#------------------------------------------------------------------------------ #$Date: 2020-08-22 05:17:39 +0300 (Sat, 22 Aug 2020) $ #$Revision: 255576 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705242.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_7705242 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_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02482A _journal_year 2020 _chemical_formula_moiety 'C38 H34 N10 Ni O4, 2(F6 P), 3(C2 H3 N)' _chemical_formula_sum 'C44 H43 F12 N13 Ni O4 P2' _chemical_formula_weight 1166.56 _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2017-02-01T06:09:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2020-07-13 deposited with the CCDC. 2020-08-21 downloaded from the CCDC. ; _cell_angle_alpha 67.053(2) _cell_angle_beta 82.782(2) _cell_angle_gamma 82.793(2) _cell_formula_units_Z 2 _cell_length_a 12.5126(3) _cell_length_b 13.9713(4) _cell_length_c 15.2848(4) _cell_measurement_reflns_used 14469 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 26.63 _cell_measurement_theta_min 1.68 _cell_volume 2432.53(12) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 123(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0965 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.921 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0566487 _diffrn_orient_matrix_UB_12 0.0130414 _diffrn_orient_matrix_UB_13 0.0002436 _diffrn_orient_matrix_UB_21 -0.0087879 _diffrn_orient_matrix_UB_22 -0.0537626 _diffrn_orient_matrix_UB_23 0.0193047 _diffrn_orient_matrix_UB_31 -0.0012863 _diffrn_orient_matrix_UB_32 -0.0006163 _diffrn_orient_matrix_UB_33 0.0467419 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_unetI/netI 0.0723 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 0.921 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 48509 _diffrn_reflns_point_group_measured_fraction_full 1 _diffrn_reflns_point_group_measured_fraction_max 0.921 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.176 _diffrn_reflns_theta_min 1.588 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_T_max 0.976 _exptl_absorpt_correction_T_min 0.923 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.593 _exptl_crystal_description prism _exptl_crystal_F_000 1192 _exptl_crystal_size_max 0.272 _exptl_crystal_size_mid 0.068 _exptl_crystal_size_min 0.046 _refine_diff_density_max 1.783 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.078 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 692 _refine_ls_number_reflns 11031 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0509 _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^)+(0.0488P)^2^+2.9726P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1118 _refine_ls_wR_factor_ref 0.1239 _reflns_Friedel_coverage 0 _reflns_number_gt 8441 _reflns_number_total 11031 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02482a2.cif _cod_data_source_block 17ma009_pm98 _cod_database_code 7705242 _shelx_res_file ; TITL 17MA009_PM98 in P-1 shelx.res created by SHELXL-2016/6 at 06:08:21 on 01-Feb-2017 CELL 0.71073 12.5126 13.9713 15.2848 67.053 82.782 82.793 ZERR 2.00 0.0003 0.0004 0.0004 0.002 0.002 0.002 LATT 1 SFAC C H F N NI O P UNIT 88 86 24 26 2 8 4 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 10 TEMP -150.00 WGHT 0.048800 2.972600 FVAR 1.84185 C1 1 0.512909 0.931521 0.181084 11.00000 0.02218 0.01849 = 0.01440 -0.00403 -0.00425 -0.00366 AFIX 43 H1 2 0.496174 0.968100 0.116851 11.00000 -1.20000 AFIX 0 C2 1 0.541311 1.099271 0.186532 11.00000 0.03711 0.01397 = 0.02599 -0.00304 -0.00741 -0.00450 AFIX 137 H2A 2 0.531616 1.122857 0.118453 11.00000 -1.50000 H2B 2 0.610616 1.119481 0.194406 11.00000 -1.50000 H2C 2 0.482395 1.131534 0.217170 11.00000 -1.50000 AFIX 0 C3 1 0.565102 0.936859 0.322392 11.00000 0.02782 0.02203 = 0.01990 -0.00988 -0.00381 -0.00397 AFIX 43 H3 2 0.582687 0.976712 0.355915 11.00000 -1.20000 AFIX 0 C4 1 0.564778 0.830323 0.366459 11.00000 0.02597 0.01983 = 0.01699 -0.00456 -0.00514 -0.00296 AFIX 43 H4 2 0.583056 0.795899 0.430466 11.00000 -1.20000 AFIX 0 C5 1 0.537855 0.773807 0.317405 11.00000 0.01811 0.01585 = 0.01815 -0.00399 0.00021 -0.00310 AFIX 43 H5 2 0.538766 0.700070 0.347814 11.00000 -1.20000 AFIX 0 C6 1 0.509028 0.823048 0.223172 11.00000 0.01415 0.01554 = 0.01569 -0.00582 0.00005 -0.00309 C7 1 0.429508 0.802846 0.098947 11.00000 0.01664 0.01774 = 0.01740 -0.00353 -0.00060 -0.00355 C8 1 0.394659 0.721740 0.068556 11.00000 0.01751 0.01775 = 0.01428 -0.00400 -0.00028 -0.00262 C9 1 0.316419 0.742186 0.005361 11.00000 0.01981 0.01952 = 0.01612 -0.00364 -0.00520 -0.00020 AFIX 43 H9 2 0.283668 0.810837 -0.024323 11.00000 -1.20000 AFIX 0 C10 1 0.287171 0.660036 -0.013438 11.00000 0.01940 0.03024 = 0.01947 -0.00832 -0.00756 -0.00272 AFIX 43 H10 2 0.233477 0.671903 -0.056129 11.00000 -1.20000 AFIX 0 C11 1 0.336357 0.560701 0.030118 11.00000 0.01978 0.02454 = 0.02127 -0.01106 -0.00411 -0.00476 AFIX 43 H11 2 0.316184 0.503653 0.018509 11.00000 -1.20000 AFIX 0 C12 1 0.415364 0.546012 0.090815 11.00000 0.01759 0.01732 = 0.01508 -0.00616 0.00073 -0.00472 C13 1 0.475080 0.441857 0.142478 11.00000 0.01878 0.01922 = 0.01689 -0.00755 0.00020 -0.00508 C14 1 0.604870 0.356827 0.251293 11.00000 0.02739 0.01914 = 0.01947 -0.01128 -0.00445 -0.00058 C15 1 0.551375 0.271307 0.316104 11.00000 0.03997 0.01998 = 0.02501 -0.00895 -0.00309 -0.00738 AFIX 43 H15 2 0.475213 0.271429 0.317721 11.00000 -1.20000 AFIX 0 C16 1 0.610308 0.186905 0.377564 11.00000 0.06159 0.02008 = 0.02837 -0.00632 -0.00764 -0.00756 AFIX 43 H16 2 0.574354 0.129300 0.422342 11.00000 -1.20000 AFIX 0 C17 1 0.720830 0.185896 0.374217 11.00000 0.06291 0.02149 = 0.03097 -0.00983 -0.02234 0.01000 AFIX 43 H17 2 0.761198 0.127748 0.416501 11.00000 -1.20000 AFIX 0 C18 1 0.890702 0.265128 0.307979 11.00000 0.03664 0.05257 = 0.05940 -0.02917 -0.02318 0.01802 AFIX 137 H18A 2 0.909526 0.282351 0.360153 11.00000 -1.50000 H18B 2 0.917831 0.316372 0.246853 11.00000 -1.50000 H18C 2 0.923506 0.195368 0.314802 11.00000 -1.50000 AFIX 0 C19 1 0.716577 0.351378 0.250609 11.00000 0.02827 0.02329 = 0.02404 -0.01224 -0.00800 0.00323 AFIX 43 H19 2 0.755025 0.407765 0.206881 11.00000 -1.20000 AFIX 0 C20 1 0.250562 0.625596 0.272094 11.00000 0.01625 0.01735 = 0.01807 -0.00310 -0.00065 -0.00339 AFIX 43 H20 2 0.284983 0.687125 0.259151 11.00000 -1.20000 AFIX 0 C21 1 0.094945 0.739395 0.199297 11.00000 0.02118 0.01896 = 0.03563 -0.00178 -0.00580 0.00168 AFIX 137 H21A 2 0.123503 0.767356 0.132287 11.00000 -1.50000 H21B 2 0.108833 0.785676 0.230288 11.00000 -1.50000 H21C 2 0.016891 0.734764 0.202985 11.00000 -1.50000 AFIX 0 C22 1 0.095952 0.549664 0.266439 11.00000 0.01626 0.02574 = 0.03645 -0.00428 -0.00599 -0.00604 AFIX 43 H22 2 0.024232 0.557294 0.248923 11.00000 -1.20000 AFIX 0 C23 1 0.146432 0.452149 0.310635 11.00000 0.02380 0.02081 = 0.04070 -0.00219 -0.00771 -0.00901 AFIX 43 H23 2 0.109081 0.392154 0.324187 11.00000 -1.20000 AFIX 0 C24 1 0.251473 0.440421 0.335683 11.00000 0.02098 0.01720 = 0.03226 -0.00618 -0.00573 -0.00221 AFIX 43 H24 2 0.285813 0.372730 0.366509 11.00000 -1.20000 AFIX 0 C25 1 0.306482 0.528702 0.315329 11.00000 0.01498 0.01703 = 0.01355 -0.00370 0.00024 -0.00126 C26 1 0.455410 0.454349 0.407363 11.00000 0.01830 0.01297 = 0.01576 -0.00703 -0.00085 -0.00086 C27 1 0.575694 0.459504 0.407584 11.00000 0.01863 0.01340 = 0.01570 -0.00752 -0.00193 -0.00123 C28 1 0.638227 0.393960 0.480042 11.00000 0.02213 0.01723 = 0.01298 -0.00313 -0.00341 -0.00027 AFIX 43 H28 2 0.607064 0.340544 0.534069 11.00000 -1.20000 AFIX 0 C29 1 0.746986 0.408188 0.471796 11.00000 0.02162 0.02085 = 0.01824 -0.00594 -0.00824 0.00414 AFIX 43 H29 2 0.790918 0.365608 0.521433 11.00000 -1.20000 AFIX 0 C30 1 0.792254 0.484792 0.390896 11.00000 0.01536 0.02177 = 0.02073 -0.00881 -0.00453 -0.00085 AFIX 43 H30 2 0.866643 0.495910 0.384848 11.00000 -1.20000 AFIX 0 C31 1 0.725846 0.544411 0.319403 11.00000 0.01478 0.01682 = 0.01615 -0.00831 -0.00148 -0.00248 C32 1 0.763234 0.624884 0.224297 11.00000 0.01627 0.01649 = 0.01755 -0.00750 -0.00056 -0.00158 C33 1 0.710040 0.727295 0.070577 11.00000 0.01448 0.01856 = 0.02000 -0.00779 0.00048 -0.00208 C34 1 0.679198 0.714509 -0.008946 11.00000 0.02168 0.02274 = 0.02056 -0.00790 -0.00236 -0.00531 AFIX 43 H34 2 0.642838 0.655369 -0.000467 11.00000 -1.20000 AFIX 0 C35 1 0.701252 0.787075 -0.099215 11.00000 0.03046 0.03102 = 0.02136 -0.01040 -0.00304 -0.00667 AFIX 43 H35 2 0.682402 0.776571 -0.152928 11.00000 -1.20000 AFIX 0 C36 1 0.750614 0.875014 -0.112069 11.00000 0.02798 0.02837 = 0.01795 -0.00502 0.00027 -0.00545 AFIX 43 H36 2 0.766125 0.925015 -0.174428 11.00000 -1.20000 AFIX 0 C37 1 0.825634 0.985358 -0.048610 11.00000 0.03072 0.02199 = 0.02970 -0.00811 0.00361 -0.01056 AFIX 137 H37A 2 0.853369 1.018853 -0.115383 11.00000 -1.50000 H37B 2 0.885170 0.967654 -0.007540 11.00000 -1.50000 H37C 2 0.770890 1.033278 -0.031640 11.00000 -1.50000 AFIX 0 C38 1 0.758363 0.818327 0.053953 11.00000 0.01764 0.02145 = 0.01828 -0.00626 -0.00123 -0.00232 AFIX 43 H38 2 0.778709 0.830481 0.106326 11.00000 -1.20000 AFIX 0 C40 1 0.978170 0.671924 -0.006219 11.00000 0.04492 0.04381 = 0.09246 -0.03010 0.01846 -0.01024 AFIX 137 H40A 2 1.054238 0.656014 -0.024293 11.00000 -1.50000 H40B 2 0.973653 0.710808 0.035581 11.00000 -1.50000 H40C 2 0.941353 0.714110 -0.063657 11.00000 -1.50000 AFIX 0 C41 1 0.926728 0.575417 0.043710 11.00000 0.04790 0.04999 = 0.06814 -0.03075 0.02061 -0.00372 C42 1 1.176930 0.269283 0.599857 11.00000 0.03096 0.03645 = 0.03924 -0.01931 -0.00297 -0.00437 AFIX 137 H42A 2 1.187555 0.202153 0.592270 11.00000 -1.50000 H42B 2 1.181885 0.257791 0.666748 11.00000 -1.50000 H42C 2 1.232819 0.314143 0.559740 11.00000 -1.50000 AFIX 0 C43 1 1.072307 0.318707 0.571767 11.00000 0.03128 0.03682 = 0.04613 -0.01021 -0.00115 -0.01209 C44 1 0.936086 0.103842 0.584312 11.00000 0.06151 0.05304 = 0.04264 -0.00698 -0.01398 -0.01989 AFIX 137 H44A 2 0.958222 0.167457 0.531811 11.00000 -1.50000 H44B 2 0.917834 0.054464 0.558393 11.00000 -1.50000 H44C 2 0.995536 0.072184 0.625326 11.00000 -1.50000 AFIX 0 C45 1 0.842898 0.129472 0.639351 11.00000 0.05419 0.03133 = 0.05664 -0.01191 -0.01899 -0.01045 F1 3 0.948705 -0.060591 0.184890 11.00000 0.04018 0.02658 = 0.07090 -0.00987 0.00305 0.00788 F2 3 0.777886 0.010952 0.158114 11.00000 0.03268 0.04616 = 0.04964 -0.02120 0.00089 -0.00808 F3 3 0.848138 -0.004587 0.292646 11.00000 0.05333 0.05931 = 0.03032 -0.00104 -0.00288 0.00493 F4 3 0.818685 0.154324 0.178036 11.00000 0.04743 0.03742 = 0.04411 -0.02261 -0.01534 0.01489 F5 3 0.990625 0.083049 0.203491 11.00000 0.03971 0.05097 = 0.04802 -0.01511 -0.01824 -0.00211 F6 3 0.918384 0.100363 0.069691 11.00000 0.04253 0.03612 = 0.03094 -0.01190 -0.00119 -0.00656 F7 3 0.836333 -0.205795 0.581463 11.00000 0.11800 0.05092 = 0.07354 -0.01762 0.00387 0.00807 F8 3 0.676739 -0.134959 0.530391 11.00000 0.09272 0.21416 = 0.07728 -0.07521 -0.00785 -0.06282 F9 3 0.692487 -0.210319 0.686018 11.00000 0.14461 0.14886 = 0.04944 -0.04900 0.03816 -0.11458 F10 3 0.668944 -0.036448 0.617839 11.00000 0.12246 0.21339 = 0.21381 -0.16084 -0.03546 0.08645 F11 3 0.824661 -0.110471 0.670314 11.00000 0.09750 0.08925 = 0.04464 -0.01601 -0.00787 -0.05218 F12 3 0.808323 -0.035611 0.513145 11.00000 0.13421 0.04013 = 0.04447 0.00489 -0.01110 -0.02597 N1 4 0.540260 0.984264 0.231238 11.00000 0.02240 0.01460 = 0.01994 -0.00608 -0.00038 -0.00446 N2 4 0.478996 0.759583 0.180469 11.00000 0.01587 0.01510 = 0.01458 -0.00499 -0.00168 -0.00320 N3 4 0.442708 0.625749 0.109178 11.00000 0.01504 0.01701 = 0.01211 -0.00411 -0.00094 -0.00549 N4 4 0.552399 0.449768 0.192291 11.00000 0.01662 0.01606 = 0.01770 -0.00835 -0.00314 -0.00110 N5 4 0.771093 0.267092 0.311211 11.00000 0.03815 0.03031 = 0.03208 -0.01723 -0.01420 0.01016 N6 4 0.148833 0.634046 0.248225 11.00000 0.01471 0.01847 = 0.02325 -0.00318 -0.00147 -0.00228 N7 4 0.414886 0.527794 0.329165 11.00000 0.01435 0.01375 = 0.01384 -0.00277 -0.00233 -0.00099 N8 4 0.620309 0.532277 0.329584 11.00000 0.01349 0.01471 = 0.01410 -0.00628 -0.00187 -0.00114 N9 4 0.689140 0.651440 0.161324 11.00000 0.01563 0.01749 = 0.01431 -0.00501 -0.00135 -0.00429 N10 4 0.776645 0.889408 -0.035458 11.00000 0.02108 0.01803 = 0.02171 -0.00597 -0.00067 -0.00533 N11 4 0.886113 0.499245 0.082121 11.00000 0.07901 0.05361 = 0.09937 -0.03492 0.04842 -0.02041 N12 4 0.988722 0.358058 0.551308 11.00000 0.03555 0.06246 = 0.09379 -0.01331 -0.01639 -0.00556 N13 4 0.770565 0.150405 0.683702 11.00000 0.06908 0.05322 = 0.10410 -0.04157 -0.01223 -0.00739 NI1 5 0.534516 0.595528 0.215835 11.00000 0.01344 0.01297 = 0.01180 -0.00285 -0.00245 -0.00294 O1 6 0.407663 0.896659 0.049509 11.00000 0.03497 0.01571 = 0.02387 -0.00164 -0.01314 -0.00148 O2 6 0.451028 0.363118 0.133090 11.00000 0.03063 0.01878 = 0.02767 -0.01100 -0.00666 -0.00554 O3 6 0.407467 0.388707 0.476484 11.00000 0.02057 0.01823 = 0.01660 0.00096 -0.00050 -0.00512 O4 6 0.855652 0.655072 0.212643 11.00000 0.01460 0.02931 = 0.02186 -0.00372 -0.00275 -0.00677 P1 7 0.884091 0.046678 0.181707 11.00000 0.02908 0.02642 = 0.02892 -0.00739 -0.00530 0.00371 P2 7 0.747957 -0.120282 0.599466 11.00000 0.06139 0.04235 = 0.03180 -0.02103 0.00571 -0.01952 HKLF 4 REM 17MA009_PM98 in P-1 REM R1 = 0.0509 for 8441 Fo > 4sig(Fo) and 0.0731 for all 11031 data REM 692 parameters refined using 0 restraints END WGHT 0.0488 2.9738 REM Highest difference peak 1.783, deepest hole -0.652, 1-sigma level 0.078 Q1 1 0.6768 -0.0897 0.5721 11.00000 0.05 1.78 Q2 1 0.8365 -0.1625 0.6278 11.00000 0.05 0.84 Q3 1 0.6136 -0.0698 0.5581 11.00000 0.05 0.74 Q4 1 0.7191 -0.0589 0.6650 11.00000 0.05 0.62 Q5 1 0.7529 -0.1993 0.5481 11.00000 0.05 0.57 Q6 1 0.6842 0.0156 0.5831 11.00000 0.05 0.55 Q7 1 0.6274 -0.1330 0.6785 11.00000 0.05 0.49 Q8 1 0.7452 0.5862 0.2738 11.00000 0.05 0.37 Q9 1 0.5183 0.4627 0.4119 11.00000 0.05 0.37 Q10 1 0.4047 0.7571 0.0893 11.00000 0.05 0.37 Q11 1 0.8582 -0.0202 0.1651 11.00000 0.05 0.35 Q12 1 0.9863 0.3322 0.5026 11.00000 0.05 0.35 Q13 1 0.7482 -0.0585 0.4694 11.00000 0.05 0.35 Q14 1 0.3354 0.6197 -0.0078 11.00000 0.05 0.34 Q15 1 0.4217 0.5012 0.1262 11.00000 0.05 0.33 Q16 1 0.6411 0.6295 0.1762 11.00000 0.05 0.33 Q17 1 0.5034 0.7881 0.1909 11.00000 0.05 0.33 Q18 1 0.6834 -0.1892 0.6203 11.00000 0.05 0.32 Q19 1 0.2742 0.5775 0.2979 11.00000 0.05 0.31 Q20 1 1.0611 0.3016 0.5300 11.00000 0.05 0.31 ; _shelx_res_checksum 38422 loop_ _symmetry_equiv_pos_as_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 C1 C 0.5129(2) 0.9315(2) 0.18108(18) 0.0186(5) Uani 1 1 d . . . . . H1 H 0.496174 0.9681 0.116851 0.022 Uiso 1 1 calc R U . . . C2 C 0.5413(3) 1.0993(2) 0.1865(2) 0.0264(6) Uani 1 1 d . . . . . H2A H 0.531616 1.122857 0.118453 0.04 Uiso 1 1 calc R U . . . H2B H 0.610616 1.119481 0.194406 0.04 Uiso 1 1 calc R U . . . H2C H 0.482395 1.131534 0.21717 0.04 Uiso 1 1 calc R U . . . C3 C 0.5651(2) 0.9369(2) 0.32239(19) 0.0223(6) Uani 1 1 d . . . . . H3 H 0.582687 0.976712 0.355915 0.027 Uiso 1 1 calc R U . . . C4 C 0.5648(2) 0.8303(2) 0.36646(19) 0.0213(6) Uani 1 1 d . . . . . H4 H 0.583056 0.795899 0.430466 0.026 Uiso 1 1 calc R U . . . C5 C 0.5379(2) 0.7738(2) 0.31740(18) 0.0181(5) Uani 1 1 d . . . . . H5 H 0.538766 0.70007 0.347814 0.022 Uiso 1 1 calc R U . . . C6 C 0.5090(2) 0.8230(2) 0.22317(17) 0.0151(5) Uani 1 1 d . . . . . C7 C 0.4295(2) 0.8028(2) 0.09895(18) 0.0181(5) Uani 1 1 d . . . . . C8 C 0.3947(2) 0.7217(2) 0.06856(18) 0.0171(5) Uani 1 1 d . . . . . C9 C 0.3164(2) 0.7422(2) 0.00536(18) 0.0192(5) Uani 1 1 d . . . . . H9 H 0.283668 0.810837 -0.024323 0.023 Uiso 1 1 calc R U . . . C10 C 0.2872(2) 0.6600(2) -0.01344(19) 0.0228(6) Uani 1 1 d . . . . . H10 H 0.233477 0.671903 -0.056129 0.027 Uiso 1 1 calc R U . . . C11 C 0.3364(2) 0.5607(2) 0.03012(19) 0.0206(6) Uani 1 1 d . . . . . H11 H 0.316184 0.503653 0.018509 0.025 Uiso 1 1 calc R U . . . C12 C 0.4154(2) 0.5460(2) 0.09082(17) 0.0166(5) Uani 1 1 d . . . . . C13 C 0.4751(2) 0.4419(2) 0.14248(18) 0.0179(5) Uani 1 1 d . . . . . C14 C 0.6049(2) 0.3568(2) 0.25129(19) 0.0207(6) Uani 1 1 d . . . . . C15 C 0.5514(3) 0.2713(2) 0.3161(2) 0.0277(7) Uani 1 1 d . . . . . H15 H 0.475213 0.271429 0.317721 0.033 Uiso 1 1 calc R U . . . C16 C 0.6103(3) 0.1869(2) 0.3776(2) 0.0368(8) Uani 1 1 d . . . . . H16 H 0.574354 0.1293 0.422342 0.044 Uiso 1 1 calc R U . . . C17 C 0.7208(3) 0.1859(2) 0.3742(2) 0.0381(8) Uani 1 1 d . . . . . H17 H 0.761198 0.127748 0.416501 0.046 Uiso 1 1 calc R U . . . C18 C 0.8907(3) 0.2651(3) 0.3080(3) 0.0473(10) Uani 1 1 d . . . . . H18A H 0.909526 0.282351 0.360153 0.071 Uiso 1 1 calc R U . . . H18B H 0.917831 0.316372 0.246853 0.071 Uiso 1 1 calc R U . . . H18C H 0.923506 0.195368 0.314802 0.071 Uiso 1 1 calc R U . . . C19 C 0.7166(2) 0.3514(2) 0.2506(2) 0.0242(6) Uani 1 1 d . . . . . H19 H 0.755025 0.407765 0.206881 0.029 Uiso 1 1 calc R U . . . C20 C 0.2506(2) 0.6256(2) 0.27209(18) 0.0182(5) Uani 1 1 d . . . . . H20 H 0.284983 0.687125 0.259151 0.022 Uiso 1 1 calc R U . . . C21 C 0.0949(2) 0.7394(2) 0.1993(2) 0.0279(7) Uani 1 1 d . . . . . H21A H 0.123503 0.767356 0.132287 0.042 Uiso 1 1 calc R U . . . H21B H 0.108833 0.785676 0.230288 0.042 Uiso 1 1 calc R U . . . H21C H 0.016891 0.734764 0.202985 0.042 Uiso 1 1 calc R U . . . C22 C 0.0960(2) 0.5497(2) 0.2664(2) 0.0277(7) Uani 1 1 d . . . . . H22 H 0.024232 0.557294 0.248923 0.033 Uiso 1 1 calc R U . . . C23 C 0.1464(2) 0.4521(2) 0.3106(2) 0.0303(7) Uani 1 1 d . . . . . H23 H 0.109081 0.392154 0.324187 0.036 Uiso 1 1 calc R U . . . C24 C 0.2515(2) 0.4404(2) 0.3357(2) 0.0241(6) Uani 1 1 d . . . . . H24 H 0.285813 0.37273 0.366509 0.029 Uiso 1 1 calc R U . . . C25 C 0.3065(2) 0.5287(2) 0.31533(17) 0.0160(5) Uani 1 1 d . . . . . C26 C 0.4554(2) 0.45435(19) 0.40736(17) 0.0153(5) Uani 1 1 d . . . . . C27 C 0.5757(2) 0.45950(19) 0.40758(17) 0.0153(5) Uani 1 1 d . . . . . C28 C 0.6382(2) 0.3940(2) 0.48004(18) 0.0182(5) Uani 1 1 d . . . . . H28 H 0.607064 0.340544 0.534069 0.022 Uiso 1 1 calc R U . . . C29 C 0.7470(2) 0.4082(2) 0.47180(19) 0.0206(6) Uani 1 1 d . . . . . H29 H 0.790918 0.365608 0.521433 0.025 Uiso 1 1 calc R U . . . C30 C 0.7923(2) 0.4848(2) 0.39090(18) 0.0188(5) Uani 1 1 d . . . . . H30 H 0.866643 0.49591 0.384848 0.023 Uiso 1 1 calc R U . . . C31 C 0.7258(2) 0.5444(2) 0.31940(17) 0.0152(5) Uani 1 1 d . . . . . C32 C 0.7632(2) 0.6249(2) 0.22430(18) 0.0165(5) Uani 1 1 d . . . . . C33 C 0.7100(2) 0.7273(2) 0.07058(18) 0.0176(5) Uani 1 1 d . . . . . C34 C 0.6792(2) 0.7145(2) -0.00895(19) 0.0214(6) Uani 1 1 d . . . . . H34 H 0.642838 0.655369 -0.000467 0.026 Uiso 1 1 calc R U . . . C35 C 0.7013(2) 0.7871(2) -0.0992(2) 0.0270(6) Uani 1 1 d . . . . . H35 H 0.682402 0.776571 -0.152928 0.032 Uiso 1 1 calc R U . . . C36 C 0.7506(2) 0.8750(2) -0.1121(2) 0.0258(6) Uani 1 1 d . . . . . H36 H 0.766125 0.925015 -0.174428 0.031 Uiso 1 1 calc R U . . . C37 C 0.8256(2) 0.9854(2) -0.0486(2) 0.0278(7) Uani 1 1 d . . . . . H37A H 0.853369 1.018853 -0.115383 0.042 Uiso 1 1 calc R U . . . H37B H 0.88517 0.967654 -0.00754 0.042 Uiso 1 1 calc R U . . . H37C H 0.77089 1.033278 -0.03164 0.042 Uiso 1 1 calc R U . . . C38 C 0.7584(2) 0.8183(2) 0.05395(19) 0.0195(6) Uani 1 1 d . . . . . H38 H 0.778709 0.830481 0.106326 0.023 Uiso 1 1 calc R U . . . C40 C 0.9782(3) 0.6719(3) -0.0062(4) 0.0607(12) Uani 1 1 d . . . . . H40A H 1.054238 0.656014 -0.024293 0.091 Uiso 1 1 calc R U . . . H40B H 0.973653 0.710808 0.035581 0.091 Uiso 1 1 calc R U . . . H40C H 0.941353 0.71411 -0.063657 0.091 Uiso 1 1 calc R U . . . C41 C 0.9267(3) 0.5754(3) 0.0437(3) 0.0552(11) Uani 1 1 d . . . . . C42 C 1.1769(3) 0.2693(3) 0.5999(2) 0.0339(7) Uani 1 1 d . . . . . H42A H 1.187555 0.202153 0.59227 0.051 Uiso 1 1 calc R U . . . H42B H 1.181885 0.257791 0.666748 0.051 Uiso 1 1 calc R U . . . H42C H 1.232819 0.314143 0.55974 0.051 Uiso 1 1 calc R U . . . C43 C 1.0723(3) 0.3187(3) 0.5718(3) 0.0391(8) Uani 1 1 d . . . . . C44 C 0.9361(3) 0.1038(3) 0.5843(3) 0.0536(11) Uani 1 1 d . . . . . H44A H 0.958222 0.167457 0.531811 0.08 Uiso 1 1 calc R U . . . H44B H 0.917834 0.054464 0.558393 0.08 Uiso 1 1 calc R U . . . H44C H 0.995536 0.072184 0.625326 0.08 Uiso 1 1 calc R U . . . C45 C 0.8429(4) 0.1295(3) 0.6394(3) 0.0469(10) Uani 1 1 d . . . . . F1 F 0.94871(16) -0.06059(15) 0.18489(16) 0.0503(6) Uani 1 1 d . . . . . F2 F 0.77789(15) 0.01095(16) 0.15811(14) 0.0419(5) Uani 1 1 d . . . . . F3 F 0.84814(18) -0.00459(18) 0.29265(14) 0.0535(6) Uani 1 1 d . . . . . F4 F 0.81868(16) 0.15432(15) 0.17804(14) 0.0414(5) Uani 1 1 d . . . . . F5 F 0.99063(16) 0.08305(16) 0.20349(15) 0.0462(5) Uani 1 1 d . . . . . F6 F 0.91838(15) 0.10036(14) 0.06969(13) 0.0367(4) Uani 1 1 d . . . . . F7 F 0.8363(3) -0.2058(2) 0.5815(2) 0.0852(9) Uani 1 1 d . . . . . F8 F 0.6767(3) -0.1350(3) 0.5304(2) 0.1173(14) Uani 1 1 d . . . . . F9 F 0.6925(3) -0.2103(3) 0.68602(18) 0.1057(13) Uani 1 1 d . . . . . F10 F 0.6689(3) -0.0364(4) 0.6178(4) 0.166(2) Uani 1 1 d . . . . . F11 F 0.8247(2) -0.1105(2) 0.67031(16) 0.0758(8) Uani 1 1 d . . . . . F12 F 0.8083(3) -0.03561(18) 0.51315(17) 0.0774(8) Uani 1 1 d . . . . . N1 N 0.54026(18) 0.98426(17) 0.23124(15) 0.0190(5) Uani 1 1 d . . . . . N2 N 0.47900(17) 0.75958(16) 0.18047(14) 0.0152(4) Uani 1 1 d . . . . . N3 N 0.44271(17) 0.62575(16) 0.10918(14) 0.0148(4) Uani 1 1 d . . . . . N4 N 0.55240(17) 0.44977(17) 0.19229(15) 0.0161(4) Uani 1 1 d . . . . . N5 N 0.7711(2) 0.2671(2) 0.31121(18) 0.0320(6) Uani 1 1 d . . . . . N6 N 0.14883(17) 0.63405(17) 0.24823(16) 0.0202(5) Uani 1 1 d . . . . . N7 N 0.41489(17) 0.52779(16) 0.32917(14) 0.0147(4) Uani 1 1 d . . . . . N8 N 0.62031(16) 0.53228(16) 0.32958(14) 0.0138(4) Uani 1 1 d . . . . . N9 N 0.68914(17) 0.65144(17) 0.16132(15) 0.0159(4) Uani 1 1 d . . . . . N10 N 0.77664(18) 0.88941(17) -0.03546(16) 0.0205(5) Uani 1 1 d . . . . . N11 N 0.8861(3) 0.4992(3) 0.0821(3) 0.0793(13) Uani 1 1 d . . . . . N12 N 0.9887(3) 0.3581(3) 0.5513(3) 0.0678(11) Uani 1 1 d . . . . . N13 N 0.7706(4) 0.1504(3) 0.6837(3) 0.0712(11) Uani 1 1 d . . . . . Ni1 Ni 0.53452(3) 0.59553(2) 0.21583(2) 0.01301(9) Uani 1 1 d . . . . . O1 O 0.40766(17) 0.89666(14) 0.04951(13) 0.0257(4) Uani 1 1 d . . . . . O2 O 0.45103(16) 0.36312(15) 0.13309(14) 0.0243(4) Uani 1 1 d . . . . . O3 O 0.40747(15) 0.38871(14) 0.47648(12) 0.0206(4) Uani 1 1 d . . . . . O4 O 0.85565(14) 0.65507(15) 0.21264(13) 0.0232(4) Uani 1 1 d . . . . . P1 P 0.88409(7) 0.04668(6) 0.18171(6) 0.02940(19) Uani 1 1 d . . . . . P2 P 0.74796(9) -0.12028(8) 0.59947(6) 0.0425(2) 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 0.0222(14) 0.0185(13) 0.0144(12) -0.0040(11) -0.0043(10) -0.0037(11) C2 0.0371(17) 0.0140(13) 0.0260(15) -0.0030(12) -0.0074(13) -0.0045(12) C3 0.0278(15) 0.0220(14) 0.0199(13) -0.0099(12) -0.0038(11) -0.0040(12) C4 0.0260(15) 0.0198(14) 0.0170(13) -0.0046(11) -0.0051(11) -0.0030(11) C5 0.0181(13) 0.0158(13) 0.0182(13) -0.0040(11) 0.0002(10) -0.0031(11) C6 0.0141(12) 0.0155(12) 0.0157(12) -0.0058(10) 0.0001(10) -0.0031(10) C7 0.0166(13) 0.0177(13) 0.0174(12) -0.0035(11) -0.0006(10) -0.0036(11) C8 0.0175(13) 0.0177(13) 0.0143(12) -0.0040(10) -0.0003(10) -0.0026(11) C9 0.0198(13) 0.0195(13) 0.0161(12) -0.0036(11) -0.0052(10) -0.0002(11) C10 0.0194(14) 0.0302(16) 0.0195(13) -0.0083(12) -0.0076(11) -0.0027(12) C11 0.0198(13) 0.0245(14) 0.0213(13) -0.0111(12) -0.0041(11) -0.0048(11) C12 0.0176(13) 0.0173(13) 0.0151(12) -0.0062(10) 0.0007(10) -0.0047(10) C13 0.0188(13) 0.0192(13) 0.0169(12) -0.0075(11) 0.0002(10) -0.0051(11) C14 0.0274(15) 0.0191(14) 0.0195(13) -0.0113(11) -0.0044(11) -0.0006(11) C15 0.0400(18) 0.0200(14) 0.0250(15) -0.0089(12) -0.0031(13) -0.0074(13) C16 0.062(2) 0.0201(15) 0.0284(16) -0.0063(13) -0.0076(16) -0.0076(15) C17 0.063(2) 0.0215(16) 0.0310(17) -0.0098(14) -0.0223(16) 0.0100(16) C18 0.037(2) 0.053(2) 0.059(2) -0.029(2) -0.0232(18) 0.0180(17) C19 0.0283(15) 0.0233(15) 0.0240(14) -0.0122(12) -0.0080(12) 0.0032(12) C20 0.0162(13) 0.0173(13) 0.0181(13) -0.0031(11) -0.0006(10) -0.0034(11) C21 0.0212(15) 0.0190(14) 0.0356(17) -0.0018(13) -0.0058(12) 0.0017(12) C22 0.0163(14) 0.0257(15) 0.0364(17) -0.0043(13) -0.0060(12) -0.0060(12) C23 0.0238(15) 0.0208(15) 0.0407(18) -0.0022(13) -0.0077(13) -0.0090(12) C24 0.0210(14) 0.0172(14) 0.0323(16) -0.0062(12) -0.0057(12) -0.0022(11) C25 0.0150(12) 0.0170(13) 0.0135(12) -0.0037(10) 0.0002(10) -0.0013(10) C26 0.0183(13) 0.0130(12) 0.0158(12) -0.0070(10) -0.0008(10) -0.0009(10) C27 0.0186(13) 0.0134(12) 0.0157(12) -0.0075(10) -0.0019(10) -0.0012(10) C28 0.0221(14) 0.0172(13) 0.0130(12) -0.0031(10) -0.0034(10) -0.0003(11) C29 0.0216(14) 0.0209(14) 0.0182(13) -0.0059(11) -0.0082(11) 0.0041(11) C30 0.0154(13) 0.0218(14) 0.0207(13) -0.0088(11) -0.0045(10) -0.0008(11) C31 0.0148(12) 0.0168(13) 0.0161(12) -0.0083(10) -0.0015(10) -0.0025(10) C32 0.0163(13) 0.0165(13) 0.0175(12) -0.0075(11) -0.0006(10) -0.0016(10) C33 0.0145(12) 0.0186(13) 0.0200(13) -0.0078(11) 0.0005(10) -0.0021(10) C34 0.0217(14) 0.0227(14) 0.0206(13) -0.0079(12) -0.0024(11) -0.0053(11) C35 0.0305(16) 0.0310(16) 0.0214(14) -0.0104(13) -0.0030(12) -0.0067(13) C36 0.0280(15) 0.0284(16) 0.0179(13) -0.0050(12) 0.0003(12) -0.0055(13) C37 0.0307(16) 0.0220(15) 0.0297(16) -0.0081(13) 0.0036(13) -0.0106(13) C38 0.0176(13) 0.0214(14) 0.0183(13) -0.0063(11) -0.0012(10) -0.0023(11) C40 0.045(2) 0.044(2) 0.092(3) -0.030(2) 0.018(2) -0.0102(19) C41 0.048(2) 0.050(2) 0.068(3) -0.031(2) 0.021(2) -0.004(2) C42 0.0310(17) 0.0364(18) 0.0392(18) -0.0193(15) -0.0030(14) -0.0044(14) C43 0.0313(19) 0.0368(19) 0.046(2) -0.0102(16) -0.0012(16) -0.0121(15) C44 0.062(3) 0.053(2) 0.043(2) -0.0070(19) -0.014(2) -0.020(2) C45 0.054(3) 0.031(2) 0.057(2) -0.0119(18) -0.019(2) -0.0104(18) F1 0.0402(12) 0.0266(10) 0.0709(15) -0.0099(10) 0.0030(11) 0.0079(9) F2 0.0327(10) 0.0462(12) 0.0496(12) -0.0212(10) 0.0009(9) -0.0081(9) F3 0.0533(13) 0.0593(14) 0.0303(11) -0.0010(10) -0.0029(10) 0.0049(11) F4 0.0474(12) 0.0374(11) 0.0441(11) -0.0226(9) -0.0153(9) 0.0149(9) F5 0.0397(11) 0.0510(13) 0.0480(12) -0.0151(10) -0.0182(9) -0.0021(10) F6 0.0425(11) 0.0361(11) 0.0309(10) -0.0119(8) -0.0012(8) -0.0066(9) F7 0.118(2) 0.0509(16) 0.0735(18) -0.0176(14) 0.0039(17) 0.0081(16) F8 0.093(2) 0.214(4) 0.077(2) -0.075(3) -0.0079(18) -0.063(3) F9 0.145(3) 0.149(3) 0.0494(15) -0.0490(18) 0.0382(17) -0.115(2) F10 0.122(3) 0.213(5) 0.214(5) -0.161(4) -0.035(3) 0.086(3) F11 0.098(2) 0.089(2) 0.0446(14) -0.0160(13) -0.0079(13) -0.0522(17) F12 0.134(3) 0.0401(13) 0.0445(14) 0.0049(11) -0.0111(15) -0.0260(15) N1 0.0224(12) 0.0146(11) 0.0199(11) -0.0061(9) -0.0004(9) -0.0045(9) N2 0.0159(11) 0.0151(11) 0.0146(10) -0.0050(9) -0.0017(8) -0.0032(9) N3 0.0150(10) 0.0170(11) 0.0121(10) -0.0041(9) -0.0009(8) -0.0055(9) N4 0.0166(11) 0.0161(11) 0.0177(11) -0.0083(9) -0.0031(9) -0.0011(9) N5 0.0381(15) 0.0303(14) 0.0321(14) -0.0172(12) -0.0142(12) 0.0102(12) N6 0.0147(11) 0.0185(12) 0.0233(12) -0.0032(10) -0.0015(9) -0.0023(9) N7 0.0143(10) 0.0138(10) 0.0138(10) -0.0028(9) -0.0023(8) -0.0010(8) N8 0.0135(10) 0.0147(10) 0.0141(10) -0.0063(9) -0.0019(8) -0.0011(8) N9 0.0156(11) 0.0175(11) 0.0143(10) -0.0050(9) -0.0013(8) -0.0043(9) N10 0.0211(12) 0.0180(11) 0.0217(11) -0.0060(10) -0.0007(9) -0.0053(9) N11 0.079(3) 0.054(2) 0.099(3) -0.035(2) 0.048(3) -0.020(2) N12 0.0355(19) 0.062(2) 0.094(3) -0.013(2) -0.0164(19) -0.0056(17) N13 0.069(3) 0.053(2) 0.104(3) -0.042(2) -0.012(2) -0.007(2) Ni1 0.01344(16) 0.01297(16) 0.01180(16) -0.00285(12) -0.00245(12) -0.00294(12) O1 0.0350(12) 0.0157(10) 0.0239(10) -0.0016(8) -0.0131(9) -0.0015(9) O2 0.0306(11) 0.0188(10) 0.0277(10) -0.0110(8) -0.0067(9) -0.0055(8) O3 0.0206(10) 0.0182(10) 0.0166(9) 0.0010(8) -0.0005(8) -0.0051(8) O4 0.0146(9) 0.0293(11) 0.0219(10) -0.0037(8) -0.0027(8) -0.0068(8) P1 0.0291(4) 0.0264(4) 0.0289(4) -0.0074(3) -0.0053(3) 0.0037(3) P2 0.0614(6) 0.0424(5) 0.0318(5) -0.0210(4) 0.0057(4) -0.0195(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 0 '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 0.006 '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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.0307 0 1 0 0.0377 1 0 0 0.0229 -1 0 0 0.0229 0 -1 -1 0.0666 -5 17 13 0.0724 1 1 1 0.08 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 N1 C1 C6 120.4(2) . . ? N1 C1 H1 119.8 . . ? C6 C1 H1 119.8 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 119.4(2) . . ? N1 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.6(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C4 C5 C6 121.2(2) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? N2 C6 C1 126.2(2) . . ? N2 C6 C5 117.1(2) . . ? C1 C6 C5 116.7(2) . . ? O1 C7 N2 129.5(2) . . ? O1 C7 C8 118.4(2) . . ? N2 C7 C8 112.1(2) . . ? N3 C8 C9 121.2(2) . . ? N3 C8 C7 115.1(2) . . ? C9 C8 C7 123.7(2) . . ? C10 C9 C8 118.4(2) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C11 C10 C9 119.9(2) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C12 C11 C10 118.8(2) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? N3 C12 C11 121.0(2) . . ? N3 C12 C13 115.1(2) . . ? C11 C12 C13 124.0(2) . . ? O2 C13 N4 128.6(3) . . ? O2 C13 C12 119.2(2) . . ? N4 C13 C12 112.2(2) . . ? C19 C14 N4 117.9(2) . . ? C19 C14 C15 117.8(3) . . ? N4 C14 C15 124.1(3) . . ? C16 C15 C14 119.5(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C17 C16 C15 120.3(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? N5 C17 C16 119.7(3) . . ? N5 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? N5 C18 H18A 109.5 . . ? N5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 C14 120.8(3) . . ? N5 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? N6 C20 C25 121.5(2) . . ? N6 C20 H20 119.2 . . ? C25 C20 H20 119.2 . . ? N6 C21 H21A 109.5 . . ? N6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 C23 119.4(3) . . ? N6 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 120.6(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 119.6(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C20 C25 N7 117.3(2) . . ? C20 C25 C24 117.2(2) . . ? N7 C25 C24 125.4(2) . . ? O3 C26 N7 128.9(2) . . ? O3 C26 C27 119.1(2) . . ? N7 C26 C27 112.0(2) . . ? N8 C27 C28 120.9(2) . . ? N8 C27 C26 114.7(2) . . ? C28 C27 C26 124.4(2) . . ? C29 C28 C27 118.5(2) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? C28 C29 C30 120.2(2) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 118.2(2) . . ? C31 C30 H30 120.9 . . ? C29 C30 H30 120.9 . . ? N8 C31 C30 121.0(2) . . ? N8 C31 C32 113.9(2) . . ? C30 C31 C32 125.1(2) . . ? O4 C32 N9 128.7(2) . . ? O4 C32 C31 119.3(2) . . ? N9 C32 C31 112.0(2) . . ? N9 C33 C38 123.4(2) . . ? N9 C33 C34 119.4(2) . . ? C38 C33 C34 117.1(2) . . ? C35 C34 C33 120.4(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 120.3(3) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? N10 C36 C35 119.4(3) . . ? N10 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? N10 C37 H37A 109.5 . . ? N10 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N10 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N10 C38 C33 121.0(2) . . ? N10 C38 H38 119.5 . . ? C33 C38 H38 119.5 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N11 C41 C40 179.2(5) . . ? C43 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C43 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N12 C43 C42 178.6(4) . . ? C45 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C45 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N13 C45 C44 178.7(4) . . ? C3 N1 C1 122.6(2) . . ? C3 N1 C2 117.6(2) . . ? C1 N1 C2 119.7(2) . . ? C7 N2 C6 119.9(2) . . ? C7 N2 Ni1 113.43(17) . . ? C6 N2 Ni1 125.37(16) . . ? C8 N3 C12 120.7(2) . . ? C8 N3 Ni1 119.27(17) . . ? C12 N3 Ni1 118.98(17) . . ? C13 N4 C14 117.1(2) . . ? C13 N4 Ni1 113.49(17) . . ? C14 N4 Ni1 124.43(16) . . ? C17 N5 C19 121.9(3) . . ? C17 N5 C18 119.3(3) . . ? C19 N5 C18 118.8(3) . . ? C22 N6 C20 121.6(2) . . ? C22 N6 C21 119.4(2) . . ? C20 N6 C21 119.0(2) . . ? C26 N7 C25 118.8(2) . . ? C26 N7 Ni1 113.99(16) . . ? C25 N7 Ni1 123.39(16) . . ? C31 N8 C27 121.2(2) . . ? C31 N8 Ni1 119.43(17) . . ? C27 N8 Ni1 117.49(16) . . ? C32 N9 C33 119.1(2) . . ? C32 N9 Ni1 116.22(16) . . ? C33 N9 Ni1 123.61(16) . . ? C36 N10 C38 121.7(2) . . ? C36 N10 C37 119.6(2) . . ? C38 N10 C37 118.7(2) . . ? N3 Ni1 N8 167.19(8) . . ? N3 Ni1 N9 110.10(8) . . ? N8 Ni1 N9 76.99(8) . . ? N3 Ni1 N7 96.80(8) . . ? N8 Ni1 N7 77.16(8) . . ? N9 Ni1 N7 152.96(8) . . ? N3 Ni1 N2 77.31(8) . . ? N8 Ni1 N2 114.55(8) . . ? N9 Ni1 N2 84.83(8) . . ? N7 Ni1 N2 98.84(8) . . ? N3 Ni1 N4 76.48(8) . . ? N8 Ni1 N4 91.85(8) . . ? N9 Ni1 N4 101.06(8) . . ? N7 Ni1 N4 87.56(8) . . ? N2 Ni1 N4 153.58(8) . . ? F3 P1 F1 90.69(12) . . ? F3 P1 F5 90.89(12) . . ? F1 P1 F5 90.22(12) . . ? F3 P1 F4 89.48(12) . . ? F1 P1 F4 179.62(13) . . ? F5 P1 F4 90.12(11) . . ? F3 P1 F2 90.01(12) . . ? F1 P1 F2 89.74(11) . . ? F5 P1 F2 179.10(12) . . ? F4 P1 F2 89.92(11) . . ? F3 P1 F6 178.78(12) . . ? F1 P1 F6 90.49(11) . . ? F5 P1 F6 89.44(11) . . ? F4 P1 F6 89.34(11) . . ? F2 P1 F6 89.66(10) . . ? F10 P2 F8 94.0(2) . . ? F10 P2 F12 91.2(3) . . ? F8 P2 F12 90.19(17) . . ? F10 P2 F9 92.0(3) . . ? F8 P2 F9 90.14(17) . . ? F12 P2 F9 176.8(2) . . ? F10 P2 F11 88.8(2) . . ? F8 P2 F11 177.1(2) . . ? F12 P2 F11 90.31(14) . . ? F9 P2 F11 89.19(14) . . ? F10 P2 F7 176.9(2) . . ? F8 P2 F7 88.8(2) . . ? F12 P2 F7 87.40(16) . . ? F9 P2 F7 89.38(19) . . ? F11 P2 F7 88.36(17) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.348(3) . ? C1 C6 1.401(4) . ? C1 H1 0.95 . ? C2 N1 1.482(3) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 N1 1.347(3) . ? C3 C4 1.374(4) . ? C3 H3 0.95 . ? C4 C5 1.375(4) . ? C4 H4 0.95 . ? C5 C6 1.405(3) . ? C5 H5 0.95 . ? C6 N2 1.396(3) . ? C7 O1 1.246(3) . ? C7 N2 1.347(3) . ? C7 C8 1.508(4) . ? C8 N3 1.337(3) . ? C8 C9 1.388(3) . ? C9 C10 1.387(4) . ? C9 H9 0.95 . ? C10 C11 1.384(4) . ? C10 H10 0.95 . ? C11 C12 1.382(3) . ? C11 H11 0.95 . ? C12 N3 1.342(3) . ? C12 C13 1.510(4) . ? C13 O2 1.240(3) . ? C13 N4 1.344(3) . ? C14 C19 1.389(4) . ? C14 N4 1.397(3) . ? C14 C15 1.403(4) . ? C15 C16 1.382(4) . ? C15 H15 0.95 . ? C16 C17 1.376(5) . ? C16 H16 0.95 . ? C17 N5 1.336(4) . ? C17 H17 0.95 . ? C18 N5 1.488(4) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 N5 1.348(4) . ? C19 H19 0.95 . ? C20 N6 1.346(3) . ? C20 C25 1.393(4) . ? C20 H20 0.95 . ? C21 N6 1.483(3) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 N6 1.341(3) . ? C22 C23 1.373(4) . ? C22 H22 0.95 . ? C23 C24 1.387(4) . ? C23 H23 0.95 . ? C24 C25 1.397(4) . ? C24 H24 0.95 . ? C25 N7 1.397(3) . ? C26 O3 1.241(3) . ? C26 N7 1.343(3) . ? C26 C27 1.516(3) . ? C27 N8 1.340(3) . ? C27 C28 1.387(3) . ? C28 C29 1.383(4) . ? C28 H28 0.95 . ? C29 C30 1.393(4) . ? C29 H29 0.95 . ? C30 C31 1.387(3) . ? C30 H30 0.95 . ? C31 N8 1.334(3) . ? C31 C32 1.511(3) . ? C32 O4 1.249(3) . ? C32 N9 1.335(3) . ? C33 N9 1.396(3) . ? C33 C38 1.396(4) . ? C33 C34 1.401(4) . ? C34 C35 1.375(4) . ? C34 H34 0.95 . ? C35 C36 1.379(4) . ? C35 H35 0.95 . ? C36 N10 1.347(3) . ? C36 H36 0.95 . ? C37 N10 1.476(3) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 N10 1.351(3) . ? C38 H38 0.95 . ? C40 C41 1.451(6) . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 N11 1.144(5) . ? C42 C43 1.435(5) . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 N12 1.139(5) . ? C44 C45 1.442(6) . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C45 N13 1.139(5) . ? F1 P1 1.597(2) . ? F2 P1 1.604(2) . ? F3 P1 1.591(2) . ? F4 P1 1.604(2) . ? F5 P1 1.600(2) . ? F6 P1 1.6040(19) . ? F7 P2 1.604(3) . ? F8 P2 1.550(3) . ? F9 P2 1.583(3) . ? F10 P2 1.525(4) . ? F11 P2 1.588(2) . ? F12 P2 1.571(3) . ? N2 Ni1 2.181(2) . ? N3 Ni1 1.992(2) . ? N4 Ni1 2.183(2) . ? N7 Ni1 2.136(2) . ? N8 Ni1 1.997(2) . ? N9 Ni1 2.125(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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C3 C4 C5 -0.8(4) . . . . ? C3 C4 C5 C6 -0.9(4) . . . . ? N1 C1 C6 N2 178.0(2) . . . . ? N1 C1 C6 C5 -1.8(4) . . . . ? C4 C5 C6 N2 -177.6(2) . . . . ? C4 C5 C6 C1 2.2(4) . . . . ? O1 C7 C8 N3 164.0(2) . . . . ? N2 C7 C8 N3 -17.7(3) . . . . ? O1 C7 C8 C9 -17.8(4) . . . . ? N2 C7 C8 C9 160.5(2) . . . . ? N3 C8 C9 C10 1.4(4) . . . . ? C7 C8 C9 C10 -176.7(2) . . . . ? C8 C9 C10 C11 -0.4(4) . . . . ? C9 C10 C11 C12 -1.0(4) . . . . ? C10 C11 C12 N3 1.4(4) . . . . ? C10 C11 C12 C13 -179.9(2) . . . . ? N3 C12 C13 O2 176.6(2) . . . . ? C11 C12 C13 O2 -2.1(4) . . . . ? N3 C12 C13 N4 -5.2(3) . . . . ? C11 C12 C13 N4 176.1(2) . . . . ? C19 C14 C15 C16 1.4(4) . . . . ? N4 C14 C15 C16 -173.9(3) . . . . ? C14 C15 C16 C17 -1.1(5) . . . . ? C15 C16 C17 N5 0.1(5) . . . . ? N4 C14 C19 N5 174.8(2) . . . . ? C15 C14 C19 N5 -0.8(4) . . . . ? N6 C22 C23 C24 -0.5(5) . . . . ? C22 C23 C24 C25 -0.3(5) . . . . ? N6 C20 C25 N7 174.1(2) . . . . ? N6 C20 C25 C24 -1.9(4) . . . . ? C23 C24 C25 C20 1.5(4) . . . . ? C23 C24 C25 N7 -174.2(3) . . . . ? O3 C26 C27 N8 179.5(2) . . . . ? N7 C26 C27 N8 -2.4(3) . . . . ? O3 C26 C27 C28 1.1(4) . . . . ? N7 C26 C27 C28 179.2(2) . . . . ? N8 C27 C28 C29 2.6(4) . . . . ? C26 C27 C28 C29 -179.1(2) . . . . ? C27 C28 C29 C30 -1.9(4) . . . . ? C28 C29 C30 C31 -0.9(4) . . . . ? C29 C30 C31 N8 3.1(4) . . . . ? C29 C30 C31 C32 -175.2(2) . . . . ? N8 C31 C32 O4 168.3(2) . . . . ? C30 C31 C32 O4 -13.2(4) . . . . ? N8 C31 C32 N9 -13.9(3) . . . . ? C30 C31 C32 N9 164.6(2) . . . . ? N9 C33 C34 C35 -178.5(3) . . . . ? C38 C33 C34 C35 3.1(4) . . . . ? C33 C34 C35 C36 -2.3(5) . . . . ? C34 C35 C36 N10 -0.3(5) . . . . ? N9 C33 C38 N10 -179.9(2) . . . . ? C34 C33 C38 N10 -1.5(4) . . . . ? C4 C3 N1 C1 1.2(4) . . . . ? C4 C3 N1 C2 179.9(3) . . . . ? C6 C1 N1 C3 0.2(4) . . . . ? C6 C1 N1 C2 -178.5(2) . . . . ? O1 C7 N2 C6 3.1(4) . . . . ? C8 C7 N2 C6 -174.9(2) . . . . ? O1 C7 N2 Ni1 -164.5(2) . . . . ? C8 C7 N2 Ni1 17.4(3) . . . . ? C1 C6 N2 C7 -13.6(4) . . . . ? C5 C6 N2 C7 166.2(2) . . . . ? C1 C6 N2 Ni1 152.5(2) . . . . ? C5 C6 N2 Ni1 -27.7(3) . . . . ? C9 C8 N3 C12 -0.9(4) . . . . ? C7 C8 N3 C12 177.3(2) . . . . ? C9 C8 N3 Ni1 -169.26(19) . . . . ? C7 C8 N3 Ni1 9.0(3) . . . . ? C11 C12 N3 C8 -0.5(4) . . . . ? C13 C12 N3 C8 -179.3(2) . . . . ? C11 C12 N3 Ni1 167.87(19) . . . . ? C13 C12 N3 Ni1 -10.9(3) . . . . ? O2 C13 N4 C14 -8.8(4) . . . . ? C12 C13 N4 C14 173.1(2) . . . . ? O2 C13 N4 Ni1 -165.1(2) . . . . ? C12 C13 N4 Ni1 16.9(3) . . . . ? C19 C14 N4 C13 136.1(3) . . . . ? C15 C14 N4 C13 -48.6(4) . . . . ? C19 C14 N4 Ni1 -70.6(3) . . . . ? C15 C14 N4 Ni1 104.7(3) . . . . ? C16 C17 N5 C19 0.6(5) . . . . ? C16 C17 N5 C18 -179.8(3) . . . . ? C14 C19 N5 C17 -0.2(4) . . . . ? C14 C19 N5 C18 -179.8(3) . . . . ? C23 C22 N6 C20 0.1(4) . . . . ? C23 C22 N6 C21 179.2(3) . . . . ? C25 C20 N6 C22 1.2(4) . . . . ? C25 C20 N6 C21 -177.9(2) . . . . ? O3 C26 N7 C25 -6.5(4) . . . . ? C27 C26 N7 C25 175.7(2) . . . . ? O3 C26 N7 Ni1 -165.3(2) . . . . ? C27 C26 N7 Ni1 16.8(3) . . . . ? C20 C25 N7 C26 145.2(2) . . . . ? C24 C25 N7 C26 -39.1(4) . . . . ? C20 C25 N7 Ni1 -58.0(3) . . . . ? C24 C25 N7 Ni1 117.7(3) . . . . ? C30 C31 N8 C27 -2.5(4) . . . . ? C32 C31 N8 C27 176.0(2) . . . . ? C30 C31 N8 Ni1 -166.49(19) . . . . ? C32 C31 N8 Ni1 12.0(3) . . . . ? C28 C27 N8 C31 -0.4(4) . . . . ? C26 C27 N8 C31 -178.9(2) . . . . ? C28 C27 N8 Ni1 163.84(19) . . . . ? C26 C27 N8 Ni1 -14.6(3) . . . . ? O4 C32 N9 C33 -4.2(4) . . . . ? C31 C32 N9 C33 178.2(2) . . . . ? O4 C32 N9 Ni1 -172.8(2) . . . . ? C31 C32 N9 Ni1 9.7(3) . . . . ? C38 C33 N9 C32 -41.3(4) . . . . ? C34 C33 N9 C32 140.4(3) . . . . ? C38 C33 N9 Ni1 126.4(2) . . . . ? C34 C33 N9 Ni1 -52.0(3) . . . . ? C35 C36 N10 C38 1.9(4) . . . . ? C35 C36 N10 C37 -177.6(3) . . . . ? C33 C38 N10 C36 -0.9(4) . . . . ? C33 C38 N10 C37 178.6(3) . . . . ?