#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:51:45 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257541 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705243.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_7705243 loop_ _publ_author_name 'Melle, Philipp' 'S\'egaud, Nathalie' 'Albrecht, Martin' _publ_section_title ; Ambidentate bonding and electrochemical implications of pincer-type pyridylidene amide ligands in complexes of nickel, cobalt and zinc. ; _journal_issue 36 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12662 _journal_page_last 12673 _journal_paper_doi 10.1039/d0dt02482a _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C38 H34 N10 Ni O4, 2(F6 P)' _chemical_formula_sum 'C38 H34 F12 N10 Ni O4 P2' _chemical_formula_weight 1043.40 _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 geom _atom_sites_solution_primary dual _audit_creation_date 2019-02-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-13 deposited with the CCDC. 2020-08-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.2670(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.9760(2) _cell_length_b 21.8343(3) _cell_length_c 16.1933(2) _cell_measurement_reflns_used 6188 _cell_measurement_temperature 173.00(10) _cell_measurement_theta_max 24.6440 _cell_measurement_theta_min 1.8580 _cell_volume 4231.03(11) _computing_cell_refinement 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 173.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0965 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.922 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -16.00 112.00 1.00 50.00 -- 27.42 77.00 150.00 128 2 \w 35.00 122.00 1.00 50.00 -- 27.42 178.00 120.00 87 3 \w -49.00 65.00 1.00 50.00 -- 27.42 -57.00 120.00 114 4 \w -10.00 103.00 1.00 50.00 -- 27.42 57.00 -90.00 113 5 \w -47.00 -6.00 1.00 50.00 -- 27.42 132.00-149.82 41 6 \w -10.00 79.00 1.00 50.00 -- 27.42 57.00 60.00 89 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0405869000 _diffrn_orient_matrix_UB_12 0.0014329000 _diffrn_orient_matrix_UB_13 -0.0306647000 _diffrn_orient_matrix_UB_21 0.0113804000 _diffrn_orient_matrix_UB_22 -0.0316294000 _diffrn_orient_matrix_UB_23 0.0056551000 _diffrn_orient_matrix_UB_31 -0.0416823000 _diffrn_orient_matrix_UB_32 -0.0072517000 _diffrn_orient_matrix_UB_33 -0.0308118000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_unetI/netI 0.0843 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.922 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 36391 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.922 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.151 _diffrn_reflns_theta_min 1.566 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.90268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.638 _exptl_crystal_description needle _exptl_crystal_F_000 2120 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.654 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.084 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 608 _refine_ls_number_reflns 9541 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.0651 _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^)+(0.0544P)^2^+5.7171P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1344 _refine_ls_wR_factor_ref 0.1578 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6036 _reflns_number_total 9541 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02482a2.cif _cod_data_source_block 19MA33_PM295 _cod_depositor_comments 'Adding full bibliography for 7705237--7705245.cif.' _cod_database_code 7705243 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula C38H34F12N10Ni1O4P2 _chemical_oxdiff_usercomment PM295 _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. ; _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C42(H42), C40(H40), C20(H20), C15(H15), C41(H41), C14(H14), C31(H31), C13(H13), C47(H47), C5(H5), C50(H50), C21(H21), C23(H23), C4(H4), C22(H22), C2(H2), C48(H48), C30(H30), C3(H3), C49(H49), C28(H28), C29(H29) 2.b Idealised Me refined as rotating group: C52(H52A,H52B,H52C), C26(H26A,H26B,H26C), C33(H33A,H33B,H33C), C25(H25A,H25B, H25C) ; _shelx_res_file ; 19ma33_c4.res created by SHELXL-2014/7 TITL 19ma33_c4_a.res in P2(1)/n REM Old TITL 19MA33_C4 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.166, Rweak 0.017, Alpha 0.048, Orientation as input REM Formula found by SHELXT: C4 N9 O6 F10 P2 Ni CELL 0.71073 11.976 21.8343 16.1933 90 92.267 90 ZERR 4 0.0002 0.0003 0.0002 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N Ni O P UNIT 152 136 48 40 4 16 8 L.S. 40 PLAN 5 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.054400 5.717100 FVAR 0.19234 NI1 5 0.424803 0.193726 0.499223 11.00000 0.02364 0.01889 = 0.02174 0.00179 0.00096 0.00163 P2 7 0.553126 0.501781 0.763624 11.00000 0.04377 0.03911 = 0.04625 -0.00430 0.00360 0.00185 P1 7 0.418809 0.144887 0.827437 11.00000 0.06260 0.03673 = 0.04076 0.00337 -0.01024 0.00346 O17 6 0.355613 0.256251 0.589871 11.00000 0.03310 0.02464 = 0.02499 -0.00033 0.00194 0.00511 O9 6 0.452349 0.162412 0.375246 11.00000 0.03285 0.02642 = 0.02055 0.00081 0.00004 0.00672 O36 6 0.761725 0.211058 0.575184 11.00000 0.02383 0.03123 = 0.04598 -0.00077 0.00146 -0.00258 O44 6 0.280810 0.029199 0.569848 11.00000 0.03075 0.02501 = 0.04621 0.00713 -0.00009 -0.00487 N11 4 0.354456 0.259476 0.429805 11.00000 0.02239 0.02149 = 0.01965 -0.00022 0.00244 0.00073 N38 4 0.511464 0.127342 0.555331 11.00000 0.02456 0.02125 = 0.01766 0.00154 0.00003 0.00101 N7 4 0.418675 0.193444 0.238193 11.00000 0.03470 0.02654 = 0.02219 0.00022 0.00316 0.00633 N45 4 0.301678 0.127132 0.516086 11.00000 0.02140 0.02094 = 0.02730 0.00278 0.00136 0.00143 N18 4 0.274051 0.354172 0.594068 11.00000 0.02921 0.02279 = 0.02707 -0.00309 0.00219 0.00037 N34 4 0.584426 0.234047 0.519838 11.00000 0.02750 0.02022 = 0.02942 0.00250 0.00212 0.00110 N24 4 0.246696 0.416717 0.704465 11.00000 0.02830 0.02673 = 0.03744 -0.00969 0.00624 0.00137 N1 4 0.471695 0.142089 0.121940 11.00000 0.03825 0.02955 = 0.02202 0.00377 0.00217 0.00942 N51 4 0.118684 0.139104 0.564186 11.00000 0.02558 0.02668 = 0.03034 0.00143 0.00140 -0.00452 F10 3 0.547223 0.512776 0.668117 11.00000 0.15365 0.05654 = 0.04611 0.00336 -0.00434 0.00796 F11 3 0.583571 0.570845 0.781946 11.00000 0.09311 0.05976 = 0.09064 -0.02932 0.02824 -0.03391 F3 3 0.529577 0.112463 0.860137 11.00000 0.04524 0.08622 = 0.13849 0.01559 -0.01637 0.00502 C8 1 0.415510 0.197890 0.320153 11.00000 0.02447 0.02432 = 0.02502 -0.00054 0.00270 0.00008 N27 4 0.620250 0.330304 0.582724 11.00000 0.04161 0.02287 = 0.04415 -0.00364 0.01392 -0.00077 F1 3 0.300196 0.173483 0.801055 11.00000 0.10606 0.09351 = 0.07573 -0.00157 -0.02772 0.04722 C16 1 0.314080 0.304254 0.558067 11.00000 0.02380 0.01982 = 0.02657 -0.00201 0.00350 0.00316 C39 1 0.461327 0.073986 0.569046 11.00000 0.02839 0.02089 = 0.02194 0.00338 0.00298 0.00155 F4 3 0.388208 0.088386 0.769071 11.00000 0.11317 0.06561 = 0.09487 -0.01952 -0.02465 0.00509 C37 1 0.621351 0.133726 0.569056 11.00000 0.02487 0.02181 = 0.02166 0.00005 0.00031 0.00210 F12 3 0.519489 0.432896 0.745339 11.00000 0.17927 0.03356 = 0.10818 -0.01511 0.06593 -0.01155 C10 1 0.360788 0.256230 0.347559 11.00000 0.02570 0.02378 = 0.02419 0.00218 -0.00006 -0.00068 C12 1 0.310157 0.308207 0.465319 11.00000 0.02132 0.02527 = 0.02684 -0.00168 0.00203 0.00132 C46 1 0.189312 0.135647 0.500262 11.00000 0.02803 0.02023 = 0.03026 -0.00039 0.00184 -0.00263 C35 1 0.664024 0.197484 0.555010 11.00000 0.02689 0.02369 = 0.02588 -0.00001 0.00509 0.00134 C42 1 0.686579 0.085148 0.595099 11.00000 0.02526 0.03003 = 0.03064 0.00308 0.00099 0.00330 AFIX 43 H42 2 0.763257 0.089892 0.604167 11.00000 -1.20000 AFIX 0 C43 1 0.337278 0.074339 0.552295 11.00000 0.02806 0.02626 = 0.02502 -0.00038 0.00281 -0.00180 F6 3 0.360780 0.108081 0.898156 11.00000 0.07464 0.16463 = 0.08388 0.05527 0.00540 -0.00365 C40 1 0.521743 0.023661 0.595852 11.00000 0.03253 0.02154 = 0.03520 0.00703 -0.00182 -0.00232 AFIX 43 H40 2 0.486113 -0.013294 0.605868 11.00000 -1.20000 AFIX 0 C6 1 0.439539 0.138954 0.202434 11.00000 0.02518 0.03191 = 0.02110 -0.00079 0.00237 0.00514 C20 1 0.259233 0.311404 0.735152 11.00000 0.04111 0.03055 = 0.02803 -0.00416 0.00674 -0.00285 AFIX 43 H20 2 0.272580 0.271235 0.719187 11.00000 -1.20000 AFIX 0 C15 1 0.320805 0.303006 0.297384 11.00000 0.03885 0.02955 = 0.02206 0.00464 0.00260 0.00575 AFIX 43 H15 2 0.324964 0.300417 0.240264 11.00000 -1.20000 AFIX 0 C32 1 0.604910 0.295672 0.513331 11.00000 0.02375 0.02486 = 0.03632 0.00165 0.00938 0.00036 C19 1 0.262660 0.358272 0.676506 11.00000 0.02276 0.02729 = 0.03123 -0.00495 0.00479 0.00039 C41 1 0.636220 0.028983 0.607627 11.00000 0.03254 0.02624 = 0.03845 0.00713 -0.00207 0.00856 AFIX 43 H41 2 0.679029 -0.004801 0.623798 11.00000 -1.20000 AFIX 0 C14 1 0.274485 0.353750 0.333633 11.00000 0.04311 0.03241 = 0.03530 0.00934 0.00264 0.01093 AFIX 43 H14 2 0.247124 0.385814 0.300887 11.00000 -1.20000 AFIX 0 C31 1 0.599246 0.325433 0.437437 11.00000 0.03188 0.03220 = 0.04710 0.00902 0.00679 -0.00078 AFIX 43 H31 2 0.587707 0.302579 0.389390 11.00000 -1.20000 AFIX 0 C13 1 0.268797 0.356882 0.418465 11.00000 0.03753 0.02672 = 0.03113 0.00199 0.00498 0.01237 AFIX 43 H13 2 0.237930 0.390862 0.443616 11.00000 -1.20000 AFIX 0 C47 1 0.145184 0.145138 0.421243 11.00000 0.03239 0.04752 = 0.02956 -0.00519 -0.00139 0.00405 AFIX 43 H47 2 0.191980 0.144069 0.376783 11.00000 -1.20000 AFIX 0 C5 1 0.422223 0.080128 0.234478 11.00000 0.05248 0.03042 = 0.02599 -0.00114 0.00710 0.00305 AFIX 43 H5 2 0.402575 0.076158 0.289210 11.00000 -1.20000 AFIX 0 C50 1 0.007813 0.148207 0.550239 11.00000 0.02635 0.03554 = 0.04410 -0.00580 0.00823 -0.00320 AFIX 43 H50 2 -0.039104 0.148293 0.594651 11.00000 -1.20000 AFIX 0 C21 1 0.236475 0.323681 0.815993 11.00000 0.03845 0.04735 = 0.03190 -0.00014 0.00517 -0.00165 AFIX 43 H21 2 0.232417 0.291963 0.854087 11.00000 -1.20000 AFIX 0 F9 3 0.427744 0.518281 0.769016 11.00000 0.04381 0.13347 = 0.22702 -0.11693 0.02108 -0.01310 C52 1 0.163577 0.136171 0.650264 11.00000 0.03832 0.04822 = 0.02557 0.00461 0.00312 0.00172 AFIX 137 H52A 2 0.180650 0.094425 0.664440 11.00000 -1.50000 H52B 2 0.108972 0.151749 0.686680 11.00000 -1.50000 H52C 2 0.230319 0.160430 0.655680 11.00000 -1.50000 AFIX 0 C26 1 0.492634 0.202730 0.085688 11.00000 0.05374 0.03626 = 0.02492 0.00914 0.00948 0.01314 AFIX 137 H26A 2 0.424765 0.226172 0.083967 11.00000 -1.50000 H26B 2 0.518106 0.197740 0.030621 11.00000 -1.50000 H26C 2 0.548669 0.223777 0.118862 11.00000 -1.50000 AFIX 0 C23 1 0.226655 0.429391 0.783732 11.00000 0.03176 0.04133 = 0.04148 -0.01965 0.00788 -0.00200 AFIX 43 H23 2 0.217569 0.469916 0.799825 11.00000 -1.20000 AFIX 0 C4 1 0.433217 0.029013 0.188242 11.00000 0.06553 0.02794 = 0.03463 0.00040 0.00707 -0.00115 AFIX 43 H4 2 0.419999 -0.009405 0.210648 11.00000 -1.20000 AFIX 0 C22 1 0.219459 0.384301 0.840518 11.00000 0.03204 0.06424 = 0.03665 -0.01748 0.00590 -0.00076 AFIX 43 H22 2 0.203488 0.393421 0.894895 11.00000 -1.20000 AFIX 0 F2 3 0.444725 0.198426 0.885188 11.00000 0.30554 0.06393 = 0.13878 -0.05570 -0.13704 0.04624 C2 1 0.482147 0.091461 0.075296 11.00000 0.06177 0.04546 = 0.02507 -0.00449 0.00229 0.01921 AFIX 43 H2 2 0.501767 0.095397 0.020553 11.00000 -1.20000 AFIX 0 F7 3 0.677964 0.485162 0.755670 11.00000 0.06037 0.23865 = 0.15071 -0.11112 -0.04051 0.07411 C48 1 0.033304 0.156115 0.407460 11.00000 0.03653 0.07419 = 0.03564 -0.01224 -0.00847 0.01307 AFIX 43 H48 2 0.004468 0.162807 0.354053 11.00000 -1.20000 AFIX 0 C33 1 0.617988 0.302240 0.665139 11.00000 0.05784 0.03682 = 0.03543 -0.00426 -0.00062 0.00295 AFIX 137 H33A 2 0.558801 0.272620 0.665944 11.00000 -1.50000 H33B 2 0.605548 0.333384 0.705600 11.00000 -1.50000 H33C 2 0.688137 0.282385 0.677705 11.00000 -1.50000 AFIX 0 C30 1 0.610270 0.387553 0.431909 11.00000 0.05505 0.03528 = 0.05866 0.01499 0.01054 0.00022 AFIX 43 H30 2 0.605291 0.407021 0.380815 11.00000 -1.20000 AFIX 0 C25 1 0.256655 0.467956 0.645642 11.00000 0.05270 0.02485 = 0.05479 -0.00333 0.00442 -0.00027 AFIX 137 H25A 2 0.332347 0.470637 0.628550 11.00000 -1.50000 H25B 2 0.236435 0.505545 0.671930 11.00000 -1.50000 H25C 2 0.207655 0.460985 0.598219 11.00000 -1.50000 AFIX 0 F5 3 0.471397 0.176175 0.755136 11.00000 0.17880 0.18187 = 0.10102 0.05960 0.02351 -0.07089 C3 1 0.464497 0.034647 0.106880 11.00000 0.07971 0.03263 = 0.03425 -0.01069 0.00893 0.00927 AFIX 43 H3 2 0.473278 0.000003 0.074362 11.00000 -1.20000 AFIX 0 C49 1 -0.036017 0.157162 0.473176 11.00000 0.02143 0.05596 = 0.05202 -0.01114 -0.00385 0.00918 AFIX 43 H49 2 -0.112248 0.163969 0.464568 11.00000 -1.20000 AFIX 0 C28 1 0.634614 0.392031 0.577173 11.00000 0.06665 0.02894 = 0.06559 -0.01424 0.01760 -0.00332 AFIX 43 H28 2 0.648607 0.414813 0.624993 11.00000 -1.20000 AFIX 0 F8 3 0.564327 0.491694 0.858349 11.00000 0.31823 0.09468 = 0.04781 0.00126 0.03546 0.04443 C29 1 0.628793 0.420646 0.503004 11.00000 0.08404 0.02268 = 0.07908 0.00931 0.02508 -0.00440 AFIX 43 H29 2 0.637398 0.462920 0.500287 11.00000 -1.20000 AFIX 0 HKLF 4 REM 19ma33_c4_a.res in P2(1)/n REM R1 = 0.0651 for 6036 Fo > 4sig(Fo) and 0.1133 for all 9541 data REM 608 parameters refined using 0 restraints END WGHT 0.0544 5.7174 REM Highest difference peak 0.654, deepest hole -0.596, 1-sigma level 0.084 Q1 1 0.4687 0.2103 0.8035 11.00000 0.05 0.65 Q2 1 0.4652 0.1214 0.7558 11.00000 0.05 0.62 Q3 1 0.6046 0.4903 0.8646 11.00000 0.05 0.62 Q4 1 0.5408 0.1257 0.7658 11.00000 0.05 0.61 Q5 1 0.6952 0.5021 0.7429 11.00000 0.05 0.59 ; _shelx_res_checksum 82863 _olex2_date_sample_data_collection 2019-02-25 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.226 _oxdiff_exptl_absorpt_empirical_full_min 0.855 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.42480(4) 0.19373(2) 0.49922(3) 0.02142(13) Uani 1 1 d . . . . . P2 P 0.55313(11) 0.50178(6) 0.76362(8) 0.0430(3) Uani 1 1 d . . . . . P1 P 0.41881(12) 0.14489(6) 0.82744(8) 0.0470(3) Uani 1 1 d . . . . . O17 O 0.3556(2) 0.25625(12) 0.58987(15) 0.0276(6) Uani 1 1 d . . . . . O9 O 0.4523(2) 0.16241(12) 0.37525(15) 0.0266(6) Uani 1 1 d . . . . . O36 O 0.7617(2) 0.21106(13) 0.57518(17) 0.0337(7) Uani 1 1 d . . . . . O44 O 0.2808(2) 0.02920(13) 0.56985(17) 0.0340(7) Uani 1 1 d . . . . . N11 N 0.3545(2) 0.25948(14) 0.42981(17) 0.0211(7) Uani 1 1 d . . . . . N38 N 0.5115(2) 0.12734(14) 0.55533(17) 0.0212(7) Uani 1 1 d . . . . . N7 N 0.4187(3) 0.19344(15) 0.23819(18) 0.0278(7) Uani 1 1 d . . . . . N45 N 0.3017(2) 0.12713(14) 0.51609(18) 0.0232(7) Uani 1 1 d . . . . . N18 N 0.2741(3) 0.35417(15) 0.59407(19) 0.0263(7) Uani 1 1 d . . . . . N34 N 0.5844(3) 0.23405(14) 0.51984(19) 0.0257(7) Uani 1 1 d . . . . . N24 N 0.2467(3) 0.41672(15) 0.7045(2) 0.0307(8) Uani 1 1 d . . . . . N1 N 0.4717(3) 0.14209(15) 0.12194(19) 0.0299(8) Uani 1 1 d . . . . . N51 N 0.1187(3) 0.13910(15) 0.56419(19) 0.0275(7) Uani 1 1 d . . . . . F10 F 0.5472(3) 0.51278(15) 0.66812(19) 0.0857(11) Uani 1 1 d . . . . . F11 F 0.5836(3) 0.57085(15) 0.7819(2) 0.0805(11) Uani 1 1 d . . . . . F3 F 0.5296(3) 0.11246(17) 0.8601(2) 0.0905(12) Uani 1 1 d . . . . . C8 C 0.4155(3) 0.19789(18) 0.3202(2) 0.0246(8) Uani 1 1 d . . . . . N27 N 0.6202(3) 0.33030(16) 0.5827(2) 0.0359(9) Uani 1 1 d . . . . . F1 F 0.3002(3) 0.17348(18) 0.8011(2) 0.0926(12) Uani 1 1 d . . . . . C16 C 0.3141(3) 0.30425(17) 0.5581(2) 0.0233(8) Uani 1 1 d . . . . . C39 C 0.4613(3) 0.07399(17) 0.5690(2) 0.0237(8) Uani 1 1 d . . . . . F4 F 0.3882(3) 0.08839(16) 0.7691(2) 0.0920(12) Uani 1 1 d . . . . . C37 C 0.6214(3) 0.13373(17) 0.5691(2) 0.0228(8) Uani 1 1 d . . . . . F12 F 0.5195(4) 0.43290(15) 0.7453(2) 0.1054(15) Uani 1 1 d . . . . . C10 C 0.3608(3) 0.25623(18) 0.3476(2) 0.0246(8) Uani 1 1 d . . . . . C12 C 0.3102(3) 0.30821(18) 0.4653(2) 0.0244(8) Uani 1 1 d . . . . . C46 C 0.1893(3) 0.13565(18) 0.5003(2) 0.0262(9) Uani 1 1 d . . . . . C35 C 0.6640(3) 0.19748(18) 0.5550(2) 0.0254(8) Uani 1 1 d . . . . . C42 C 0.6866(3) 0.08515(18) 0.5951(2) 0.0286(9) Uani 1 1 d . . . . . H42 H 0.7633 0.0899 0.6042 0.034 Uiso 1 1 calc R . . . . C43 C 0.3373(3) 0.07434(18) 0.5523(2) 0.0264(9) Uani 1 1 d . . . . . F6 F 0.3608(3) 0.1081(2) 0.8982(2) 0.1077(15) Uani 1 1 d . . . . . C40 C 0.5217(3) 0.02366(19) 0.5959(2) 0.0298(9) Uani 1 1 d . . . . . H40 H 0.4861 -0.0133 0.6059 0.036 Uiso 1 1 calc R . . . . C6 C 0.4395(3) 0.13895(19) 0.2024(2) 0.0260(9) Uani 1 1 d . . . . . C20 C 0.2592(3) 0.3114(2) 0.7352(2) 0.0331(10) Uani 1 1 d . . . . . H20 H 0.2726 0.2712 0.7192 0.040 Uiso 1 1 calc R . . . . C15 C 0.3208(3) 0.30301(19) 0.2974(2) 0.0301(9) Uani 1 1 d . . . . . H15 H 0.3250 0.3004 0.2403 0.036 Uiso 1 1 calc R . . . . C32 C 0.6049(3) 0.29567(18) 0.5133(2) 0.0281(9) Uani 1 1 d . . . . . C19 C 0.2627(3) 0.35827(18) 0.6765(2) 0.0270(9) Uani 1 1 d . . . . . C41 C 0.6362(3) 0.02898(19) 0.6076(2) 0.0325(10) Uani 1 1 d . . . . . H41 H 0.6790 -0.0048 0.6238 0.039 Uiso 1 1 calc R . . . . C14 C 0.2745(4) 0.3538(2) 0.3336(3) 0.0369(10) Uani 1 1 d . . . . . H14 H 0.2471 0.3858 0.3009 0.044 Uiso 1 1 calc R . . . . C31 C 0.5992(3) 0.3254(2) 0.4374(3) 0.0369(10) Uani 1 1 d . . . . . H31 H 0.5877 0.3026 0.3894 0.044 Uiso 1 1 calc R . . . . C13 C 0.2688(3) 0.35688(19) 0.4185(2) 0.0317(9) Uani 1 1 d . . . . . H13 H 0.2379 0.3909 0.4436 0.038 Uiso 1 1 calc R . . . . C47 C 0.1452(3) 0.1451(2) 0.4212(3) 0.0366(10) Uani 1 1 d . . . . . H47 H 0.1920 0.1441 0.3768 0.044 Uiso 1 1 calc R . . . . C5 C 0.4222(4) 0.0801(2) 0.2345(3) 0.0362(10) Uani 1 1 d . . . . . H5 H 0.4026 0.0762 0.2892 0.043 Uiso 1 1 calc R . . . . C50 C 0.0078(3) 0.1482(2) 0.5502(3) 0.0351(10) Uani 1 1 d . . . . . H50 H -0.0391 0.1483 0.5947 0.042 Uiso 1 1 calc R . . . . C21 C 0.2365(4) 0.3237(2) 0.8160(3) 0.0391(11) Uani 1 1 d . . . . . H21 H 0.2324 0.2920 0.8541 0.047 Uiso 1 1 calc R . . . . F9 F 0.4277(3) 0.5183(2) 0.7690(3) 0.134(2) Uani 1 1 d . . . . . C52 C 0.1636(4) 0.1362(2) 0.6503(2) 0.0373(10) Uani 1 1 d . . . . . H52A H 0.1806 0.0944 0.6644 0.056 Uiso 1 1 calc GR . . . . H52B H 0.1090 0.1517 0.6867 0.056 Uiso 1 1 calc GR . . . . H52C H 0.2303 0.1604 0.6557 0.056 Uiso 1 1 calc GR . . . . C26 C 0.4926(4) 0.2027(2) 0.0857(2) 0.0381(11) Uani 1 1 d . . . . . H26A H 0.4248 0.2262 0.0840 0.057 Uiso 1 1 calc GR . . . . H26B H 0.5181 0.1977 0.0306 0.057 Uiso 1 1 calc GR . . . . H26C H 0.5487 0.2238 0.1189 0.057 Uiso 1 1 calc GR . . . . C23 C 0.2267(3) 0.4294(2) 0.7837(3) 0.0380(11) Uani 1 1 d . . . . . H23 H 0.2176 0.4699 0.7998 0.046 Uiso 1 1 calc R . . . . C4 C 0.4332(4) 0.0290(2) 0.1882(3) 0.0426(11) Uani 1 1 d . . . . . H4 H 0.4200 -0.0094 0.2106 0.051 Uiso 1 1 calc R . . . . C22 C 0.2195(4) 0.3843(2) 0.8405(3) 0.0442(12) Uani 1 1 d . . . . . H22 H 0.2035 0.3934 0.8949 0.053 Uiso 1 1 calc R . . . . F2 F 0.4447(6) 0.19843(19) 0.8852(3) 0.173(3) Uani 1 1 d . . . . . C2 C 0.4821(4) 0.0915(2) 0.0753(3) 0.0441(12) Uani 1 1 d . . . . . H2 H 0.5018 0.0954 0.0206 0.053 Uiso 1 1 calc R . . . . F7 F 0.6780(3) 0.4852(3) 0.7557(3) 0.151(2) Uani 1 1 d . . . . . C48 C 0.0333(4) 0.1561(2) 0.4075(3) 0.0491(13) Uani 1 1 d . . . . . H48 H 0.0045 0.1628 0.3541 0.059 Uiso 1 1 calc R . . . . C33 C 0.6180(4) 0.3022(2) 0.6651(3) 0.0434(11) Uani 1 1 d . . . . . H33A H 0.5588 0.2726 0.6659 0.065 Uiso 1 1 calc GR . . . . H33B H 0.6055 0.3334 0.7056 0.065 Uiso 1 1 calc GR . . . . H33C H 0.6881 0.2824 0.6777 0.065 Uiso 1 1 calc GR . . . . C30 C 0.6103(4) 0.3876(2) 0.4319(3) 0.0494(13) Uani 1 1 d . . . . . H30 H 0.6053 0.4070 0.3808 0.059 Uiso 1 1 calc R . . . . C25 C 0.2567(4) 0.4680(2) 0.6456(3) 0.0441(11) Uani 1 1 d . . . . . H25A H 0.3323 0.4706 0.6285 0.066 Uiso 1 1 calc GR . . . . H25B H 0.2364 0.5055 0.6719 0.066 Uiso 1 1 calc GR . . . . H25C H 0.2077 0.4610 0.5982 0.066 Uiso 1 1 calc GR . . . . F5 F 0.4714(5) 0.1762(3) 0.7551(3) 0.153(2) Uani 1 1 d . . . . . C3 C 0.4645(4) 0.0346(2) 0.1069(3) 0.0487(13) Uani 1 1 d . . . . . H3 H 0.4733 0.0000 0.0744 0.058 Uiso 1 1 calc R . . . . C49 C -0.0360(3) 0.1572(2) 0.4732(3) 0.0433(12) Uani 1 1 d . . . . . H49 H -0.1122 0.1640 0.4646 0.052 Uiso 1 1 calc R . . . . C28 C 0.6346(4) 0.3920(2) 0.5772(3) 0.0533(14) Uani 1 1 d . . . . . H28 H 0.6486 0.4148 0.6250 0.064 Uiso 1 1 calc R . . . . F8 F 0.5643(5) 0.4917(2) 0.8583(2) 0.153(2) Uani 1 1 d . . . . . C29 C 0.6288(5) 0.4206(2) 0.5030(4) 0.0614(15) Uani 1 1 d . . . . . H29 H 0.6374 0.4629 0.5003 0.074 Uiso 1 1 calc 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 0.0236(2) 0.0189(3) 0.0217(2) 0.0018(2) 0.00096(18) 0.0016(2) P2 0.0438(7) 0.0391(7) 0.0462(7) -0.0043(6) 0.0036(5) 0.0019(6) P1 0.0626(9) 0.0367(7) 0.0408(7) 0.0034(6) -0.0102(6) 0.0035(7) O17 0.0331(15) 0.0246(15) 0.0250(14) -0.0003(12) 0.0019(11) 0.0051(12) O9 0.0329(15) 0.0264(15) 0.0206(13) 0.0008(12) 0.0000(11) 0.0067(12) O36 0.0238(14) 0.0312(16) 0.0460(17) -0.0008(14) 0.0015(12) -0.0026(13) O44 0.0308(15) 0.0250(16) 0.0462(17) 0.0071(13) -0.0001(13) -0.0049(13) N11 0.0224(16) 0.0215(17) 0.0196(15) -0.0002(13) 0.0024(12) 0.0007(13) N38 0.0246(16) 0.0212(17) 0.0177(15) 0.0015(13) 0.0000(12) 0.0010(14) N7 0.0347(18) 0.0265(18) 0.0222(16) 0.0002(14) 0.0032(13) 0.0063(16) N45 0.0214(15) 0.0209(17) 0.0273(17) 0.0028(14) 0.0014(12) 0.0014(14) N18 0.0292(18) 0.0228(18) 0.0271(17) -0.0031(14) 0.0022(13) 0.0004(15) N34 0.0275(17) 0.0202(17) 0.0294(18) 0.0025(14) 0.0021(14) 0.0011(14) N24 0.0283(18) 0.0267(19) 0.0374(19) -0.0097(16) 0.0062(14) 0.0014(15) N1 0.0383(19) 0.0296(19) 0.0220(17) 0.0038(15) 0.0022(14) 0.0094(16) N51 0.0256(17) 0.0267(19) 0.0303(18) 0.0014(15) 0.0014(13) -0.0045(15) F10 0.154(4) 0.057(2) 0.0461(19) 0.0034(16) -0.004(2) 0.008(2) F11 0.093(3) 0.060(2) 0.091(2) -0.0293(19) 0.028(2) -0.034(2) F3 0.0452(18) 0.086(3) 0.138(3) 0.016(2) -0.0164(19) 0.0050(19) C8 0.0245(19) 0.024(2) 0.0250(19) -0.0005(17) 0.0027(15) 0.0001(17) N27 0.042(2) 0.0229(19) 0.044(2) -0.0036(17) 0.0139(17) -0.0008(17) F1 0.106(3) 0.094(3) 0.076(2) -0.002(2) -0.028(2) 0.047(2) C16 0.0238(18) 0.020(2) 0.0266(19) -0.0020(17) 0.0035(15) 0.0032(17) C39 0.028(2) 0.021(2) 0.0219(19) 0.0034(16) 0.0030(15) 0.0016(17) F4 0.113(3) 0.066(2) 0.095(3) -0.020(2) -0.025(2) 0.005(2) C37 0.0249(19) 0.022(2) 0.0217(18) 0.0001(16) 0.0003(15) 0.0021(16) F12 0.179(4) 0.0336(19) 0.108(3) -0.0151(19) 0.066(3) -0.012(2) C10 0.026(2) 0.024(2) 0.0242(19) 0.0022(16) -0.0001(15) -0.0007(17) C12 0.0213(18) 0.025(2) 0.0268(19) -0.0017(17) 0.0020(15) 0.0013(17) C46 0.028(2) 0.020(2) 0.030(2) -0.0004(17) 0.0018(16) -0.0026(17) C35 0.027(2) 0.024(2) 0.0259(19) 0.0000(17) 0.0051(15) 0.0013(17) C42 0.025(2) 0.030(2) 0.031(2) 0.0031(18) 0.0010(16) 0.0033(18) C43 0.028(2) 0.026(2) 0.025(2) -0.0004(17) 0.0028(16) -0.0018(18) F6 0.075(2) 0.165(4) 0.084(3) 0.055(3) 0.005(2) -0.004(3) C40 0.033(2) 0.022(2) 0.035(2) 0.0070(18) -0.0018(17) -0.0023(18) C6 0.025(2) 0.032(2) 0.0211(19) -0.0008(17) 0.0024(15) 0.0051(18) C20 0.041(2) 0.031(2) 0.028(2) -0.0042(19) 0.0067(18) -0.003(2) C15 0.039(2) 0.030(2) 0.0221(19) 0.0046(18) 0.0026(16) 0.006(2) C32 0.0237(19) 0.025(2) 0.036(2) 0.0017(18) 0.0094(16) 0.0004(17) C19 0.0228(19) 0.027(2) 0.031(2) -0.0050(18) 0.0048(16) 0.0004(17) C41 0.033(2) 0.026(2) 0.038(2) 0.0071(19) -0.0021(18) 0.0086(19) C14 0.043(3) 0.032(2) 0.035(2) 0.009(2) 0.0026(19) 0.011(2) C31 0.032(2) 0.032(2) 0.047(3) 0.009(2) 0.0068(19) -0.001(2) C13 0.038(2) 0.027(2) 0.031(2) 0.0020(18) 0.0050(17) 0.0124(19) C47 0.032(2) 0.048(3) 0.030(2) -0.005(2) -0.0014(17) 0.004(2) C5 0.052(3) 0.030(2) 0.026(2) -0.0011(19) 0.0071(19) 0.003(2) C50 0.026(2) 0.036(3) 0.044(3) -0.006(2) 0.0082(18) -0.0032(19) C21 0.038(2) 0.047(3) 0.032(2) 0.000(2) 0.0052(19) -0.002(2) F9 0.044(2) 0.133(4) 0.227(5) -0.117(4) 0.021(3) -0.013(2) C52 0.038(2) 0.048(3) 0.026(2) 0.005(2) 0.0031(18) 0.002(2) C26 0.054(3) 0.036(3) 0.025(2) 0.0091(19) 0.0095(19) 0.013(2) C23 0.032(2) 0.041(3) 0.041(3) -0.020(2) 0.0079(19) -0.002(2) C4 0.066(3) 0.028(2) 0.035(2) 0.000(2) 0.007(2) -0.001(2) C22 0.032(2) 0.064(4) 0.037(3) -0.017(2) 0.0059(19) -0.001(2) F2 0.306(7) 0.064(3) 0.139(4) -0.056(3) -0.137(5) 0.046(4) C2 0.062(3) 0.045(3) 0.025(2) -0.004(2) 0.002(2) 0.019(3) F7 0.060(2) 0.239(6) 0.151(4) -0.111(4) -0.041(2) 0.074(3) C48 0.037(3) 0.074(4) 0.036(3) -0.012(3) -0.008(2) 0.013(3) C33 0.058(3) 0.037(3) 0.035(2) -0.004(2) -0.001(2) 0.003(2) C30 0.055(3) 0.035(3) 0.059(3) 0.015(3) 0.011(2) 0.000(2) C25 0.053(3) 0.025(2) 0.055(3) -0.003(2) 0.004(2) 0.000(2) F5 0.179(5) 0.182(5) 0.101(3) 0.060(3) 0.024(3) -0.071(4) C3 0.080(4) 0.033(3) 0.034(3) -0.011(2) 0.009(2) 0.009(3) C49 0.021(2) 0.056(3) 0.052(3) -0.011(2) -0.0039(19) 0.009(2) C28 0.067(4) 0.029(3) 0.066(3) -0.014(3) 0.018(3) -0.003(3) F8 0.318(7) 0.095(3) 0.048(2) 0.001(2) 0.035(3) 0.044(4) C29 0.084(4) 0.023(3) 0.079(4) 0.009(3) 0.025(3) -0.004(3) 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' F F 0.0171 0.0103 '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' 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' 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 O9 Ni1 O17 153.66(10) . . ? N11 Ni1 O17 76.47(11) . . ? N11 Ni1 O9 77.29(11) . . ? N11 Ni1 N45 106.84(12) . . ? N11 Ni1 N34 98.53(12) . . ? N38 Ni1 O17 110.70(11) . . ? N38 Ni1 O9 95.63(11) . . ? N38 Ni1 N11 171.43(12) . . ? N38 Ni1 N45 77.96(12) . . ? N38 Ni1 N34 77.22(12) . . ? N45 Ni1 O17 93.34(11) . . ? N45 Ni1 O9 92.04(11) . . ? N45 Ni1 N34 154.48(12) . . ? N34 Ni1 O17 89.90(11) . . ? N34 Ni1 O9 96.20(11) . . ? F10 P2 F11 92.31(19) . . ? F10 P2 F12 87.7(2) . . ? F11 P2 F12 178.6(2) . . ? F9 P2 F10 90.8(3) . . ? F9 P2 F11 89.1(2) . . ? F9 P2 F12 89.5(2) . . ? F9 P2 F8 91.3(3) . . ? F7 P2 F10 87.7(3) . . ? F7 P2 F11 91.3(3) . . ? F7 P2 F12 90.1(3) . . ? F7 P2 F9 178.5(3) . . ? F7 P2 F8 90.2(3) . . ? F8 P2 F10 177.5(3) . . ? F8 P2 F11 86.5(2) . . ? F8 P2 F12 93.5(2) . . ? F3 P1 F1 174.1(2) . . ? F3 P1 F4 91.3(2) . . ? F3 P1 F6 85.2(2) . . ? F4 P1 F1 87.9(2) . . ? F6 P1 F1 88.9(2) . . ? F6 P1 F4 86.5(2) . . ? F2 P1 F3 89.4(3) . . ? F2 P1 F1 91.2(3) . . ? F2 P1 F4 178.0(3) . . ? F2 P1 F6 91.7(3) . . ? F5 P1 F3 95.3(3) . . ? F5 P1 F1 90.5(3) . . ? F5 P1 F4 89.1(3) . . ? F5 P1 F6 175.5(3) . . ? F5 P1 F2 92.7(4) . . ? C16 O17 Ni1 113.4(2) . . ? C8 O9 Ni1 113.9(2) . . ? C10 N11 Ni1 119.0(2) . . ? C12 N11 Ni1 120.0(2) . . ? C12 N11 C10 120.8(3) . . ? C39 N38 Ni1 119.0(2) . . ? C39 N38 C37 120.8(3) . . ? C37 N38 Ni1 119.7(3) . . ? C8 N7 C6 120.3(3) . . ? C46 N45 Ni1 124.8(3) . . ? C43 N45 Ni1 115.8(2) . . ? C43 N45 C46 119.1(3) . . ? C16 N18 C19 122.6(3) . . ? C35 N34 Ni1 116.0(2) . . ? C35 N34 C32 119.1(3) . . ? C32 N34 Ni1 123.9(3) . . ? C19 N24 C25 118.5(3) . . ? C23 N24 C19 122.7(4) . . ? C23 N24 C25 118.8(4) . . ? C6 N1 C26 118.7(3) . . ? C2 N1 C6 121.7(4) . . ? C2 N1 C26 119.5(3) . . ? C46 N51 C52 120.0(3) . . ? C50 N51 C46 121.0(3) . . ? C50 N51 C52 118.9(3) . . ? O9 C8 N7 130.0(4) . . ? O9 C8 C10 117.3(3) . . ? N7 C8 C10 112.6(3) . . ? C32 N27 C33 120.8(4) . . ? C32 N27 C28 120.6(4) . . ? C28 N27 C33 118.6(4) . . ? O17 C16 N18 130.0(3) . . ? O17 C16 C12 116.9(3) . . ? N18 C16 C12 113.1(3) . . ? N38 C39 C43 114.5(3) . . ? N38 C39 C40 121.0(3) . . ? C40 C39 C43 124.5(4) . . ? N38 C37 C35 114.3(3) . . ? N38 C37 C42 121.1(4) . . ? C42 C37 C35 124.7(3) . . ? N11 C10 C8 112.3(3) . . ? N11 C10 C15 121.0(4) . . ? C15 C10 C8 126.7(3) . . ? N11 C12 C16 112.9(3) . . ? N11 C12 C13 121.1(3) . . ? C13 C12 C16 126.0(3) . . ? N45 C46 C47 122.0(4) . . ? N51 C46 N45 119.9(3) . . ? N51 C46 C47 118.0(4) . . ? O36 C35 N34 127.8(4) . . ? O36 C35 C37 120.3(3) . . ? N34 C35 C37 111.9(3) . . ? C37 C42 H42 120.6 . . ? C37 C42 C41 118.9(4) . . ? C41 C42 H42 120.6 . . ? O44 C43 N45 127.8(4) . . ? O44 C43 C39 120.1(4) . . ? N45 C43 C39 112.0(3) . . ? C39 C40 H40 120.6 . . ? C39 C40 C41 118.9(4) . . ? C41 C40 H40 120.6 . . ? N7 C6 N1 115.2(3) . . ? N7 C6 C5 127.9(3) . . ? N1 C6 C5 116.5(4) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C21 C20 C19 121.1(4) . . ? C10 C15 H15 120.7 . . ? C10 C15 C14 118.7(4) . . ? C14 C15 H15 120.7 . . ? N34 C32 C31 121.6(4) . . ? N27 C32 N34 120.0(4) . . ? N27 C32 C31 118.1(4) . . ? N18 C19 N24 114.2(4) . . ? N18 C19 C20 129.1(4) . . ? N24 C19 C20 116.7(3) . . ? C42 C41 H41 120.3 . . ? C40 C41 C42 119.3(4) . . ? C40 C41 H41 120.3 . . ? C15 C14 H14 120.0 . . ? C13 C14 C15 120.0(4) . . ? C13 C14 H14 120.0 . . ? C32 C31 H31 119.3 . . ? C30 C31 C32 121.4(5) . . ? C30 C31 H31 119.3 . . ? C12 C13 H13 120.8 . . ? C14 C13 C12 118.4(4) . . ? C14 C13 H13 120.8 . . ? C46 C47 H47 119.6 . . ? C48 C47 C46 120.9(4) . . ? C48 C47 H47 119.6 . . ? C6 C5 H5 119.0 . . ? C4 C5 C6 122.1(4) . . ? C4 C5 H5 119.0 . . ? N51 C50 H50 119.4 . . ? C49 C50 N51 121.3(4) . . ? C49 C50 H50 119.4 . . ? C20 C21 H21 120.3 . . ? C20 C21 C22 119.4(4) . . ? C22 C21 H21 120.3 . . ? N51 C52 H52A 109.5 . . ? N51 C52 H52B 109.5 . . ? N51 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N1 C26 H26A 109.5 . . ? N1 C26 H26B 109.5 . . ? N1 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N24 C23 H23 119.4 . . ? N24 C23 C22 121.2(4) . . ? C22 C23 H23 119.4 . . ? C5 C4 H4 120.4 . . ? C5 C4 C3 119.2(4) . . ? C3 C4 H4 120.4 . . ? C21 C22 H22 120.6 . . ? C23 C22 C21 118.8(4) . . ? C23 C22 H22 120.6 . . ? N1 C2 H2 119.4 . . ? N1 C2 C3 121.2(4) . . ? C3 C2 H2 119.4 . . ? C47 C48 H48 120.2 . . ? C47 C48 C49 119.5(4) . . ? C49 C48 H48 120.2 . . ? N27 C33 H33A 109.5 . . ? N27 C33 H33B 109.5 . . ? N27 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C30 H30 120.6 . . ? C31 C30 C29 118.8(5) . . ? C29 C30 H30 120.6 . . ? N24 C25 H25A 109.5 . . ? N24 C25 H25B 109.5 . . ? N24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C4 C3 H3 120.4 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3 120.4 . . ? C50 C49 C48 119.3(4) . . ? C50 C49 H49 120.4 . . ? C48 C49 H49 120.4 . . ? N27 C28 H28 119.6 . . ? C29 C28 N27 120.9(5) . . ? C29 C28 H28 119.6 . . ? C30 C29 H29 119.9 . . ? C28 C29 C30 120.2(5) . . ? C28 C29 H29 119.9 . . ? 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 O17 2.191(3) . ? Ni1 O9 2.159(2) . ? Ni1 N11 1.990(3) . ? Ni1 N38 1.982(3) . ? Ni1 N45 2.096(3) . ? Ni1 N34 2.119(3) . ? P2 F10 1.564(3) . ? P2 F11 1.577(3) . ? P2 F12 1.582(4) . ? P2 F9 1.550(4) . ? P2 F7 1.549(4) . ? P2 F8 1.550(4) . ? P1 F3 1.577(3) . ? P1 F1 1.594(3) . ? P1 F4 1.588(4) . ? P1 F6 1.582(4) . ? P1 F2 1.521(4) . ? P1 F5 1.514(4) . ? O17 C16 1.261(4) . ? O9 C8 1.249(4) . ? O36 C35 1.238(4) . ? O44 C43 1.235(4) . ? N11 C10 1.339(4) . ? N11 C12 1.330(5) . ? N38 C39 1.333(5) . ? N38 C37 1.333(4) . ? N7 C8 1.333(5) . ? N7 C6 1.351(5) . ? N45 C46 1.373(5) . ? N45 C43 1.354(5) . ? N18 C16 1.334(5) . ? N18 C19 1.350(5) . ? N34 C35 1.352(5) . ? N34 C32 1.373(5) . ? N24 C19 1.370(5) . ? N24 C23 1.344(5) . ? N24 C25 1.477(5) . ? N1 C6 1.375(5) . ? N1 C26 1.474(5) . ? N1 C2 1.347(5) . ? N51 C46 1.365(5) . ? N51 C50 1.353(5) . ? N51 C52 1.475(5) . ? C8 C10 1.507(5) . ? N27 C32 1.361(5) . ? N27 C33 1.470(5) . ? N27 C28 1.362(6) . ? C16 C12 1.503(5) . ? C39 C43 1.500(5) . ? C39 C40 1.376(5) . ? C37 C35 1.503(5) . ? C37 C42 1.374(5) . ? C10 C15 1.379(5) . ? C12 C13 1.386(5) . ? C46 C47 1.381(5) . ? C42 H42 0.9300 . ? C42 C41 1.385(6) . ? C40 H40 0.9300 . ? C40 C41 1.382(5) . ? C6 C5 1.404(6) . ? C20 H20 0.9300 . ? C20 C19 1.398(6) . ? C20 C21 1.374(5) . ? C15 H15 0.9300 . ? C15 C14 1.380(6) . ? C32 C31 1.389(6) . ? C41 H41 0.9300 . ? C14 H14 0.9300 . ? C14 C13 1.380(5) . ? C31 H31 0.9300 . ? C31 C30 1.366(6) . ? C13 H13 0.9300 . ? C47 H47 0.9300 . ? C47 C48 1.371(6) . ? C5 H5 0.9300 . ? C5 C4 1.353(6) . ? C50 H50 0.9300 . ? C50 C49 1.349(6) . ? C21 H21 0.9300 . ? C21 C22 1.399(6) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C23 H23 0.9300 . ? C23 C22 1.352(7) . ? C4 H4 0.9300 . ? C4 C3 1.389(6) . ? C22 H22 0.9300 . ? C2 H2 0.9300 . ? C2 C3 1.361(6) . ? C48 H48 0.9300 . ? C48 C49 1.376(6) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C30 H30 0.9300 . ? C30 C29 1.370(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C3 H3 0.9300 . ? C49 H49 0.9300 . ? C28 H28 0.9300 . ? C28 C29 1.353(7) . ? C29 H29 0.9300 . ?