#------------------------------------------------------------------------------ #$Date: 2020-11-06 14:12:09 +0200 (Fri, 06 Nov 2020) $ #$Revision: 258830 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705315.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_7705315 loop_ _publ_author_name 'Tretiakov, Serhii' 'Damen, Johannes A. M.' 'Lutz, Martin' 'Moret, Marc-Etienne' _publ_section_title ; A dianionic C3-symmetric scorpionate: synthesis and coordination chemistry. ; _journal_issue 39 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 13549 _journal_page_last 13556 _journal_paper_doi 10.1039/d0dt02601h _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C43 H39 N6 Ni P, 0.3(C6 H14)' _chemical_formula_sum 'C44.8 H43.2 N6 Ni P' _chemical_formula_weight 755.33 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-06-19 deposited with the CCDC. 2020-08-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 113.027(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 24.314(3) _cell_length_b 17.888(2) _cell_length_c 19.297(2) _cell_measurement_reflns_used 4663 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 20.77 _cell_measurement_theta_min 2.30 _cell_volume 7724.1(15) _computing_cell_refinement 'SAINT V8.37A' _computing_data_collection Apex3 _computing_data_reduction 'SAINT V8.37A' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution SHELXT _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker Kappa ApexII' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.2211 _diffrn_reflns_av_unetI/netI 0.1920 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 66286 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 23.297 _diffrn_reflns_theta_max 23.297 _diffrn_reflns_theta_min 0.910 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_T_max 0.9996 _exptl_absorpt_correction_T_min 0.8158 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.299 _exptl_crystal_description needle _exptl_crystal_F_000 3176 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.266 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.119 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 982 _refine_ls_number_reflns 11139 _refine_ls_number_restraints 1829 _refine_ls_restrained_S_all 0.963 _refine_ls_R_factor_all 0.1954 _refine_ls_R_factor_gt 0.0877 _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^)+(0.1032P)^2^+11.9404P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1806 _refine_ls_wR_factor_ref 0.2320 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5916 _reflns_number_total 11139 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02601h2.cif _cod_data_source_block l1011a _cod_depositor_comments 'Adding full bibliography for 7705312--7705317.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'C44.80 H43.20 N6 Ni P' _cod_database_code 7705315 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL l1011a l1011a.res created by SHELXL-2018/3 at 15:44:12 on 16-Nov-2018 CELL 0.71073 24.3137 17.8884 19.2969 90.0000 113.0266 90.0000 ZERR 8 0.0028 0.0020 0.0021 0.0000 0.0033 0.0000 LATT 1 SYMM -x, y+0.5, 0.5-z SFAC C H N NI P UNIT 358.4 345.6 48 8 8 TEMP -123 L.S. 15 FMAP 2 PLAN -20 ACTA BOND $H CONF TWIN -1 0 -1 0 -1 0 0 0 1 DFIX 1.54 0.01 C19 C29 C29 C39 C39 C49 C49 C59 C59 C69 SADI 0.01 C19 C39 C29 C49 C39 C59 C49 C69 RIGU C11 > C154 RIGU C15 > C158 ISOR 0.02 C11 > C154 ISOR 0.02 C15 > C158 ISOR 0.01 C19 > C69 WGHT 0.103200 11.940399 BASF 0.23611 FVAR 0.21092 NI1 4 0.457500 0.196347 0.286014 11.00000 0.02365 0.01742 = 0.01842 -0.00018 0.00741 -0.00211 P1 5 0.346616 0.154576 0.129932 11.00000 0.02170 0.01929 = 0.01508 -0.00145 0.00206 -0.00032 C1 1 0.286258 0.131163 0.044198 11.00000 0.02449 0.02983 = 0.03491 -0.00499 0.00705 -0.00038 AFIX 137 H1A 2 0.291543 0.156449 0.002170 11.00000 -1.50000 H1B 2 0.248521 0.147195 0.046659 11.00000 -1.50000 H1C 2 0.285469 0.076950 0.036552 11.00000 -1.50000 AFIX 0 N11 3 0.397732 0.105143 0.270637 11.00000 0.01978 0.01694 = 0.01317 0.00308 -0.00052 -0.00087 C11 1 0.347547 0.096475 0.204199 11.00000 0.02036 0.02623 = 0.01287 -0.00288 0.01049 -0.00410 C21 1 0.309882 0.038796 0.206074 11.00000 0.02069 0.02162 = 0.02715 -0.00863 0.01187 -0.00562 C31 1 0.337936 0.008455 0.279674 11.00000 0.02760 0.02322 = 0.02515 -0.00314 0.01330 -0.00644 C41 1 0.324214 -0.052478 0.316684 11.00000 0.03878 0.03401 = 0.02993 0.00025 0.01809 -0.01142 AFIX 43 H41 2 0.288757 -0.080617 0.291947 11.00000 -1.20000 AFIX 0 C51 1 0.362002 -0.070695 0.387918 11.00000 0.05487 0.03367 = 0.03220 0.01389 0.02165 -0.00676 AFIX 43 H51 2 0.352982 -0.112043 0.412544 11.00000 -1.20000 AFIX 0 C61 1 0.414609 -0.028657 0.425691 11.00000 0.05179 0.02261 = 0.02445 0.00783 0.01398 0.00312 AFIX 43 H61 2 0.440336 -0.041732 0.475610 11.00000 -1.20000 AFIX 0 C71 1 0.428805 0.030830 0.390867 11.00000 0.03615 0.01824 = 0.02257 -0.00302 0.01021 -0.00143 AFIX 43 H71 2 0.464072 0.058914 0.416817 11.00000 -1.20000 AFIX 0 C81 1 0.391463 0.050052 0.317392 11.00000 0.03005 0.01217 = 0.01651 -0.00479 0.01379 0.00216 C91 1 0.251697 0.010982 0.148135 11.00000 0.02801 0.03008 = 0.03943 0.00509 0.00479 -0.01031 AFIX 137 H91A 2 0.224114 0.053086 0.128814 11.00000 -1.50000 H91B 2 0.234169 -0.025719 0.171254 11.00000 -1.50000 H91C 2 0.258890 -0.012545 0.106582 11.00000 -1.50000 AFIX 0 SAME 0.01 N11 > C91 N12 3 0.382982 0.265426 0.228149 11.00000 0.03130 0.01291 = 0.01931 0.00106 0.00563 -0.00187 C12 1 0.342210 0.248648 0.156271 11.00000 0.01995 0.01854 = 0.01674 0.00081 0.00699 -0.00471 C22 1 0.303859 0.306890 0.120559 11.00000 0.02525 0.01780 = 0.02173 0.00305 0.01222 -0.00263 C32 1 0.321770 0.366157 0.173568 11.00000 0.02024 0.01897 = 0.02643 0.00109 0.00948 -0.00106 C42 1 0.300602 0.439627 0.172973 11.00000 0.03429 0.02046 = 0.02911 0.01267 0.01995 0.00485 AFIX 43 H42 2 0.268131 0.457812 0.130103 11.00000 -1.20000 AFIX 0 C52 1 0.326926 0.484347 0.234125 11.00000 0.03981 0.02032 = 0.04474 0.00320 0.02820 0.00593 AFIX 43 H52 2 0.313043 0.534084 0.233497 11.00000 -1.20000 AFIX 0 C62 1 0.374857 0.457429 0.298741 11.00000 0.04973 0.02539 = 0.02955 -0.00465 0.02289 -0.00161 AFIX 43 H62 2 0.392927 0.489394 0.340912 11.00000 -1.20000 AFIX 0 C72 1 0.395485 0.385524 0.301038 11.00000 0.03132 0.02479 = 0.01948 -0.00388 0.00892 0.00654 AFIX 43 H72 2 0.426839 0.367461 0.345151 11.00000 -1.20000 AFIX 0 C82 1 0.370249 0.339266 0.238461 11.00000 0.02613 0.01760 = 0.01874 0.00328 0.01019 0.00072 C92 1 0.256941 0.313896 0.042639 11.00000 0.02984 0.01686 = 0.02947 -0.00159 -0.00092 -0.00413 AFIX 137 H92A 2 0.252959 0.266224 0.016083 11.00000 -1.50000 H92B 2 0.268437 0.353109 0.015439 11.00000 -1.50000 H92C 2 0.218680 0.326948 0.045328 11.00000 -1.50000 AFIX 0 SAME 0.01 N11 > C91 N13 3 0.464830 0.168981 0.182119 11.00000 0.02431 0.02294 = 0.01374 0.00248 0.00665 0.00256 C13 1 0.415827 0.143086 0.121179 11.00000 0.02702 0.01202 = 0.01826 0.00076 0.00491 -0.00204 C23 1 0.430495 0.111700 0.064674 11.00000 0.03502 0.01014 = 0.01192 0.00654 0.00629 -0.00197 C33 1 0.492949 0.122740 0.089122 11.00000 0.03493 0.01795 = 0.02006 0.00356 0.01225 0.00196 C43 1 0.533726 0.110095 0.054785 11.00000 0.03577 0.02430 = 0.02424 0.00979 0.01385 0.00848 AFIX 43 H43 2 0.520652 0.087880 0.006273 11.00000 -1.20000 AFIX 0 C53 1 0.592012 0.130006 0.091775 11.00000 0.03047 0.04042 = 0.03530 0.01063 0.02168 0.00953 AFIX 43 H53 2 0.619719 0.121514 0.068969 11.00000 -1.20000 AFIX 0 C63 1 0.611591 0.163245 0.163916 11.00000 0.03076 0.04153 = 0.03016 0.00869 0.01526 0.00136 AFIX 43 H63 2 0.652406 0.176864 0.188958 11.00000 -1.20000 AFIX 0 C73 1 0.572771 0.176153 0.198329 11.00000 0.02455 0.02805 = 0.03222 -0.00230 0.00867 0.00272 AFIX 43 H73 2 0.586700 0.198133 0.246999 11.00000 -1.20000 AFIX 0 C83 1 0.512663 0.156869 0.161569 11.00000 0.02408 0.01646 = 0.01824 0.00959 0.00942 0.00793 C93 1 0.391149 0.079163 -0.010265 11.00000 0.03278 0.03297 = 0.02022 -0.00508 0.00799 -0.00697 AFIX 137 H93A 2 0.361997 0.045203 -0.003530 11.00000 -1.50000 H93B 2 0.415760 0.051503 -0.031410 11.00000 -1.50000 H93C 2 0.370057 0.119586 -0.044676 11.00000 -1.50000 AFIX 0 N14 3 0.536022 0.127702 0.341458 11.00000 0.03016 0.02843 = 0.02408 0.00028 0.01330 0.00268 C14 1 0.531702 0.055127 0.321080 11.00000 0.03347 0.03415 = 0.02379 -0.00519 0.01869 0.00392 AFIX 43 H14 2 0.496205 0.038932 0.281135 11.00000 -1.20000 AFIX 0 C24 1 0.576043 0.003064 0.355088 11.00000 0.04206 0.03658 = 0.04309 -0.00606 0.01781 0.01292 AFIX 43 H24 2 0.570751 -0.047714 0.339431 11.00000 -1.20000 AFIX 0 C34 1 0.628125 0.026278 0.412205 11.00000 0.04221 0.05010 = 0.02416 0.00695 0.01770 0.01556 AFIX 43 H34 2 0.658568 -0.008479 0.439013 11.00000 -1.20000 AFIX 0 C44 1 0.634699 0.100924 0.429177 11.00000 0.03330 0.05563 = 0.03182 -0.00803 0.00886 0.00112 AFIX 43 H44 2 0.671156 0.119149 0.465881 11.00000 -1.20000 AFIX 0 C54 1 0.588278 0.149680 0.392883 11.00000 0.03045 0.03956 = 0.02674 -0.00013 0.01534 -0.00780 AFIX 43 H54 2 0.593943 0.201294 0.405227 11.00000 -1.20000 AFIX 0 SAME 0.01 N14 > C54 N24 3 0.512439 0.296230 0.302817 11.00000 0.03843 0.02163 = 0.01071 -0.00016 0.01029 -0.00407 C64 1 0.539231 0.332895 0.368209 11.00000 0.04570 0.01924 = 0.01283 -0.00191 0.00974 -0.00786 AFIX 43 H64 2 0.535967 0.312950 0.412070 11.00000 -1.20000 AFIX 0 C74 1 0.571219 0.397995 0.374884 11.00000 0.05293 0.02714 = 0.02534 -0.01008 0.01234 -0.01528 AFIX 43 H74 2 0.588071 0.423275 0.421824 11.00000 -1.20000 AFIX 0 C84 1 0.578332 0.425747 0.312422 11.00000 0.04606 0.02558 = 0.04120 -0.00187 0.02021 -0.02047 AFIX 43 H84 2 0.601942 0.468996 0.315890 11.00000 -1.20000 AFIX 0 C94 1 0.550420 0.389358 0.244744 11.00000 0.05184 0.02381 = 0.02977 0.00312 0.02386 -0.00491 AFIX 43 H94 2 0.553660 0.407836 0.200339 11.00000 -1.20000 AFIX 0 C104 1 0.517667 0.325659 0.242321 11.00000 0.03708 0.01417 = 0.01749 0.00019 0.01039 0.00136 AFIX 43 H104 2 0.497874 0.301631 0.195140 11.00000 -1.20000 AFIX 0 SAME 0.01 N14 > C54 N34 3 0.449234 0.213390 0.396576 11.00000 0.02948 0.01877 = 0.02177 0.00106 0.00761 -0.00488 C114 1 0.490239 0.201358 0.466066 11.00000 0.03197 0.02562 = 0.02254 0.00454 0.00794 0.00283 AFIX 43 H114 2 0.530820 0.195976 0.472484 11.00000 -1.20000 AFIX 0 C124 1 0.476456 0.196388 0.528833 11.00000 0.04896 0.02704 = 0.01869 -0.00518 0.01078 -0.00521 AFIX 43 H124 2 0.507247 0.189354 0.577270 11.00000 -1.20000 AFIX 0 C134 1 0.417700 0.201704 0.520743 11.00000 0.05680 0.03953 = 0.02747 -0.00798 0.02298 -0.00173 AFIX 43 H134 2 0.407090 0.198620 0.563097 11.00000 -1.20000 AFIX 0 C144 1 0.375093 0.211589 0.449544 11.00000 0.04435 0.03209 = 0.02846 -0.01455 0.01906 -0.00930 AFIX 43 H144 2 0.334006 0.214467 0.441400 11.00000 -1.20000 AFIX 0 C154 1 0.392653 0.217311 0.389792 11.00000 0.02820 0.02166 = 0.02665 0.00384 0.00932 -0.00049 AFIX 43 H154 2 0.362546 0.224478 0.340885 11.00000 -1.20000 AFIX 0 NI2 4 0.048740 0.303252 0.335609 11.00000 0.02297 0.01601 = 0.01884 0.00070 0.00884 0.00076 P2 5 0.157657 0.344740 0.283828 11.00000 0.02821 0.01739 = 0.02321 -0.00020 0.01363 -0.00104 C2 1 0.217520 0.366459 0.255718 11.00000 0.02989 0.03895 = 0.03376 -0.00768 0.02528 -0.01052 AFIX 137 H2A 2 0.213168 0.337287 0.210883 11.00000 -1.50000 H2B 2 0.255676 0.354121 0.296676 11.00000 -1.50000 H2C 2 0.216608 0.419901 0.244149 11.00000 -1.50000 AFIX 0 SAME 0.01 N11 > C91 N15 3 0.107189 0.396197 0.373824 11.00000 0.03092 0.01855 = 0.01792 0.00628 0.00808 -0.00104 C15 1 0.155700 0.407165 0.353992 11.00000 0.02523 0.02560 = 0.02025 0.00408 0.01617 -0.00411 C25 1 0.188825 0.471058 0.385298 11.00000 0.02679 0.02042 = 0.02061 0.00538 0.00712 -0.00343 C35 1 0.158872 0.503409 0.427793 11.00000 0.02469 0.02425 = 0.01636 0.00496 0.00149 0.00154 C45 1 0.167378 0.570848 0.469016 11.00000 0.03936 0.03114 = 0.03040 -0.00226 0.01112 -0.00668 AFIX 43 H45 2 0.199385 0.603540 0.473489 11.00000 -1.20000 AFIX 0 C55 1 0.128660 0.587959 0.502210 11.00000 0.04234 0.03372 = 0.03204 -0.00798 0.00834 -0.00484 AFIX 43 H55 2 0.133976 0.633123 0.529985 11.00000 -1.20000 AFIX 0 C65 1 0.080776 0.539917 0.496174 11.00000 0.04119 0.03096 = 0.02319 -0.00109 0.02239 0.00556 AFIX 43 H65 2 0.055462 0.552290 0.521518 11.00000 -1.20000 AFIX 0 C75 1 0.070468 0.475673 0.454152 11.00000 0.03032 0.02961 = 0.01309 0.00341 0.00800 0.00836 AFIX 43 H75 2 0.037283 0.444664 0.448595 11.00000 -1.20000 AFIX 0 C85 1 0.109323 0.456493 0.419716 11.00000 0.03180 0.02105 = 0.01176 -0.00120 0.00989 0.00342 C95 1 0.241866 0.505768 0.375922 11.00000 0.02924 0.04969 = 0.02894 0.00225 0.01449 -0.00941 AFIX 137 H95A 2 0.269597 0.466379 0.375033 11.00000 -1.50000 H95B 2 0.262182 0.539723 0.418081 11.00000 -1.50000 H95C 2 0.228367 0.533808 0.328544 11.00000 -1.50000 AFIX 0 SAME 0.01 N11 > C91 N16 3 0.122852 0.234579 0.351341 11.00000 0.01970 0.02642 = 0.01232 0.00142 0.00288 0.00383 C16 1 0.163347 0.251812 0.319130 11.00000 0.02727 0.02114 = 0.01703 -0.00552 0.00794 0.00088 C26 1 0.200240 0.193125 0.317587 11.00000 0.02368 0.03253 = 0.02479 -0.00147 0.00971 0.00369 C36 1 0.184823 0.134427 0.356393 11.00000 0.02812 0.02514 = 0.01613 -0.00395 0.00587 0.00613 C46 1 0.207895 0.061854 0.378056 11.00000 0.03262 0.02999 = 0.02045 -0.00724 0.00608 0.00699 AFIX 43 H46 2 0.240465 0.044248 0.367074 11.00000 -1.20000 AFIX 0 C56 1 0.182714 0.017520 0.414932 11.00000 0.04612 0.01900 = 0.02939 -0.00343 0.00987 0.01143 AFIX 43 H56 2 0.197527 -0.031688 0.429142 11.00000 -1.20000 AFIX 0 C66 1 0.134736 0.043788 0.432383 11.00000 0.04376 0.01856 = 0.02743 -0.00842 0.01230 -0.00202 AFIX 43 H66 2 0.118021 0.011867 0.458385 11.00000 -1.20000 AFIX 0 C76 1 0.111718 0.114648 0.412496 11.00000 0.02802 0.02791 = 0.03974 0.00121 0.02101 0.00553 AFIX 43 H76 2 0.079322 0.131480 0.424260 11.00000 -1.20000 AFIX 0 C86 1 0.136917 0.161274 0.374711 11.00000 0.02425 0.02379 = 0.01697 -0.00256 0.00513 0.00253 C96 1 0.244210 0.184400 0.280927 11.00000 0.02527 0.04116 = 0.01782 0.00670 0.00874 0.01843 AFIX 137 H96A 2 0.223347 0.166487 0.229194 11.00000 -1.50000 H96B 2 0.275048 0.148241 0.309424 11.00000 -1.50000 H96C 2 0.262902 0.232784 0.280261 11.00000 -1.50000 AFIX 0 SAME 0.01 N11 > C91 N17 3 0.040090 0.326742 0.222639 11.00000 0.02793 0.02174 = 0.02845 0.00874 0.00763 0.00034 C17 1 0.088159 0.353948 0.208327 11.00000 0.02958 0.01338 = 0.02306 -0.00086 0.01065 0.00031 C27 1 0.072413 0.384405 0.136937 11.00000 0.04231 0.01584 = 0.02574 0.00352 0.01674 0.00415 C37 1 0.009747 0.373776 0.102323 11.00000 0.04173 0.01098 = 0.02745 0.00025 0.01446 0.00852 C47 1 -0.032474 0.387493 0.028646 11.00000 0.05425 0.02939 = 0.02511 -0.00373 0.01306 0.00662 AFIX 43 H47 2 -0.020791 0.411408 -0.007413 11.00000 -1.20000 AFIX 0 C57 1 -0.090260 0.365881 0.010073 11.00000 0.04948 0.03615 = 0.02437 -0.00180 -0.00125 0.01014 AFIX 43 H57 2 -0.118632 0.373233 -0.039894 11.00000 -1.20000 AFIX 0 C67 1 -0.108642 0.332683 0.064024 11.00000 0.03443 0.03742 = 0.04174 0.00181 0.00254 0.00724 AFIX 43 H67 2 -0.149420 0.319480 0.050079 11.00000 -1.20000 AFIX 0 C77 1 -0.068491 0.319164 0.136375 11.00000 0.03390 0.02370 = 0.03267 0.00049 0.00563 0.00149 AFIX 43 H77 2 -0.081214 0.297158 0.172412 11.00000 -1.20000 AFIX 0 C87 1 -0.008802 0.338431 0.155653 11.00000 0.02892 0.01794 = 0.02236 -0.00149 0.00906 0.01254 C97 1 0.110160 0.418376 0.099290 11.00000 0.04646 0.03833 = 0.03288 0.00984 0.01885 0.00306 AFIX 137 H97A 2 0.136258 0.456719 0.132150 11.00000 -1.50000 H97B 2 0.084213 0.441179 0.051473 11.00000 -1.50000 H97C 2 0.134611 0.379371 0.089710 11.00000 -1.50000 AFIX 0 SAME 0.01 N14 > C54 N18 3 -0.030150 0.371332 0.311369 11.00000 0.02622 0.02244 = 0.02459 -0.01176 0.00928 -0.00484 C18 1 -0.028591 0.440480 0.283645 11.00000 0.02399 0.03088 = 0.03542 -0.00096 0.00848 -0.00015 AFIX 43 H18 2 0.006125 0.454752 0.275697 11.00000 -1.20000 AFIX 0 C28 1 -0.074581 0.491159 0.266376 11.00000 0.03633 0.03407 = 0.02055 0.00920 0.01256 0.00578 AFIX 43 H28 2 -0.071992 0.538454 0.245462 11.00000 -1.20000 AFIX 0 C38 1 -0.124428 0.472353 0.279840 11.00000 0.03850 0.04033 = 0.04145 0.01423 0.02257 0.01635 AFIX 43 H38 2 -0.156050 0.507083 0.270782 11.00000 -1.20000 AFIX 0 C48 1 -0.127129 0.401982 0.306727 11.00000 0.02698 0.04364 = 0.03542 0.01181 0.01839 0.00610 AFIX 43 H48 2 -0.161110 0.386933 0.315988 11.00000 -1.20000 AFIX 0 C58 1 -0.080123 0.353404 0.320152 11.00000 0.02789 0.02595 = 0.02261 0.00151 0.01009 -0.00092 AFIX 43 H58 2 -0.083594 0.304249 0.336637 11.00000 -1.20000 AFIX 0 SAME 0.01 N14 > C54 N28 3 -0.006580 0.204249 0.302333 11.00000 0.02738 0.02180 = 0.01980 -0.00246 0.00874 0.00163 C68 1 -0.032764 0.168764 0.342682 11.00000 0.02283 0.02629 = 0.02224 -0.00110 0.00311 -0.00093 AFIX 43 H68 2 -0.029672 0.190216 0.389098 11.00000 -1.20000 AFIX 0 C78 1 -0.063907 0.102755 0.320099 11.00000 0.03168 0.02872 = 0.02359 -0.00482 0.01037 -0.00464 AFIX 43 H78 2 -0.080620 0.078613 0.351196 11.00000 -1.20000 AFIX 0 C88 1 -0.070424 0.072353 0.251831 11.00000 0.04580 0.02691 = 0.02679 -0.00887 0.01621 -0.01064 AFIX 43 H88 2 -0.092612 0.027650 0.234238 11.00000 -1.20000 AFIX 0 C98 1 -0.044079 0.108168 0.209652 11.00000 0.03884 0.02442 = 0.01653 -0.00887 0.00689 -0.00640 AFIX 43 H98 2 -0.048131 0.088903 0.162019 11.00000 -1.20000 AFIX 0 C108 1 -0.011572 0.172707 0.237659 11.00000 0.02691 0.01731 = 0.02094 -0.00149 0.00768 -0.00035 AFIX 43 H108 2 0.008157 0.195636 0.209324 11.00000 -1.20000 AFIX 0 SAME 0.01 N14 > C54 N38 3 0.061578 0.290715 0.456163 11.00000 0.02428 0.01262 = 0.01646 -0.00506 0.00750 -0.00080 C118 1 0.021837 0.298421 0.488028 11.00000 0.02494 0.02691 = 0.02375 -0.00001 0.01259 0.00025 AFIX 43 H118 2 -0.019431 0.299225 0.456151 11.00000 -1.20000 AFIX 0 C128 1 0.037628 0.305257 0.564702 11.00000 0.04328 0.02738 = 0.02584 0.00144 0.01936 0.00178 AFIX 43 H128 2 0.008023 0.311708 0.584886 11.00000 -1.20000 AFIX 0 C138 1 0.097160 0.302501 0.611034 11.00000 0.05220 0.02897 = 0.01476 0.00535 0.01256 -0.00200 AFIX 43 H138 2 0.109637 0.307380 0.664023 11.00000 -1.20000 AFIX 0 C148 1 0.138266 0.292581 0.579451 11.00000 0.03856 0.02853 = 0.01306 0.00637 0.00337 0.00715 AFIX 43 H148 2 0.179614 0.288952 0.610483 11.00000 -1.20000 AFIX 0 C158 1 0.119010 0.287902 0.501998 11.00000 0.02823 0.02877 = 0.01681 0.00570 0.00890 0.00169 AFIX 43 H158 2 0.147994 0.282456 0.480666 11.00000 -1.20000 AFIX 0 C19 1 0.245049 0.745622 0.370154 10.60000 0.07340 0.07525 = 0.09664 0.00019 0.04886 0.01596 AFIX 33 H19A 2 0.228020 0.760405 0.406498 10.60000 -1.50000 H19B 2 0.277226 0.709359 0.393561 10.60000 -1.50000 H19C 2 0.261113 0.789810 0.354528 10.60000 -1.50000 AFIX 0 C29 1 0.196588 0.710362 0.301638 10.60000 0.05540 0.05861 = 0.06459 0.00506 0.02008 0.01760 AFIX 23 H29A 2 0.163916 0.747189 0.279942 10.60000 -1.20000 H29B 2 0.179977 0.666998 0.318849 10.60000 -1.20000 AFIX 0 C39 1 0.215541 0.683986 0.239121 10.60000 0.04523 0.08092 = 0.07296 -0.00484 0.02123 0.00186 AFIX 23 H39A 2 0.181223 0.658006 0.200565 10.60000 -1.20000 H39B 2 0.247957 0.646801 0.260658 10.60000 -1.20000 AFIX 0 C49 1 0.237120 0.744505 0.199995 10.60000 0.05743 0.06128 = 0.06393 0.00350 0.01500 0.03183 AFIX 23 H49A 2 0.270279 0.772215 0.238559 10.60000 -1.20000 H49B 2 0.204087 0.780320 0.175810 10.60000 -1.20000 AFIX 0 C59 1 0.258780 0.714910 0.139836 10.60000 0.04833 0.06563 = 0.04891 0.00462 0.01100 0.01520 AFIX 23 H59A 2 0.290642 0.677459 0.163394 10.60000 -1.20000 H59B 2 0.225126 0.689262 0.099929 10.60000 -1.20000 AFIX 0 C69 1 0.282974 0.776359 0.103386 10.60000 0.06058 0.06347 = 0.09159 0.02451 0.01707 0.04682 AFIX 33 H69A 2 0.295888 0.753855 0.065936 10.60000 -1.50000 H69B 2 0.251421 0.813066 0.078750 10.60000 -1.50000 H69C 2 0.317005 0.801250 0.142282 10.60000 -1.50000 AFIX 0 HKLF 4 REM l1011a REM wR2 = 0.2320, GooF = S = 1.034, Restrained GooF = 0.963 for all data REM R1 = 0.0877 for 5916 Fo > 4sig(Fo) and 0.1954 for all 11139 data REM 982 parameters refined using 1829 restraints END WGHT 0.1015 12.6814 REM Highest difference peak 1.266, deepest hole -0.862, 1-sigma level 0.119 Q1 1 0.0470 0.1980 0.3376 11.00000 0.05 1.27 Q2 1 0.4588 0.3029 0.2764 11.00000 0.05 1.09 Q3 1 0.2561 0.7745 0.1511 11.00000 0.05 0.76 Q4 1 0.2795 0.7800 0.2010 11.00000 0.05 0.75 Q5 1 0.2483 0.7459 0.0897 11.00000 0.05 0.67 Q6 1 0.2461 0.7608 0.3021 11.00000 0.05 0.65 Q7 1 0.2177 0.7133 0.2211 11.00000 0.05 0.64 Q8 1 0.2167 0.7500 0.3336 11.00000 0.05 0.63 Q9 1 0.2355 0.7791 0.2429 11.00000 0.05 0.60 Q10 1 0.2735 0.7424 0.0222 11.00000 0.05 0.58 Q11 1 0.2049 0.7026 0.3615 11.00000 0.05 0.58 Q12 1 0.2898 0.7935 0.0002 11.00000 0.05 0.56 Q13 1 0.2204 0.7171 0.1673 11.00000 0.05 0.55 Q14 1 0.5033 0.1921 0.2980 11.00000 0.05 0.55 Q15 1 0.1492 0.1560 0.2847 11.00000 0.05 0.55 Q16 1 0.3419 0.3424 0.1401 11.00000 0.05 0.53 Q17 1 0.2133 0.6467 0.1885 11.00000 0.05 0.52 Q18 1 0.5302 0.1910 0.2522 11.00000 0.05 0.52 Q19 1 0.2891 0.7353 0.1295 11.00000 0.05 0.51 Q20 1 0.2316 0.7102 0.4295 11.00000 0.05 0.49 ; _shelx_res_checksum 54600 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.45750(6) 0.19635(8) 0.28601(8) 0.0201(4) Uani 1 1 d . . . . . P1 P 0.34662(13) 0.15458(17) 0.12993(17) 0.0203(8) Uani 1 1 d . . . . . C1 C 0.2863(5) 0.1312(7) 0.0442(7) 0.031(3) Uani 1 1 d . . . . . H1A H 0.291543 0.156449 0.002170 0.047 Uiso 1 1 calc R U . . . H1B H 0.248521 0.147195 0.046659 0.047 Uiso 1 1 calc R U . . . H1C H 0.285469 0.076950 0.036552 0.047 Uiso 1 1 calc R U . . . N11 N 0.3977(3) 0.1051(4) 0.2706(4) 0.019(2) Uani 1 1 d D . . . . C11 C 0.3475(4) 0.0965(5) 0.2042(4) 0.019(3) Uani 1 1 d D U . . . C21 C 0.3099(4) 0.0388(5) 0.2061(5) 0.022(2) Uani 1 1 d D U . . . C31 C 0.3379(4) 0.0085(5) 0.2797(5) 0.024(3) Uani 1 1 d D U . . . C41 C 0.3242(4) -0.0525(5) 0.3167(5) 0.033(3) Uani 1 1 d D U . . . H41 H 0.288757 -0.080617 0.291947 0.039 Uiso 1 1 calc R U . . . C51 C 0.3620(5) -0.0707(6) 0.3879(5) 0.039(3) Uani 1 1 d D U . . . H51 H 0.352982 -0.112043 0.412544 0.047 Uiso 1 1 calc R U . . . C61 C 0.4146(4) -0.0287(5) 0.4257(5) 0.033(3) Uani 1 1 d D U . . . H61 H 0.440336 -0.041732 0.475610 0.040 Uiso 1 1 calc R U . . . C71 C 0.4288(4) 0.0308(5) 0.3909(5) 0.026(3) Uani 1 1 d D U . . . H71 H 0.464072 0.058914 0.416817 0.031 Uiso 1 1 calc R U . . . C81 C 0.3915(4) 0.0501(5) 0.3174(4) 0.018(2) Uani 1 1 d D U . . . C91 C 0.2517(4) 0.0110(6) 0.1481(6) 0.035(3) Uani 1 1 d D U . . . H91A H 0.224114 0.053086 0.128814 0.053 Uiso 1 1 calc R U . . . H91B H 0.234169 -0.025719 0.171254 0.053 Uiso 1 1 calc R U . . . H91C H 0.258890 -0.012545 0.106582 0.053 Uiso 1 1 calc R U . . . N12 N 0.3830(4) 0.2654(4) 0.2281(4) 0.022(2) Uani 1 1 d D U . . . C12 C 0.3422(4) 0.2486(4) 0.1563(5) 0.018(3) Uani 1 1 d D U . . . C22 C 0.3039(4) 0.3069(4) 0.1206(4) 0.021(2) Uani 1 1 d D U . . . C32 C 0.3218(4) 0.3662(4) 0.1736(5) 0.022(2) Uani 1 1 d D U . . . C42 C 0.3006(4) 0.4396(4) 0.1730(5) 0.026(3) Uani 1 1 d D U . . . H42 H 0.268131 0.457812 0.130103 0.031 Uiso 1 1 calc R U . . . C52 C 0.3269(5) 0.4843(5) 0.2341(5) 0.031(3) Uani 1 1 d D U . . . H52 H 0.313043 0.534084 0.233497 0.038 Uiso 1 1 calc R U . . . C62 C 0.3749(5) 0.4574(5) 0.2987(5) 0.033(3) Uani 1 1 d D U . . . H62 H 0.392927 0.489394 0.340912 0.039 Uiso 1 1 calc R U . . . C72 C 0.3955(4) 0.3855(5) 0.3010(5) 0.026(3) Uani 1 1 d D U . . . H72 H 0.426839 0.367461 0.345151 0.031 Uiso 1 1 calc R U . . . C82 C 0.3702(4) 0.3393(4) 0.2385(4) 0.020(2) Uani 1 1 d D U . . . C92 C 0.2569(4) 0.3139(6) 0.0426(5) 0.029(3) Uani 1 1 d D U . . . H92A H 0.252959 0.266224 0.016083 0.044 Uiso 1 1 calc R U . . . H92B H 0.268437 0.353109 0.015439 0.044 Uiso 1 1 calc R U . . . H92C H 0.218680 0.326948 0.045328 0.044 Uiso 1 1 calc R U . . . N13 N 0.4648(3) 0.1690(5) 0.1821(4) 0.021(2) Uani 1 1 d D U . . . C13 C 0.4158(3) 0.1431(6) 0.1212(5) 0.020(2) Uani 1 1 d D U . . . C23 C 0.4305(3) 0.1117(5) 0.0647(4) 0.020(2) Uani 1 1 d D U . . . C33 C 0.4929(3) 0.1227(6) 0.0891(5) 0.024(2) Uani 1 1 d D U . . . C43 C 0.5337(4) 0.1101(6) 0.0548(5) 0.027(3) Uani 1 1 d D U . . . H43 H 0.520652 0.087880 0.006273 0.033 Uiso 1 1 calc R U . . . C53 C 0.5920(4) 0.1300(6) 0.0918(5) 0.033(3) Uani 1 1 d D U . . . H53 H 0.619719 0.121514 0.068969 0.039 Uiso 1 1 calc R U . . . C63 C 0.6116(4) 0.1632(6) 0.1639(5) 0.033(3) Uani 1 1 d D U . . . H63 H 0.652406 0.176864 0.188958 0.040 Uiso 1 1 calc R U . . . C73 C 0.5728(3) 0.1762(6) 0.1983(5) 0.029(3) Uani 1 1 d D U . . . H73 H 0.586700 0.198133 0.246999 0.035 Uiso 1 1 calc R U . . . C83 C 0.5127(3) 0.1569(5) 0.1616(5) 0.019(2) Uani 1 1 d D U . . . C93 C 0.3911(4) 0.0792(6) -0.0103(5) 0.029(3) Uani 1 1 d D U . . . H93A H 0.361997 0.045203 -0.003530 0.044 Uiso 1 1 calc R U . . . H93B H 0.415760 0.051503 -0.031410 0.044 Uiso 1 1 calc R U . . . H93C H 0.370057 0.119586 -0.044676 0.044 Uiso 1 1 calc R U . . . N14 N 0.5360(3) 0.1277(4) 0.3415(5) 0.027(2) Uani 1 1 d D U . . . C14 C 0.5317(4) 0.0551(5) 0.3211(6) 0.028(3) Uani 1 1 d D U . . . H14 H 0.496205 0.038932 0.281135 0.034 Uiso 1 1 calc R U . . . C24 C 0.5760(4) 0.0031(5) 0.3551(6) 0.040(3) Uani 1 1 d D U . . . H24 H 0.570751 -0.047714 0.339431 0.048 Uiso 1 1 calc R U . . . C34 C 0.6281(4) 0.0263(6) 0.4122(6) 0.037(3) Uani 1 1 d D U . . . H34 H 0.658568 -0.008479 0.439013 0.045 Uiso 1 1 calc R U . . . C44 C 0.6347(4) 0.1009(6) 0.4292(6) 0.041(3) Uani 1 1 d D U . . . H44 H 0.671156 0.119149 0.465881 0.050 Uiso 1 1 calc R U . . . C54 C 0.5883(4) 0.1497(5) 0.3929(6) 0.031(3) Uani 1 1 d D U . . . H54 H 0.593943 0.201294 0.405227 0.037 Uiso 1 1 calc R U . . . N24 N 0.5124(4) 0.2962(4) 0.3028(4) 0.023(2) Uani 1 1 d D U . . . C64 C 0.5392(5) 0.3329(5) 0.3682(5) 0.026(3) Uani 1 1 d D U . . . H64 H 0.535967 0.312950 0.412070 0.032 Uiso 1 1 calc R U . . . C74 C 0.5712(5) 0.3980(6) 0.3749(5) 0.036(3) Uani 1 1 d D U . . . H74 H 0.588071 0.423275 0.421824 0.043 Uiso 1 1 calc R U . . . C84 C 0.5783(5) 0.4257(6) 0.3124(5) 0.037(3) Uani 1 1 d D U . . . H84 H 0.601942 0.468996 0.315890 0.044 Uiso 1 1 calc R U . . . C94 C 0.5504(5) 0.3894(5) 0.2447(5) 0.033(3) Uani 1 1 d D U . . . H94 H 0.553660 0.407836 0.200339 0.039 Uiso 1 1 calc R U . . . C104 C 0.5177(5) 0.3257(5) 0.2423(5) 0.023(3) Uani 1 1 d D U . . . H104 H 0.497874 0.301631 0.195140 0.028 Uiso 1 1 calc R U . . . N34 N 0.4492(3) 0.2134(5) 0.3966(4) 0.024(2) Uani 1 1 d D U . . . C114 C 0.4902(4) 0.2014(6) 0.4661(5) 0.028(3) Uani 1 1 d D U . . . H114 H 0.530820 0.195976 0.472484 0.033 Uiso 1 1 calc R U . . . C124 C 0.4765(4) 0.1964(6) 0.5288(5) 0.032(3) Uani 1 1 d D U . . . H124 H 0.507247 0.189354 0.577270 0.039 Uiso 1 1 calc R U . . . C134 C 0.4177(4) 0.2017(7) 0.5207(5) 0.039(3) Uani 1 1 d D U . . . H134 H 0.407090 0.198620 0.563097 0.047 Uiso 1 1 calc R U . . . C144 C 0.3751(4) 0.2116(6) 0.4495(5) 0.033(3) Uani 1 1 d D U . . . H144 H 0.334006 0.214467 0.441400 0.040 Uiso 1 1 calc R U . . . C154 C 0.3927(4) 0.2173(6) 0.3898(5) 0.026(3) Uani 1 1 d D U . . . H154 H 0.362546 0.224478 0.340885 0.031 Uiso 1 1 calc R U . . . Ni2 Ni 0.04874(6) 0.30325(8) 0.33561(8) 0.0191(4) Uani 1 1 d . . . . . P2 P 0.15766(13) 0.34474(17) 0.28383(17) 0.0218(8) Uani 1 1 d . . . . . C2 C 0.2175(5) 0.3665(7) 0.2557(7) 0.030(3) Uani 1 1 d . . . . . H2A H 0.213168 0.337287 0.210883 0.045 Uiso 1 1 calc R U . . . H2B H 0.255676 0.354121 0.296676 0.045 Uiso 1 1 calc R U . . . H2C H 0.216608 0.419901 0.244149 0.045 Uiso 1 1 calc R U . . . N15 N 0.1072(3) 0.3962(4) 0.3738(5) 0.023(2) Uani 1 1 d D . . . . C15 C 0.1557(4) 0.4072(5) 0.3540(6) 0.021(3) Uani 1 1 d D U . . . C25 C 0.1888(4) 0.4711(5) 0.3853(6) 0.023(3) Uani 1 1 d D U . . . C35 C 0.1589(4) 0.5034(5) 0.4278(5) 0.024(2) Uani 1 1 d D U . . . C45 C 0.1674(5) 0.5708(5) 0.4690(6) 0.034(3) Uani 1 1 d D U . . . H45 H 0.199385 0.603540 0.473489 0.041 Uiso 1 1 calc R U . . . C55 C 0.1287(4) 0.5880(6) 0.5022(6) 0.038(3) Uani 1 1 d D U . . . H55 H 0.133976 0.633123 0.529985 0.046 Uiso 1 1 calc R U . . . C65 C 0.0808(4) 0.5399(5) 0.4962(6) 0.029(3) Uani 1 1 d D U . . . H65 H 0.055462 0.552290 0.521518 0.035 Uiso 1 1 calc R U . . . C75 C 0.0705(4) 0.4757(5) 0.4542(5) 0.024(3) Uani 1 1 d D U . . . H75 H 0.037283 0.444664 0.448595 0.029 Uiso 1 1 calc R U . . . C85 C 0.1093(4) 0.4565(5) 0.4197(5) 0.021(3) Uani 1 1 d D U . . . C95 C 0.2419(4) 0.5058(7) 0.3759(7) 0.035(3) Uani 1 1 d D U . . . H95A H 0.269597 0.466379 0.375033 0.052 Uiso 1 1 calc R U . . . H95B H 0.262182 0.539723 0.418081 0.052 Uiso 1 1 calc R U . . . H95C H 0.228367 0.533808 0.328544 0.052 Uiso 1 1 calc R U . . . N16 N 0.1229(3) 0.2346(4) 0.3513(5) 0.021(2) Uani 1 1 d D U . . . C16 C 0.1633(4) 0.2518(4) 0.3191(6) 0.022(3) Uani 1 1 d D U . . . C26 C 0.2002(4) 0.1931(5) 0.3176(6) 0.027(3) Uani 1 1 d D U . . . C36 C 0.1848(4) 0.1344(4) 0.3564(6) 0.024(2) Uani 1 1 d D U . . . C46 C 0.2079(4) 0.0619(5) 0.3781(6) 0.029(3) Uani 1 1 d D U . . . H46 H 0.240465 0.044248 0.367074 0.035 Uiso 1 1 calc R U . . . C56 C 0.1827(5) 0.0175(5) 0.4149(6) 0.033(3) Uani 1 1 d D U . . . H56 H 0.197527 -0.031688 0.429142 0.040 Uiso 1 1 calc R U . . . C66 C 0.1347(5) 0.0438(5) 0.4324(6) 0.030(3) Uani 1 1 d D U . . . H66 H 0.118021 0.011867 0.458385 0.036 Uiso 1 1 calc R U . . . C76 C 0.1117(4) 0.1146(5) 0.4125(6) 0.030(3) Uani 1 1 d D U . . . H76 H 0.079322 0.131480 0.424260 0.035 Uiso 1 1 calc R U . . . C86 C 0.1369(4) 0.1613(4) 0.3747(6) 0.023(2) Uani 1 1 d D U . . . C96 C 0.2442(4) 0.1844(6) 0.2809(6) 0.028(3) Uani 1 1 d D U . . . H96A H 0.223347 0.166487 0.229194 0.042 Uiso 1 1 calc R U . . . H96B H 0.275048 0.148241 0.309424 0.042 Uiso 1 1 calc R U . . . H96C H 0.262902 0.232784 0.280261 0.042 Uiso 1 1 calc R U . . . N17 N 0.0401(3) 0.3267(5) 0.2226(4) 0.027(2) Uani 1 1 d D U . . . C17 C 0.0882(3) 0.3539(6) 0.2083(5) 0.022(2) Uani 1 1 d D U . . . C27 C 0.0724(3) 0.3844(6) 0.1369(5) 0.027(3) Uani 1 1 d D U . . . C37 C 0.0097(3) 0.3738(6) 0.1023(4) 0.026(2) Uani 1 1 d D U . . . C47 C -0.0325(4) 0.3875(6) 0.0286(5) 0.037(3) Uani 1 1 d D U . . . H47 H -0.020791 0.411408 -0.007413 0.044 Uiso 1 1 calc R U . . . C57 C -0.0903(4) 0.3659(7) 0.0101(6) 0.041(3) Uani 1 1 d D U . . . H57 H -0.118632 0.373233 -0.039894 0.050 Uiso 1 1 calc R U . . . C67 C -0.1086(4) 0.3327(7) 0.0640(5) 0.042(3) Uani 1 1 d D U . . . H67 H -0.149420 0.319480 0.050079 0.050 Uiso 1 1 calc R U . . . C77 C -0.0685(3) 0.3192(6) 0.1364(5) 0.032(3) Uani 1 1 d D U . . . H77 H -0.081214 0.297158 0.172412 0.039 Uiso 1 1 calc R U . . . C87 C -0.0088(3) 0.3384(6) 0.1557(4) 0.023(2) Uani 1 1 d D U . . . C97 C 0.1102(5) 0.4184(7) 0.0993(6) 0.038(3) Uani 1 1 d D U . . . H97A H 0.136258 0.456719 0.132150 0.057 Uiso 1 1 calc R U . . . H97B H 0.084213 0.441179 0.051473 0.057 Uiso 1 1 calc R U . . . H97C H 0.134611 0.379371 0.089710 0.057 Uiso 1 1 calc R U . . . N18 N -0.0301(3) 0.3713(4) 0.3114(5) 0.025(2) Uani 1 1 d D U . . . C18 C -0.0286(4) 0.4405(5) 0.2836(7) 0.031(3) Uani 1 1 d D U . . . H18 H 0.006125 0.454752 0.275697 0.037 Uiso 1 1 calc R U . . . C28 C -0.0746(4) 0.4912(5) 0.2664(6) 0.030(3) Uani 1 1 d D U . . . H28 H -0.071992 0.538454 0.245462 0.036 Uiso 1 1 calc R U . . . C38 C -0.1244(4) 0.4724(5) 0.2798(7) 0.038(3) Uani 1 1 d D U . . . H38 H -0.156050 0.507083 0.270782 0.046 Uiso 1 1 calc R U . . . C48 C -0.1271(4) 0.4020(5) 0.3067(7) 0.033(3) Uani 1 1 d D U . . . H48 H -0.161110 0.386933 0.315988 0.040 Uiso 1 1 calc R U . . . C58 C -0.0801(4) 0.3534(5) 0.3202(6) 0.025(3) Uani 1 1 d D U . . . H58 H -0.083594 0.304249 0.336637 0.031 Uiso 1 1 calc R U . . . N28 N -0.0066(4) 0.2042(4) 0.3023(4) 0.023(2) Uani 1 1 d D U . . . C68 C -0.0328(4) 0.1688(5) 0.3427(5) 0.026(3) Uani 1 1 d D U . . . H68 H -0.029672 0.190216 0.389098 0.031 Uiso 1 1 calc R U . . . C78 C -0.0639(5) 0.1028(5) 0.3201(5) 0.028(3) Uani 1 1 d D U . . . H78 H -0.080620 0.078613 0.351196 0.034 Uiso 1 1 calc R U . . . C88 C -0.0704(5) 0.0724(6) 0.2518(5) 0.033(3) Uani 1 1 d D U . . . H88 H -0.092612 0.027650 0.234238 0.039 Uiso 1 1 calc R U . . . C98 C -0.0441(5) 0.1082(5) 0.2097(5) 0.028(3) Uani 1 1 d D U . . . H98 H -0.048131 0.088903 0.162019 0.033 Uiso 1 1 calc R U . . . C108 C -0.0116(4) 0.1727(5) 0.2377(5) 0.022(3) Uani 1 1 d D U . . . H108 H 0.008157 0.195636 0.209324 0.027 Uiso 1 1 calc R U . . . N38 N 0.0616(3) 0.2907(4) 0.4562(4) 0.018(2) Uani 1 1 d D U . . . C118 C 0.0218(4) 0.2984(6) 0.4880(5) 0.024(2) Uani 1 1 d D U . . . H118 H -0.019431 0.299225 0.456151 0.029 Uiso 1 1 calc R U . . . C128 C 0.0376(4) 0.3053(6) 0.5647(5) 0.030(3) Uani 1 1 d D U . . . H128 H 0.008023 0.311708 0.584886 0.036 Uiso 1 1 calc R U . . . C138 C 0.0972(4) 0.3025(6) 0.6110(5) 0.032(3) Uani 1 1 d D U . . . H138 H 0.109637 0.307380 0.664023 0.039 Uiso 1 1 calc R U . . . C148 C 0.1383(4) 0.2926(6) 0.5795(5) 0.029(3) Uani 1 1 d D U . . . H148 H 0.179614 0.288952 0.610483 0.035 Uiso 1 1 calc R U . . . C158 C 0.1190(4) 0.2879(6) 0.5020(5) 0.025(3) Uani 1 1 d D U . . . H158 H 0.147994 0.282456 0.480666 0.029 Uiso 1 1 calc R U . . . C19 C 0.2450(10) 0.7456(15) 0.3702(12) 0.077(9) Uani 0.6 1 d D U P . . H19A H 0.228020 0.760405 0.406498 0.115 Uiso 0.6 1 calc R U P . . H19B H 0.277226 0.709359 0.393561 0.115 Uiso 0.6 1 calc R U P . . H19C H 0.261113 0.789810 0.354528 0.115 Uiso 0.6 1 calc R U P . . C29 C 0.1966(8) 0.7104(12) 0.3016(11) 0.061(7) Uani 0.6 1 d D U P . . H29A H 0.163916 0.747189 0.279942 0.073 Uiso 0.6 1 calc R U P . . H29B H 0.179977 0.666998 0.318849 0.073 Uiso 0.6 1 calc R U P . . C39 C 0.2155(10) 0.6840(10) 0.2391(10) 0.067(8) Uani 0.6 1 d D U P . . H39A H 0.181223 0.658006 0.200565 0.080 Uiso 0.6 1 calc R U P . . H39B H 0.247957 0.646801 0.260658 0.080 Uiso 0.6 1 calc R U P . . C49 C 0.2371(10) 0.7445(9) 0.2000(11) 0.064(7) Uani 0.6 1 d D U P . . H49A H 0.270279 0.772215 0.238559 0.076 Uiso 0.6 1 calc R U P . . H49B H 0.204087 0.780320 0.175810 0.076 Uiso 0.6 1 calc R U P . . C59 C 0.2588(10) 0.7149(10) 0.1398(11) 0.057(7) Uani 0.6 1 d D U P . . H59A H 0.290642 0.677459 0.163394 0.068 Uiso 0.6 1 calc R U P . . H59B H 0.225126 0.689262 0.099929 0.068 Uiso 0.6 1 calc R U P . . C69 C 0.2830(10) 0.7764(12) 0.1034(14) 0.076(9) Uani 0.6 1 d D U P . . H69A H 0.295888 0.753855 0.065936 0.114 Uiso 0.6 1 calc R U P . . H69B H 0.251421 0.813066 0.078750 0.114 Uiso 0.6 1 calc R U P . . H69C H 0.317005 0.801250 0.142282 0.114 Uiso 0.6 1 calc R U P . . 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(9) 0.0174(9) 0.0184(9) -0.0002(7) 0.0074(7) -0.0021(7) P1 0.0217(17) 0.0193(18) 0.0151(18) -0.0015(15) 0.0021(14) -0.0003(14) C1 0.024(7) 0.030(7) 0.035(8) -0.005(6) 0.007(6) 0.000(6) N11 0.020(5) 0.017(5) 0.013(6) 0.003(5) -0.001(4) -0.001(4) C11 0.020(6) 0.026(6) 0.013(6) -0.003(5) 0.010(5) -0.004(4) C21 0.021(5) 0.022(6) 0.027(5) -0.009(5) 0.012(4) -0.006(4) C31 0.028(6) 0.023(6) 0.025(5) -0.003(4) 0.013(4) -0.006(4) C41 0.039(6) 0.034(6) 0.030(6) 0.000(5) 0.018(5) -0.011(5) C51 0.055(7) 0.034(7) 0.032(6) 0.014(5) 0.022(5) -0.007(5) C61 0.052(7) 0.023(6) 0.024(7) 0.008(5) 0.014(5) 0.003(5) C71 0.036(6) 0.018(6) 0.023(5) -0.003(5) 0.010(4) -0.001(5) C81 0.030(5) 0.012(5) 0.017(5) -0.005(4) 0.014(4) 0.002(4) C91 0.028(6) 0.030(7) 0.039(7) 0.005(6) 0.005(5) -0.010(5) N12 0.031(5) 0.013(4) 0.019(5) 0.001(4) 0.006(4) -0.002(4) C12 0.020(6) 0.019(5) 0.017(5) 0.001(4) 0.007(4) -0.005(4) C22 0.025(5) 0.018(5) 0.022(5) 0.003(4) 0.012(4) -0.003(4) C32 0.020(5) 0.019(4) 0.026(5) 0.001(4) 0.009(4) -0.001(4) C42 0.034(6) 0.020(5) 0.029(6) 0.013(4) 0.020(5) 0.005(4) C52 0.040(7) 0.020(6) 0.045(6) 0.003(5) 0.028(5) 0.006(5) C62 0.050(7) 0.025(5) 0.030(6) -0.005(5) 0.023(5) -0.002(5) C72 0.031(6) 0.025(5) 0.019(6) -0.004(4) 0.009(5) 0.007(5) C82 0.026(6) 0.018(5) 0.019(5) 0.003(4) 0.010(4) 0.001(4) C92 0.030(6) 0.017(6) 0.029(6) -0.002(5) -0.001(5) -0.004(5) N13 0.024(4) 0.023(5) 0.014(5) 0.002(4) 0.007(4) 0.003(4) C13 0.027(5) 0.012(6) 0.018(5) 0.001(5) 0.005(4) -0.002(4) C23 0.035(5) 0.010(5) 0.012(5) 0.007(4) 0.006(4) -0.002(4) C33 0.035(5) 0.018(6) 0.020(5) 0.004(5) 0.012(4) 0.002(5) C43 0.036(5) 0.024(6) 0.024(6) 0.010(5) 0.014(4) 0.008(5) C53 0.030(5) 0.040(7) 0.035(6) 0.011(5) 0.022(5) 0.010(5) C63 0.031(6) 0.042(7) 0.030(6) 0.009(5) 0.015(5) 0.001(5) C73 0.025(5) 0.028(7) 0.032(7) -0.002(5) 0.009(4) 0.003(5) C83 0.024(4) 0.016(6) 0.018(5) 0.010(4) 0.009(4) 0.008(4) C93 0.033(6) 0.033(7) 0.020(6) -0.005(5) 0.008(5) -0.007(6) N14 0.030(5) 0.028(5) 0.024(6) 0.000(4) 0.013(4) 0.003(4) C14 0.033(6) 0.034(5) 0.024(7) -0.005(5) 0.019(5) 0.004(5) C24 0.042(6) 0.037(7) 0.043(8) -0.006(6) 0.018(5) 0.013(5) C34 0.042(6) 0.050(6) 0.024(7) 0.007(6) 0.018(5) 0.016(5) C44 0.033(6) 0.056(6) 0.032(8) -0.008(6) 0.009(5) 0.001(5) C54 0.030(5) 0.040(6) 0.027(7) 0.000(5) 0.015(5) -0.008(4) N24 0.038(6) 0.022(5) 0.011(4) 0.000(4) 0.010(4) -0.004(4) C64 0.046(7) 0.019(6) 0.013(5) -0.002(4) 0.010(5) -0.008(5) C74 0.053(8) 0.027(6) 0.025(6) -0.010(5) 0.012(6) -0.015(5) C84 0.046(7) 0.026(7) 0.041(6) -0.002(5) 0.020(6) -0.020(6) C94 0.052(8) 0.024(6) 0.030(6) 0.003(5) 0.024(6) -0.005(5) C104 0.037(7) 0.014(5) 0.017(5) 0.000(4) 0.010(5) 0.001(4) N34 0.029(4) 0.019(5) 0.022(5) 0.001(4) 0.008(4) -0.005(4) C114 0.032(5) 0.026(6) 0.023(5) 0.005(5) 0.008(4) 0.003(5) C124 0.049(6) 0.027(6) 0.019(6) -0.005(6) 0.011(5) -0.005(6) C134 0.057(6) 0.040(7) 0.027(5) -0.008(6) 0.023(5) -0.002(6) C144 0.044(6) 0.032(7) 0.028(6) -0.015(6) 0.019(4) -0.009(6) C154 0.028(5) 0.022(6) 0.027(6) 0.004(5) 0.009(5) 0.000(5) Ni2 0.0230(8) 0.0160(9) 0.0188(9) 0.0007(7) 0.0088(7) 0.0008(7) P2 0.0282(18) 0.0174(17) 0.0232(19) -0.0002(15) 0.0136(15) -0.0010(14) C2 0.030(7) 0.039(8) 0.034(8) -0.008(7) 0.025(6) -0.011(6) N15 0.031(6) 0.019(6) 0.018(6) 0.006(5) 0.008(5) -0.001(5) C15 0.025(6) 0.026(6) 0.020(7) 0.004(5) 0.016(5) -0.004(5) C25 0.027(6) 0.020(6) 0.021(6) 0.005(5) 0.007(5) -0.003(4) C35 0.025(5) 0.024(5) 0.016(6) 0.005(4) 0.001(5) 0.002(4) C45 0.039(7) 0.031(6) 0.030(7) -0.002(5) 0.011(5) -0.007(5) C55 0.042(7) 0.034(6) 0.032(7) -0.008(6) 0.008(6) -0.005(5) C65 0.041(6) 0.031(6) 0.023(7) -0.001(5) 0.022(6) 0.006(5) C75 0.030(6) 0.030(6) 0.013(6) 0.003(5) 0.008(5) 0.008(5) C85 0.032(6) 0.021(6) 0.012(6) -0.001(5) 0.010(5) 0.003(4) C95 0.029(6) 0.050(8) 0.029(8) 0.002(7) 0.014(6) -0.009(6) N16 0.020(5) 0.026(4) 0.012(5) 0.001(4) 0.003(4) 0.004(4) C16 0.027(6) 0.021(5) 0.017(7) -0.006(5) 0.008(5) 0.001(4) C26 0.024(6) 0.033(6) 0.025(7) -0.001(5) 0.010(5) 0.004(5) C36 0.028(6) 0.025(5) 0.016(6) -0.004(4) 0.006(5) 0.006(4) C46 0.033(7) 0.030(5) 0.020(7) -0.007(5) 0.006(5) 0.007(5) C56 0.046(7) 0.019(6) 0.029(7) -0.003(5) 0.010(6) 0.011(5) C66 0.044(7) 0.019(5) 0.027(7) -0.008(5) 0.012(6) -0.002(5) C76 0.028(6) 0.028(5) 0.040(8) 0.001(5) 0.021(6) 0.006(5) C86 0.024(6) 0.024(5) 0.017(6) -0.003(5) 0.005(5) 0.003(4) C96 0.025(6) 0.041(8) 0.018(7) 0.007(6) 0.009(5) 0.018(6) N17 0.028(5) 0.022(5) 0.028(5) 0.009(4) 0.008(4) 0.000(4) C17 0.030(5) 0.013(6) 0.023(5) -0.001(5) 0.011(4) 0.000(5) C27 0.042(5) 0.016(6) 0.026(6) 0.004(5) 0.017(4) 0.004(5) C37 0.042(5) 0.011(6) 0.027(5) 0.000(5) 0.014(4) 0.009(5) C47 0.054(6) 0.029(7) 0.025(6) -0.004(6) 0.013(5) 0.007(5) C57 0.049(6) 0.036(7) 0.024(6) -0.002(6) -0.001(5) 0.010(6) C67 0.034(6) 0.037(7) 0.042(6) 0.002(6) 0.003(5) 0.007(6) C77 0.034(5) 0.024(7) 0.033(6) 0.000(5) 0.006(4) 0.001(5) C87 0.029(4) 0.018(6) 0.022(5) -0.001(5) 0.009(4) 0.013(4) C97 0.046(7) 0.038(8) 0.033(8) 0.010(6) 0.019(6) 0.003(6) N18 0.026(5) 0.022(5) 0.025(6) -0.012(4) 0.009(4) -0.005(4) C18 0.024(6) 0.031(6) 0.035(8) -0.001(5) 0.008(5) 0.000(5) C28 0.036(6) 0.034(6) 0.021(7) 0.009(5) 0.013(5) 0.006(5) C38 0.039(6) 0.040(6) 0.041(8) 0.014(6) 0.023(6) 0.016(5) C48 0.027(6) 0.044(6) 0.035(8) 0.012(6) 0.018(6) 0.006(5) C58 0.028(5) 0.026(6) 0.023(7) 0.002(5) 0.010(5) -0.001(4) N28 0.027(5) 0.022(5) 0.020(5) -0.002(4) 0.009(4) 0.002(4) C68 0.023(6) 0.026(6) 0.022(6) -0.001(5) 0.003(5) -0.001(4) C78 0.032(7) 0.029(6) 0.024(6) -0.005(5) 0.010(5) -0.005(5) C88 0.046(7) 0.027(6) 0.027(6) -0.009(5) 0.016(6) -0.011(5) C98 0.039(7) 0.024(6) 0.017(6) -0.009(5) 0.007(5) -0.006(5) C108 0.027(6) 0.017(5) 0.021(6) -0.001(4) 0.008(5) 0.000(4) N38 0.024(4) 0.013(5) 0.016(5) -0.005(4) 0.008(3) -0.001(4) C118 0.025(5) 0.027(6) 0.024(5) 0.000(5) 0.013(4) 0.000(5) C128 0.043(5) 0.027(6) 0.026(5) 0.001(6) 0.019(5) 0.002(6) C138 0.052(6) 0.029(6) 0.015(6) 0.005(6) 0.013(4) -0.002(6) C148 0.039(6) 0.029(7) 0.013(5) 0.006(5) 0.003(4) 0.007(5) C158 0.028(5) 0.029(7) 0.017(5) 0.006(5) 0.009(4) 0.002(5) C19 0.073(15) 0.075(16) 0.097(18) 0.000(13) 0.049(14) 0.016(13) C29 0.055(10) 0.059(11) 0.065(11) 0.005(8) 0.020(8) 0.018(8) C39 0.045(10) 0.081(11) 0.073(11) -0.005(9) 0.021(8) 0.002(8) C49 0.057(10) 0.061(10) 0.064(11) 0.004(8) 0.015(8) 0.032(8) C59 0.048(10) 0.066(11) 0.049(10) 0.005(8) 0.011(8) 0.015(8) C69 0.061(14) 0.063(14) 0.092(17) 0.025(13) 0.017(12) 0.047(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 N12 Ni1 N11 88.7(3) . . ? N12 Ni1 N13 90.4(3) . . ? N11 Ni1 N13 89.8(3) . . ? N12 Ni1 N14 177.0(4) . . ? N11 Ni1 N14 93.2(3) . . ? N13 Ni1 N14 87.3(3) . . ? N12 Ni1 N24 87.0(3) . . ? N11 Ni1 N24 174.8(3) . . ? N13 Ni1 N24 93.2(3) . . ? N14 Ni1 N24 91.2(3) . . ? N12 Ni1 N34 92.6(3) . . ? N11 Ni1 N34 85.8(3) . . ? N13 Ni1 N34 174.6(3) . . ? N14 Ni1 N34 89.8(3) . . ? N24 Ni1 N34 91.4(3) . . ? C11 P1 C13 107.4(5) . . ? C11 P1 C12 108.0(5) . . ? C13 P1 C12 107.7(5) . . ? C11 P1 C1 111.1(5) . . ? C13 P1 C1 110.7(5) . . ? C12 P1 C1 111.7(5) . . ? P1 C1 H1A 109.5 . . ? P1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? P1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C81 N11 C11 103.9(6) . . ? C81 N11 Ni1 134.3(5) . . ? C11 N11 Ni1 121.3(5) . . ? C21 C11 N11 114.1(6) . . ? C21 C11 P1 131.3(6) . . ? N11 C11 P1 114.3(5) . . ? C11 C21 C31 104.2(6) . . ? C11 C21 C91 131.6(7) . . ? C31 C21 C91 124.1(7) . . ? C41 C31 C21 133.2(7) . . ? C41 C31 C81 119.5(6) . . ? C21 C31 C81 107.2(6) . . ? C51 C41 C31 119.7(7) . . ? C51 C41 H41 120.1 . . ? C31 C41 H41 120.1 . . ? C41 C51 C61 120.7(8) . . ? C41 C51 H51 119.7 . . ? C61 C51 H51 119.7 . . ? C71 C61 C51 120.6(8) . . ? C71 C61 H61 119.7 . . ? C51 C61 H61 119.7 . . ? C61 C71 C81 120.0(7) . . ? C61 C71 H71 120.0 . . ? C81 C71 H71 120.0 . . ? N11 C81 C71 130.1(7) . . ? N11 C81 C31 110.5(6) . . ? C71 C81 C31 119.4(6) . . ? C21 C91 H91A 109.5 . . ? C21 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C21 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C12 N12 C82 103.7(6) . . ? C12 N12 Ni1 122.1(5) . . ? C82 N12 Ni1 132.3(5) . . ? N12 C12 C22 114.4(6) . . ? N12 C12 P1 113.1(5) . . ? C22 C12 P1 132.4(6) . . ? C12 C22 C32 104.2(6) . . ? C12 C22 C92 131.5(7) . . ? C32 C22 C92 124.1(7) . . ? C42 C32 C22 133.1(7) . . ? C42 C32 C82 119.7(6) . . ? C22 C32 C82 107.2(6) . . ? C52 C42 C32 119.6(7) . . ? C52 C42 H42 120.2 . . ? C32 C42 H42 120.2 . . ? C42 C52 C62 120.6(7) . . ? C42 C52 H52 119.7 . . ? C62 C52 H52 119.7 . . ? C72 C62 C52 120.7(8) . . ? C72 C62 H62 119.7 . . ? C52 C62 H62 119.7 . . ? C62 C72 C82 119.8(7) . . ? C62 C72 H72 120.1 . . ? C82 C72 H72 120.1 . . ? N12 C82 C72 129.9(7) . . ? N12 C82 C32 110.4(6) . . ? C72 C82 C32 119.6(6) . . ? C22 C92 H92A 109.5 . . ? C22 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C22 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C83 N13 C13 104.1(6) . . ? C83 N13 Ni1 133.8(5) . . ? C13 N13 Ni1 120.9(5) . . ? N13 C13 C23 113.6(6) . . ? N13 C13 P1 114.5(5) . . ? C23 C13 P1 131.9(6) . . ? C13 C23 C33 104.6(6) . . ? C13 C23 C93 130.4(7) . . ? C33 C23 C93 124.7(7) . . ? C43 C33 C23 132.9(7) . . ? C43 C33 C83 120.1(6) . . ? C23 C33 C83 107.0(6) . . ? C53 C43 C33 119.4(7) . . ? C53 C43 H43 120.3 . . ? C33 C43 H43 120.3 . . ? C43 C53 C63 120.4(8) . . ? C43 C53 H53 119.8 . . ? C63 C53 H53 119.8 . . ? C73 C63 C53 121.2(8) . . ? C73 C63 H63 119.4 . . ? C53 C63 H63 119.4 . . ? C63 C73 C83 119.7(8) . . ? C63 C73 H73 120.2 . . ? C83 C73 H73 120.2 . . ? N13 C83 C73 130.2(7) . . ? N13 C83 C33 110.5(6) . . ? C73 C83 C33 119.2(6) . . ? C23 C93 H93A 109.5 . . ? C23 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C23 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C54 N14 C14 116.4(7) . . ? C54 N14 Ni1 126.9(6) . . ? C14 N14 Ni1 116.6(6) . . ? N14 C14 C24 123.6(8) . . ? N14 C14 H14 118.2 . . ? C24 C14 H14 118.2 . . ? C34 C24 C14 118.6(8) . . ? C34 C24 H24 120.7 . . ? C14 C24 H24 120.7 . . ? C44 C34 C24 118.0(8) . . ? C44 C34 H34 121.0 . . ? C24 C34 H34 121.0 . . ? C34 C44 C54 119.9(8) . . ? C34 C44 H44 120.0 . . ? C54 C44 H44 120.0 . . ? N14 C54 C44 123.0(8) . . ? N14 C54 H54 118.5 . . ? C44 C54 H54 118.5 . . ? C104 N24 C64 116.9(7) . . ? C104 N24 Ni1 117.2(6) . . ? C64 N24 Ni1 125.8(6) . . ? N24 C64 C74 123.3(8) . . ? N24 C64 H64 118.3 . . ? C74 C64 H64 118.3 . . ? C84 C74 C64 118.9(8) . . ? C84 C74 H74 120.6 . . ? C64 C74 H74 120.6 . . ? C74 C84 C94 118.4(7) . . ? C74 C84 H84 120.8 . . ? C94 C84 H84 120.8 . . ? C84 C94 C104 119.1(8) . . ? C84 C94 H94 120.5 . . ? C104 C94 H94 120.5 . . ? N24 C104 C94 123.3(8) . . ? N24 C104 H104 118.4 . . ? C94 C104 H104 118.4 . . ? C154 N34 C114 116.3(7) . . ? C154 N34 Ni1 112.8(6) . . ? C114 N34 Ni1 128.5(6) . . ? N34 C114 C124 123.2(8) . . ? N34 C114 H114 118.4 . . ? C124 C114 H114 118.4 . . ? C134 C124 C114 119.5(8) . . ? C134 C124 H124 120.2 . . ? C114 C124 H124 120.2 . . ? C144 C134 C124 117.8(8) . . ? C144 C134 H134 121.1 . . ? C124 C134 H134 121.1 . . ? C134 C144 C154 119.2(8) . . ? C134 C144 H144 120.4 . . ? C154 C144 H144 120.4 . . ? N34 C154 C144 124.0(8) . . ? N34 C154 H154 118.0 . . ? C144 C154 H154 118.0 . . ? N16 Ni2 N15 89.3(3) . . ? N16 Ni2 N17 89.9(3) . . ? N15 Ni2 N17 89.2(3) . . ? N16 Ni2 N18 176.0(3) . . ? N15 Ni2 N18 92.9(3) . . ? N17 Ni2 N18 86.8(3) . . ? N16 Ni2 N28 87.9(3) . . ? N15 Ni2 N28 176.3(3) . . ? N17 Ni2 N28 93.2(3) . . ? N18 Ni2 N28 90.1(3) . . ? N16 Ni2 N38 91.6(3) . . ? N15 Ni2 N38 85.1(3) . . ? N17 Ni2 N38 174.1(3) . . ? N18 Ni2 N38 91.9(3) . . ? N28 Ni2 N38 92.5(3) . . ? C17 P2 C15 105.7(5) . . ? C17 P2 C16 108.1(5) . . ? C15 P2 C16 108.5(5) . . ? C17 P2 C2 111.2(5) . . ? C15 P2 C2 111.4(5) . . ? C16 P2 C2 111.7(5) . . ? P2 C2 H2A 109.5 . . ? P2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? P2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C85 N15 C15 104.1(6) . . ? C85 N15 Ni2 133.3(5) . . ? C15 N15 Ni2 122.7(5) . . ? N15 C15 C25 113.9(6) . . ? N15 C15 P2 113.7(5) . . ? C25 C15 P2 131.7(6) . . ? C15 C25 C35 104.2(6) . . ? C15 C25 C95 131.6(7) . . ? C35 C25 C95 124.1(7) . . ? C45 C35 C25 132.8(7) . . ? C45 C35 C85 119.7(7) . . ? C25 C35 C85 107.5(6) . . ? C55 C45 C35 118.6(8) . . ? C55 C45 H45 120.7 . . ? C35 C45 H45 120.7 . . ? C45 C55 C65 121.4(8) . . ? C45 C55 H55 119.3 . . ? C65 C55 H55 119.3 . . ? C75 C65 C55 120.8(8) . . ? C75 C65 H65 119.6 . . ? C55 C65 H65 119.6 . . ? C65 C75 C85 119.1(7) . . ? C65 C75 H75 120.4 . . ? C85 C75 H75 120.4 . . ? N15 C85 C75 129.4(7) . . ? N15 C85 C35 110.3(6) . . ? C75 C85 C35 120.3(6) . . ? C25 C95 H95A 109.5 . . ? C25 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C25 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C86 N16 C16 103.2(6) . . ? C86 N16 Ni2 133.5(5) . . ? C16 N16 Ni2 121.5(5) . . ? C26 C16 N16 114.7(6) . . ? C26 C16 P2 130.7(6) . . ? N16 C16 P2 114.6(5) . . ? C16 C26 C36 104.0(6) . . ? C16 C26 C96 132.3(7) . . ? C36 C26 C96 123.6(7) . . ? C46 C36 C26 132.8(7) . . ? C46 C36 C86 120.3(6) . . ? C26 C36 C86 106.9(6) . . ? C56 C46 C36 118.9(7) . . ? C56 C46 H46 120.6 . . ? C36 C46 H46 120.6 . . ? C46 C56 C66 120.8(8) . . ? C46 C56 H56 119.6 . . ? C66 C56 H56 119.6 . . ? C76 C66 C56 121.5(8) . . ? C76 C66 H66 119.3 . . ? C56 C66 H66 119.3 . . ? C66 C76 C86 118.8(7) . . ? C66 C76 H76 120.6 . . ? C86 C76 H76 120.6 . . ? N16 C86 C76 129.2(7) . . ? N16 C86 C36 111.1(6) . . ? C76 C86 C36 119.7(6) . . ? C26 C96 H96A 109.5 . . ? C26 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C26 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C87 N17 C17 104.0(6) . . ? C87 N17 Ni2 133.1(5) . . ? C17 N17 Ni2 120.9(5) . . ? C27 C17 N17 114.1(6) . . ? C27 C17 P2 131.5(6) . . ? N17 C17 P2 114.4(5) . . ? C17 C27 C37 104.1(6) . . ? C17 C27 C97 130.9(7) . . ? C37 C27 C97 125.0(7) . . ? C47 C37 C27 132.5(7) . . ? C47 C37 C87 119.6(7) . . ? C27 C37 C87 107.8(6) . . ? C57 C47 C37 119.0(8) . . ? C57 C47 H47 120.5 . . ? C37 C47 H47 120.5 . . ? C47 C57 C67 121.0(8) . . ? C47 C57 H57 119.5 . . ? C67 C57 H57 119.5 . . ? C77 C67 C57 121.2(8) . . ? C77 C67 H67 119.4 . . ? C57 C67 H67 119.4 . . ? C67 C77 C87 118.6(8) . . ? C67 C77 H77 120.7 . . ? C87 C77 H77 120.7 . . ? N17 C87 C77 129.4(7) . . ? N17 C87 C37 110.0(6) . . ? C77 C87 C37 120.6(7) . . ? C27 C97 H97A 109.5 . . ? C27 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C27 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C58 N18 C18 116.0(7) . . ? C58 N18 Ni2 127.9(6) . . ? C18 N18 Ni2 116.1(6) . . ? N18 C18 C28 123.5(8) . . ? N18 C18 H18 118.2 . . ? C28 C18 H18 118.2 . . ? C18 C28 C38 119.0(8) . . ? C18 C28 H28 120.5 . . ? C38 C28 H28 120.5 . . ? C48 C38 C28 118.1(8) . . ? C48 C38 H38 120.9 . . ? C28 C38 H38 120.9 . . ? C38 C48 C58 119.4(8) . . ? C38 C48 H48 120.3 . . ? C58 C48 H48 120.3 . . ? N18 C58 C48 123.8(8) . . ? N18 C58 H58 118.1 . . ? C48 C58 H58 118.1 . . ? C108 N28 C68 117.0(7) . . ? C108 N28 Ni2 116.3(6) . . ? C68 N28 Ni2 126.6(6) . . ? N28 C68 C78 123.2(8) . . ? N28 C68 H68 118.4 . . ? C78 C68 H68 118.4 . . ? C88 C78 C68 119.0(8) . . ? C88 C78 H78 120.5 . . ? C68 C78 H78 120.5 . . ? C98 C88 C78 118.5(7) . . ? C98 C88 H88 120.8 . . ? C78 C88 H88 120.8 . . ? C88 C98 C108 119.0(8) . . ? C88 C98 H98 120.5 . . ? C108 C98 H98 120.5 . . ? N28 C108 C98 123.3(8) . . ? N28 C108 H108 118.4 . . ? C98 C108 H108 118.4 . . ? C158 N38 C118 117.2(7) . . ? C158 N38 Ni2 112.3(5) . . ? C118 N38 Ni2 129.4(6) . . ? N38 C118 C128 123.5(7) . . ? N38 C118 H118 118.2 . . ? C128 C118 H118 118.2 . . ? C138 C128 C118 118.4(7) . . ? C138 C128 H128 120.8 . . ? C118 C128 H128 120.8 . . ? C148 C138 C128 118.8(8) . . ? C148 C138 H138 120.6 . . ? C128 C138 H138 120.6 . . ? C138 C148 C158 119.4(8) . . ? C138 C148 H148 120.3 . . ? C158 C148 H148 120.3 . . ? N38 C158 C148 122.7(7) . . ? N38 C158 H158 118.7 . . ? C148 C158 H158 118.7 . . ? C29 C19 H19A 109.5 . . ? C29 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C29 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19 C29 C39 116.4(11) . . ? C19 C29 H29A 108.2 . . ? C39 C29 H29A 108.2 . . ? C19 C29 H29B 108.2 . . ? C39 C29 H29B 108.2 . . ? H29A C29 H29B 107.3 . . ? C29 C39 C49 116.2(11) . . ? C29 C39 H39A 108.2 . . ? C49 C39 H39A 108.2 . . ? C29 C39 H39B 108.2 . . ? C49 C39 H39B 108.2 . . ? H39A C39 H39B 107.4 . . ? C39 C49 C59 114.4(12) . . ? C39 C49 H49A 108.7 . . ? C59 C49 H49A 108.7 . . ? C39 C49 H49B 108.7 . . ? C59 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? C69 C59 C49 113.7(11) . . ? C69 C59 H59A 108.8 . . ? C49 C59 H59A 108.8 . . ? C69 C59 H59B 108.8 . . ? C49 C59 H59B 108.8 . . ? H59A C59 H59B 107.7 . . ? C59 C69 H69A 109.5 . . ? C59 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C59 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? 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 N12 2.115(7) . ? Ni1 N11 2.127(7) . ? Ni1 N13 2.138(7) . ? Ni1 N14 2.168(8) . ? Ni1 N24 2.178(7) . ? Ni1 N34 2.241(8) . ? P1 C11 1.763(8) . ? P1 C13 1.768(8) . ? P1 C12 1.773(8) . ? P1 C1 1.780(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? N11 C81 1.384(7) . ? N11 C11 1.390(7) . ? C11 C21 1.389(8) . ? C21 C31 1.421(8) . ? C21 C91 1.504(8) . ? C31 C41 1.413(8) . ? C31 C81 1.427(8) . ? C41 C51 1.361(8) . ? C41 H41 0.9500 . ? C51 C61 1.415(8) . ? C51 H51 0.9500 . ? C61 C71 1.373(8) . ? C61 H61 0.9500 . ? C71 C81 1.395(8) . ? C71 H71 0.9500 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? N12 C12 1.386(7) . ? N12 C82 1.389(7) . ? C12 C22 1.388(8) . ? C22 C32 1.418(8) . ? C22 C92 1.495(8) . ? C32 C42 1.410(8) . ? C32 C82 1.426(8) . ? C42 C52 1.361(8) . ? C42 H42 0.9500 . ? C52 C62 1.417(8) . ? C52 H52 0.9500 . ? C62 C72 1.375(8) . ? C62 H62 0.9500 . ? C72 C82 1.393(8) . ? C72 H72 0.9500 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? N13 C83 1.385(7) . ? N13 C13 1.386(7) . ? C13 C23 1.391(8) . ? C23 C33 1.417(8) . ? C23 C93 1.504(8) . ? C33 C43 1.410(8) . ? C33 C83 1.426(8) . ? C43 C53 1.361(8) . ? C43 H43 0.9500 . ? C53 C63 1.414(8) . ? C53 H53 0.9500 . ? C63 C73 1.370(8) . ? C63 H63 0.9500 . ? C73 C83 1.395(8) . ? C73 H73 0.9500 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? N14 C54 1.329(8) . ? N14 C14 1.349(8) . ? C14 C24 1.381(8) . ? C14 H14 0.9500 . ? C24 C34 1.378(8) . ? C24 H24 0.9500 . ? C34 C44 1.369(8) . ? C34 H34 0.9500 . ? C44 C54 1.381(8) . ? C44 H44 0.9500 . ? C54 H54 0.9500 . ? N24 C104 1.331(7) . ? N24 C64 1.343(7) . ? C64 C74 1.378(8) . ? C64 H64 0.9500 . ? C74 C84 1.376(8) . ? C74 H74 0.9500 . ? C84 C94 1.377(8) . ? C84 H84 0.9500 . ? C94 C104 1.380(8) . ? C94 H94 0.9500 . ? C104 H104 0.9500 . ? N34 C154 1.332(8) . ? N34 C114 1.339(7) . ? C114 C124 1.380(8) . ? C114 H114 0.9500 . ? C124 C134 1.378(8) . ? C124 H124 0.9500 . ? C134 C144 1.371(8) . ? C134 H134 0.9500 . ? C144 C154 1.381(8) . ? C144 H144 0.9500 . ? C154 H154 0.9500 . ? Ni2 N16 2.102(7) . ? Ni2 N15 2.123(7) . ? Ni2 N17 2.148(7) . ? Ni2 N18 2.163(8) . ? Ni2 N28 2.164(7) . ? Ni2 N38 2.234(7) . ? P2 C17 1.755(8) . ? P2 C15 1.770(8) . ? P2 C16 1.781(8) . ? P2 C2 1.784(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? N15 C85 1.384(7) . ? N15 C15 1.389(7) . ? C15 C25 1.393(8) . ? C25 C35 1.416(8) . ? C25 C95 1.505(8) . ? C35 C45 1.415(8) . ? C35 C85 1.426(8) . ? C45 C55 1.365(8) . ? C45 H45 0.9500 . ? C55 C65 1.415(8) . ? C55 H55 0.9500 . ? C65 C75 1.372(8) . ? C65 H65 0.9500 . ? C75 C85 1.394(8) . ? C75 H75 0.9500 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? N16 C86 1.385(7) . ? N16 C16 1.389(7) . ? C16 C26 1.389(8) . ? C26 C36 1.422(8) . ? C26 C96 1.503(8) . ? C36 C46 1.411(8) . ? C36 C86 1.426(8) . ? C46 C56 1.360(8) . ? C46 H46 0.9500 . ? C56 C66 1.415(8) . ? C56 H56 0.9500 . ? C66 C76 1.378(8) . ? C66 H66 0.9500 . ? C76 C86 1.397(8) . ? C76 H76 0.9500 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? N17 C87 1.388(7) . ? N17 C17 1.390(7) . ? C17 C27 1.389(8) . ? C27 C37 1.417(8) . ? C27 C97 1.504(8) . ? C37 C47 1.412(8) . ? C37 C87 1.423(8) . ? C47 C57 1.363(8) . ? C47 H47 0.9500 . ? C57 C67 1.414(8) . ? C57 H57 0.9500 . ? C67 C77 1.376(8) . ? C67 H67 0.9500 . ? C77 C87 1.393(8) . ? C77 H77 0.9500 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? N18 C58 1.330(7) . ? N18 C18 1.354(8) . ? C18 C28 1.375(8) . ? C18 H18 0.9500 . ? C28 C38 1.377(8) . ? C28 H28 0.9500 . ? C38 C48 1.373(8) . ? C38 H38 0.9500 . ? C48 C58 1.377(8) . ? C48 H48 0.9500 . ? C58 H58 0.9500 . ? N28 C108 1.331(7) . ? N28 C68 1.342(8) . ? C68 C78 1.378(8) . ? C68 H68 0.9500 . ? C78 C88 1.376(8) . ? C78 H78 0.9500 . ? C88 C98 1.375(8) . ? C88 H88 0.9500 . ? C98 C108 1.384(8) . ? C98 H98 0.9500 . ? C108 H108 0.9500 . ? N38 C158 1.330(7) . ? N38 C118 1.340(7) . ? C118 C128 1.381(8) . ? C118 H118 0.9500 . ? C128 C138 1.373(8) . ? C128 H128 0.9500 . ? C138 C148 1.371(8) . ? C138 H138 0.9500 . ? C148 C158 1.383(8) . ? C148 H148 0.9500 . ? C158 H158 0.9500 . ? C19 C29 1.522(10) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C29 C39 1.525(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C39 C49 1.526(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C49 C59 1.544(10) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C59 C69 1.540(10) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? 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 C81 N11 C11 C21 -0.2(12) . . . . ? Ni1 N11 C11 C21 -173.6(7) . . . . ? C81 N11 C11 P1 -174.5(7) . . . . ? Ni1 N11 C11 P1 12.1(11) . . . . ? C13 P1 C11 C21 -122.1(11) . . . . ? C12 P1 C11 C21 122.0(11) . . . . ? C1 P1 C11 C21 -0.8(13) . . . . ? C13 P1 C11 N11 51.0(9) . . . . ? C12 P1 C11 N11 -64.9(9) . . . . ? C1 P1 C11 N11 172.3(8) . . . . ? N11 C11 C21 C31 0.4(13) . . . . ? P1 C11 C21 C31 173.5(9) . . . . ? N11 C11 C21 C91 179.4(11) . . . . ? P1 C11 C21 C91 -8(2) . . . . ? C11 C21 C31 C41 -177.2(13) . . . . ? C91 C21 C31 C41 4(2) . . . . ? C11 C21 C31 C81 -0.4(12) . . . . ? C91 C21 C31 C81 -179.5(11) . . . . ? C21 C31 C41 C51 176.7(13) . . . . ? C81 C31 C41 C51 0.2(18) . . . . ? C31 C41 C51 C61 0.7(19) . . . . ? C41 C51 C61 C71 -0.7(19) . . . . ? C51 C61 C71 C81 -0.4(18) . . . . ? C11 N11 C81 C71 178.7(11) . . . . ? Ni1 N11 C81 C71 -9.2(18) . . . . ? C11 N11 C81 C31 -0.1(12) . . . . ? Ni1 N11 C81 C31 172.0(8) . . . . ? C61 C71 C81 N11 -177.3(11) . . . . ? C61 C71 C81 C31 1.4(16) . . . . ? C41 C31 C81 N11 177.6(10) . . . . ? C21 C31 C81 N11 0.3(13) . . . . ? C41 C31 C81 C71 -1.3(17) . . . . ? C21 C31 C81 C71 -178.6(10) . . . . ? C82 N12 C12 C22 -0.7(13) . . . . ? Ni1 N12 C12 C22 -166.9(7) . . . . ? C82 N12 C12 P1 -177.4(7) . . . . ? Ni1 N12 C12 P1 16.5(11) . . . . ? C11 P1 C12 N12 48.1(9) . . . . ? C13 P1 C12 N12 -67.6(9) . . . . ? C1 P1 C12 N12 170.6(8) . . . . ? C11 P1 C12 C22 -127.7(11) . . . . ? C13 P1 C12 C22 116.5(11) . . . . ? C1 P1 C12 C22 -5.2(13) . . . . ? N12 C12 C22 C32 0.5(13) . . . . ? P1 C12 C22 C32 176.3(9) . . . . ? N12 C12 C22 C92 175.5(11) . . . . ? P1 C12 C22 C92 -9(2) . . . . ? C12 C22 C32 C42 -178.7(12) . . . . ? C92 C22 C32 C42 6(2) . . . . ? C12 C22 C32 C82 -0.1(12) . . . . ? C92 C22 C32 C82 -175.6(10) . . . . ? C22 C32 C42 C52 179.0(12) . . . . ? C82 C32 C42 C52 0.5(17) . . . . ? C32 C42 C52 C62 -0.9(17) . . . . ? C42 C52 C62 C72 -0.3(18) . . . . ? C52 C62 C72 C82 1.9(18) . . . . ? C12 N12 C82 C72 177.7(12) . . . . ? Ni1 N12 C82 C72 -18.2(18) . . . . ? C12 N12 C82 C32 0.7(12) . . . . ? Ni1 N12 C82 C32 164.8(8) . . . . ? C62 C72 C82 N12 -179.0(11) . . . . ? C62 C72 C82 C32 -2.2(17) . . . . ? C42 C32 C82 N12 178.5(10) . . . . ? C22 C32 C82 N12 -0.4(13) . . . . ? C42 C32 C82 C72 1.1(17) . . . . ? C22 C32 C82 C72 -177.8(10) . . . . ? C83 N13 C13 C23 3.1(12) . . . . ? Ni1 N13 C13 C23 -165.9(7) . . . . ? C83 N13 C13 P1 -177.8(7) . . . . ? Ni1 N13 C13 P1 13.2(11) . . . . ? C11 P1 C13 N13 -66.2(9) . . . . ? C12 P1 C13 N13 49.9(9) . . . . ? C1 P1 C13 N13 172.3(8) . . . . ? C11 P1 C13 C23 112.7(11) . . . . ? C12 P1 C13 C23 -131.2(10) . . . . ? C1 P1 C13 C23 -8.8(13) . . . . ? N13 C13 C23 C33 -4.0(12) . . . . ? P1 C13 C23 C33 177.2(9) . . . . ? N13 C13 C23 C93 -178.5(10) . . . . ? P1 C13 C23 C93 2.6(19) . . . . ? C13 C23 C33 C43 -173.3(12) . . . . ? C93 C23 C33 C43 1.6(19) . . . . ? C13 C23 C33 C83 3.1(11) . . . . ? C93 C23 C33 C83 178.0(10) . . . . ? C23 C33 C43 C53 176.8(11) . . . . ? C83 C33 C43 C53 0.7(16) . . . . ? C33 C43 C53 C63 -0.1(17) . . . . ? C43 C53 C63 C73 0.1(18) . . . . ? C53 C63 C73 C83 -0.6(18) . . . . ? C13 N13 C83 C73 175.4(11) . . . . ? Ni1 N13 C83 C73 -17.8(18) . . . . ? C13 N13 C83 C33 -0.9(12) . . . . ? Ni1 N13 C83 C33 165.9(7) . . . . ? C63 C73 C83 N13 -174.9(11) . . . . ? C63 C73 C83 C33 1.1(16) . . . . ? C43 C33 C83 N13 175.6(10) . . . . ? C23 C33 C83 N13 -1.4(12) . . . . ? C43 C33 C83 C73 -1.2(16) . . . . ? C23 C33 C83 C73 -178.2(10) . . . . ? C54 N14 C14 C24 5.8(17) . . . . ? Ni1 N14 C14 C24 -174.9(9) . . . . ? N14 C14 C24 C34 -1.1(19) . . . . ? C14 C24 C34 C44 -4.0(19) . . . . ? C24 C34 C44 C54 4.3(19) . . . . ? C14 N14 C54 C44 -5.4(17) . . . . ? Ni1 N14 C54 C44 175.3(9) . . . . ? C34 C44 C54 N14 1(2) . . . . ? C104 N24 C64 C74 -0.2(17) . . . . ? Ni1 N24 C64 C74 -176.8(9) . . . . ? N24 C64 C74 C84 -2.6(19) . . . . ? C64 C74 C84 C94 3.4(19) . . . . ? C74 C84 C94 C104 -1.5(19) . . . . ? C64 N24 C104 C94 2.2(16) . . . . ? Ni1 N24 C104 C94 179.1(9) . . . . ? C84 C94 C104 N24 -1.4(18) . . . . ? C154 N34 C114 C124 -2.8(16) . . . . ? Ni1 N34 C114 C124 -163.8(9) . . . . ? N34 C114 C124 C134 2.0(18) . . . . ? C114 C124 C134 C144 0.2(18) . . . . ? C124 C134 C144 C154 -1.3(17) . . . . ? C114 N34 C154 C144 1.6(16) . . . . ? Ni1 N34 C154 C144 165.6(9) . . . . ? C134 C144 C154 N34 0.4(18) . . . . ? C85 N15 C15 C25 0.4(12) . . . . ? Ni2 N15 C15 C25 -179.5(7) . . . . ? C85 N15 C15 P2 -171.4(7) . . . . ? Ni2 N15 C15 P2 8.7(11) . . . . ? C17 P2 C15 N15 54.5(9) . . . . ? C16 P2 C15 N15 -61.3(9) . . . . ? C2 P2 C15 N15 175.4(8) . . . . ? C17 P2 C15 C25 -115.4(11) . . . . ? C16 P2 C15 C25 128.8(11) . . . . ? C2 P2 C15 C25 5.5(13) . . . . ? N15 C15 C25 C35 -0.4(13) . . . . ? P2 C15 C25 C35 169.5(9) . . . . ? N15 C15 C25 C95 -176.5(11) . . . . ? P2 C15 C25 C95 -7(2) . . . . ? C15 C25 C35 C45 -175.4(12) . . . . ? C95 C25 C35 C45 1(2) . . . . ? C15 C25 C35 C85 0.3(12) . . . . ? C95 C25 C35 C85 176.7(10) . . . . ? C25 C35 C45 C55 177.4(12) . . . . ? C85 C35 C45 C55 2.1(17) . . . . ? C35 C45 C55 C65 0.0(18) . . . . ? C45 C55 C65 C75 -2.5(18) . . . . ? C55 C65 C75 C85 2.6(17) . . . . ? C15 N15 C85 C75 177.9(11) . . . . ? Ni2 N15 C85 C75 -2.2(18) . . . . ? C15 N15 C85 C35 -0.2(12) . . . . ? Ni2 N15 C85 C35 179.7(7) . . . . ? C65 C75 C85 N15 -178.3(11) . . . . ? C65 C75 C85 C35 -0.4(16) . . . . ? C45 C35 C85 N15 176.3(10) . . . . ? C25 C35 C85 N15 0.0(13) . . . . ? C45 C35 C85 C75 -2.0(16) . . . . ? C25 C35 C85 C75 -178.3(10) . . . . ? C86 N16 C16 C26 2.8(13) . . . . ? Ni2 N16 C16 C26 -164.0(8) . . . . ? C86 N16 C16 P2 -179.2(8) . . . . ? Ni2 N16 C16 P2 14.1(11) . . . . ? C17 P2 C16 C26 112.1(12) . . . . ? C15 P2 C16 C26 -133.7(11) . . . . ? C2 P2 C16 C26 -10.6(13) . . . . ? C17 P2 C16 N16 -65.6(9) . . . . ? C15 P2 C16 N16 48.6(10) . . . . ? C2 P2 C16 N16 171.8(8) . . . . ? N16 C16 C26 C36 -3.9(14) . . . . ? P2 C16 C26 C36 178.5(9) . . . . ? N16 C16 C26 C96 171.8(11) . . . . ? P2 C16 C26 C96 -6(2) . . . . ? C16 C26 C36 C46 -175.8(12) . . . . ? C96 C26 C36 C46 8(2) . . . . ? C16 C26 C36 C86 3.3(12) . . . . ? C96 C26 C36 C86 -172.9(10) . . . . ? C26 C36 C46 C56 -179.4(12) . . . . ? C86 C36 C46 C56 1.6(17) . . . . ? C36 C46 C56 C66 -0.9(18) . . . . ? C46 C56 C66 C76 0.3(18) . . . . ? C56 C66 C76 C86 -0.4(18) . . . . ? C16 N16 C86 C76 178.5(12) . . . . ? Ni2 N16 C86 C76 -17.1(18) . . . . ? C16 N16 C86 C36 -0.5(12) . . . . ? Ni2 N16 C86 C36 163.9(8) . . . . ? C66 C76 C86 N16 -177.8(11) . . . . ? C66 C76 C86 C36 1.1(17) . . . . ? C46 C36 C86 N16 177.4(10) . . . . ? C26 C36 C86 N16 -1.8(13) . . . . ? C46 C36 C86 C76 -1.7(16) . . . . ? C26 C36 C86 C76 179.1(10) . . . . ? C87 N17 C17 C27 1.9(13) . . . . ? Ni2 N17 C17 C27 -164.1(8) . . . . ? C87 N17 C17 P2 -178.8(7) . . . . ? Ni2 N17 C17 P2 15.1(11) . . . . ? C15 P2 C17 C27 110.5(11) . . . . ? C16 P2 C17 C27 -133.5(11) . . . . ? C2 P2 C17 C27 -10.5(13) . . . . ? C15 P2 C17 N17 -68.6(9) . . . . ? C16 P2 C17 N17 47.4(9) . . . . ? C2 P2 C17 N17 170.3(8) . . . . ? N17 C17 C27 C37 -1.8(13) . . . . ? P2 C17 C27 C37 179.0(9) . . . . ? N17 C17 C27 C97 -179.1(11) . . . . ? P2 C17 C27 C97 2(2) . . . . ? C17 C27 C37 C47 -175.0(12) . . . . ? C97 C27 C37 C47 3(2) . . . . ? C17 C27 C37 C87 0.9(12) . . . . ? C97 C27 C37 C87 178.5(11) . . . . ? C27 C37 C47 C57 175.0(12) . . . . ? C87 C37 C47 C57 -0.5(17) . . . . ? C37 C47 C57 C67 2.3(19) . . . . ? C47 C57 C67 C77 -1.9(19) . . . . ? C57 C67 C77 C87 -0.4(18) . . . . ? C17 N17 C87 C77 177.1(11) . . . . ? Ni2 N17 C87 C77 -19.3(18) . . . . ? C17 N17 C87 C37 -1.2(12) . . . . ? Ni2 N17 C87 C37 162.4(8) . . . . ? C67 C77 C87 N17 -176.0(11) . . . . ? C67 C77 C87 C37 2.2(17) . . . . ? C47 C37 C87 N17 176.7(10) . . . . ? C27 C37 C87 N17 0.2(12) . . . . ? C47 C37 C87 C77 -1.8(16) . . . . ? C27 C37 C87 C77 -178.3(10) . . . . ? C58 N18 C18 C28 1.3(17) . . . . ? Ni2 N18 C18 C28 -179.0(9) . . . . ? N18 C18 C28 C38 2.1(19) . . . . ? C18 C28 C38 C48 -3.1(18) . . . . ? C28 C38 C48 C58 0.8(19) . . . . ? C18 N18 C58 C48 -3.7(17) . . . . ? Ni2 N18 C58 C48 176.6(9) . . . . ? C38 C48 C58 N18 2.7(19) . . . . ? C108 N28 C68 C78 -0.2(16) . . . . ? Ni2 N28 C68 C78 -175.1(8) . . . . ? N28 C68 C78 C88 -2.1(17) . . . . ? C68 C78 C88 C98 1.8(18) . . . . ? C78 C88 C98 C108 0.7(18) . . . . ? C68 N28 C108 C98 2.8(16) . . . . ? Ni2 N28 C108 C98 178.4(8) . . . . ? C88 C98 C108 N28 -3.2(17) . . . . ? C158 N38 C118 C128 1.6(16) . . . . ? Ni2 N38 C118 C128 -165.3(8) . . . . ? N38 C118 C128 C138 -1.4(17) . . . . ? C118 C128 C138 C148 -0.5(17) . . . . ? C128 C138 C148 C158 1.9(17) . . . . ? C118 N38 C158 C148 0.0(15) . . . . ? Ni2 N38 C158 C148 169.1(9) . . . . ? C138 C148 C158 N38 -1.8(17) . . . . ? C19 C29 C39 C49 -63(3) . . . . ? C29 C39 C49 C59 177.1(19) . . . . ? C39 C49 C59 C69 -177(2) . . . . ?