.50000 AFIX 3 H25 2 0.391611 0.312415 0.708008 11.00000 0.06361 AFIX 3 H26 2 0.580701 0.175315 0.631008 11.00000 0.04625 AFIX 0 HKLF 4 REM C:\XRay\LNK007\P-1_a.res in P-1 REM wR2 = 0.1483, GooF = S = 0.964, Restrained GooF = 0.964 for all data REM R1 = 0.0644 for 3550 Fo > 4sig(Fo) and 0.1592 for all 7148 data REM 404 parameters refined using 0 restraints END WGHT 0.0593 0.0000 REM Highest difference peak 0.396, deepest hole -0.453, 1-sigma level 0.079 Q1 1 0.9573 0.4228 0.5539 11.00000 0.05 0.40 Q2 1 0.9142 0.4576 0.4801 11.00000 0.05 0.39 Q3 1 0.8593 0.3386 0.8380 11.00000 0.05 0.37 Q4 1 0.8339 0.5771 0.5403 11.00000 0.05 0.37 Q5 1 0.7931 0.6327 0.4045 11.00000 0.05 0.35 Q6 1 0.9126 0.5383 0.5553 11.00000 0.05 0.34 Q7 1 0.8609 0.4212 0.6692 11.00000 0.05 0.34 Q8 1 0.9212 0.4841 0.3337 11.00000 0.05 0.34 Q9 1 1.0011 0.3969 0.7019 11.00000 0.05 0.32 Q10 1 0.9791 0.0648 0.5350 11.00000 0.05 0.32 Q11 1 0.7178 0.9788 0.6663 11.00000 0.05 0.32 Q12 1 0.9271 0.3757 0.5119 11.00000 0.05 0.31 Q13 1 0.9049 0.7207 0.2305 11.00000 0.05 0.31 Q14 1 0.7381 0.4358 0.5970 11.00000 0.05 0.31 Q15 1 0.4710 1.3409 0.1284 11.00000 0.05 0.31 Q16 1 0.8742 0.3513 0.7411 11.00000 0.05 0.30 Q17 1 0.8294 1.2595 -0.2145 11.00000 0.05 0.30 Q18 1 0.8581 0.3942 0.6119 11.00000 0.05 0.30 Q19 1 0.8638 0.3465 0.6495 11.00000 0.05 0.30 Q20 1 0.9521 0.3642 0.6542 11.00000 0.05 0.30 ; _shelx_res_checksum 89617 _shelx_hkl_file ; -7 -7 7 -23.80 44.00 -7 -2 7 -5.80 45.90 -7 0 8 48.10 49.50 -7 1 9 -24.80 46.20 -7 2 10 34.40 49.90 -6 -7 4 36.40 34.80 -6 -1 5 214.08 43.20 -6 1 6 533.75 57.59 -6 5 10 -10.60 46.90 -5 7 10 73.99 44.60 -4 -13 4 -9.30 34.90 -4 -12 3 8.60 27.70 -4 1 3 66.99 36.20 -4 4 5 257.77 39.10 -3 1 2 178.18 30.60 -2 4 3 12.20 24.20 -1 12 10 43.70 31.60 0 14 12 29.80 26.00 1 -3 -1 1996.70 29.60 2 13 9 18.00 14.90 3 -11 0 68.49 26.40 6 4 2 341.87 38.60 -7 -8 7 8.60 47.20 -7 -4 6 -22.00 47.60 -7 -1 7 -32.40 50.39 -7 3 11 -56.19 49.40 -6 -8 4 15.80 35.00 -6 -3 4 74.39 41.10 -6 6 11 -29.60 48.60 -5 -10 3 13.70 31.70 -5 9 13 11.00 52.69 -4 -5 1 404.96 33.90 -4 10 12 -5.90 47.00 0 12 9 23.10 23.20 2 -13 1 29.50 20.60 2 -3 -1 675.33 26.70 3 -7 -1 209.08 26.50 -7 -3 6 24.00 48.50 -7 4 12 16.40 46.90 -6 -10 5 87.69 43.70 -5 1 4 22.00 38.80 -4 3 4 13.20 35.10 -4 9 10 33.80 37.00 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44.60 4 10 19 -51.79 45.40 4 13 16 32.50 42.40 4 14 14 48.00 45.20 5 0 -9 41.80 24.30 5 16 10 12.90 44.10 5 16 11 11.70 37.30 5 16 12 -45.40 39.10 5 16 13 -29.70 43.70 6 15 3 7.10 32.40 6 17 9 12.10 41.20 7 14 0 40.00 28.20 1 -8 3 22.80 22.00 1 -5 -4 156.18 27.80 1 -1 -4 11.60 16.80 2 -1 -6 683.93 30.70 2 10 12 19.10 43.10 3 3 18 -2.10 28.60 3 6 18 25.00 34.30 3 9 17 83.39 40.20 4 11 0 205.08 25.30 5 14 3 43.90 29.60 5 16 14 68.09 43.60 6 16 5 -11.30 33.30 6 17 8 21.70 46.70 0 -4 1 5.90 16.90 0 -2 7 255.17 14.00 0 3 3 40.10 21.50 0 3 7 1646.74 41.20 1 -1 12 108.79 20.70 1 8 6 8.10 33.60 1 8 7 75.29 35.30 1 8 8 351.06 41.60 2 -8 8 -9.00 20.00 2 10 4 39.70 31.00 3 2 18 -3.90 25.60 3 7 -3 8.30 11.40 3 12 14 208.58 45.80 3 13 8 392.36 49.20 3 13 9 18.90 35.40 3 13 11 75.99 42.30 4 13 17 -38.70 40.20 4 14 15 45.10 43.40 5 13 1 56.29 29.70 5 15 5 48.40 34.40 5 16 15 -30.60 42.80 6 14 1 26.70 27.50 7 16 3 5.90 30.80 0 -3 0 202.28 15.80 0 2 8 2194.88 44.30 1 -8 1 230.58 24.60 1 -8 2 -14.00 19.30 1 -7 -2 514.05 35.10 1 -4 -4 219.08 23.40 1 3 13 11.30 29.40 1 6 1 475.85 27.90 1 6 12 72.39 29.00 1 7 11 -20.90 30.80 1 8 5 173.38 39.20 1 8 9 186.58 36.20 2 -9 6 -10.10 22.70 2 -5 -6 9.90 24.70 2 3 16 -17.30 27.80 2 4 16 4.30 28.10 2 9 14 -40.30 32.60 2 10 13 76.99 42.00 2 11 8 -19.00 34.90 2 11 9 181.18 40.90 2 11 10 -29.90 38.50 3 0 -7 14.20 20.50 3 8 18 62.59 38.60 3 11 16 11.40 40.30 3 13 12 23.50 41.40 4 0 -8 251.17 28.90 4 11 19 40.70 46.30 4 13 3 21.90 26.40 4 15 10 4.40 43.90 4 15 11 4.40 40.70 4 15 12 2.90 43.20 0 -4 2 110.79 15.70 0 -4 3 -13.90 12.90 0 3 8 192.48 30.60 0 4 5 22.90 26.00 0 4 6 795.52 35.40 1 -3 -4 145.69 19.50 1 -2 -4 21.30 18.10 1 2 13 -20.50 23.70 1 4 13 131.09 29.60 1 8 10 0.60 35.90 2 -4 -6 300.17 29.40 2 -2 -6 237.58 24.10 2 6 16 3.60 30.40 2 11 11 52.09 36.80 3 9 -1 636.84 27.20 3 12 15 69.19 42.80 3 13 7 397.36 42.20 3 13 13 5.70 42.80 4 14 5 28.40 31.90 4 14 16 3.70 44.30 4 15 9 121.19 41.20 4 15 13 -9.30 43.20 5 16 7 62.19 40.40 6 17 7 98.29 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5 12.60 19.30 -1 7 6 2.00 24.00 0 -12 2 119.79 25.00 0 -11 1 128.19 22.00 0 -5 -1 177.88 15.60 1 -11 0 92.69 27.30 2 -13 1 28.40 29.00 2 -12 0 69.49 25.10 3 -9 -2 213.38 34.30 3 -1 -2 168.38 24.60 6 5 0 138.39 19.10 7 -11 -1 83.49 48.30 8 -10 -1 -16.50 49.30 8 -7 -2 72.49 49.10 10 -7 -1 -9.10 53.29 -1 5 4 108.09 23.50 2 -7 -2 69.79 31.70 2 -3 -2 -23.00 21.50 6 -9 -2 23.00 46.30 6 0 -2 15.80 28.00 7 -8 -2 25.00 46.40 8 -6 -2 83.49 46.00 8 -2 -2 67.39 40.60 9 4 0 0.20 26.70 9 6 1 61.29 28.50 10 -6 -1 66.09 53.69 10 3 0 68.39 37.30 -2 3 4 16.50 22.20 0 4 2 10.20 17.40 1 -12 1 17.50 24.80 3 -14 2 25.90 35.00 4 -9 -2 -18.90 31.20 5 -9 -2 14.00 39.40 7 -1 -2 195.08 37.20 8 -5 -2 50.39 46.70 8 -4 -2 38.40 48.50 8 -3 -2 304.27 48.60 9 -8 -1 44.20 52.39 10 -5 -1 108.69 58.29 10 -2 -1 186.18 55.19 11 1 0 52.89 43.80 11 4 1 32.40 40.60 12 5 2 -33.30 41.10 -3 3 6 349.27 27.70 2 -6 -2 -11.60 27.80 2 -4 -2 514.75 30.30 3 -12 0 9.30 31.60 3 -8 -2 65.39 31.00 6 -8 -2 63.19 41.50 7 -7 -2 77.19 43.90 8 -11 0 -21.40 46.10 8 -9 -1 18.70 50.39 10 -3 -1 148.89 51.49 12 2 1 -11.80 49.70 -3 0 4 242.48 20.40 1 -1 -1 1363.56 22.90 2 -5 -2 456.25 31.50 4 -1 -2 919.61 38.90 5 -8 -2 232.38 41.00 6 -1 -2 112.19 32.50 7 -6 -2 269.27 45.60 7 -2 -2 46.20 36.30 9 -7 -1 85.29 50.89 11 0 0 21.50 46.40 -8 10 -1 -6.50 19.00 -7 1 1 40.40 19.90 -4 -7 -2 1764.02 43.90 -4 11 0 30.40 21.10 -3 -5 -1 409.36 25.00 -3 -3 0 692.43 22.70 -3 9 1 245.48 22.70 -3 11 0 49.80 22.80 -2 14 -3 2.80 35.20 0 9 0 445.56 33.80 0 12 -2 116.49 36.90 0 14 -5 138.39 40.40 1 -12 -11 62.69 22.00 1 -10 -8 266.57 23.80 1 11 -2 56.89 28.30 1 12 -3 38.90 36.80 2 12 -5 -21.80 34.70 3 0 -3 129.29 16.10 3 8 -3 -1.20 30.70 3 11 -6 21.10 34.20 4 3 -4 257.07 28.90 4 5 -4 40.60 28.70 4 9 -7 100.99 40.60 5 -4 -13 2.90 21.00 5 2 -7 74.29 24.00 5 3 -7 24.20 22.80 -5 12 -1 20.00 25.20 -4 14 -3 -17.40 38.30 -3 14 -3 -5.10 38.10 -2 12 -1 8.90 24.90 -2 13 -2 -35.70 31.00 -1 7 1 74.09 21.70 -1 10 0 483.45 35.90 1 3 0 280.67 21.40 1 6 0 742.93 31.20 1 13 -5 106.29 37.70 2 6 -1 8.90 25.80 2 9 -2 120.29 28.80 3 10 -5 -9.10 34.80 3 11 -7 69.39 38.40 4 4 -4 131.99 25.20 4 7 -5 102.39 34.60 5 -4 -14 -22.80 23.50 5 -3 -11 46.10 20.80 5 0 -8 64.49 21.90 -8 -2 0 103.89 22.70 -7 -3 0 69.39 21.80 -7 9 0 8.60 17.30 -5 13 -2 22.50 28.40 -2 -9 -4 41.80 23.50 0 -12 -9 27.40 21.10 1 4 0 144.39 18.80 1 5 0 189.68 22.50 1 9 -1 441.46 33.50 2 3 -1 15.90 16.80 2 10 -3 37.60 29.10 3 9 -4 9.80 29.80 3 11 -8 -15.60 36.40 4 8 -6 74.49 33.60 4 9 -9 1.50 34.30 4 9 -8 -11.20 32.40 5 -2 -10 17.40 20.60 5 6 -11 -2.30 37.50 5 6 -10 28.20 31.70 -7 12 -2 15.60 23.40 -4 -1 1 230.38 19.80 -4 12 -1 8.10 26.30 -4 13 -2 1.80 29.60 -3 -7 -2 1316.77 39.20 -3 12 -1 33.50 24.00 -3 13 -2 27.10 30.90 -2 14 -4 -7.80 38.40 -1 -7 -3 1200.18 30.30 0 -6 -3 2123.99 32.80 1 12 -4 7.40 35.20 2 4 -1 317.57 24.50 2 5 -1 203.28 26.00 3 7 -3 -25.10 26.40 4 6 -5 134.89 32.80 5 1 -8 20.80 19.40 5 3 -8 182.78 29.00 5 4 -8 49.90 22.90 5 5 -9 96.49 33.90 -6 7 1 78.49 12.90 -1 6 1 751.62 25.40 -1 11 -1 28.00 25.40 0 8 0 348.77 29.50 0 10 -1 95.99 27.00 1 -11 -9 4.40 20.20 1 10 -2 171.58 31.70 1 11 -3 97.29 38.50 1 13 -7 41.60 34.90 2 11 -5 42.10 36.90 2 12 -8 -22.80 35.30 3 10 -6 -9.30 33.50 4 -5 -9 10.00 12.00 4 -3 -7 4.30 11.40 4 8 -7 297.47 42.00 5 -3 -12 16.30 21.20 5 2 -8 16.80 21.00 5 4 -9 98.39 28.30 5 5 -11 27.90 36.10 5 5 -10 -1.20 30.10 -7 0 1 180.18 23.20 -5 -4 0 19.40 16.00 -3 14 -4 48.20 38.40 -2 -8 -3 65.19 19.60 -1 -4 -1 81.29 19.40 0 11 -2 306.87 37.20 0 12 -3 58.49 33.80 0 13 -5 109.39 37.90 2 -8 -7 107.99 14.10 2 -7 -6 138.49 12.00 3 6 -3 396.66 34.50 3 8 -4 96.09 31.80 3 10 -7 43.90 35.30 4 5 -5 7.60 30.00 4 8 -8 179.68 38.40 5 -3 -13 6.30 20.10 5 4 -10 24.40 30.70 -6 -1 1 183.28 18.90 -6 11 -1 2.40 20.80 -5 10 0 38.80 22.40 -4 -6 -1 217.48 22.90 -4 -4 0 214.28 20.70 -4 8 1 19.40 14.30 -2 -5 -1 303.87 21.50 -2 13 -3 -29.20 33.40 -2 14 -5 -84.99 38.30 -1 9 0 415.96 28.50 1 8 -1 105.69 28.10 1 12 -5 99.29 37.00 2 -11 -11 41.70 17.20 2 9 -3 336.87 37.70 2 10 -4 2.90 29.90 2 11 -6 -29.50 35.10 3 1 -3 749.82 24.30 3 10 -8 30.90 37.00 4 -4 -8 23.90 11.90 4 4 -5 123.79 28.50 4 7 -7 171.68 37.50 4 8 -10 -11.30 36.10 5 -3 -14 15.50 21.50 5 -2 -11 7.00 20.80 5 -1 -10 16.10 23.10 5 1 -9 -0.90 21.40 5 2 -9 263.77 29.70 5 3 -9 77.59 27.20 5 4 -12 25.60 37.30 5 4 -11 19.80 32.80 -6 12 -2 -6.40 25.80 -4 10 0 40.60 21.00 -3 -1 1 4136.09 38.20 -3 10 0 18.10 22.10 -2 7 1 634.94 26.20 -2 12 -2 -5.50 28.20 -1 5 1 1886.11 28.00 0 13 -6 55.59 36.30 2 7 -2 33.20 27.10 3 5 -3 55.89 27.20 3 9 -6 9.10 32.00 3 10 -9 18.90 35.10 4 3 -5 361.26 30.20 4 6 -6 41.20 26.90 5 3 -11 9.10 30.20 5 3 -10 -3.80 28.80 -8 2 1 67.29 18.50 -8 3 1 101.09 14.30 -5 13 -3 -5.10 29.90 -4 13 -3 15.80 32.20 -3 13 -3 39.90 31.60 -2 0 1 1725.73 19.30 -1 -6 -2 278.27 19.60 0 7 0 380.16 27.50 0 12 -4 51.19 37.20 1 9 -2 133.49 30.70 1 12 -6 28.70 35.10 2 -9 -8 12.40 15.10 2 11 -7 -20.90 38.60 3 7 -4 24.40 25.40 4 -1 -6 221.88 17.80 4 7 -8 209.98 41.10 5 -2 -14 8.60 24.20 5 -2 -13 20.10 21.50 5 -2 -12 43.60 19.50 5 -1 -11 26.20 21.50 5 0 -10 48.40 21.20 5 1 -10 92.89 27.70 5 2 -10 138.39 29.20 5 3 -12 10.80 30.90 -10 2 0 24.40 16.80 -5 11 -1 8.80 23.40 -5 12 -2 3.20 27.20 -3 -6 -1 1288.67 35.80 -3 11 -1 4.60 21.50 -3 12 -2 106.59 29.90 -2 -7 -2 45.40 21.00 -2 13 -4 -36.50 35.30 -1 -2 0 16.80 14.70 -1 10 -1 195.78 31.30 -1 12 -3 65.49 31.20 -1 13 -5 28.80 35.20 0 -11 -7 75.89 23.20 0 -10 -6 90.99 18.50 0 -9 -5 59.39 17.30 0 13 -7 43.70 30.90 1 -12 -10 58.79 22.10 1 -5 -3 1488.95 23.40 1 7 -1 44.00 26.70 1 10 -3 124.79 30.50 1 12 -7 -5.90 34.70 2 -6 -5 159.98 10.70 2 10 -5 6.90 32.80 2 11 -9 -1.30 35.20 2 11 -8 3.30 35.00 3 2 -3 155.78 20.80 3 4 -3 -17.70 23.40 3 9 -7 78.99 35.50 4 5 -6 166.38 29.00 4 6 -7 -7.50 31.10 4 7 -9 22.10 32.10 5 -1 -12 7.40 22.80 5 0 -14 10.20 27.90 5 0 -11 6.00 24.60 5 1 -13 2.20 28.80 5 1 -11 125.99 30.80 5 2 -12 3.20 29.50 5 2 -11 15.70 27.80 -8 1 1 270.47 24.10 -7 -1 1 155.38 23.50 -5 -2 1 23.90 16.70 -4 11 -1 3.30 20.60 -4 12 -2 29.90 25.90 -3 -4 0 445.16 22.00 -1 -9 -4 158.88 21.50 0 10 -2 -10.30 25.30 0 11 -3 110.99 31.40 1 12 -8 3.40 33.40 2 6 -2 59.89 26.60 2 8 -3 15.70 25.60 2 9 -4 24.00 29.60 3 9 -8 4.60 35.60 5 -1 -13 27.40 25.30 5 0 -13 6.30 27.60 5 0 -12 -1.60 26.20 5 1 -12 12.50 27.30 -6 -2 1 259.17 20.70 -4 -2 1 2216.48 36.90 -1 8 0 236.68 24.20 -1 13 -6 48.20 39.60 0 -12 -8 81.09 22.10 0 -5 -2 580.24 19.90 0 -3 -1 5762.32 35.80 0 6 0 298.27 27.50 0 12 -5 236.78 43.80 1 11 -5 17.70 33.70 2 0 -2 468.05 16.90 2 10 -6 131.39 38.70 3 6 -4 82.39 28.00 3 8 -6 35.80 30.00 3 9 -10 7.60 32.00 3 9 -9 35.00 33.00 4 -7 -13 7.50 13.70 4 4 -6 211.38 26.80 4 6 -8 66.39 30.30 -7 11 -2 -17.70 20.00 -5 -5 0 -6.20 19.60 -5 7 1 64.79 13.20 -3 -8 -2 498.15 29.00 -3 13 -4 18.20 33.20 -2 6 1 181.18 17.60 1 6 -1 370.56 31.60 2 -10 -9 138.69 18.80 3 7 -5 134.79 31.50 4 3 -6 549.95 34.40 4 5 -7 -7.00 24.80 4 6 -12 -48.60 37.80 -8 0 1 368.56 26.60 -8 9 -1 4.10 17.40 -5 13 -4 40.30 35.50 -4 -5 0 57.59 21.80 -4 13 -4 1.50 38.50 -3 9 0 306.17 26.30 0 8 -1 661.93 38.10 0 11 -4 64.19 35.50 0 12 -6 149.09 39.20 1 -10 -7 483.65 28.20 1 8 -2 122.59 29.20 1 9 -3 334.07 36.50 1 10 -4 5.40 28.50 1 11 -6 138.39 38.00 2 5 -2 342.37 28.40 2 7 -3 41.40 27.20 2 9 -5 179.18 33.40 2 10 -8 1.40 35.70 3 -1 -4 24.80 14.00 3 8 -7 -2.50 34.00 4 -6 -11 28.10 13.50 4 -2 -7 10.90 12.70 -8 7 0 35.10 12.40 -7 -2 1 41.30 20.40 -7 8 0 11.70 15.50 -5 9 0 27.40 17.60 -3 12 -3 21.40 30.00 -2 -9 -3 123.39 25.50 -1 -8 -3 113.69 16.90 -1 9 -1 464.75 33.20 -1 11 -3 83.49 32.30 0 12 -7 10.30 34.10 1 -13 -11 41.60 22.50 1 -8 -5 173.48 18.20 1 11 -7 40.40 34.30 2 8 -4 -19.70 28.30 2 10 -10 8.20 32.30 2 10 -9 17.50 35.30 3 7 -6 58.69 30.90 3 8 -8 8.80 33.10 4 4 -7 85.49 25.40 4 5 -8 42.50 27.40 -8 -1 1 83.49 23.10 -6 10 -1 9.90 20.40 -6 12 -3 29.10 25.80 -4 9 0 392.36 26.50 -3 13 -5 49.60 33.30 -1 10 -2 196.98 31.30 0 5 0 46.80 20.00 0 10 -3 64.69 27.80 0 12 -8 10.60 34.20 1 -11 -8 -2.90 20.10 1 10 -5 102.09 37.50 1 11 -9 -7.40 36.10 2 4 -2 2.90 22.50 2 9 -6 136.69 33.60 3 6 -5 30.70 24.60 3 8 -11 -11.30 30.70 3 8 -10 -0.10 31.50 3 8 -9 21.30 32.80 4 5 -12 14.10 35.40 4 5 -11 0.50 32.40 -6 11 -2 31.40 23.70 -5 -3 1 60.99 18.90 -5 12 -3 10.70 28.30 -4 12 -3 2.90 28.50 -4 13 -5 102.69 39.40 -3 -2 1 359.66 18.60 -3 10 -1 11.50 22.00 -2 -6 -1 114.39 21.90 -1 7 0 479.05 27.80 0 -7 -3 1.10 15.40 0 11 -5 126.09 38.40 1 5 -1 109.69 24.00 2 1 -2 328.17 17.90 3 4 -4 25.60 24.50 3 7 -7 16.00 33.20 4 -3 -8 111.99 14.90 -5 10 -1 33.40 23.00 -5 11 -2 64.39 28.90 -4 10 -1 37.80 21.80 -4 11 -2 15.10 25.70 -3 -7 -1 457.95 27.80 -3 -5 0 420.16 26.80 -3 13 -6 -3.90 37.20 -2 -4 0 242.98 18.80 -1 -5 -1 197.48 16.90 -1 12 -6 41.80 34.40 1 7 -2 180.68 29.00 1 9 -4 74.49 32.50 2 2 -2 903.81 24.70 2 3 -2 59.89 19.10 2 6 -3 82.29 28.10 2 8 -5 76.19 29.20 3 3 -4 223.28 28.00 4 -5 -10 90.99 15.50 4 4 -13 31.90 34.20 -7 -3 1 155.68 25.50 -4 -3 1 360.36 21.10 -3 12 -4 -1.20 32.40 -2 -8 -2 63.49 20.10 -2 -1 1 3996.60 32.80 -2 5 1 539.65 18.90 -1 11 -4 -17.60 27.40 0 7 -1 168.38 24.80 0 11 -6 214.98 39.20 1 -12 -9 -14.00 19.90 1 8 -3 633.54 36.60 1 10 -6 196.78 36.50 2 -11 -10 193.78 20.70 2 7 -4 9.40 25.10 2 9 -11 5.00 31.10 2 9 -10 17.00 34.60 2 9 -8 12.90 32.10 3 0 -4 240.18 17.60 3 5 -5 61.09 26.20 3 6 -6 25.40 27.20 3 7 -8 -3.70 33.00 4 -4 -9 135.29 16.40 4 0 -7 356.26 25.70 4 4 -12 -3.50 31.50 4 4 -11 24.60 29.50 4 4 -10 8.90 29.80 -8 -2 1 7.90 18.00 -2 9 -1 475.95 33.60 -1 -7 -2 1413.76 32.90 -1 12 -7 35.20 34.50 0 4 0 183.28 16.50 0 10 -4 -15.40 28.60 1 10 -7 13.40 34.30 3 1 -4 0.30 19.20 3 2 -4 70.69 20.00 3 7 -10 -6.50 32.10 3 7 -9 42.40 32.60 -9 1 1 47.60 19.90 -4 -6 0 51.49 20.30 -4 12 -4 27.10 31.90 -1 8 -1 230.98 28.40 0 -11 -6 108.59 23.90 0 9 -3 9.40 29.10 0 11 -8 -1.70 36.20 0 11 -7 106.49 37.10 1 9 -5 88.29 35.20 1 10 -10 -24.60 36.50 1 10 -9 12.40 36.20 1 10 -8 58.79 35.40 2 5 -3 81.39 26.70 2 8 -6 192.48 33.00 3 6 -7 27.90 26.60 4 3 -13 6.00 32.40 -9 0 1 103.09 22.30 -7 11 -3 15.00 24.10 -5 -4 1 17.90 18.90 -5 12 -4 82.39 32.60 -3 11 -3 15.20 26.70 -3 12 -5 38.30 35.90 -1 -3 0 327.97 19.50 -1 9 -2 -25.70 28.00 -1 11 -5 3.70 32.60 0 -10 -5 185.38 21.00 0 11 -9 7.00 34.10 1 6 -2 120.69 27.00 2 7 -5 109.39 31.40 2 8 -7 22.90 35.60 3 5 -6 2.60 28.40 4 -2 -8 215.28 18.40 4 2 -14 8.10 34.20 4 3 -12 -6.00 27.40 4 3 -11 -5.60 28.40 4 3 -10 -2.30 21.80 -9 -1 1 70.39 22.50 -7 10 -2 10.40 19.50 -3 -3 1 1156.88 28.60 -2 12 -7 -2.60 33.60 -1 6 0 52.29 18.40 0 3 0 224.38 19.70 0 10 -5 69.59 31.20 1 0 -1 19.50 9.50 1 3 -1 270.97 19.60 1 8 -4 297.47 32.10 2 6 -4 -2.80 27.20 2 8 -8 13.00 33.60 3 6 -11 -1.60 32.40 3 6 -9 26.70 33.50 3 6 -8 24.00 27.40 4 -1 -8 350.16 23.60 4 0 -8 228.28 25.10 4 1 -8 39.50 22.60 4 2 -13 14.10 29.50 4 2 -9 139.49 27.20 -6 11 -3 9.30 26.60 -4 -4 1 199.38 22.50 -4 8 0 200.98 20.70 -4 11 -3 48.40 26.20 -4 12 -5 10.60 34.60 -3 10 -2 13.30 23.60 -2 7 0 16.70 18.90 -2 12 -8 6.30 32.80 -1 -9 -3 117.79 20.00 -1 11 -6 92.99 38.10 0 -6 -2 3058.09 38.80 0 6 -1 1426.76 39.00 1 7 -3 277.97 31.00 1 9 -6 183.08 31.80 2 8 -11 -8.50 31.00 2 8 -10 28.80 32.80 2 8 -9 -35.10 32.20 3 3 -5 -7.90 26.20 3 6 -10 -32.60 30.90 4 1 -14 42.50 33.20 4 2 -12 -22.70 30.10 4 2 -11 7.60 24.30 4 2 -10 72.99 25.80 -6 12 -5 31.60 33.10 -5 11 -3 47.20 27.90 -5 12 -5 123.19 37.20 -3 -6 0 8.10 20.50 -3 12 -6 -1.30 34.30 -2 -7 -1 713.53 28.90 -1 10 -4 14.70 27.30 -1 11 -7 98.69 37.50 0 -4 -1 1187.28 22.20 0 9 -4 58.79 34.00 0 10 -6 244.48 41.30 1 2 -1 975.20 23.70 1 9 -7 154.08 36.90 2 4 -3 108.79 24.90 2 7 -6 85.79 31.70 3 5 -7 35.60 25.50 -2 -5 0 572.34 26.80 -2 10 -3 266.97 30.30 -2 11 -5 22.40 29.70 0 10 -7 216.68 38.50 1 9 -8 44.10 32.70 3 4 -6 33.50 23.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 7578 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 0.88528(7) 0.45134(4) 0.57029(5) 0.0331(2) Uani 1 1 d . . . . . P1 P 0.89485(13) 0.53970(9) 0.40595(10) 0.0324(3) Uani 1 1 d . . . . . P2 P 0.91430(14) 0.43249(9) 0.71687(10) 0.0350(3) Uani 1 1 d . . . . . O1 O 0.7772(3) 0.6247(2) 0.5727(2) 0.0347(8) Uani 1 1 d . . . . . N2 N 0.7331(4) 0.2836(3) 0.5981(3) 0.0377(10) Uani 1 1 d . . . . . N1 N 0.5822(4) 0.3947(3) 0.6566(3) 0.0371(10) Uani 1 1 d . . . . . C1 C 0.7771(5) 0.7053(3) 0.4807(4) 0.0337(12) Uani 1 1 d . . . . . C12 C 0.8626(5) 0.5676(3) 0.7168(4) 0.0331(11) Uani 1 1 d . . . . . O2 O 0.5949(5) 1.2447(3) -0.0173(3) 0.0726(13) Uani 1 1 d . . . . . C2 C 0.8276(5) 0.6760(3) 0.3965(4) 0.0335(12) Uani 1 1 d . . . . . C6 C 0.7281(5) 0.8061(3) 0.4792(4) 0.0347(12) Uani 1 1 d . . . . . C13 C 0.7999(5) 0.6485(3) 0.6474(4) 0.0334(12) Uani 1 1 d . . . . . C24 C 0.7249(5) 0.3751(3) 0.6124(4) 0.0323(11) Uani 1 1 d . . . . . C3 C 0.8228(5) 0.7552(3) 0.3067(4) 0.0349(12) Uani 1 1 d . . . . . H3 H 0.854674 0.738213 0.247569 0.042 Uiso 1 1 calc R U . . . C7 C 0.6743(5) 0.8275(3) 0.5779(4) 0.0367(12) Uani 1 1 d . . . . . C4 C 0.7737(5) 0.8586(3) 0.2983(4) 0.0353(12) Uani 1 1 d . . . . . C5 C 0.7270(5) 0.8824(3) 0.3859(4) 0.0367(12) Uani 1 1 d . . . . . H5 H 0.693510 0.952451 0.381910 0.044 Uiso 1 1 calc R U . . . C11 C 0.8855(5) 0.5924(4) 0.7907(4) 0.0406(13) Uani 1 1 d . . . . . H11 H 0.926965 0.538736 0.839525 0.049 Uiso 1 1 calc R U . . . C10 C 0.8510(5) 0.6920(4) 0.7976(4) 0.0372(12) Uani 1 1 d . . . . . C27 C 0.5142(5) 0.4885(4) 0.6809(4) 0.0432(13) Uani 1 1 d . . . . . H27 H 0.590510 0.520121 0.686345 0.052 Uiso 1 1 calc R U . . . C9 C 0.7849(5) 0.7691(4) 0.7266(4) 0.0407(13) Uani 1 1 d . . . . . H9 H 0.757719 0.837020 0.730091 0.049 Uiso 1 1 calc R U . . . C8 C 0.7582(5) 0.7481(4) 0.6511(4) 0.0369(12) Uani 1 1 d . . . . . C20 C 0.8873(6) 0.7153(4) 0.8772(4) 0.0429(13) Uani 1 1 d . . . . . C14 C 0.7697(5) 0.9460(3) 0.1973(4) 0.0391(13) Uani 1 1 d . . . . . C30 C 0.8660(6) 0.2276(4) 0.5556(4) 0.0465(14) Uani 1 1 d . . . . . H30 H 0.946431 0.268764 0.538858 0.056 Uiso 1 1 calc R U . . . C19 C 0.6917(6) 0.9401(3) 0.5610(4) 0.0445(14) Uani 1 1 d . . . . . H19A H 0.793224 0.951259 0.531422 0.067 Uiso 1 1 calc R U . . . H19B H 0.657845 0.951579 0.625128 0.067 Uiso 1 1 calc R U . . . H19C H 0.634968 0.988854 0.515809 0.067 Uiso 1 1 calc R U . . . C26 C 0.5981(5) 0.2493(4) 0.6308(4) 0.0430(14) Uani 1 1 d . . . . . C17 C 0.6144(6) 0.9988(4) 0.2000(4) 0.0518(15) Uani 1 1 d . . . . . H17A H 0.578965 1.028086 0.253677 0.078 Uiso 1 1 calc R U . . . H17B H 0.552687 0.947234 0.212053 0.078 Uiso 1 1 calc R U . . . H17C H 0.613057 1.054508 0.135846 0.078 Uiso 1 1 calc R U . . . C18 C 0.5146(5) 0.8096(4) 0.6254(4) 0.0475(14) Uani 1 1 d . . . . . H18A H 0.458616 0.853351 0.577814 0.071 Uiso 1 1 calc R U . . . H18B H 0.478837 0.827606 0.686126 0.071 Uiso 1 1 calc R U . . . H18C H 0.504951 0.736288 0.642246 0.071 Uiso 1 1 calc R U . . . C25 C 0.5049(6) 0.3179(4) 0.6673(4) 0.0427(13) Uani 1 1 d . . . . . C32 C 0.8605(6) 0.2204(4) 0.4594(4) 0.0578(17) Uani 1 1 d . . . . . H32A H 0.779386 0.183345 0.472857 0.087 Uiso 1 1 calc R U . . . H32B H 0.950222 0.182568 0.432060 0.087 Uiso 1 1 calc R U . . . H32C H 0.848210 0.290516 0.411039 0.087 Uiso 1 1 calc R U . . . C29 C 0.4532(6) 0.5667(4) 0.5967(5) 0.0627(18) Uani 1 1 d . . . . . H29A H 0.529609 0.581488 0.534009 0.094 Uiso 1 1 calc R U . . . H29B H 0.413625 0.631114 0.611187 0.094 Uiso 1 1 calc R U . . . H29C H 0.376843 0.538124 0.590345 0.094 Uiso 1 1 calc R U . . . C15 C 0.8235(6) 0.9049(4) 0.1099(4) 0.0557(16) Uani 1 1 d . . . . . H15A H 0.822870 0.963133 0.047150 0.084 Uiso 1 1 calc R U . . . H15B H 0.760243 0.855476 0.119371 0.084 Uiso 1 1 calc R U . . . H15C H 0.921551 0.869999 0.107298 0.084 Uiso 1 1 calc R U . . . C23 C 0.8280(7) 0.8254(4) 0.8784(5) 0.0628(17) Uani 1 1 d . . . . . H23A H 0.868201 0.876267 0.813202 0.094 Uiso 1 1 calc R U . . . H23B H 0.854825 0.836457 0.930336 0.094 Uiso 1 1 calc R U . . . H23C H 0.723014 0.834044 0.892414 0.094 Uiso 1 1 calc R U . . . C21 C 1.0506(6) 0.7035(5) 0.8570(5) 0.0654(18) Uani 1 1 d . . . . . H21A H 1.090111 0.632404 0.859167 0.098 Uiso 1 1 calc R U . . . H21B H 1.074957 0.717976 0.908098 0.098 Uiso 1 1 calc R U . . . H21C H 1.091517 0.752703 0.790957 0.098 Uiso 1 1 calc R U . . . C31 C 0.8960(6) 0.1222(4) 0.6322(5) 0.0624(18) Uani 1 1 d . . . . . H31A H 0.908035 0.131841 0.689949 0.094 Uiso 1 1 calc R U . . . H31B H 0.984027 0.084834 0.602319 0.094 Uiso 1 1 calc R U . . . H31C H 0.815224 0.081882 0.653882 0.094 Uiso 1 1 calc R U . . . C16 C 0.8649(7) 1.0270(4) 0.1775(4) 0.0671(19) Uani 1 1 d . . . . . H16A H 0.860470 1.083380 0.114286 0.101 Uiso 1 1 calc R U . . . H16B H 0.964302 0.994572 0.173623 0.101 Uiso 1 1 calc R U . . . H16C H 0.831131 1.055218 0.232005 0.101 Uiso 1 1 calc R U . . . C28 C 0.4013(7) 0.4624(5) 0.7812(5) 0.075(2) Uani 1 1 d . . . . . H28A H 0.319443 0.439222 0.775586 0.113 Uiso 1 1 calc R U . . . H28B H 0.368622 0.524398 0.800631 0.113 Uiso 1 1 calc R U . . . H28C H 0.443218 0.406917 0.831959 0.113 Uiso 1 1 calc R U . . . C35 C 0.6561(7) 1.3257(5) -0.0165(5) 0.077(2) Uani 1 1 d . . . . . H35A H 0.651981 1.387272 -0.077333 0.093 Uiso 1 1 calc R U . . . H35B H 0.758259 1.302911 -0.016352 0.093 Uiso 1 1 calc R U . . . C22 C 0.8231(7) 0.6391(4) 0.9811(4) 0.072(2) Uani 1 1 d . . . . . H22A H 0.717968 0.650044 0.995906 0.108 Uiso 1 1 calc R U . . . H22B H 0.853041 0.651131 1.031256 0.108 Uiso 1 1 calc R U . . . H22C H 0.857217 0.567625 0.982498 0.108 Uiso 1 1 calc R U . . . C34 C 0.6737(7) 1.2057(5) -0.0955(5) 0.0735(19) Uani 1 1 d . . . . . H34A H 0.771380 1.175704 -0.087522 0.088 Uiso 1 1 calc R U . . . H34B H 0.683101 1.263018 -0.160735 0.088 Uiso 1 1 calc R U . . . C36 C 0.5764(9) 1.3535(6) 0.0734(6) 0.105(3) Uani 1 1 d . . . . . H36A H 0.474941 1.374542 0.073715 0.157 Uiso 1 1 calc R U . . . H36B H 0.617107 1.411097 0.072654 0.157 Uiso 1 1 calc R U . . . H36C H 0.584225 1.293145 0.133462 0.157 Uiso 1 1 calc R U . . . C33 C 0.5977(8) 1.1241(5) -0.0928(5) 0.087(2) Uani 1 1 d . . . . . H33A H 0.596724 1.064643 -0.030838 0.130 Uiso 1 1 calc R U . . . H33B H 0.647694 1.101473 -0.150194 0.130 Uiso 1 1 calc R U . . . H33C H 0.498695 1.152749 -0.095738 0.130 Uiso 1 1 calc R U . . . H25 H 0.391611 0.312415 0.708008 0.064(16) Uiso 1 1 d R . . . . H26 H 0.580701 0.175315 0.631008 0.046(14) 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 0.0311(4) 0.0367(3) 0.0371(4) -0.0121(3) -0.0144(3) -0.0075(3) P1 0.0316(7) 0.0367(7) 0.0359(8) -0.0129(6) -0.0157(6) -0.0061(5) P2 0.0351(8) 0.0351(7) 0.0376(9) -0.0105(6) -0.0146(6) -0.0053(6) O1 0.041(2) 0.0323(17) 0.037(2) -0.0117(15) -0.0212(16) -0.0002(14) N2 0.038(3) 0.038(2) 0.041(3) -0.010(2) -0.017(2) -0.0091(19) N1 0.032(2) 0.048(2) 0.037(3) -0.012(2) -0.015(2) -0.0099(19) C1 0.031(3) 0.034(3) 0.041(3) -0.012(2) -0.021(2) 0.001(2) C12 0.032(3) 0.042(3) 0.029(3) -0.010(2) -0.015(2) -0.006(2) O2 0.075(3) 0.095(3) 0.058(3) -0.015(3) -0.026(3) -0.038(3) C2 0.032(3) 0.037(3) 0.041(3) -0.016(2) -0.015(2) -0.009(2) C6 0.033(3) 0.039(3) 0.039(3) -0.018(2) -0.016(2) -0.001(2) C13 0.034(3) 0.039(3) 0.034(3) -0.018(2) -0.012(2) -0.003(2) C24 0.031(3) 0.035(3) 0.029(3) -0.002(2) -0.015(2) -0.007(2) C3 0.032(3) 0.037(3) 0.040(3) -0.013(2) -0.013(2) -0.008(2) C7 0.040(3) 0.033(3) 0.045(3) -0.015(2) -0.021(3) 0.001(2) C4 0.033(3) 0.041(3) 0.038(3) -0.013(2) -0.018(2) -0.004(2) C5 0.042(3) 0.029(2) 0.041(3) -0.011(2) -0.019(3) 0.000(2) C11 0.038(3) 0.045(3) 0.041(4) -0.012(2) -0.017(3) -0.003(2) C10 0.035(3) 0.042(3) 0.042(3) -0.021(2) -0.015(2) -0.001(2) C27 0.033(3) 0.053(3) 0.054(4) -0.025(3) -0.014(3) -0.009(2) C9 0.041(3) 0.038(3) 0.051(4) -0.020(3) -0.022(3) 0.002(2) C8 0.034(3) 0.040(3) 0.042(3) -0.018(2) -0.014(2) -0.003(2) C20 0.048(3) 0.052(3) 0.038(3) -0.018(3) -0.021(3) -0.004(3) C14 0.045(3) 0.032(3) 0.041(3) -0.007(2) -0.020(3) -0.004(2) C30 0.041(3) 0.042(3) 0.063(4) -0.018(3) -0.021(3) -0.006(2) C19 0.057(4) 0.037(3) 0.047(4) -0.017(2) -0.024(3) 0.002(2) C26 0.041(3) 0.044(3) 0.049(4) -0.006(3) -0.021(3) -0.017(3) C17 0.057(4) 0.056(3) 0.043(4) -0.016(3) -0.028(3) 0.012(3) C18 0.043(3) 0.054(3) 0.052(4) -0.022(3) -0.024(3) 0.006(3) C25 0.034(3) 0.051(3) 0.045(4) -0.009(3) -0.016(3) -0.015(3) C32 0.050(4) 0.064(4) 0.069(5) -0.035(3) -0.018(3) 0.000(3) C29 0.061(4) 0.054(3) 0.095(5) -0.034(3) -0.052(4) 0.013(3) C15 0.066(4) 0.052(3) 0.043(4) -0.012(3) -0.020(3) 0.004(3) C23 0.084(5) 0.066(4) 0.065(5) -0.035(3) -0.041(4) -0.005(3) C21 0.059(4) 0.080(4) 0.081(5) -0.042(4) -0.037(4) 0.000(3) C31 0.059(4) 0.051(3) 0.082(5) -0.014(3) -0.040(4) 0.001(3) C16 0.090(5) 0.060(4) 0.052(4) 0.006(3) -0.032(4) -0.038(3) C28 0.062(4) 0.099(5) 0.074(5) -0.052(4) 0.009(4) -0.026(4) C35 0.074(5) 0.101(5) 0.072(5) -0.029(4) -0.029(4) -0.026(4) C22 0.110(6) 0.077(4) 0.044(4) -0.017(3) -0.030(4) -0.031(4) C34 0.071(5) 0.087(5) 0.065(5) -0.018(4) -0.025(4) -0.018(4) C36 0.113(7) 0.153(7) 0.075(6) -0.054(6) -0.012(5) -0.056(6) C33 0.103(6) 0.098(5) 0.073(5) -0.013(4) -0.044(5) -0.037(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 C24 Ni1 P2 101.22(15) . . ? C24 Ni1 P1 101.52(15) . . ? P2 Ni1 P1 153.45(5) . . ? C24 Ni1 P1 147.39(14) . 2_766 ? P2 Ni1 P1 55.92(6) . 2_766 ? P1 Ni1 P1 107.43(6) . 2_766 ? C24 Ni1 Ni1 152.84(15) . 2_766 ? P2 Ni1 Ni1 105.11(5) . 2_766 ? P1 Ni1 Ni1 55.09(5) . 2_766 ? P1 Ni1 Ni1 52.34(4) 2_766 2_766 ? C2 P1 P2 98.32(17) . 2_766 ? C2 P1 Ni1 105.59(17) . . ? P2 P1 Ni1 126.69(7) 2_766 . ? C2 P1 Ni1 93.20(16) . 2_766 ? P2 P1 Ni1 58.98(5) 2_766 2_766 ? Ni1 P1 Ni1 72.57(6) . 2_766 ? C12 P2 P1 97.49(16) . 2_766 ? C12 P2 Ni1 100.92(16) . . ? P1 P2 Ni1 65.10(6) 2_766 . ? C13 O1 C1 117.7(4) . . ? C24 N2 C26 111.2(4) . . ? C24 N2 C30 124.8(4) . . ? C26 N2 C30 124.0(4) . . ? C24 N1 C25 111.1(4) . . ? C24 N1 C27 125.5(4) . . ? C25 N1 C27 123.1(4) . . ? C6 C1 C2 124.7(5) . . ? C6 C1 O1 119.3(4) . . ? C2 C1 O1 116.0(4) . . ? C11 C12 C13 116.1(4) . . ? C11 C12 P2 119.1(4) . . ? C13 C12 P2 124.8(4) . . ? C35 O2 C34 113.5(5) . . ? C3 C2 C1 115.6(4) . . ? C3 C2 P1 123.0(4) . . ? C1 C2 P1 121.4(4) . . ? C1 C6 C5 116.7(5) . . ? C1 C6 C7 119.3(4) . . ? C5 C6 C7 124.0(4) . . ? C8 C13 O1 119.9(4) . . ? C8 C13 C12 123.5(5) . . ? O1 C13 C12 116.6(4) . . ? N2 C24 N1 103.5(4) . . ? N2 C24 Ni1 123.9(3) . . ? N1 C24 Ni1 132.5(3) . . ? C2 C3 C4 123.6(5) . . ? C6 C7 C8 108.6(4) . . ? C6 C7 C18 109.6(4) . . ? C8 C7 C18 106.8(4) . . ? C6 C7 C19 111.0(4) . . ? C8 C7 C19 111.2(4) . . ? C18 C7 C19 109.5(4) . . ? C3 C4 C5 117.6(5) . . ? C3 C4 C14 122.8(5) . . ? C5 C4 C14 119.6(4) . . ? C4 C5 C6 121.9(4) . . ? C12 C11 C10 123.9(5) . . ? C11 C10 C9 116.9(5) . . ? C11 C10 C20 121.1(5) . . ? C9 C10 C20 122.0(4) . . ? N1 C27 C29 109.8(4) . . ? N1 C27 C28 111.2(4) . . ? C29 C27 C28 112.4(5) . . ? C8 C9 C10 121.6(4) . . ? C13 C8 C9 118.0(5) . . ? C13 C8 C7 118.8(4) . . ? C9 C8 C7 123.1(4) . . ? C10 C20 C21 108.9(4) . . ? C10 C20 C23 112.8(4) . . ? C21 C20 C23 108.3(5) . . ? C10 C20 C22 110.0(4) . . ? C21 C20 C22 109.5(5) . . ? C23 C20 C22 107.3(5) . . ? C16 C14 C15 108.2(5) . . ? C16 C14 C17 109.0(4) . . ? C15 C14 C17 107.9(4) . . ? C16 C14 C4 109.5(4) . . ? C15 C14 C4 112.1(4) . . ? C17 C14 C4 110.0(4) . . ? N2 C30 C32 110.6(4) . . ? N2 C30 C31 110.3(5) . . ? C32 C30 C31 113.0(5) . . ? C25 C26 N2 107.0(4) . . ? C26 C25 N1 107.2(4) . . ? O2 C35 C36 109.7(6) . . ? O2 C34 C33 109.5(6) . . ? 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 C24 1.916(5) . ? Ni1 P2 2.2292(16) . ? Ni1 P1 2.2781(17) . ? Ni1 P1 2.3594(15) 2_766 ? Ni1 Ni1 2.7453(18) 2_766 ? P1 C2 1.846(4) . ? P1 P2 2.155(2) 2_766 ? P2 C12 1.853(5) . ? O1 C13 1.391(5) . ? O1 C1 1.407(5) . ? N2 C24 1.367(6) . ? N2 C26 1.394(6) . ? N2 C30 1.462(6) . ? N1 C24 1.367(6) . ? N1 C25 1.394(6) . ? N1 C27 1.464(6) . ? C1 C6 1.384(6) . ? C1 C2 1.392(6) . ? C12 C11 1.387(6) . ? C12 C13 1.396(6) . ? O2 C35 1.415(7) . ? O2 C34 1.418(7) . ? C2 C3 1.383(6) . ? C6 C5 1.399(6) . ? C6 C7 1.534(7) . ? C13 C8 1.386(6) . ? C3 C4 1.393(6) . ? C7 C8 1.539(6) . ? C7 C18 1.544(7) . ? C7 C19 1.544(6) . ? C4 C5 1.396(7) . ? C4 C14 1.545(6) . ? C11 C10 1.401(6) . ? C10 C9 1.406(6) . ? C10 C20 1.525(7) . ? C27 C29 1.514(7) . ? C27 C28 1.525(7) . ? C9 C8 1.397(7) . ? C20 C21 1.529(7) . ? C20 C23 1.533(7) . ? C20 C22 1.534(7) . ? C14 C16 1.522(7) . ? C14 C15 1.536(7) . ? C14 C17 1.544(6) . ? C30 C32 1.513(7) . ? C30 C31 1.518(7) . ? C26 C25 1.329(7) . ? C35 C36 1.481(9) . ? C34 C33 1.492(8) . ?