#------------------------------------------------------------------------------ #$Date: 2015-07-24 07:07:09 +0300 (Fri, 24 Jul 2015) $ #$Revision: 152503 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/03/59/7035949.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_7035949 loop_ _publ_author_name 'Castellanos-Blanco, Nahury' 'Flores-\'Alamo, Marcos' 'Garcia, Juventino J.' _publ_section_title ; Tandem Hydrogenation and Condensation of Fluorinated \a,\b-Unsaturated Ketones With Primary Amines, Catalyzed by Nickel ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C5DT02366A _journal_year 2015 _chemical_absolute_configuration syn _chemical_formula_moiety 'C45 H76 F2 Ni2 O P4' _chemical_formula_sum 'C45 H76 F2 Ni2 O P4' _chemical_formula_weight 912.35 _chemical_name_systematic ; ? ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2015-06-18T23:20:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2015-06-19 deposited with the CCDC. 2015-07-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.4964(8) _cell_length_b 15.4616(9) _cell_length_c 21.4898(11) _cell_measurement_reflns_used 3419 _cell_measurement_temperature 130(2) _cell_measurement_theta_max 25.2395 _cell_measurement_theta_min 3.3842 _cell_volume 4816.7(5) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 130(2) _diffrn_detector_area_resol_mean 10.4685 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0175384 _diffrn_orient_matrix_UB_12 -0.0407367 _diffrn_orient_matrix_UB_13 -0.0095071 _diffrn_orient_matrix_UB_21 -0.0065275 _diffrn_orient_matrix_UB_22 0.011752 _diffrn_orient_matrix_UB_23 -0.0316084 _diffrn_orient_matrix_UB_31 0.0452281 _diffrn_orient_matrix_UB_32 0.0175026 _diffrn_orient_matrix_UB_33 -0.0008647 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1483 _diffrn_reflns_av_unetI/netI 0.2717 _diffrn_reflns_laue_measured_fraction_full 0.996 _diffrn_reflns_laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 37408 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.288 _diffrn_reflns_theta_min 3.39 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_T_max 0.973 _exptl_absorpt_correction_T_min 0.843 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.258 _exptl_crystal_description needle _exptl_crystal_F_000 1952 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.648 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.082 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.52(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 504 _refine_ls_number_reflns 8745 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.991 _refine_ls_R_factor_all 0.1201 _refine_ls_R_factor_gt 0.0659 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0907 _refine_ls_wR_factor_ref 0.1045 _reflns_Friedel_coverage 0.806 _reflns_friedel_fraction_full 0.999 _reflns_friedel_fraction_max 0.999 _reflns_number_gt 5747 _reflns_number_total 8745 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5dt02366a2.cif _cod_data_source_block 2b _cod_database_code 7035949 _shelx_estimated_absorpt_t_min 0.744 _shelx_estimated_absorpt_t_max 0.972 _shelx_res_file ; TITL nycb24-c in P212121 #19 CELL 0.71073 14.4964 15.4616 21.4898 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0009 0.0011 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O NI P F UNIT 180 304 4 8 16 8 MERG 2 TWIN SHEL 100 0.83 FMAP 2 PLAN 5 SIZE 0.030 0.040 0.330 ACTA BOND BOND $H CONF LIST 4 WPDB -2 L.S. 20 TEMP -143.00 WGHT 0.024400 BASF 0.51630 FVAR 0.22236 C1 1 0.865838 -0.027301 0.923409 11.00000 0.04285 0.02517 = 0.03057 -0.00527 -0.00838 -0.00985 C2 1 0.947683 -0.037695 0.891357 11.00000 0.04161 0.03431 = 0.04054 -0.00150 -0.00777 0.00306 AFIX 43 H2 2 0.964125 0.003480 0.860476 11.00000 -1.20000 AFIX 0 C3 1 1.006200 -0.106149 0.902916 11.00000 0.04491 0.04110 = 0.06271 -0.00637 -0.02606 0.00657 AFIX 43 H3 2 1.061706 -0.111993 0.879795 11.00000 -1.20000 AFIX 0 C4 1 0.984754 -0.164548 0.946840 11.00000 0.06821 0.02935 = 0.05901 -0.00571 -0.03357 0.00373 C5 1 0.905786 -0.156147 0.981175 11.00000 0.08092 0.04045 = 0.04899 0.01838 -0.02492 -0.02519 AFIX 43 H5 2 0.892310 -0.196895 1.012988 11.00000 -1.20000 AFIX 0 C6 1 0.845325 -0.088500 0.969801 11.00000 0.05507 0.04223 = 0.04285 0.00540 -0.00824 -0.02055 AFIX 43 H6 2 0.790094 -0.083492 0.993320 11.00000 -1.20000 AFIX 0 C7 1 0.757888 0.415245 0.796400 11.00000 0.04093 0.03634 = 0.02591 -0.00684 -0.00831 -0.00117 C8 1 0.847821 0.434227 0.776550 11.00000 0.04477 0.05809 = 0.03415 0.01597 0.00316 0.00714 AFIX 43 H8 2 0.897965 0.400622 0.791567 11.00000 -1.20000 AFIX 0 C9 1 0.864611 0.501866 0.735007 11.00000 0.06769 0.06682 = 0.03632 0.00712 0.01223 -0.01170 AFIX 43 H9 2 0.925815 0.515325 0.722519 11.00000 -1.20000 AFIX 0 C10 1 0.792869 0.547660 0.712946 11.00000 0.08733 0.04071 = 0.02276 0.01820 -0.00503 -0.00863 C11 1 0.705749 0.531235 0.729436 11.00000 0.05978 0.04209 = 0.03663 0.00880 -0.01736 -0.00796 AFIX 43 H11 2 0.656488 0.564390 0.712674 11.00000 -1.20000 AFIX 0 C12 1 0.688371 0.465350 0.771206 11.00000 0.04495 0.03959 = 0.03871 0.00933 -0.01009 -0.00684 AFIX 43 H12 2 0.626388 0.454072 0.783044 11.00000 -1.20000 AFIX 0 C13 1 0.797535 0.041825 0.908471 11.00000 0.03165 0.03123 = 0.02406 -0.01055 0.00455 -0.00877 AFIX 13 H13 2 0.745581 0.045649 0.938959 11.00000 -1.20000 AFIX 0 C14 1 0.820216 0.122355 0.880270 11.00000 0.02823 0.02778 = 0.02673 -0.00681 0.00774 0.00048 AFIX 13 H14 2 0.887100 0.134258 0.872762 11.00000 -1.20000 AFIX 0 C15 1 0.759499 0.195514 0.881754 11.00000 0.02707 0.04164 = 0.01437 -0.00953 0.00148 -0.00458 C16 1 0.794322 0.276979 0.854815 11.00000 0.02767 0.03474 = 0.02530 -0.00093 0.00120 -0.00154 AFIX 13 H16 2 0.849721 0.271576 0.827361 11.00000 -1.20000 AFIX 0 C17 1 0.736223 0.349030 0.842845 11.00000 0.02534 0.03410 = 0.02917 0.00691 -0.00829 0.00236 AFIX 13 H17 2 0.668859 0.336885 0.847754 11.00000 -1.20000 AFIX 0 C18 1 0.659384 0.016749 0.687168 11.00000 0.05675 0.07286 = 0.03936 -0.01625 -0.02088 0.00664 AFIX 23 H18A 2 0.593993 0.034653 0.690426 11.00000 -1.20000 H18B 2 0.676288 0.017150 0.642534 11.00000 -1.20000 AFIX 0 C19 1 0.669047 -0.076598 0.712383 11.00000 0.04375 0.05694 = 0.05598 -0.02369 -0.01039 0.00015 AFIX 23 H19A 2 0.718277 -0.106903 0.689059 11.00000 -1.20000 H19B 2 0.610541 -0.108172 0.705413 11.00000 -1.20000 AFIX 0 C20 1 0.585597 -0.105775 0.833411 11.00000 0.03386 0.04109 = 0.07965 -0.02308 -0.00393 -0.01181 AFIX 13 H20 2 0.557859 -0.155751 0.810556 11.00000 -1.20000 AFIX 0 C21 1 0.521094 -0.028480 0.827589 11.00000 0.03597 0.07977 = 0.05442 -0.01351 -0.00405 0.00615 AFIX 137 H21A 2 0.461221 -0.042791 0.846093 11.00000 -1.50000 H21B 2 0.512712 -0.014122 0.783533 11.00000 -1.50000 H21C 2 0.547831 0.021224 0.849394 11.00000 -1.50000 AFIX 0 C22 1 0.597861 -0.131175 0.901567 11.00000 0.03730 0.04798 = 0.06979 0.00582 0.00932 -0.00582 AFIX 137 H22A 2 0.627106 -0.083485 0.924218 11.00000 -1.50000 H22B 2 0.636913 -0.182777 0.904260 11.00000 -1.50000 H22C 2 0.537436 -0.143568 0.919969 11.00000 -1.50000 AFIX 0 C23 1 0.764440 -0.179036 0.805415 11.00000 0.05631 0.03413 = 0.05010 -0.01453 -0.00571 0.01220 AFIX 13 H23 2 0.779935 -0.183788 0.850630 11.00000 -1.20000 AFIX 0 C24 1 0.856179 -0.174003 0.770891 11.00000 0.04636 0.07354 = 0.06503 -0.01315 0.00390 0.01906 AFIX 137 H24A 2 0.894890 -0.223288 0.782738 11.00000 -1.50000 H24B 2 0.887677 -0.120013 0.781810 11.00000 -1.50000 H24C 2 0.844930 -0.175473 0.725936 11.00000 -1.50000 AFIX 0 C25 1 0.712697 -0.261830 0.788447 11.00000 0.07399 0.03615 = 0.08927 -0.02080 -0.00475 -0.00111 AFIX 137 H25A 2 0.693969 -0.259423 0.744663 11.00000 -1.50000 H25B 2 0.657839 -0.267342 0.814800 11.00000 -1.50000 H25C 2 0.753094 -0.311830 0.794994 11.00000 -1.50000 AFIX 0 C26 1 0.831249 0.112219 0.676747 11.00000 0.07772 0.05945 = 0.02442 -0.00428 0.00962 -0.00527 AFIX 13 H26 2 0.807886 0.124793 0.633908 11.00000 -1.20000 AFIX 0 C27 1 0.887151 0.028015 0.674726 11.00000 0.06741 0.08441 = 0.07459 -0.02978 0.03978 0.00183 AFIX 137 H27A 2 0.941450 0.036037 0.648180 11.00000 -1.50000 H27B 2 0.848725 -0.018521 0.657794 11.00000 -1.50000 H27C 2 0.906989 0.012740 0.716914 11.00000 -1.50000 AFIX 0 C28 1 0.892542 0.186103 0.697044 11.00000 0.07997 0.07898 = 0.05645 -0.00226 0.02343 -0.01928 AFIX 137 H28A 2 0.918589 0.173275 0.738102 11.00000 -1.50000 H28B 2 0.856132 0.239416 0.699294 11.00000 -1.50000 H28C 2 0.942645 0.193521 0.666897 11.00000 -1.50000 AFIX 0 C29 1 0.664583 0.198802 0.720291 11.00000 0.07110 0.06622 = 0.02635 -0.00432 -0.00839 0.00478 AFIX 13 H29 2 0.704504 0.245792 0.737530 11.00000 -1.20000 AFIX 0 C30 1 0.578246 0.197468 0.760080 11.00000 0.05481 0.07701 = 0.04741 -0.01180 -0.01930 0.02853 AFIX 137 H30A 2 0.550307 0.255183 0.760445 11.00000 -1.50000 H30B 2 0.594384 0.180613 0.802672 11.00000 -1.50000 H30C 2 0.534231 0.155747 0.742846 11.00000 -1.50000 AFIX 0 C31 1 0.643191 0.224354 0.653636 11.00000 0.12590 0.09259 = 0.04194 0.01061 -0.02251 0.03673 AFIX 137 H31A 2 0.606041 0.179012 0.633955 11.00000 -1.50000 H31B 2 0.700960 0.231648 0.630539 11.00000 -1.50000 H31C 2 0.608762 0.278900 0.653381 11.00000 -1.50000 AFIX 0 C32 1 0.871972 0.399742 1.061545 11.00000 0.02990 0.03059 = 0.02640 -0.00230 -0.00614 -0.00441 AFIX 23 H32A 2 0.825075 0.371714 1.088282 11.00000 -1.20000 H32B 2 0.928368 0.408286 1.086788 11.00000 -1.20000 AFIX 0 C33 1 0.835528 0.488519 1.039935 11.00000 0.02984 0.03264 = 0.04376 -0.01187 0.00238 -0.00115 AFIX 23 H33A 2 0.888350 0.527506 1.031823 11.00000 -1.20000 H33B 2 0.797883 0.514472 1.073532 11.00000 -1.20000 AFIX 0 C34 1 1.022817 0.343474 0.976850 11.00000 0.01827 0.04244 = 0.03502 0.01561 -0.00871 -0.00014 AFIX 13 H34 2 1.059532 0.308950 1.007427 11.00000 -1.20000 AFIX 0 C35 1 1.041878 0.307133 0.912185 11.00000 0.02306 0.05273 = 0.02958 0.00527 0.00484 -0.00361 AFIX 137 H35A 2 1.010960 0.343035 0.880921 11.00000 -1.50000 H35B 2 1.018433 0.247790 0.909631 11.00000 -1.50000 H35C 2 1.108495 0.307209 0.904426 11.00000 -1.50000 AFIX 0 C36 1 1.053951 0.437330 0.981703 11.00000 0.02791 0.05364 = 0.05497 0.00451 -0.00058 -0.01286 AFIX 137 H36A 2 1.118278 0.442108 0.968107 11.00000 -1.50000 H36B 2 1.048733 0.456706 1.024980 11.00000 -1.50000 H36C 2 1.014872 0.473557 0.955145 11.00000 -1.50000 AFIX 0 C37 1 0.896947 0.220735 1.033118 11.00000 0.02026 0.03085 = 0.02644 0.00989 -0.00170 -0.00348 AFIX 13 H37 2 0.924003 0.178799 1.002756 11.00000 -1.20000 AFIX 0 C38 1 0.797989 0.191134 1.046192 11.00000 0.03423 0.03259 = 0.03079 0.00554 -0.00236 -0.00511 AFIX 137 H38A 2 0.798182 0.129898 1.057958 11.00000 -1.50000 H38B 2 0.760376 0.198991 1.008724 11.00000 -1.50000 H38C 2 0.772099 0.225576 1.080259 11.00000 -1.50000 AFIX 0 C39 1 0.954077 0.214593 1.092587 11.00000 0.02699 0.04580 = 0.02946 0.01692 0.00572 0.00087 AFIX 137 H39A 2 0.924451 0.248546 1.125503 11.00000 -1.50000 H39B 2 1.016136 0.237297 1.084821 11.00000 -1.50000 H39C 2 0.958339 0.153991 1.105633 11.00000 -1.50000 AFIX 0 C40 1 0.644251 0.480914 0.996970 11.00000 0.03403 0.03651 = 0.04166 -0.01027 0.00745 0.00712 AFIX 13 H40 2 0.638649 0.526825 1.029527 11.00000 -1.20000 AFIX 0 C41 1 0.620808 0.393636 1.026119 11.00000 0.03034 0.05739 = 0.04603 0.00697 0.01012 -0.00866 AFIX 137 H41A 2 0.559446 0.396506 1.045144 11.00000 -1.50000 H41B 2 0.666649 0.379529 1.058062 11.00000 -1.50000 H41C 2 0.621276 0.348825 0.993868 11.00000 -1.50000 AFIX 0 C42 1 0.575634 0.500845 0.943945 11.00000 0.03225 0.04712 = 0.06442 0.00795 0.00699 0.00836 AFIX 137 H42A 2 0.583756 0.458650 0.910360 11.00000 -1.50000 H42B 2 0.587170 0.559187 0.927912 11.00000 -1.50000 H42C 2 0.512414 0.497350 0.959901 11.00000 -1.50000 AFIX 0 C43 1 0.777311 0.586685 0.931284 11.00000 0.04197 0.02824 = 0.04814 0.00357 0.00117 -0.00642 AFIX 13 H43 2 0.734349 0.587723 0.894884 11.00000 -1.20000 AFIX 0 C44 1 0.874751 0.599745 0.905066 11.00000 0.04957 0.03984 = 0.06369 0.01202 0.00432 -0.00807 AFIX 137 H44A 2 0.876498 0.652997 0.880363 11.00000 -1.50000 H44B 2 0.891108 0.550433 0.878625 11.00000 -1.50000 H44C 2 0.918891 0.604146 0.939461 11.00000 -1.50000 AFIX 0 C45 1 0.749370 0.662280 0.973279 11.00000 0.06286 0.02299 = 0.09551 -0.00081 0.00488 0.00630 AFIX 137 H45A 2 0.785517 0.660374 1.011791 11.00000 -1.50000 H45B 2 0.683576 0.657863 0.983266 11.00000 -1.50000 H45C 2 0.761134 0.716984 0.951656 11.00000 -1.50000 AFIX 0 O1 3 0.679831 0.190961 0.904323 11.00000 0.02479 0.04781 = 0.02879 -0.00442 0.00143 -0.00796 NI1 4 0.756906 0.044497 0.820142 11.00000 0.02497 0.03283 = 0.02539 -0.00838 -0.00143 -0.00047 NI2 4 0.803800 0.362047 0.922053 11.00000 0.02042 0.02632 = 0.02100 0.00078 -0.00094 0.00099 P1 5 0.898647 0.328307 0.995563 11.00000 0.01897 0.03108 = 0.02242 0.00365 -0.00115 -0.00160 P2 5 0.764175 0.479204 0.968002 11.00000 0.02641 0.02403 = 0.03107 -0.00272 0.00275 -0.00008 P3 5 0.697144 -0.078181 0.796543 11.00000 0.03069 0.04002 = 0.03854 -0.01537 -0.00208 -0.00012 P4 5 0.731692 0.096493 0.728621 11.00000 0.04366 0.04743 = 0.02570 -0.00700 -0.00463 0.00688 F1 6 1.041717 -0.232719 0.958036 11.00000 0.09990 0.04170 = 0.11384 0.00693 -0.05167 0.01354 F2 6 0.812639 0.615882 0.673600 11.00000 0.10204 0.07053 = 0.04047 0.02019 -0.00547 -0.01100 HKLF 4 REM nycb24-c in P212121 #19 REM R1 = 0.0659 for 5747 Fo > 4sig(Fo) and 0.1201 for all 8745 data REM 504 parameters refined using 0 restraints END WGHT 0.0245 0.0000 REM Highest difference peak 0.648, deepest hole -0.396, 1-sigma level 0.082 Q1 1 0.7142 0.3675 0.9181 11.00000 0.05 0.54 Q2 1 0.7479 0.0949 0.7886 11.00000 0.05 0.43 Q3 1 0.7789 0.0486 0.7737 11.00000 0.05 0.41 Q4 1 0.7091 0.0520 0.7867 11.00000 0.05 0.38 Q5 1 0.7610 -0.0018 0.8721 11.00000 0.05 0.38 ; _shelx_res_checksum 69133 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, 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 C1 C 0.8658(6) -0.0273(5) 0.9234(4) 0.033(2) Uani 1 1 d . . C2 C 0.9477(6) -0.0377(6) 0.8914(4) 0.039(2) Uani 1 1 d . . H2 H 0.9641 0.0035 0.8605 0.047 Uiso 1 1 calc R U C3 C 1.0062(7) -0.1061(6) 0.9029(5) 0.050(3) Uani 1 1 d . . H3 H 1.0617 -0.112 0.8798 0.059 Uiso 1 1 calc R U C4 C 0.9848(8) -0.1645(6) 0.9468(5) 0.052(3) Uani 1 1 d . . C5 C 0.9058(8) -0.1561(6) 0.9812(5) 0.057(3) Uani 1 1 d . . H5 H 0.8923 -0.1969 1.013 0.068 Uiso 1 1 calc R U C6 C 0.8453(7) -0.0885(6) 0.9698(4) 0.047(3) Uani 1 1 d . . H6 H 0.7901 -0.0835 0.9933 0.056 Uiso 1 1 calc R U C7 C 0.7579(6) 0.4152(5) 0.7964(4) 0.034(2) Uani 1 1 d . . C8 C 0.8478(7) 0.4342(6) 0.7766(4) 0.046(3) Uani 1 1 d . . H8 H 0.898 0.4006 0.7916 0.055 Uiso 1 1 calc R U C9 C 0.8646(8) 0.5019(7) 0.7350(5) 0.057(3) Uani 1 1 d . . H9 H 0.9258 0.5153 0.7225 0.068 Uiso 1 1 calc R U C10 C 0.7929(9) 0.5477(6) 0.7129(4) 0.050(3) Uani 1 1 d . . C11 C 0.7057(8) 0.5312(6) 0.7294(4) 0.046(3) Uani 1 1 d . . H11 H 0.6565 0.5644 0.7127 0.055 Uiso 1 1 calc R U C12 C 0.6884(6) 0.4654(6) 0.7712(4) 0.041(2) Uani 1 1 d . . H12 H 0.6264 0.4541 0.783 0.049 Uiso 1 1 calc R U C13 C 0.7975(6) 0.0418(5) 0.9085(3) 0.029(2) Uani 1 1 d . . H13 H 0.7456 0.0456 0.939 0.035 Uiso 1 1 calc R U C14 C 0.8202(6) 0.1224(5) 0.8803(4) 0.028(2) Uani 1 1 d . . H14 H 0.8871 0.1343 0.8728 0.033 Uiso 1 1 calc R U C15 C 0.7595(6) 0.1955(5) 0.8818(3) 0.028(2) Uani 1 1 d . . C16 C 0.7943(6) 0.2770(5) 0.8548(4) 0.029(2) Uani 1 1 d . . H16 H 0.8497 0.2716 0.8274 0.035 Uiso 1 1 calc R U C17 C 0.7362(6) 0.3490(5) 0.8428(3) 0.030(2) Uani 1 1 d . . H17 H 0.6689 0.3369 0.8478 0.035 Uiso 1 1 calc R U C18 C 0.6594(7) 0.0167(6) 0.6872(5) 0.056(3) Uani 1 1 d . . H18A H 0.594 0.0347 0.6904 0.068 Uiso 1 1 calc R U H18B H 0.6763 0.0172 0.6425 0.068 Uiso 1 1 calc R U C19 C 0.6690(6) -0.0766(6) 0.7124(4) 0.052(3) Uani 1 1 d . . H19A H 0.7183 -0.1069 0.6891 0.063 Uiso 1 1 calc R U H19B H 0.6105 -0.1082 0.7054 0.063 Uiso 1 1 calc R U C20 C 0.5856(6) -0.1058(6) 0.8334(5) 0.052(3) Uani 1 1 d . . H20 H 0.5579 -0.1558 0.8106 0.062 Uiso 1 1 calc R U C21 C 0.5211(6) -0.0285(7) 0.8276(5) 0.057(3) Uani 1 1 d . . H21A H 0.4612 -0.0428 0.8461 0.085 Uiso 1 1 calc R U H21B H 0.5127 -0.0141 0.7835 0.085 Uiso 1 1 calc R U H21C H 0.5478 0.0212 0.8494 0.085 Uiso 1 1 calc R U C22 C 0.5979(6) -0.1312(6) 0.9016(5) 0.052(3) Uani 1 1 d . . H22A H 0.6271 -0.0835 0.9242 0.078 Uiso 1 1 calc R U H22B H 0.6369 -0.1828 0.9043 0.078 Uiso 1 1 calc R U H22C H 0.5374 -0.1436 0.92 0.078 Uiso 1 1 calc R U C23 C 0.7644(6) -0.1790(5) 0.8054(4) 0.047(3) Uani 1 1 d . . H23 H 0.7799 -0.1838 0.8506 0.056 Uiso 1 1 calc R U C24 C 0.8562(6) -0.1740(7) 0.7709(5) 0.062(3) Uani 1 1 d . . H24A H 0.8949 -0.2233 0.7827 0.092 Uiso 1 1 calc R U H24B H 0.8877 -0.12 0.7818 0.092 Uiso 1 1 calc R U H24C H 0.8449 -0.1755 0.7259 0.092 Uiso 1 1 calc R U C25 C 0.7127(7) -0.2618(6) 0.7884(5) 0.066(3) Uani 1 1 d . . H25A H 0.694 -0.2594 0.7447 0.1 Uiso 1 1 calc R U H25B H 0.6578 -0.2673 0.8148 0.1 Uiso 1 1 calc R U H25C H 0.7531 -0.3118 0.795 0.1 Uiso 1 1 calc R U C26 C 0.8312(7) 0.1122(6) 0.6767(4) 0.054(3) Uani 1 1 d . . H26 H 0.8079 0.1248 0.6339 0.065 Uiso 1 1 calc R U C27 C 0.8872(7) 0.0280(7) 0.6747(5) 0.075(4) Uani 1 1 d . . H27A H 0.9414 0.036 0.6482 0.113 Uiso 1 1 calc R U H27B H 0.8487 -0.0185 0.6578 0.113 Uiso 1 1 calc R U H27C H 0.907 0.0127 0.7169 0.113 Uiso 1 1 calc R U C28 C 0.8925(7) 0.1861(7) 0.6970(5) 0.072(3) Uani 1 1 d . . H28A H 0.9186 0.1733 0.7381 0.108 Uiso 1 1 calc R U H28B H 0.8561 0.2394 0.6993 0.108 Uiso 1 1 calc R U H28C H 0.9426 0.1935 0.6669 0.108 Uiso 1 1 calc R U C29 C 0.6646(7) 0.1988(7) 0.7203(4) 0.055(3) Uani 1 1 d . . H29 H 0.7045 0.2458 0.7375 0.065 Uiso 1 1 calc R U C30 C 0.5782(6) 0.1975(7) 0.7601(5) 0.060(3) Uani 1 1 d . . H30A H 0.5503 0.2552 0.7604 0.09 Uiso 1 1 calc R U H30B H 0.5944 0.1806 0.8027 0.09 Uiso 1 1 calc R U H30C H 0.5342 0.1557 0.7428 0.09 Uiso 1 1 calc R U C31 C 0.6432(9) 0.2244(8) 0.6536(5) 0.087(4) Uani 1 1 d . . H31A H 0.606 0.179 0.634 0.13 Uiso 1 1 calc R U H31B H 0.701 0.2316 0.6305 0.13 Uiso 1 1 calc R U H31C H 0.6088 0.2789 0.6534 0.13 Uiso 1 1 calc R U C32 C 0.8720(6) 0.3997(5) 1.0615(4) 0.029(2) Uani 1 1 d . . H32A H 0.8251 0.3717 1.0883 0.035 Uiso 1 1 calc R U H32B H 0.9284 0.4083 1.0868 0.035 Uiso 1 1 calc R U C33 C 0.8355(6) 0.4885(5) 1.0399(4) 0.035(2) Uani 1 1 d . . H33A H 0.8884 0.5275 1.0318 0.042 Uiso 1 1 calc R U H33B H 0.7979 0.5145 1.0735 0.042 Uiso 1 1 calc R U C34 C 1.0228(5) 0.3435(5) 0.9768(4) 0.032(2) Uani 1 1 d . . H34 H 1.0595 0.3089 1.0074 0.038 Uiso 1 1 calc R U C35 C 1.0419(5) 0.3071(6) 0.9122(4) 0.035(2) Uani 1 1 d . . H35A H 1.011 0.343 0.8809 0.053 Uiso 1 1 calc R U H35B H 1.0184 0.2478 0.9096 0.053 Uiso 1 1 calc R U H35C H 1.1085 0.3072 0.9044 0.053 Uiso 1 1 calc R U C36 C 1.0540(6) 0.4373(6) 0.9817(5) 0.046(3) Uani 1 1 d . . H36A H 1.1183 0.4421 0.9681 0.068 Uiso 1 1 calc R U H36B H 1.0487 0.4567 1.025 0.068 Uiso 1 1 calc R U H36C H 1.0149 0.4736 0.9551 0.068 Uiso 1 1 calc R U C37 C 0.8969(5) 0.2207(5) 1.0331(4) 0.026(2) Uani 1 1 d . . H37 H 0.924 0.1788 1.0028 0.031 Uiso 1 1 calc R U C38 C 0.7980(6) 0.1911(5) 1.0462(4) 0.033(2) Uani 1 1 d . . H38A H 0.7982 0.1299 1.058 0.049 Uiso 1 1 calc R U H38B H 0.7604 0.199 1.0087 0.049 Uiso 1 1 calc R U H38C H 0.7721 0.2256 1.0803 0.049 Uiso 1 1 calc R U C39 C 0.9541(5) 0.2146(6) 1.0926(4) 0.034(2) Uani 1 1 d . . H39A H 0.9245 0.2485 1.1255 0.051 Uiso 1 1 calc R U H39B H 1.0161 0.2373 1.0848 0.051 Uiso 1 1 calc R U H39C H 0.9583 0.154 1.1056 0.051 Uiso 1 1 calc R U C40 C 0.6443(6) 0.4809(5) 0.9970(4) 0.037(2) Uani 1 1 d . . H40 H 0.6386 0.5268 1.0295 0.045 Uiso 1 1 calc R U C41 C 0.6208(6) 0.3936(6) 1.0261(4) 0.045(3) Uani 1 1 d . . H41A H 0.5594 0.3965 1.0451 0.067 Uiso 1 1 calc R U H41B H 0.6666 0.3795 1.0581 0.067 Uiso 1 1 calc R U H41C H 0.6213 0.3488 0.9939 0.067 Uiso 1 1 calc R U C42 C 0.5756(6) 0.5008(6) 0.9439(5) 0.048(3) Uani 1 1 d . . H42A H 0.5838 0.4587 0.9104 0.072 Uiso 1 1 calc R U H42B H 0.5872 0.5592 0.9279 0.072 Uiso 1 1 calc R U H42C H 0.5124 0.4974 0.9599 0.072 Uiso 1 1 calc R U C43 C 0.7773(6) 0.5867(5) 0.9313(4) 0.039(2) Uani 1 1 d . . H43 H 0.7343 0.5877 0.8949 0.047 Uiso 1 1 calc R U C44 C 0.8748(6) 0.5997(6) 0.9051(5) 0.051(3) Uani 1 1 d . . H44A H 0.8765 0.653 0.8804 0.077 Uiso 1 1 calc R U H44B H 0.8911 0.5504 0.8786 0.077 Uiso 1 1 calc R U H44C H 0.9189 0.6041 0.9395 0.077 Uiso 1 1 calc R U C45 C 0.7494(7) 0.6623(5) 0.9733(5) 0.060(3) Uani 1 1 d . . H45A H 0.7855 0.6604 1.0118 0.091 Uiso 1 1 calc R U H45B H 0.6836 0.6579 0.9833 0.091 Uiso 1 1 calc R U H45C H 0.7611 0.717 0.9517 0.091 Uiso 1 1 calc R U O1 O 0.6798(4) 0.1910(4) 0.9043(2) 0.0338(15) Uani 1 1 d . . Ni1 Ni 0.75691(7) 0.04450(6) 0.82014(5) 0.0277(3) Uani 1 1 d . . Ni2 Ni 0.80380(7) 0.36205(6) 0.92205(5) 0.0226(3) Uani 1 1 d . . P1 P 0.89865(14) 0.32831(14) 0.99556(10) 0.0242(5) Uani 1 1 d . . P2 P 0.76418(15) 0.47920(13) 0.96800(10) 0.0272(5) Uani 1 1 d . . P3 P 0.69714(16) -0.07818(14) 0.79654(11) 0.0364(6) Uani 1 1 d . . P4 P 0.73169(16) 0.09649(15) 0.72862(11) 0.0389(6) Uani 1 1 d . . F1 F 1.0417(5) -0.2327(4) 0.9580(3) 0.085(2) Uani 1 1 d . . F2 F 0.8126(4) 0.6159(3) 0.6736(2) 0.0710(17) Uani 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 0.043(5) 0.025(5) 0.031(5) -0.005(5) -0.008(5) -0.010(4) C2 0.042(6) 0.034(6) 0.041(6) -0.001(5) -0.008(5) 0.003(5) C3 0.045(6) 0.041(6) 0.063(8) -0.006(6) -0.026(6) 0.007(5) C4 0.068(8) 0.029(6) 0.059(8) -0.006(6) -0.034(7) 0.004(6) C5 0.081(8) 0.040(7) 0.049(7) 0.018(6) -0.025(7) -0.025(7) C6 0.055(6) 0.042(6) 0.043(6) 0.005(5) -0.008(5) -0.021(6) C7 0.041(5) 0.036(5) 0.026(5) -0.007(4) -0.008(5) -0.001(5) C8 0.045(6) 0.058(7) 0.034(6) 0.016(5) 0.003(5) 0.007(5) C9 0.068(8) 0.067(8) 0.036(7) 0.007(6) 0.012(6) -0.012(6) C10 0.087(8) 0.041(6) 0.023(5) 0.018(5) -0.005(6) -0.009(7) C11 0.060(7) 0.042(6) 0.037(6) 0.009(5) -0.017(6) -0.008(6) C12 0.045(6) 0.040(6) 0.039(6) 0.009(5) -0.010(5) -0.007(5) C13 0.032(5) 0.031(5) 0.024(5) -0.011(4) 0.005(4) -0.009(5) C14 0.028(5) 0.028(5) 0.027(5) -0.007(4) 0.008(4) 0.000(4) C15 0.027(5) 0.042(5) 0.014(4) -0.010(4) 0.001(4) -0.005(5) C16 0.028(5) 0.035(5) 0.025(5) -0.001(4) 0.001(4) -0.002(5) C17 0.025(5) 0.034(5) 0.029(5) 0.007(4) -0.008(4) 0.002(4) C18 0.057(7) 0.073(8) 0.039(6) -0.016(6) -0.021(6) 0.007(6) C19 0.044(6) 0.057(7) 0.056(7) -0.024(6) -0.010(5) 0.000(5) C20 0.034(5) 0.041(6) 0.080(9) -0.023(6) -0.004(6) -0.012(5) C21 0.036(5) 0.080(8) 0.054(7) -0.014(7) -0.004(5) 0.006(6) C22 0.037(6) 0.048(6) 0.070(8) 0.006(6) 0.009(6) -0.006(5) C23 0.056(6) 0.034(5) 0.050(6) -0.015(5) -0.006(6) 0.012(5) C24 0.046(6) 0.074(8) 0.065(8) -0.013(6) 0.004(6) 0.019(6) C25 0.074(8) 0.036(6) 0.089(9) -0.021(6) -0.005(7) -0.001(6) C26 0.078(8) 0.059(7) 0.024(5) -0.004(5) 0.010(6) -0.005(6) C27 0.067(7) 0.084(9) 0.075(9) -0.030(8) 0.040(7) 0.002(7) C28 0.080(8) 0.079(8) 0.056(8) -0.002(7) 0.023(7) -0.019(7) C29 0.071(8) 0.066(8) 0.026(6) -0.004(5) -0.008(6) 0.005(6) C30 0.055(7) 0.077(8) 0.047(7) -0.012(6) -0.019(6) 0.029(6) C31 0.126(11) 0.093(9) 0.042(7) 0.011(7) -0.023(8) 0.037(8) C32 0.030(5) 0.031(5) 0.026(5) -0.002(4) -0.006(4) -0.004(4) C33 0.030(5) 0.033(5) 0.044(6) -0.012(4) 0.002(4) -0.001(4) C34 0.018(4) 0.042(6) 0.035(6) 0.016(5) -0.009(4) 0.000(4) C35 0.023(5) 0.053(6) 0.030(6) 0.005(5) 0.005(4) -0.004(4) C36 0.028(5) 0.054(7) 0.055(7) 0.005(6) -0.001(5) -0.013(5) C37 0.020(4) 0.031(5) 0.026(5) 0.010(4) -0.002(4) -0.003(4) C38 0.034(5) 0.033(5) 0.031(5) 0.006(4) -0.002(4) -0.005(5) C39 0.027(5) 0.046(6) 0.029(6) 0.017(5) 0.006(4) 0.001(4) C40 0.034(5) 0.037(6) 0.042(6) -0.010(5) 0.007(5) 0.007(4) C41 0.030(5) 0.057(7) 0.046(6) 0.007(5) 0.010(5) -0.009(5) C42 0.032(5) 0.047(6) 0.064(7) 0.008(5) 0.007(5) 0.008(5) C43 0.042(6) 0.028(5) 0.048(6) 0.004(5) 0.001(5) -0.006(4) C44 0.050(6) 0.040(6) 0.064(8) 0.012(5) 0.004(6) -0.008(5) C45 0.063(6) 0.023(5) 0.096(8) -0.001(5) 0.005(7) 0.006(5) O1 0.025(3) 0.048(4) 0.029(4) -0.004(3) 0.001(3) -0.008(3) Ni1 0.0250(6) 0.0328(6) 0.0254(6) -0.0084(5) -0.0014(5) -0.0005(6) Ni2 0.0204(5) 0.0263(6) 0.0210(6) 0.0008(5) -0.0009(5) 0.0010(5) P1 0.0190(11) 0.0311(13) 0.0224(12) 0.0036(11) -0.0011(10) -0.0016(10) P2 0.0264(13) 0.0240(12) 0.0311(13) -0.0027(10) 0.0028(11) -0.0001(11) P3 0.0307(13) 0.0400(15) 0.0385(15) -0.0154(12) -0.0021(13) -0.0001(12) P4 0.0437(16) 0.0474(15) 0.0257(13) -0.0070(11) -0.0046(12) 0.0069(13) F1 0.100(5) 0.042(4) 0.114(6) 0.007(4) -0.052(4) 0.014(4) F2 0.102(4) 0.071(4) 0.040(3) 0.020(3) -0.005(4) -0.011(4) 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -2 30 0.0185 0 2 -30 0.0185 19 8 1 0.1449 -19 -8 -1 0.1449 1 22 1 0.0152 -1 -22 -1 0.0152 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 C1 C6 117.2(9) C2 C1 C13 123.1(8) C6 C1 C13 119.6(8) C3 C2 C1 121.9(9) C3 C2 H2 119.1 C1 C2 H2 119.1 C4 C3 C2 120.0(10) C4 C3 H3 120 C2 C3 H3 120 C3 C4 F1 120.3(11) C3 C4 C5 120.6(10) F1 C4 C5 119.1(11) C4 C5 C6 120.4(9) C4 C5 H5 119.8 C6 C5 H5 119.8 C5 C6 C1 119.9(9) C5 C6 H6 120 C1 C6 H6 120 C12 C7 C8 116.2(8) C12 C7 C17 120.2(8) C8 C7 C17 123.6(8) C9 C8 C7 120.9(9) C9 C8 H8 119.6 C7 C8 H8 119.6 C10 C9 C8 119.0(10) C10 C9 H9 120.5 C8 C9 H9 120.5 C11 C10 C9 122.5(9) C11 C10 F2 120.2(10) C9 C10 F2 117.2(10) C10 C11 C12 119.0(9) C10 C11 H11 120.5 C12 C11 H11 120.5 C11 C12 C7 122.4(9) C11 C12 H12 118.8 C7 C12 H12 118.8 C14 C13 C1 124.4(7) C14 C13 Ni1 69.1(4) C1 C13 Ni1 114.6(5) C14 C13 H13 113.7 C1 C13 H13 113.7 Ni1 C13 H13 113.7 C13 C14 C15 122.6(7) C13 C14 Ni1 68.9(4) C15 C14 Ni1 102.0(5) C13 C14 H14 117 C15 C14 H14 117 Ni1 C14 H14 117 O1 C15 C14 122.0(8) O1 C15 C16 121.0(8) C14 C15 C16 117.1(7) C17 C16 C15 122.5(7) C17 C16 Ni2 69.4(4) C15 C16 Ni2 107.9(5) C17 C16 H16 115.8 C15 C16 H16 115.8 Ni2 C16 H16 115.8 C16 C17 C7 123.0(8) C16 C17 Ni2 68.3(4) C7 C17 Ni2 114.2(5) C16 C17 H17 114.4 C7 C17 H17 114.4 Ni2 C17 H17 114.4 C19 C18 P4 113.7(6) C19 C18 H18A 108.8 P4 C18 H18A 108.8 C19 C18 H18B 108.8 P4 C18 H18B 108.8 H18A C18 H18B 107.7 C18 C19 P3 111.9(6) C18 C19 H19A 109.2 P3 C19 H19A 109.2 C18 C19 H19B 109.2 P3 C19 H19B 109.2 H19A C19 H19B 107.9 C21 C20 C22 110.6(8) C21 C20 P3 108.7(7) C22 C20 P3 111.6(6) C21 C20 H20 108.6 C22 C20 H20 108.6 P3 C20 H20 108.6 C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C20 C22 H22A 109.5 C20 C22 H22B 109.5 H22A C22 H22B 109.5 C20 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C24 C23 C25 110.8(8) C24 C23 P3 111.5(7) C25 C23 P3 115.0(6) C24 C23 H23 106.3 C25 C23 H23 106.3 P3 C23 H23 106.3 C23 C24 H24A 109.5 C23 C24 H24B 109.5 H24A C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C23 C25 H25A 109.5 C23 C25 H25B 109.5 H25A C25 H25B 109.5 C23 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C28 C26 C27 109.8(9) C28 C26 P4 112.7(7) C27 C26 P4 108.6(7) C28 C26 H26 108.5 C27 C26 H26 108.5 P4 C26 H26 108.5 C26 C27 H27A 109.5 C26 C27 H27B 109.5 H27A C27 H27B 109.5 C26 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C26 C28 H28A 109.5 C26 C28 H28B 109.5 H28A C28 H28B 109.5 C26 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C30 C29 C31 111.5(9) C30 C29 P4 111.4(7) C31 C29 P4 114.7(7) C30 C29 H29 106.2 C31 C29 H29 106.2 P4 C29 H29 106.2 C29 C30 H30A 109.5 C29 C30 H30B 109.5 H30A C30 H30B 109.5 C29 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C29 C31 H31A 109.5 C29 C31 H31B 109.5 H31A C31 H31B 109.5 C29 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C33 C32 P1 112.0(6) C33 C32 H32A 109.2 P1 C32 H32A 109.2 C33 C32 H32B 109.2 P1 C32 H32B 109.2 H32A C32 H32B 107.9 C32 C33 P2 111.8(5) C32 C33 H33A 109.3 P2 C33 H33A 109.3 C32 C33 H33B 109.3 P2 C33 H33B 109.3 H33A C33 H33B 107.9 C36 C34 C35 111.1(7) C36 C34 P1 113.1(6) C35 C34 P1 109.0(6) C36 C34 H34 107.8 C35 C34 H34 107.8 P1 C34 H34 107.8 C34 C35 H35A 109.5 C34 C35 H35B 109.5 H35A C35 H35B 109.5 C34 C35 H35C 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 C34 C36 H36A 109.5 C34 C36 H36B 109.5 H36A C36 H36B 109.5 C34 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C39 C37 C38 109.6(6) C39 C37 P1 114.5(6) C38 C37 P1 111.2(5) C39 C37 H37 107.1 C38 C37 H37 107.1 P1 C37 H37 107.1 C37 C38 H38A 109.5 C37 C38 H38B 109.5 H38A C38 H38B 109.5 C37 C38 H38C 109.5 H38A C38 H38C 109.5 H38B C38 H38C 109.5 C37 C39 H39A 109.5 C37 C39 H39B 109.5 H39A C39 H39B 109.5 C37 C39 H39C 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 C41 C40 C42 109.6(7) C41 C40 P2 109.6(6) C42 C40 P2 111.1(6) C41 C40 H40 108.8 C42 C40 H40 108.8 P2 C40 H40 108.8 C40 C41 H41A 109.5 C40 C41 H41B 109.5 H41A C41 H41B 109.5 C40 C41 H41C 109.5 H41A C41 H41C 109.5 H41B C41 H41C 109.5 C40 C42 H42A 109.5 C40 C42 H42B 109.5 H42A C42 H42B 109.5 C40 C42 H42C 109.5 H42A C42 H42C 109.5 H42B C42 H42C 109.5 C45 C43 C44 111.1(7) C45 C43 P2 114.0(6) C44 C43 P2 111.7(6) C45 C43 H43 106.5 C44 C43 H43 106.5 P2 C43 H43 106.5 C43 C44 H44A 109.5 C43 C44 H44B 109.5 H44A C44 H44B 109.5 C43 C44 H44C 109.5 H44A C44 H44C 109.5 H44B C44 H44C 109.5 C43 C45 H45A 109.5 C43 C45 H45B 109.5 H45A C45 H45B 109.5 C43 C45 H45C 109.5 H45A C45 H45C 109.5 H45B C45 H45C 109.5 C13 Ni1 C14 41.9(3) C13 Ni1 P3 109.1(2) C14 Ni1 P3 150.9(2) C13 Ni1 P4 158.3(2) C14 Ni1 P4 116.4(2) P3 Ni1 P4 92.61(10) C16 Ni2 C17 42.3(3) C16 Ni2 P2 152.8(3) C17 Ni2 P2 110.5(2) C16 Ni2 P1 115.0(2) C17 Ni2 P1 157.3(2) P2 Ni2 P1 92.17(9) C32 P1 C37 101.6(4) C32 P1 C34 107.1(4) C37 P1 C34 102.8(4) C32 P1 Ni2 106.6(3) C37 P1 Ni2 121.9(3) C34 P1 Ni2 115.3(3) C40 P2 C43 103.2(4) C40 P2 C33 104.0(4) C43 P2 C33 103.1(4) C40 P2 Ni2 114.8(3) C43 P2 Ni2 122.4(3) C33 P2 Ni2 107.4(3) C23 P3 C20 102.9(4) C23 P3 C19 103.2(4) C20 P3 C19 103.2(5) C23 P3 Ni1 120.5(3) C20 P3 Ni1 117.1(3) C19 P3 Ni1 107.9(3) C26 P4 C18 104.0(5) C26 P4 C29 103.8(5) C18 P4 C29 102.9(5) C26 P4 Ni1 118.0(3) C18 P4 Ni1 106.7(3) C29 P4 Ni1 119.5(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.381(11) C1 C6 1.406(12) C1 C13 1.492(11) C2 C3 1.379(11) C2 H2 0.95 C3 C4 1.343(13) C3 H3 0.95 C4 F1 1.360(11) C4 C5 1.368(14) C5 C6 1.386(13) C5 H5 0.95 C6 H6 0.95 C7 C12 1.382(11) C7 C8 1.403(11) C7 C17 1.464(10) C8 C9 1.396(12) C8 H8 0.95 C9 C10 1.345(13) C9 H9 0.95 C10 C11 1.336(13) C10 F2 1.382(10) C11 C12 1.381(12) C11 H11 0.95 C12 H12 0.95 C13 C14 1.423(10) C13 Ni1 1.988(8) C13 H13 1 C14 C15 1.434(10) C14 Ni1 1.990(8) C14 H14 1 C15 O1 1.255(9) C15 C16 1.475(10) C16 C17 1.420(10) C16 Ni2 1.959(8) C16 H16 1 C17 Ni2 1.974(7) C17 H17 1 C18 C19 1.548(12) C18 P4 1.847(9) C18 H18A 0.99 C18 H18B 0.99 C19 P3 1.854(10) C19 H19A 0.99 C19 H19B 0.99 C20 C21 1.523(12) C20 C22 1.527(13) C20 P3 1.851(9) C20 H20 1 C21 H21A 0.98 C21 H21B 0.98 C21 H21C 0.98 C22 H22A 0.98 C22 H22B 0.98 C22 H22C 0.98 C23 C24 1.525(12) C23 C25 1.528(11) C23 P3 1.849(8) C23 H23 1 C24 H24A 0.98 C24 H24B 0.98 C24 H24C 0.98 C25 H25A 0.98 C25 H25B 0.98 C25 H25C 0.98 C26 C28 1.512(13) C26 C27 1.534(13) C26 P4 1.840(9) C26 H26 1 C27 H27A 0.98 C27 H27B 0.98 C27 H27C 0.98 C28 H28A 0.98 C28 H28B 0.98 C28 H28C 0.98 C29 C30 1.516(13) C29 C31 1.518(13) C29 P4 1.866(10) C29 H29 1 C30 H30A 0.98 C30 H30B 0.98 C30 H30C 0.98 C31 H31A 0.98 C31 H31B 0.98 C31 H31C 0.98 C32 C33 1.542(10) C32 P1 1.838(8) C32 H32A 0.99 C32 H32B 0.99 C33 P2 1.866(8) C33 H33A 0.99 C33 H33B 0.99 C34 C36 1.523(11) C34 C35 1.524(11) C34 P1 1.859(8) C34 H34 1 C35 H35A 0.98 C35 H35B 0.98 C35 H35C 0.98 C36 H36A 0.98 C36 H36B 0.98 C36 H36C 0.98 C37 C39 1.526(10) C37 C38 1.532(11) C37 P1 1.849(8) C37 H37 1 C38 H38A 0.98 C38 H38B 0.98 C38 H38C 0.98 C39 H39A 0.98 C39 H39B 0.98 C39 H39C 0.98 C40 C41 1.526(11) C40 C42 1.544(12) C40 P2 1.847(8) C40 H40 1 C41 H41A 0.98 C41 H41B 0.98 C41 H41C 0.98 C42 H42A 0.98 C42 H42B 0.98 C42 H42C 0.98 C43 C45 1.531(11) C43 C44 1.534(11) C43 P2 1.849(8) C43 H43 1 C44 H44A 0.98 C44 H44B 0.98 C44 H44C 0.98 C45 H45A 0.98 C45 H45B 0.98 C45 H45C 0.98 Ni1 P3 2.146(2) Ni1 P4 2.156(3) Ni2 P2 2.142(2) Ni2 P1 2.158(2) 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 C6 C1 C2 C3 1.6(13) C13 C1 C2 C3 -174.9(8) C1 C2 C3 C4 -0.7(13) C2 C3 C4 F1 179.3(8) C2 C3 C4 C5 -1.1(14) C3 C4 C5 C6 1.9(15) F1 C4 C5 C6 -178.5(8) C4 C5 C6 C1 -1.0(14) C2 C1 C6 C5 -0.7(12) C13 C1 C6 C5 175.9(8) C12 C7 C8 C9 1.8(13) C17 C7 C8 C9 -175.9(8) C7 C8 C9 C10 -1.5(15) C8 C9 C10 C11 0.3(16) C8 C9 C10 F2 177.9(8) C9 C10 C11 C12 0.7(16) F2 C10 C11 C12 -176.8(7) C10 C11 C12 C7 -0.4(15) C8 C7 C12 C11 -0.8(13) C17 C7 C12 C11 177.0(8) C2 C1 C13 C14 -26.7(12) C6 C1 C13 C14 157.0(8) C2 C1 C13 Ni1 54.1(9) C6 C1 C13 Ni1 -122.3(7) C1 C13 C14 C15 -162.7(7) Ni1 C13 C14 C15 91.1(7) C1 C13 C14 Ni1 106.2(7) C13 C14 C15 O1 -5.1(12) Ni1 C14 C15 O1 67.5(8) C13 C14 C15 C16 175.6(7) Ni1 C14 C15 C16 -111.9(6) O1 C15 C16 C17 -11.3(11) C14 C15 C16 C17 168.0(7) O1 C15 C16 Ni2 65.3(8) C14 C15 C16 Ni2 -115.4(7) C15 C16 C17 C7 -155.8(7) Ni2 C16 C17 C7 105.5(7) C15 C16 C17 Ni2 98.7(7) C12 C7 C17 C16 157.5(8) C8 C7 C17 C16 -25.0(12) C12 C7 C17 Ni2 -123.6(7) C8 C7 C17 Ni2 54.0(10) P4 C18 C19 P3 29.9(9) P1 C32 C33 P2 34.7(7) C33 C32 P1 C37 -159.8(6) C33 C32 P1 C34 92.8(6) C33 C32 P1 Ni2 -31.2(6) C39 C37 P1 C32 -49.6(6) C38 C37 P1 C32 75.3(6) C39 C37 P1 C34 61.2(7) C38 C37 P1 C34 -173.9(6) C39 C37 P1 Ni2 -167.7(5) C38 C37 P1 Ni2 -42.8(7) C36 C34 P1 C32 -39.5(7) C35 C34 P1 C32 -163.6(6) C36 C34 P1 C37 -146.1(6) C35 C34 P1 C37 89.8(6) C36 C34 P1 Ni2 79.0(7) C35 C34 P1 Ni2 -45.2(6) C41 C40 P2 C43 177.2(6) C42 C40 P2 C43 55.8(7) C41 C40 P2 C33 -75.5(7) C42 C40 P2 C33 163.2(6) C41 C40 P2 Ni2 41.6(7) C42 C40 P2 Ni2 -79.8(6) C45 C43 P2 C40 51.7(8) C44 C43 P2 C40 178.6(7) C45 C43 P2 C33 -56.3(7) C44 C43 P2 C33 70.6(7) C45 C43 P2 Ni2 -177.1(6) C44 C43 P2 Ni2 -50.1(8) C32 C33 P2 C40 99.2(6) C32 C33 P2 C43 -153.4(6) C32 C33 P2 Ni2 -22.9(6) C24 C23 P3 C20 173.2(7) C25 C23 P3 C20 46.0(8) C24 C23 P3 C19 66.1(7) C25 C23 P3 C19 -61.1(8) C24 C23 P3 Ni1 -54.2(7) C25 C23 P3 Ni1 178.6(6) C21 C20 P3 C23 -178.2(7) C22 C20 P3 C23 59.6(7) C21 C20 P3 C19 -71.1(7) C22 C20 P3 C19 166.6(7) C21 C20 P3 Ni1 47.3(8) C22 C20 P3 Ni1 -75.0(7) C18 C19 P3 C23 -150.4(7) C18 C19 P3 C20 102.8(7) C18 C19 P3 Ni1 -21.8(7) C28 C26 P4 C18 170.9(7) C27 C26 P4 C18 -67.1(8) C28 C26 P4 C29 63.6(8) C27 C26 P4 C29 -174.5(7) C28 C26 P4 Ni1 -71.2(8) C27 C26 P4 Ni1 50.7(8) C19 C18 P4 C26 100.9(8) C19 C18 P4 C29 -151.1(7) C19 C18 P4 Ni1 -24.5(8) C30 C29 P4 C26 179.7(7) C31 C29 P4 C26 51.8(10) C30 C29 P4 C18 71.5(8) C31 C29 P4 C18 -56.3(10) C30 C29 P4 Ni1 -46.4(8) C31 C29 P4 Ni1 -174.3(7)