# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hiroki Oshio' _publ_contact_author_email OSHIO@CHEM.TSUKUBA.AC.JP _publ_section_title ; Ferromagnetically Coupled Chiral Cyanide-bridged {Ni6Fe4} Cages ; loop_ _publ_author_name 'Hiroki Oshio' 'Leroy Cronin' 'Jennifer S. Mathieson' 'Graham Newton' 'Masayuki Nihei' 'Takuya Shiga' ; T.Tetsuka ; data_1R _database_code_depnum_ccdc_archive 'CCDC 756354' #TrackingRef 'Combined_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H56 Cl2 N8 Ni2, C28 H28 Cl2 N4 Ni, 3(C H4 O), 2(Cl)' _chemical_formula_sum 'C87 H96 Cl6 N12 Ni3 O3' _chemical_formula_weight 1746.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.3057(17) _cell_length_b 14.806(2) _cell_length_c 15.877(3) _cell_angle_alpha 107.701(2) _cell_angle_beta 107.261(2) _cell_angle_gamma 99.251(2) _cell_volume 2118.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 968 _cell_measurement_theta_min 3.7925 _cell_measurement_theta_max 23.233 _exptl_crystal_description Blocks _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7135 _exptl_absorpt_correction_T_max 0.7605 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8735 _diffrn_reflns_av_R_equivalents 0.0143 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 23.27 _reflns_number_total 7157 _reflns_number_gt 6978 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.010(8) _chemical_absolute_configuration rmad _refine_ls_number_reflns 7157 _refine_ls_number_parameters 1010 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0709 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.77863(4) 0.54735(3) 0.81967(3) 0.02588(12) Uani 1 1 d . . . Ni2 Ni 0.56264(4) 0.33639(3) 0.83123(3) 0.02594(12) Uani 1 1 d . . . Ni3 Ni 0.87854(5) 0.86395(3) 0.51902(3) 0.02871(13) Uani 1 1 d . . . C1 C 0.6010(5) 0.4393(3) 0.6034(3) 0.0420(11) Uani 1 1 d . . . H1 H 0.6098 0.3805 0.6112 0.050 Uiso 1 1 calc R . . C2 C 0.5296(6) 0.4357(4) 0.5137(3) 0.0566(15) Uani 1 1 d . . . H2 H 0.4921 0.3759 0.4622 0.068 Uiso 1 1 calc R . . C3 C 0.5147(7) 0.5219(4) 0.5013(3) 0.0706(19) Uani 1 1 d . . . H3 H 0.4648 0.5215 0.4418 0.085 Uiso 1 1 calc R . . C4 C 0.5751(5) 0.6082(4) 0.5788(3) 0.0518(13) Uani 1 1 d . . . H4 H 0.5682 0.6676 0.5718 0.062 Uiso 1 1 calc R . . C5 C 0.6455(4) 0.6078(3) 0.6665(3) 0.0333(10) Uani 1 1 d . . . C6 C 0.7068(4) 0.6974(3) 0.7524(3) 0.0306(9) Uani 1 1 d . . . H6 H 0.7005 0.7582 0.7490 0.037 Uiso 1 1 calc R . . C7 C 0.8210(4) 0.7795(3) 0.9207(3) 0.0313(9) Uani 1 1 d . . . H7 H 0.7903 0.7595 0.9667 0.038 Uiso 1 1 calc R . . C8 C 0.7628(5) 0.8666(3) 0.9121(3) 0.0421(11) Uani 1 1 d . . . H8A H 0.7923 0.8894 0.8685 0.063 Uiso 1 1 calc R . . H8B H 0.7982 0.9192 0.9734 0.063 Uiso 1 1 calc R . . H8C H 0.6614 0.8459 0.8892 0.063 Uiso 1 1 calc R . . C9 C 0.9812(4) 0.8133(3) 0.9622(3) 0.0300(9) Uani 1 1 d . . . C10 C 1.0513(5) 0.8425(3) 1.0579(3) 0.0413(11) Uani 1 1 d . . . H10 H 1.0000 0.8378 1.0965 0.050 Uiso 1 1 calc R . . C11 C 1.1948(5) 0.8786(4) 1.0982(4) 0.0553(13) Uani 1 1 d . . . H11 H 1.2406 0.8988 1.1636 0.066 Uiso 1 1 calc R . . C12 C 1.2714(5) 0.8851(4) 1.0417(4) 0.0568(14) Uani 1 1 d . . . H12 H 1.3695 0.9077 1.0686 0.068 Uiso 1 1 calc R . . C13 C 1.2030(5) 0.8581(4) 0.9454(3) 0.0481(12) Uani 1 1 d . . . H13 H 1.2548 0.8641 0.9074 0.058 Uiso 1 1 calc R . . C14 C 1.0581(5) 0.8222(3) 0.9052(3) 0.0387(10) Uani 1 1 d . . . H14 H 1.0119 0.8039 0.8401 0.046 Uiso 1 1 calc R . . C15 C 0.8929(5) 0.6011(3) 1.0378(3) 0.0367(10) Uani 1 1 d . . . H15 H 0.7999 0.5927 1.0347 0.044 Uiso 1 1 calc R . . C16 C 0.9994(6) 0.6255(3) 1.1250(3) 0.0490(12) Uani 1 1 d . . . H16 H 0.9780 0.6351 1.1794 0.059 Uiso 1 1 calc R . . C17 C 1.1350(6) 0.6353(4) 1.1306(3) 0.0566(14) Uani 1 1 d . . . H17 H 1.2069 0.6481 1.1880 0.068 Uiso 1 1 calc R . . C18 C 1.1642(5) 0.6260(3) 1.0493(3) 0.0479(12) Uani 1 1 d . . . H18 H 1.2569 0.6346 1.0518 0.057 Uiso 1 1 calc R . . C19 C 1.0552(5) 0.6039(3) 0.9649(3) 0.0343(10) Uani 1 1 d . . . C20 C 1.0773(4) 0.5976(3) 0.8767(3) 0.0342(10) Uani 1 1 d . . . H20 H 1.1687 0.6130 0.8772 0.041 Uiso 1 1 calc R . . C21 C 0.9910(5) 0.5650(3) 0.7086(3) 0.0380(10) Uani 1 1 d . . . H21 H 0.9153 0.5873 0.6738 0.046 Uiso 1 1 calc R . . C22 C 0.9664(6) 0.4572(3) 0.6502(4) 0.0590(15) Uani 1 1 d . . . H22A H 1.0442 0.4346 0.6784 0.088 Uiso 1 1 calc R . . H22B H 0.9587 0.4500 0.5866 0.088 Uiso 1 1 calc R . . H22C H 0.8805 0.4189 0.6486 0.088 Uiso 1 1 calc R . . C23 C 1.1298(5) 0.6300(3) 0.7201(3) 0.0339(10) Uani 1 1 d . . . C24 C 1.1301(5) 0.7158(3) 0.7020(3) 0.0385(10) Uani 1 1 d . . . H24 H 1.0460 0.7327 0.6834 0.046 Uiso 1 1 calc R . . C25 C 1.2549(5) 0.7764(4) 0.7115(4) 0.0516(13) Uani 1 1 d . . . H25 H 1.2542 0.8334 0.6983 0.062 Uiso 1 1 calc R . . C26 C 1.3770(5) 0.7531(4) 0.7398(4) 0.0646(17) Uani 1 1 d . . . H26 H 1.4605 0.7944 0.7464 0.078 Uiso 1 1 calc R . . C27 C 1.3799(5) 0.6692(4) 0.7589(4) 0.0656(17) Uani 1 1 d . . . H27 H 1.4651 0.6539 0.7789 0.079 Uiso 1 1 calc R . . C28 C 1.2558(5) 0.6074(4) 0.7483(4) 0.0495(12) Uani 1 1 d . . . H28 H 1.2575 0.5499 0.7603 0.059 Uiso 1 1 calc R . . C29 C 0.3409(5) 0.3559(3) 0.6600(3) 0.0342(10) Uani 1 1 d . . . H29 H 0.3725 0.4237 0.6935 0.041 Uiso 1 1 calc R . . C30 C 0.2338(5) 0.3200(3) 0.5726(3) 0.0397(10) Uani 1 1 d . . . H30 H 0.1942 0.3630 0.5479 0.048 Uiso 1 1 calc R . . C31 C 0.1855(5) 0.2206(4) 0.5219(3) 0.0446(12) Uani 1 1 d . . . H31 H 0.1144 0.1948 0.4619 0.053 Uiso 1 1 calc R . . C32 C 0.2450(5) 0.1598(3) 0.5622(3) 0.0441(11) Uani 1 1 d . . . H32 H 0.2124 0.0918 0.5304 0.053 Uiso 1 1 calc R . . C33 C 0.3542(4) 0.2006(3) 0.6506(3) 0.0324(9) Uani 1 1 d . . . C34 C 0.4283(4) 0.1410(3) 0.6942(3) 0.0328(9) Uani 1 1 d . . . H34 H 0.4007 0.0728 0.6634 0.039 Uiso 1 1 calc R . . C35 C 0.6166(5) 0.1225(3) 0.8133(3) 0.0345(9) Uani 1 1 d . . . H35 H 0.7156 0.1566 0.8296 0.041 Uiso 1 1 calc R . . C36 C 0.5892(6) 0.0180(3) 0.7442(3) 0.0483(12) Uani 1 1 d . . . H36A H 0.4956 -0.0198 0.7309 0.073 Uiso 1 1 calc R . . H36B H 0.6571 -0.0122 0.7719 0.073 Uiso 1 1 calc R . . H36C H 0.5975 0.0201 0.6861 0.073 Uiso 1 1 calc R . . C37 C 0.6018(5) 0.1189(3) 0.9047(3) 0.0347(10) Uani 1 1 d . . . C38 C 0.7200(6) 0.1318(4) 0.9803(3) 0.0519(12) Uani 1 1 d . . . H38 H 0.8088 0.1466 0.9765 0.062 Uiso 1 1 calc R . . C39 C 0.7086(7) 0.1231(4) 1.0622(4) 0.0643(15) Uani 1 1 d . . . H39 H 0.7891 0.1329 1.1137 0.077 Uiso 1 1 calc R . . C40 C 0.5771(7) 0.1000(4) 1.0667(4) 0.0686(17) Uani 1 1 d . . . H40 H 0.5688 0.0927 1.1212 0.082 Uiso 1 1 calc R . . C41 C 0.4585(7) 0.0876(4) 0.9926(4) 0.0616(15) Uani 1 1 d . . . H41 H 0.3701 0.0737 0.9971 0.074 Uiso 1 1 calc R . . C42 C 0.4708(5) 0.0960(3) 0.9102(3) 0.0449(11) Uani 1 1 d . . . H42 H 0.3901 0.0860 0.8587 0.054 Uiso 1 1 calc R . . C43 C 0.8426(4) 0.3694(3) 0.9948(3) 0.0321(9) Uani 1 1 d . . . H43 H 0.8865 0.3637 0.9508 0.039 Uiso 1 1 calc R . . C44 C 0.9239(5) 0.3869(4) 1.0876(3) 0.0488(12) Uani 1 1 d . . . H44 H 1.0204 0.3932 1.1057 0.059 Uiso 1 1 calc R . . C45 C 0.8592(6) 0.3949(4) 1.1526(3) 0.0627(15) Uani 1 1 d . . . H45 H 0.9111 0.4061 1.2155 0.075 Uiso 1 1 calc R . . C46 C 0.7163(6) 0.3861(4) 1.1234(3) 0.0569(14) Uani 1 1 d . . . H46 H 0.6705 0.3932 1.1665 0.068 Uiso 1 1 calc R . . C47 C 0.6427(5) 0.3665(3) 1.0291(3) 0.0363(10) Uani 1 1 d . . . C48 C 0.4894(5) 0.3498(3) 0.9922(3) 0.0353(10) Uani 1 1 d . . . H48 H 0.4401 0.3542 1.0331 0.042 Uiso 1 1 calc R . . C49 C 0.2681(5) 0.3129(3) 0.8668(3) 0.0380(10) Uani 1 1 d . . . H49 H 0.2362 0.2862 0.7973 0.046 Uiso 1 1 calc R . . C50 C 0.2333(5) 0.4101(4) 0.8953(4) 0.0571(14) Uani 1 1 d . . . H50A H 0.2613 0.4379 0.9631 0.086 Uiso 1 1 calc R . . H50B H 0.1334 0.3998 0.8660 0.086 Uiso 1 1 calc R . . H50C H 0.2831 0.4545 0.8748 0.086 Uiso 1 1 calc R . . C51 C 0.1920(4) 0.2362(3) 0.8952(3) 0.0341(10) Uani 1 1 d . . . C52 C 0.1423(5) 0.1388(3) 0.8340(3) 0.0486(12) Uani 1 1 d . . . H52 H 0.1497 0.1212 0.7745 0.058 Uiso 1 1 calc R . . C53 C 0.0800(5) 0.0656(4) 0.8613(4) 0.0580(14) Uani 1 1 d . . . H53 H 0.0473 -0.0002 0.8203 0.070 Uiso 1 1 calc R . . C54 C 0.0683(6) 0.0926(4) 0.9485(5) 0.0629(15) Uani 1 1 d . . . H54 H 0.0274 0.0448 0.9668 0.075 Uiso 1 1 calc R . . C55 C 0.1157(5) 0.1885(4) 1.0087(4) 0.0526(13) Uani 1 1 d . . . H55 H 0.1080 0.2058 1.0681 0.063 Uiso 1 1 calc R . . C56 C 0.1759(5) 0.2614(3) 0.9821(3) 0.0432(11) Uani 1 1 d . . . H56 H 0.2053 0.3271 1.0229 0.052 Uiso 1 1 calc R . . C57 C 0.9983(6) 0.6869(3) 0.4727(3) 0.0443(11) Uani 1 1 d . . . H57 H 1.0873 0.7320 0.5051 0.053 Uiso 1 1 calc R . . C58 C 0.9890(7) 0.5873(4) 0.4365(4) 0.0580(14) Uani 1 1 d . . . H58 H 1.0704 0.5659 0.4454 0.070 Uiso 1 1 calc R . . C59 C 0.8584(7) 0.5207(4) 0.3874(4) 0.0645(16) Uani 1 1 d . . . H59 H 0.8497 0.4535 0.3631 0.077 Uiso 1 1 calc R . . C60 C 0.7411(7) 0.5546(3) 0.3747(3) 0.0566(14) Uani 1 1 d . . . H60 H 0.6515 0.5106 0.3410 0.068 Uiso 1 1 calc R . . C61 C 0.7567(5) 0.6545(3) 0.4122(3) 0.0410(11) Uani 1 1 d . . . C62 C 0.6359(5) 0.6969(3) 0.4073(3) 0.0424(11) Uani 1 1 d . . . H62 H 0.5440 0.6560 0.3749 0.051 Uiso 1 1 calc R . . C63 C 0.5391(5) 0.8302(4) 0.4551(3) 0.0438(11) Uani 1 1 d . . . H63 H 0.5638 0.8662 0.5232 0.053 Uiso 1 1 calc R . . C64 C 0.3958(6) 0.7550(4) 0.4209(4) 0.0686(16) Uani 1 1 d . . . H64A H 0.3684 0.7157 0.3547 0.103 Uiso 1 1 calc R . . H64B H 0.3261 0.7890 0.4296 0.103 Uiso 1 1 calc R . . H64C H 0.4030 0.7130 0.4568 0.103 Uiso 1 1 calc R . . C65 C 0.5254(5) 0.9056(3) 0.4095(3) 0.0403(11) Uani 1 1 d . . . C66 C 0.4857(5) 0.9872(4) 0.4503(3) 0.0516(13) Uani 1 1 d . . . H66 H 0.4703 0.9960 0.5067 0.062 Uiso 1 1 calc R . . C67 C 0.4681(6) 1.0566(4) 0.4088(4) 0.0651(15) Uani 1 1 d . . . H67 H 0.4384 1.1105 0.4362 0.078 Uiso 1 1 calc R . . C68 C 0.4950(6) 1.0448(4) 0.3263(4) 0.0608(14) Uani 1 1 d . . . H68 H 0.4881 1.0924 0.2995 0.073 Uiso 1 1 calc R . . C69 C 0.5314(5) 0.9640(4) 0.2849(3) 0.0549(13) Uani 1 1 d . . . H69 H 0.5472 0.9556 0.2287 0.066 Uiso 1 1 calc R . . C70 C 0.5456(5) 0.8930(4) 0.3250(3) 0.0458(11) Uani 1 1 d . . . H70 H 0.5686 0.8370 0.2948 0.055 Uiso 1 1 calc R . . C71 C 0.8409(5) 1.0581(3) 0.6338(3) 0.0355(10) Uani 1 1 d . . . H71 H 0.8416 1.0317 0.6801 0.043 Uiso 1 1 calc R . . C72 C 0.8258(5) 1.1516(3) 0.6496(3) 0.0461(12) Uani 1 1 d . . . H72 H 0.8173 1.1875 0.7060 0.055 Uiso 1 1 calc R . . C73 C 0.8231(6) 1.1916(3) 0.5826(4) 0.0488(12) Uani 1 1 d . . . H73 H 0.8110 1.2543 0.5920 0.059 Uiso 1 1 calc R . . C74 C 0.8388(5) 1.1367(3) 0.4997(3) 0.0419(11) Uani 1 1 d . . . H74 H 0.8381 1.1623 0.4529 0.050 Uiso 1 1 calc R . . C75 C 0.8555(4) 1.0431(3) 0.4884(3) 0.0323(9) Uani 1 1 d . . . C76 C 0.8801(5) 0.9827(3) 0.4071(3) 0.0359(10) Uani 1 1 d . . . H76 H 0.8864 1.0060 0.3599 0.043 Uiso 1 1 calc R . . C77 C 0.9250(5) 0.8355(3) 0.3208(3) 0.0373(10) Uani 1 1 d . . . H77 H 0.9402 0.7765 0.3335 0.045 Uiso 1 1 calc R . . C78 C 1.0641(5) 0.8891(4) 0.3192(3) 0.0463(11) Uani 1 1 d . . . H78A H 1.0514 0.9442 0.3011 0.069 Uiso 1 1 calc R . . H78B H 1.0917 0.8444 0.2743 0.069 Uiso 1 1 calc R . . H78C H 1.1364 0.9120 0.3814 0.069 Uiso 1 1 calc R . . C79 C 0.8007(5) 0.8005(3) 0.2282(3) 0.0380(10) Uani 1 1 d . . . C80 C 0.7083(6) 0.7064(3) 0.1938(3) 0.0501(13) Uani 1 1 d . . . H80 H 0.7261 0.6656 0.2277 0.060 Uiso 1 1 calc R . . C81 C 0.5912(6) 0.6724(4) 0.1106(4) 0.0610(15) Uani 1 1 d . . . H81 H 0.5316 0.6092 0.0890 0.073 Uiso 1 1 calc R . . C82 C 0.5629(6) 0.7320(5) 0.0600(4) 0.0630(16) Uani 1 1 d . . . H82 H 0.4843 0.7094 0.0039 0.076 Uiso 1 1 calc R . . C83 C 0.6515(5) 0.8253(4) 0.0929(3) 0.0518(13) Uani 1 1 d . . . H83 H 0.6314 0.8661 0.0592 0.062 Uiso 1 1 calc R . . C84 C 0.7707(5) 0.8594(3) 0.1757(3) 0.0416(11) Uani 1 1 d . . . H84 H 0.8308 0.9222 0.1962 0.050 Uiso 1 1 calc R . . N1 N 0.6583(4) 0.5228(2) 0.6796(2) 0.0305(8) Uani 1 1 d . . . N2 N 0.7690(3) 0.6914(2) 0.8319(2) 0.0253(7) Uani 1 1 d . . . N3 N 0.9188(4) 0.5893(2) 0.9582(2) 0.0291(8) Uani 1 1 d . . . N4 N 0.9726(4) 0.5712(2) 0.7995(2) 0.0298(8) Uani 1 1 d . . . N5 N 0.4013(4) 0.2987(2) 0.6986(2) 0.0288(8) Uani 1 1 d . . . N6 N 0.5296(4) 0.1810(2) 0.7734(2) 0.0304(8) Uani 1 1 d . . . N7 N 0.7048(4) 0.3602(2) 0.9655(2) 0.0277(8) Uani 1 1 d . . . N8 N 0.4233(4) 0.3293(2) 0.9040(2) 0.0304(8) Uani 1 1 d . . . N9 N 0.8855(4) 0.7200(2) 0.4627(2) 0.0350(9) Uani 1 1 d . . . N10 N 0.6568(4) 0.7876(3) 0.4467(2) 0.0332(8) Uani 1 1 d . . . N11 N 0.8545(3) 1.0040(2) 0.5551(2) 0.0277(8) Uani 1 1 d . . . N12 N 0.8928(4) 0.8973(2) 0.4013(2) 0.0309(8) Uani 1 1 d . . . Cl1 Cl 0.57803(10) 0.51362(7) 0.86607(7) 0.0294(2) Uani 1 1 d . . . Cl2 Cl 0.75729(10) 0.36945(7) 0.77838(7) 0.0305(2) Uani 1 1 d . . . Cl3 Cl 0.84270(11) 0.83975(7) 0.65570(7) 0.0365(2) Uani 1 1 d . . . Cl4 Cl 1.13414(11) 0.93315(8) 0.59176(8) 0.0424(3) Uani 1 1 d . . . Cl5 Cl 0.38478(16) 0.49872(10) 0.18551(10) 0.0661(4) Uani 1 1 d . . . Cl6 Cl -0.1336(2) 0.26723(12) 0.34389(13) 0.0867(5) Uani 1 1 d . . . C1S C 0.0929(9) 0.1208(5) 0.2402(6) 0.104(3) Uani 1 1 d . . . H1S1 H 0.0637 0.1509 0.1946 0.156 Uiso 1 1 calc R . . H1S2 H 0.1172 0.0622 0.2114 0.156 Uiso 1 1 calc R . . H1S3 H 0.1736 0.1662 0.2938 0.156 Uiso 1 1 calc R . . O2S O 0.5559(11) 0.2917(9) 0.3258(7) 0.229(5) Uani 1 1 d . . . H2S H 0.6350 0.2985 0.3233 0.343 Uiso 1 1 calc R . . C3S C 0.1806(9) 0.3938(6) 0.3207(9) 0.186(7) Uani 1 1 d . . . H3S1 H 0.2501 0.3615 0.3078 0.278 Uiso 1 1 calc R . . H3S2 H 0.0885 0.3550 0.2747 0.278 Uiso 1 1 calc R . . H3S3 H 0.1827 0.4009 0.3833 0.278 Uiso 1 1 calc R . . O1S O -0.0192(5) 0.0959(3) 0.2706(3) 0.0747(11) Uani 1 1 d . . . H1S H -0.0486 0.1441 0.2872 0.112 Uiso 1 1 calc R . . C2S C 0.4517(13) 0.2680(7) 0.2319(6) 0.136(4) Uani 1 1 d . . . H2S1 H 0.3798 0.3007 0.2375 0.204 Uiso 1 1 calc R . . H2S2 H 0.4097 0.1980 0.2024 0.204 Uiso 1 1 calc R . . H2S3 H 0.4969 0.2895 0.1939 0.204 Uiso 1 1 calc R . . O3S O 0.2127(6) 0.4948(5) 0.3147(4) 0.127(2) Uani 1 1 d . . . H3S H 0.2519 0.4936 0.2764 0.190 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0250(3) 0.0240(3) 0.0277(3) 0.0080(2) 0.0107(2) 0.0055(2) Ni2 0.0259(3) 0.0247(3) 0.0275(2) 0.0099(2) 0.0101(2) 0.0066(2) Ni3 0.0332(3) 0.0242(3) 0.0280(2) 0.0094(2) 0.0097(2) 0.0096(2) C1 0.046(3) 0.038(3) 0.037(2) 0.013(2) 0.014(2) 0.002(2) C2 0.071(4) 0.047(3) 0.027(2) 0.004(2) 0.009(3) -0.009(3) C3 0.088(4) 0.061(4) 0.032(3) 0.023(3) -0.009(3) -0.013(3) C4 0.058(3) 0.048(3) 0.041(3) 0.027(2) 0.004(2) -0.002(2) C5 0.027(2) 0.035(2) 0.037(2) 0.0162(19) 0.0125(19) 0.0012(18) C6 0.025(2) 0.029(2) 0.040(2) 0.0150(19) 0.0140(19) 0.0060(17) C7 0.032(2) 0.029(2) 0.032(2) 0.0102(18) 0.0125(19) 0.0043(17) C8 0.041(3) 0.035(3) 0.054(3) 0.017(2) 0.019(2) 0.015(2) C9 0.029(2) 0.0192(19) 0.037(2) 0.0038(17) 0.0122(19) 0.0073(16) C10 0.040(3) 0.041(3) 0.039(2) 0.011(2) 0.014(2) 0.007(2) C11 0.043(3) 0.062(3) 0.043(3) 0.011(2) 0.007(2) 0.005(2) C12 0.030(3) 0.058(3) 0.060(3) 0.012(3) 0.003(3) 0.000(2) C13 0.032(3) 0.054(3) 0.051(3) 0.013(2) 0.018(2) 0.001(2) C14 0.034(3) 0.033(2) 0.041(2) 0.0050(19) 0.014(2) 0.0026(19) C15 0.042(3) 0.031(2) 0.033(2) 0.0084(18) 0.013(2) 0.0084(19) C16 0.060(4) 0.047(3) 0.035(2) 0.009(2) 0.016(2) 0.016(2) C17 0.050(4) 0.073(4) 0.039(3) 0.019(3) 0.002(2) 0.025(3) C18 0.034(3) 0.049(3) 0.048(3) 0.008(2) 0.005(2) 0.017(2) C19 0.035(3) 0.029(2) 0.036(2) 0.0092(18) 0.010(2) 0.0123(18) C20 0.022(2) 0.028(2) 0.052(3) 0.011(2) 0.015(2) 0.0099(18) C21 0.035(3) 0.038(2) 0.045(2) 0.013(2) 0.022(2) 0.0093(19) C22 0.066(4) 0.042(3) 0.067(3) 0.004(2) 0.049(3) -0.002(2) C23 0.034(2) 0.033(2) 0.042(2) 0.016(2) 0.020(2) 0.0129(18) C24 0.033(3) 0.048(3) 0.041(2) 0.023(2) 0.012(2) 0.018(2) C25 0.047(3) 0.046(3) 0.066(3) 0.039(3) 0.011(3) 0.007(2) C26 0.029(3) 0.084(4) 0.095(4) 0.066(4) 0.015(3) 0.003(3) C27 0.026(3) 0.098(4) 0.111(5) 0.074(4) 0.035(3) 0.029(3) C28 0.046(3) 0.058(3) 0.079(3) 0.047(3) 0.039(3) 0.028(2) C29 0.036(2) 0.030(2) 0.038(2) 0.0145(19) 0.013(2) 0.0097(19) C30 0.040(3) 0.051(3) 0.037(2) 0.024(2) 0.015(2) 0.019(2) C31 0.036(3) 0.053(3) 0.040(2) 0.021(2) 0.006(2) 0.008(2) C32 0.041(3) 0.037(2) 0.041(2) 0.009(2) 0.008(2) 0.000(2) C33 0.029(2) 0.032(2) 0.033(2) 0.0107(19) 0.0125(19) 0.0023(17) C34 0.032(2) 0.025(2) 0.038(2) 0.0087(18) 0.014(2) 0.0040(18) C35 0.031(2) 0.030(2) 0.046(2) 0.0154(19) 0.016(2) 0.0093(18) C36 0.061(4) 0.037(3) 0.054(3) 0.016(2) 0.026(3) 0.024(2) C37 0.040(3) 0.024(2) 0.041(2) 0.0141(18) 0.013(2) 0.0132(18) C38 0.052(3) 0.053(3) 0.053(3) 0.027(2) 0.014(3) 0.019(2) C39 0.067(4) 0.077(4) 0.054(3) 0.040(3) 0.010(3) 0.027(3) C40 0.104(5) 0.076(4) 0.055(3) 0.044(3) 0.042(4) 0.038(4) C41 0.073(4) 0.067(4) 0.064(3) 0.039(3) 0.037(3) 0.019(3) C42 0.046(3) 0.046(3) 0.052(3) 0.027(2) 0.021(2) 0.012(2) C43 0.025(2) 0.034(2) 0.035(2) 0.0120(18) 0.0085(19) 0.0102(17) C44 0.042(3) 0.060(3) 0.043(3) 0.017(2) 0.010(2) 0.025(2) C45 0.049(3) 0.099(5) 0.034(3) 0.024(3) 0.005(3) 0.028(3) C46 0.049(3) 0.088(4) 0.034(2) 0.020(3) 0.019(2) 0.018(3) C47 0.038(3) 0.038(2) 0.031(2) 0.0111(19) 0.012(2) 0.0109(19) C48 0.036(3) 0.043(2) 0.034(2) 0.0168(19) 0.019(2) 0.012(2) C49 0.032(3) 0.048(3) 0.041(2) 0.021(2) 0.018(2) 0.013(2) C50 0.046(3) 0.059(3) 0.095(4) 0.051(3) 0.036(3) 0.026(2) C51 0.026(2) 0.033(2) 0.041(2) 0.0111(19) 0.012(2) 0.0067(18) C52 0.033(3) 0.053(3) 0.045(3) 0.005(2) 0.009(2) 0.010(2) C53 0.037(3) 0.034(3) 0.077(4) 0.011(3) 0.001(3) -0.002(2) C54 0.044(3) 0.053(3) 0.087(4) 0.030(3) 0.024(3) -0.002(3) C55 0.048(3) 0.056(3) 0.060(3) 0.025(3) 0.030(3) 0.006(2) C56 0.039(3) 0.034(2) 0.056(3) 0.011(2) 0.025(2) 0.004(2) C57 0.062(3) 0.038(3) 0.039(2) 0.015(2) 0.020(2) 0.023(2) C58 0.078(4) 0.053(3) 0.055(3) 0.022(3) 0.028(3) 0.041(3) C59 0.102(5) 0.038(3) 0.053(3) 0.014(3) 0.025(3) 0.032(3) C60 0.084(4) 0.027(2) 0.048(3) 0.007(2) 0.022(3) 0.005(3) C61 0.059(3) 0.035(2) 0.028(2) 0.0121(19) 0.015(2) 0.011(2) C62 0.047(3) 0.036(3) 0.030(2) 0.010(2) 0.004(2) -0.002(2) C63 0.035(3) 0.055(3) 0.041(2) 0.020(2) 0.011(2) 0.014(2) C64 0.045(3) 0.082(4) 0.087(4) 0.047(4) 0.020(3) 0.015(3) C65 0.029(2) 0.049(3) 0.036(2) 0.013(2) 0.0049(19) 0.013(2) C66 0.057(3) 0.057(3) 0.040(3) 0.013(2) 0.018(2) 0.021(3) C67 0.067(4) 0.053(3) 0.075(4) 0.020(3) 0.023(3) 0.031(3) C68 0.063(4) 0.066(4) 0.063(3) 0.038(3) 0.015(3) 0.029(3) C69 0.048(3) 0.076(4) 0.042(3) 0.026(3) 0.010(2) 0.025(3) C70 0.041(3) 0.058(3) 0.036(2) 0.017(2) 0.006(2) 0.025(2) C71 0.042(3) 0.030(2) 0.033(2) 0.0072(18) 0.015(2) 0.0107(19) C72 0.063(3) 0.036(3) 0.043(3) 0.009(2) 0.028(2) 0.019(2) C73 0.063(3) 0.025(2) 0.062(3) 0.011(2) 0.031(3) 0.016(2) C74 0.047(3) 0.035(2) 0.052(3) 0.024(2) 0.020(2) 0.016(2) C75 0.030(2) 0.028(2) 0.034(2) 0.0113(18) 0.0075(19) 0.0056(17) C76 0.039(3) 0.036(3) 0.036(2) 0.0177(19) 0.013(2) 0.0111(19) C77 0.049(3) 0.036(2) 0.033(2) 0.0119(19) 0.020(2) 0.019(2) C78 0.043(3) 0.059(3) 0.039(2) 0.014(2) 0.019(2) 0.018(2) C79 0.044(3) 0.040(3) 0.032(2) 0.0078(19) 0.021(2) 0.012(2) C80 0.064(3) 0.039(3) 0.046(3) 0.004(2) 0.034(3) 0.007(2) C81 0.050(3) 0.056(3) 0.054(3) -0.004(3) 0.024(3) -0.004(3) C82 0.039(3) 0.090(4) 0.037(3) -0.002(3) 0.014(2) 0.010(3) C83 0.049(3) 0.078(4) 0.038(3) 0.025(3) 0.024(2) 0.020(3) C84 0.038(3) 0.052(3) 0.037(2) 0.014(2) 0.020(2) 0.012(2) N1 0.0246(19) 0.034(2) 0.0282(17) 0.0079(15) 0.0114(15) 0.0013(15) N2 0.0188(17) 0.0279(18) 0.0321(19) 0.0123(15) 0.0118(15) 0.0069(14) N3 0.029(2) 0.0242(18) 0.0331(19) 0.0095(15) 0.0109(16) 0.0085(14) N4 0.0254(19) 0.0267(18) 0.042(2) 0.0120(15) 0.0173(18) 0.0106(14) N5 0.031(2) 0.032(2) 0.0275(17) 0.0109(15) 0.0151(15) 0.0103(15) N6 0.031(2) 0.0259(18) 0.0329(19) 0.0098(15) 0.0130(18) 0.0047(15) N7 0.030(2) 0.0252(17) 0.0258(17) 0.0086(14) 0.0077(16) 0.0077(14) N8 0.031(2) 0.0297(18) 0.0344(19) 0.0134(15) 0.0150(17) 0.0096(15) N9 0.049(2) 0.030(2) 0.0292(18) 0.0095(16) 0.0177(18) 0.0154(18) N10 0.034(2) 0.035(2) 0.0265(17) 0.0127(16) 0.0057(16) 0.0071(15) N11 0.0299(19) 0.0262(18) 0.0266(17) 0.0081(15) 0.0105(15) 0.0097(14) N12 0.036(2) 0.0288(19) 0.0285(17) 0.0100(15) 0.0113(16) 0.0118(15) Cl1 0.0291(5) 0.0258(5) 0.0354(5) 0.0107(4) 0.0153(4) 0.0081(4) Cl2 0.0340(6) 0.0249(5) 0.0362(5) 0.0102(4) 0.0182(5) 0.0094(4) Cl3 0.0425(6) 0.0353(5) 0.0319(5) 0.0156(4) 0.0121(5) 0.0086(5) Cl4 0.0348(6) 0.0393(6) 0.0498(6) 0.0214(5) 0.0074(5) 0.0076(5) Cl5 0.0707(9) 0.0537(8) 0.0622(8) 0.0160(6) 0.0155(7) 0.0142(7) Cl6 0.1236(15) 0.0741(10) 0.1077(13) 0.0578(10) 0.0680(12) 0.0501(10) C1S 0.127(7) 0.077(5) 0.144(7) 0.053(5) 0.084(6) 0.034(4) O2S 0.181(9) 0.219(10) 0.216(10) -0.034(8) 0.110(8) 0.027(8) C3S 0.090(6) 0.057(5) 0.295(15) 0.066(7) -0.074(8) -0.005(4) O1S 0.096(3) 0.055(2) 0.087(3) 0.036(2) 0.042(3) 0.022(2) C2S 0.198(11) 0.096(6) 0.097(6) 0.046(5) 0.021(7) 0.040(7) O3S 0.093(4) 0.154(6) 0.103(4) 0.015(4) 0.029(3) 0.032(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 N3 2.075(3) . ? Ni1 N1 2.084(3) . ? Ni1 N2 2.104(3) . ? Ni1 N4 2.108(3) . ? Ni1 Cl1 2.4211(10) . ? Ni1 Cl2 2.4687(11) . ? Ni2 N7 2.083(3) . ? Ni2 N8 2.102(3) . ? Ni2 N5 2.103(3) . ? Ni2 N6 2.129(3) . ? Ni2 Cl2 2.4291(10) . ? Ni2 Cl1 2.4796(11) . ? Ni3 N11 2.053(3) . ? Ni3 N9 2.067(3) . ? Ni3 N12 2.112(3) . ? Ni3 N10 2.154(3) . ? Ni3 Cl3 2.4250(11) . ? Ni3 Cl4 2.4352(12) . ? C1 N1 1.331(5) . ? C1 C2 1.376(7) . ? C2 C3 1.374(8) . ? C3 C4 1.366(7) . ? C4 C5 1.369(6) . ? C5 N1 1.357(5) . ? C5 C6 1.462(6) . ? C6 N2 1.271(5) . ? C7 N2 1.478(5) . ? C7 C9 1.517(6) . ? C7 C8 1.533(6) . ? C9 C10 1.366(6) . ? C9 C14 1.390(6) . ? C10 C11 1.364(7) . ? C11 C12 1.372(7) . ? C12 C13 1.376(7) . ? C13 C14 1.375(6) . ? C15 N3 1.335(5) . ? C15 C16 1.385(7) . ? C16 C17 1.354(7) . ? C17 C18 1.382(7) . ? C18 C19 1.375(6) . ? C19 N3 1.354(5) . ? C19 C20 1.462(6) . ? C20 N4 1.268(5) . ? C21 N4 1.488(5) . ? C21 C23 1.517(6) . ? C21 C22 1.517(6) . ? C23 C28 1.372(7) . ? C23 C24 1.384(6) . ? C24 C25 1.384(6) . ? C25 C26 1.343(7) . ? C26 C27 1.368(7) . ? C27 C28 1.380(7) . ? C29 N5 1.318(5) . ? C29 C30 1.371(6) . ? C30 C31 1.367(6) . ? C31 C32 1.374(7) . ? C32 C33 1.389(6) . ? C33 N5 1.345(5) . ? C33 C34 1.454(6) . ? C34 N6 1.261(5) . ? C35 N6 1.483(5) . ? C35 C37 1.519(6) . ? C35 C36 1.524(6) . ? C37 C38 1.372(7) . ? C37 C42 1.373(6) . ? C38 C39 1.381(7) . ? C39 C40 1.372(8) . ? C40 C41 1.362(8) . ? C41 C42 1.392(7) . ? C43 N7 1.326(5) . ? C43 C44 1.381(6) . ? C44 C45 1.372(7) . ? C45 C46 1.377(8) . ? C46 C47 1.376(6) . ? C47 N7 1.335(5) . ? C47 C48 1.462(6) . ? C48 N8 1.274(5) . ? C49 N8 1.481(6) . ? C49 C50 1.506(7) . ? C49 C51 1.532(6) . ? C51 C52 1.379(6) . ? C51 C56 1.383(6) . ? C52 C53 1.415(7) . ? C53 C54 1.368(8) . ? C54 C55 1.358(7) . ? C55 C56 1.394(6) . ? C57 N9 1.319(6) . ? C57 C58 1.387(7) . ? C58 C59 1.369(8) . ? C59 C60 1.365(8) . ? C60 C61 1.378(6) . ? C61 N9 1.352(6) . ? C61 C62 1.475(7) . ? C62 N10 1.248(5) . ? C63 N10 1.476(6) . ? C63 C65 1.507(6) . ? C63 C64 1.531(7) . ? C65 C66 1.374(7) . ? C65 C70 1.380(6) . ? C66 C67 1.387(7) . ? C67 C68 1.385(8) . ? C68 C69 1.347(8) . ? C69 C70 1.389(7) . ? C71 N11 1.324(5) . ? C71 C72 1.373(6) . ? C72 C73 1.362(6) . ? C73 C74 1.391(7) . ? C74 C75 1.388(6) . ? C75 N11 1.356(5) . ? C75 C76 1.447(6) . ? C76 N12 1.271(5) . ? C77 N12 1.489(5) . ? C77 C79 1.509(6) . ? C77 C78 1.534(6) . ? C79 C84 1.388(6) . ? C79 C80 1.396(6) . ? C80 C81 1.381(8) . ? C81 C82 1.373(8) . ? C82 C83 1.374(8) . ? C83 C84 1.391(7) . ? C1S O1S 1.417(8) . ? O2S C2S 1.452(13) . ? C3S O3S 1.517(9) . ? 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 N3 Ni1 N1 171.33(13) . . ? N3 Ni1 N2 94.71(13) . . ? N1 Ni1 N2 79.41(13) . . ? N3 Ni1 N4 79.74(13) . . ? N1 Ni1 N4 93.97(13) . . ? N2 Ni1 N4 91.61(12) . . ? N3 Ni1 Cl1 91.44(10) . . ? N1 Ni1 Cl1 95.26(9) . . ? N2 Ni1 Cl1 93.64(9) . . ? N4 Ni1 Cl1 170.09(10) . . ? N3 Ni1 Cl2 95.08(9) . . ? N1 Ni1 Cl2 90.99(10) . . ? N2 Ni1 Cl2 170.14(9) . . ? N4 Ni1 Cl2 91.33(9) . . ? Cl1 Ni1 Cl2 84.91(3) . . ? N7 Ni2 N8 79.75(13) . . ? N7 Ni2 N5 172.54(12) . . ? N8 Ni2 N5 94.46(13) . . ? N7 Ni2 N6 96.50(13) . . ? N8 Ni2 N6 94.66(12) . . ? N5 Ni2 N6 79.16(13) . . ? N7 Ni2 Cl2 90.43(10) . . ? N8 Ni2 Cl2 168.23(10) . . ? N5 Ni2 Cl2 95.83(9) . . ? N6 Ni2 Cl2 92.88(9) . . ? N7 Ni2 Cl1 94.33(9) . . ? N8 Ni2 Cl1 89.75(9) . . ? N5 Ni2 Cl1 90.33(9) . . ? N6 Ni2 Cl1 168.88(9) . . ? Cl2 Ni2 Cl1 84.50(3) . . ? N11 Ni3 N9 171.71(13) . . ? N11 Ni3 N12 79.16(12) . . ? N9 Ni3 N12 94.25(13) . . ? N11 Ni3 N10 96.42(14) . . ? N9 Ni3 N10 78.74(14) . . ? N12 Ni3 N10 92.85(13) . . ? N11 Ni3 Cl3 94.40(9) . . ? N9 Ni3 Cl3 91.83(9) . . ? N12 Ni3 Cl3 172.63(10) . . ? N10 Ni3 Cl3 84.24(9) . . ? N11 Ni3 Cl4 89.69(10) . . ? N9 Ni3 Cl4 94.97(11) . . ? N12 Ni3 Cl4 86.43(10) . . ? N10 Ni3 Cl4 173.61(10) . . ? Cl3 Ni3 Cl4 97.21(4) . . ? N1 C1 C2 123.3(4) . . ? C3 C2 C1 119.0(4) . . ? C4 C3 C2 118.3(5) . . ? C3 C4 C5 120.5(5) . . ? N1 C5 C4 121.6(4) . . ? N1 C5 C6 115.6(4) . . ? C4 C5 C6 122.8(4) . . ? N2 C6 C5 119.4(4) . . ? N2 C7 C9 111.1(3) . . ? N2 C7 C8 115.0(3) . . ? C9 C7 C8 109.7(3) . . ? C10 C9 C14 119.1(4) . . ? C10 C9 C7 120.0(4) . . ? C14 C9 C7 120.8(4) . . ? C11 C10 C9 121.4(4) . . ? C10 C11 C12 119.6(5) . . ? C11 C12 C13 120.0(5) . . ? C14 C13 C12 120.1(4) . . ? C13 C14 C9 119.7(4) . . ? N3 C15 C16 122.3(4) . . ? C17 C16 C15 119.7(4) . . ? C16 C17 C18 118.7(5) . . ? C19 C18 C17 119.4(5) . . ? N3 C19 C18 122.0(4) . . ? N3 C19 C20 115.0(4) . . ? C18 C19 C20 123.0(4) . . ? N4 C20 C19 120.4(4) . . ? N4 C21 C23 114.7(4) . . ? N4 C21 C22 108.1(3) . . ? C23 C21 C22 112.9(4) . . ? C28 C23 C24 118.5(4) . . ? C28 C23 C21 122.6(4) . . ? C24 C23 C21 119.0(4) . . ? C25 C24 C23 120.4(4) . . ? C26 C25 C24 120.1(4) . . ? C25 C26 C27 120.8(4) . . ? C26 C27 C28 119.6(5) . . ? C23 C28 C27 120.7(4) . . ? N5 C29 C30 123.0(4) . . ? C31 C30 C29 119.6(4) . . ? C30 C31 C32 118.1(4) . . ? C31 C32 C33 119.7(4) . . ? N5 C33 C32 121.2(4) . . ? N5 C33 C34 116.3(3) . . ? C32 C33 C34 122.5(4) . . ? N6 C34 C33 120.7(4) . . ? N6 C35 C37 112.1(3) . . ? N6 C35 C36 114.3(4) . . ? C37 C35 C36 109.4(3) . . ? C38 C37 C42 119.5(4) . . ? C38 C37 C35 119.5(4) . . ? C42 C37 C35 120.8(4) . . ? C37 C38 C39 120.6(5) . . ? C40 C39 C38 119.3(5) . . ? C41 C40 C39 121.0(5) . . ? C40 C41 C42 119.4(5) . . ? C37 C42 C41 120.2(5) . . ? N7 C43 C44 123.1(4) . . ? C45 C44 C43 118.5(5) . . ? C44 C45 C46 119.1(5) . . ? C47 C46 C45 118.5(5) . . ? N7 C47 C46 122.9(4) . . ? N7 C47 C48 115.8(4) . . ? C46 C47 C48 121.3(4) . . ? N8 C48 C47 120.1(4) . . ? N8 C49 C50 109.8(4) . . ? N8 C49 C51 111.9(3) . . ? C50 C49 C51 113.5(4) . . ? C52 C51 C56 119.0(4) . . ? C52 C51 C49 119.2(4) . . ? C56 C51 C49 121.7(4) . . ? C51 C52 C53 120.3(5) . . ? C54 C53 C52 119.3(5) . . ? C55 C54 C53 120.7(5) . . ? C54 C55 C56 120.5(5) . . ? C51 C56 C55 120.2(4) . . ? N9 C57 C58 122.3(5) . . ? C59 C58 C57 119.1(5) . . ? C60 C59 C58 119.0(5) . . ? C59 C60 C61 119.4(5) . . ? N9 C61 C60 121.6(5) . . ? N9 C61 C62 115.2(4) . . ? C60 C61 C62 123.0(5) . . ? N10 C62 C61 120.1(4) . . ? N10 C63 C65 112.4(4) . . ? N10 C63 C64 115.2(4) . . ? C65 C63 C64 110.3(4) . . ? C66 C65 C70 118.5(4) . . ? C66 C65 C63 119.6(4) . . ? C70 C65 C63 121.9(4) . . ? C65 C66 C67 121.2(5) . . ? C68 C67 C66 119.3(5) . . ? C69 C68 C67 119.8(5) . . ? C68 C69 C70 121.0(5) . . ? C65 C70 C69 120.2(5) . . ? N11 C71 C72 122.5(4) . . ? C73 C72 C71 119.9(4) . . ? C72 C73 C74 118.7(4) . . ? C75 C74 C73 118.7(4) . . ? N11 C75 C74 121.6(4) . . ? N11 C75 C76 115.7(4) . . ? C74 C75 C76 122.7(4) . . ? N12 C76 C75 119.0(4) . . ? N12 C77 C79 111.3(4) . . ? N12 C77 C78 110.5(3) . . ? C79 C77 C78 114.6(3) . . ? C84 C79 C80 117.5(4) . . ? C84 C79 C77 122.6(4) . . ? C80 C79 C77 119.8(4) . . ? C81 C80 C79 121.7(5) . . ? C82 C81 C80 119.9(5) . . ? C81 C82 C83 119.5(5) . . ? C82 C83 C84 120.9(5) . . ? C79 C84 C83 120.4(4) . . ? C1 N1 C5 117.4(4) . . ? C1 N1 Ni1 130.1(3) . . ? C5 N1 Ni1 112.4(3) . . ? C6 N2 C7 120.4(3) . . ? C6 N2 Ni1 112.9(3) . . ? C7 N2 Ni1 126.7(2) . . ? C15 N3 C19 117.8(4) . . ? C15 N3 Ni1 129.6(3) . . ? C19 N3 Ni1 112.6(3) . . ? C20 N4 C21 121.9(3) . . ? C20 N4 Ni1 111.9(3) . . ? C21 N4 Ni1 126.1(3) . . ? C29 N5 C33 118.4(3) . . ? C29 N5 Ni2 129.7(3) . . ? C33 N5 Ni2 111.8(3) . . ? C34 N6 C35 121.1(3) . . ? C34 N6 Ni2 111.7(3) . . ? C35 N6 Ni2 127.0(3) . . ? C43 N7 C47 117.8(4) . . ? C43 N7 Ni2 129.8(3) . . ? C47 N7 Ni2 112.4(3) . . ? C48 N8 C49 120.0(3) . . ? C48 N8 Ni2 111.7(3) . . ? C49 N8 Ni2 128.0(3) . . ? C57 N9 C61 118.5(4) . . ? C57 N9 Ni3 127.6(3) . . ? C61 N9 Ni3 113.8(3) . . ? C62 N10 C63 121.1(4) . . ? C62 N10 Ni3 112.2(3) . . ? C63 N10 Ni3 125.8(3) . . ? C71 N11 C75 118.6(3) . . ? C71 N11 Ni3 128.1(3) . . ? C75 N11 Ni3 113.3(3) . . ? C76 N12 C77 120.0(3) . . ? C76 N12 Ni3 112.8(3) . . ? C77 N12 Ni3 127.1(3) . . ? Ni1 Cl1 Ni2 95.21(4) . . ? Ni2 Cl2 Ni1 95.29(4) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.500 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.044 data_1S _database_code_depnum_ccdc_archive 'CCDC 756355' #TrackingRef 'Combined_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H56 Cl2 N8 Ni2, C28 H28 Cl2 N4 Ni, 3(C H4 O), 2(Cl)' _chemical_formula_sum 'C87 H96 Cl6 N12 Ni3 O3' _chemical_formula_weight 1746.53 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.3220(17) _cell_length_b 14.819(3) _cell_length_c 15.883(3) _cell_angle_alpha 107.650(3) _cell_angle_beta 107.289(2) _cell_angle_gamma 99.278(3) _cell_volume 2124.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6611 _exptl_absorpt_correction_T_max 0.8544 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8716 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 23.27 _reflns_number_total 7152 _reflns_number_gt 6618 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration rmad _refine_ls_abs_structure_Flack 0.000(11) _refine_ls_number_reflns 7152 _refine_ls_number_parameters 1009 _refine_ls_number_restraints 669 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.44369(7) 0.33522(5) 0.83773(5) 0.02961(18) Uani 1 1 d U . . Ni2 Ni 0.54324(6) 0.65202(5) 0.53711(4) 0.02681(18) Uani 1 1 d U . . Ni3 Ni 0.75909(6) 0.86305(5) 0.52546(4) 0.02678(18) Uani 1 1 d U . . N1 N 0.4669(5) 0.1950(3) 0.8014(3) 0.0276(11) Uani 1 1 d U . . N2 N 0.4294(5) 0.3017(4) 0.9551(3) 0.0320(11) Uani 1 1 d U . . N3 N 0.4381(6) 0.4784(4) 0.8939(3) 0.0365(13) Uani 1 1 d U . . N4 N 0.6656(5) 0.4106(4) 0.9094(3) 0.0350(12) Uani 1 1 d U . . N5 N 0.4022(5) 0.6100(3) 0.3983(3) 0.0279(11) Uani 1 1 d U . . N6 N 0.3492(5) 0.6275(3) 0.5568(3) 0.0291(11) Uani 1 1 d U . . N7 N 0.6633(5) 0.6762(4) 0.6772(3) 0.0313(12) Uani 1 1 d U . . N8 N 0.5518(5) 0.5068(3) 0.5237(3) 0.0268(11) Uani 1 1 d U . . N9 N 0.6178(5) 0.8397(3) 0.3915(3) 0.0277(11) Uani 1 1 d U . . N10 N 0.8998(5) 0.8702(3) 0.4532(3) 0.0305(11) Uani 1 1 d U . . N11 N 0.9192(5) 0.9007(4) 0.6575(3) 0.0290(11) Uani 1 1 d U . . N12 N 0.7920(5) 1.0175(4) 0.5832(3) 0.0293(12) Uani 1 1 d U . . O1S O 0.3416(6) 0.1033(4) 0.0861(4) 0.0759(16) Uani 1 1 d U . . H1 H 0.3716 0.0556 0.0693 0.114 Uiso 1 1 calc R . . O2S O 0.1111(9) 0.7032(9) 0.0429(6) 0.160(4) Uani 1 1 d U . . H2 H 0.0786 0.7108 0.0850 0.240 Uiso 1 1 calc R . . O3S O 0.8830(17) 0.9273(12) 0.1249(9) 0.271(9) Uani 1 1 d U . . H3 H 0.9561 0.9610 0.1271 0.406 Uiso 1 1 calc R . . C1 C 0.4805(6) 0.1406(5) 0.7226(4) 0.0386(15) Uani 1 1 d U . . H1A H 0.4801 0.1666 0.6762 0.046 Uiso 1 1 calc R . . C2 C 0.4950(7) 0.0476(5) 0.7077(5) 0.0506(18) Uani 1 1 d U . . H2A H 0.5018 0.0111 0.6509 0.061 Uiso 1 1 calc R . . C3 C 0.4995(8) 0.0080(5) 0.7748(5) 0.0467(18) Uani 1 1 d U . . H3A H 0.5134 -0.0542 0.7661 0.056 Uiso 1 1 calc R . . C4 C 0.4829(7) 0.0628(5) 0.8563(4) 0.0413(16) Uani 1 1 d U . . H4 H 0.4832 0.0374 0.9032 0.050 Uiso 1 1 calc R . . C5 C 0.4658(6) 0.1551(5) 0.8676(4) 0.0336(14) Uani 1 1 d U . . C6 C 0.4406(6) 0.2162(5) 0.9488(4) 0.0369(15) Uani 1 1 d U . . H6 H 0.4327 0.1927 0.9956 0.044 Uiso 1 1 calc R . . C7 C 0.3951(7) 0.3632(5) 1.0359(4) 0.0388(16) Uani 1 1 d U . . H7 H 0.3788 0.4218 1.0228 0.047 Uiso 1 1 calc R . . C8 C 0.2578(6) 0.3098(5) 1.0375(4) 0.0426(16) Uani 1 1 d U . . H8A H 0.2698 0.2528 1.0524 0.064 Uiso 1 1 calc R . . H8B H 0.1844 0.2896 0.9763 0.064 Uiso 1 1 calc R . . H8C H 0.2326 0.3531 1.0848 0.064 Uiso 1 1 calc R . . C9 C 0.5212(6) 0.3998(5) 1.1287(4) 0.0357(15) Uani 1 1 d U . . C10 C 0.6124(8) 0.4936(5) 1.1625(5) 0.0496(18) Uani 1 1 d U . . H10 H 0.5943 0.5342 1.1284 0.060 Uiso 1 1 calc R . . C11 C 0.7292(8) 0.5275(6) 1.2454(5) 0.065(2) Uani 1 1 d U . . H11 H 0.7884 0.5908 1.2671 0.079 Uiso 1 1 calc R . . C12 C 0.7581(8) 0.4678(7) 1.2962(5) 0.064(2) Uani 1 1 d U . . H12 H 0.8370 0.4905 1.3521 0.077 Uiso 1 1 calc R . . C13 C 0.6702(7) 0.3745(6) 1.2641(5) 0.055(2) Uani 1 1 d U . . H13 H 0.6899 0.3340 1.2982 0.066 Uiso 1 1 calc R . . C14 C 0.5519(7) 0.3404(5) 1.1807(4) 0.0422(16) Uani 1 1 d U . . H14 H 0.4928 0.2772 1.1594 0.051 Uiso 1 1 calc R . . C15 C 0.3243(8) 0.5130(5) 0.8840(4) 0.0441(17) Uani 1 1 d U . . H15 H 0.2352 0.4684 0.8509 0.053 Uiso 1 1 calc R . . C16 C 0.3342(9) 0.6122(6) 0.9210(5) 0.060(2) Uani 1 1 d U . . H16 H 0.2529 0.6334 0.9132 0.071 Uiso 1 1 calc R . . C17 C 0.4644(10) 0.6790(6) 0.9691(5) 0.066(2) Uani 1 1 d U . . H17 H 0.4735 0.7462 0.9926 0.079 Uiso 1 1 calc R . . C18 C 0.5827(9) 0.6437(5) 0.9817(4) 0.0561(19) Uani 1 1 d U . . H18 H 0.6725 0.6873 1.0153 0.067 Uiso 1 1 calc R . . C19 C 0.5665(7) 0.5455(5) 0.9447(4) 0.0410(16) Uani 1 1 d U . . C20 C 0.6867(7) 0.5015(5) 0.9491(4) 0.0411(16) Uani 1 1 d U . . H20 H 0.7787 0.5419 0.9816 0.049 Uiso 1 1 calc R . . C21 C 0.7832(7) 0.3677(5) 0.9014(5) 0.0444(17) Uani 1 1 d U . . H21 H 0.7588 0.3314 0.8334 0.053 Uiso 1 1 calc R . . C22 C 0.9273(8) 0.4432(7) 0.9359(6) 0.073(2) Uani 1 1 d U . . H22A H 0.9545 0.4826 1.0020 0.110 Uiso 1 1 calc R . . H22B H 0.9203 0.4850 0.8998 0.110 Uiso 1 1 calc R . . H22C H 0.9969 0.4092 0.9274 0.110 Uiso 1 1 calc R . . C23 C 0.7972(6) 0.2933(5) 0.9476(4) 0.0405(16) Uani 1 1 d U . . C24 C 0.7755(7) 0.3055(5) 1.0317(4) 0.0456(17) Uani 1 1 d U . . H24 H 0.7513 0.3613 1.0611 0.055 Uiso 1 1 calc R . . C25 C 0.7895(7) 0.2354(6) 1.0724(5) 0.055(2) Uani 1 1 d U . . H25 H 0.7739 0.2444 1.1287 0.066 Uiso 1 1 calc R . . C26 C 0.8258(8) 0.1533(6) 1.0311(5) 0.062(2) Uani 1 1 d U . . H26 H 0.8331 0.1058 1.0580 0.075 Uiso 1 1 calc R . . C27 C 0.8516(8) 0.1418(6) 0.9480(6) 0.065(2) Uani 1 1 d U . . H27 H 0.8803 0.0876 0.9205 0.078 Uiso 1 1 calc R . . C28 C 0.8350(7) 0.2111(6) 0.9054(5) 0.0513(18) Uani 1 1 d U . . H28 H 0.8495 0.2019 0.8487 0.062 Uiso 1 1 calc R . . C29 C 0.4298(6) 0.5985(4) 0.3194(4) 0.0353(14) Uani 1 1 d U . . H29 H 0.5228 0.6074 0.3229 0.042 Uiso 1 1 calc R . . C30 C 0.3223(8) 0.5734(5) 0.2319(4) 0.0490(18) Uani 1 1 d U . . H30 H 0.3437 0.5638 0.1775 0.059 Uiso 1 1 calc R . . C31 C 0.1850(8) 0.5629(6) 0.2257(5) 0.055(2) Uani 1 1 d U . . H31 H 0.1129 0.5489 0.1680 0.066 Uiso 1 1 calc R . . C32 C 0.1565(7) 0.5735(5) 0.3073(5) 0.0514(19) Uani 1 1 d U . . H32 H 0.0644 0.5668 0.3056 0.062 Uiso 1 1 calc R . . C33 C 0.2672(6) 0.5945(5) 0.3920(4) 0.0378(15) Uani 1 1 d U . . C34 C 0.2446(7) 0.6018(4) 0.4806(4) 0.0368(15) Uani 1 1 d U . . H34 H 0.1534 0.5876 0.4805 0.044 Uiso 1 1 calc R . . C35 C 0.3312(6) 0.6349(4) 0.6482(4) 0.0364(15) Uani 1 1 d U . . H35 H 0.4065 0.6123 0.6827 0.044 Uiso 1 1 calc R . . C36 C 0.3574(8) 0.7412(5) 0.7066(5) 0.059(2) Uani 1 1 d U . . H36A H 0.2806 0.7648 0.6787 0.088 Uiso 1 1 calc R . . H36B H 0.4438 0.7790 0.7086 0.088 Uiso 1 1 calc R . . H36C H 0.3644 0.7480 0.7700 0.088 Uiso 1 1 calc R . . C37 C 0.1926(6) 0.5697(5) 0.6370(4) 0.0366(15) Uani 1 1 d U . . C38 C 0.1917(6) 0.4833(5) 0.6547(4) 0.0358(15) Uani 1 1 d U . . H38 H 0.2752 0.4655 0.6723 0.043 Uiso 1 1 calc R . . C39 C 0.0661(8) 0.4232(6) 0.6463(5) 0.056(2) Uani 1 1 d U . . H39 H 0.0668 0.3670 0.6609 0.067 Uiso 1 1 calc R . . C40 C -0.0561(7) 0.4463(6) 0.6171(6) 0.068(2) Uani 1 1 d U . . H40 H -0.1401 0.4048 0.6095 0.081 Uiso 1 1 calc R . . C41 C -0.0574(7) 0.5307(7) 0.5984(6) 0.071(3) Uani 1 1 d U . . H41 H -0.1422 0.5462 0.5781 0.085 Uiso 1 1 calc R . . C42 C 0.0665(7) 0.5927(5) 0.6097(5) 0.0516(19) Uani 1 1 d U . . H42 H 0.0650 0.6507 0.5988 0.062 Uiso 1 1 calc R . . C43 C 0.7207(7) 0.7602(5) 0.7528(4) 0.0440(16) Uani 1 1 d U . . H43 H 0.7120 0.8188 0.7448 0.053 Uiso 1 1 calc R . . C44 C 0.7927(8) 0.7636(6) 0.8426(4) 0.059(2) Uani 1 1 d U . . H44 H 0.8300 0.8233 0.8942 0.071 Uiso 1 1 calc R . . C45 C 0.8084(9) 0.6775(6) 0.8548(5) 0.071(3) Uani 1 1 d U . . H45 H 0.8589 0.6782 0.9143 0.085 Uiso 1 1 calc R . . C46 C 0.7486(8) 0.5906(5) 0.7779(4) 0.0529(19) Uani 1 1 d U . . H46 H 0.7563 0.5315 0.7852 0.063 Uiso 1 1 calc R . . C47 C 0.6766(6) 0.5906(5) 0.6893(4) 0.0342(14) Uani 1 1 d U . . C48 C 0.6154(6) 0.5017(4) 0.6050(4) 0.0318(14) Uani 1 1 d U . . H48 H 0.6216 0.4412 0.6091 0.038 Uiso 1 1 calc R . . C49 C 0.5010(6) 0.4205(4) 0.4367(4) 0.0315(14) Uani 1 1 d U . . H49 H 0.5315 0.4407 0.3907 0.038 Uiso 1 1 calc R . . C50 C 0.5582(7) 0.3330(5) 0.4442(5) 0.0400(16) Uani 1 1 d U . . H50A H 0.5257 0.3082 0.4858 0.060 Uiso 1 1 calc R . . H50B H 0.6595 0.3540 0.4693 0.060 Uiso 1 1 calc R . . H50C H 0.5253 0.2819 0.3824 0.060 Uiso 1 1 calc R . . C51 C 0.3411(6) 0.3855(4) 0.3944(4) 0.0308(13) Uani 1 1 d U . . C52 C 0.2630(6) 0.3773(4) 0.4515(4) 0.0370(15) Uani 1 1 d U . . H52 H 0.3087 0.3967 0.5167 0.044 Uiso 1 1 calc R . . C53 C 0.1180(7) 0.3405(5) 0.4106(5) 0.0488(17) Uani 1 1 d U . . H53 H 0.0662 0.3339 0.4484 0.059 Uiso 1 1 calc R . . C54 C 0.0503(7) 0.3137(6) 0.3153(5) 0.058(2) Uani 1 1 d U . . H54 H -0.0477 0.2911 0.2885 0.069 Uiso 1 1 calc R . . C55 C 0.1277(8) 0.3201(5) 0.2582(5) 0.0565(19) Uani 1 1 d U . . H55 H 0.0817 0.2997 0.1928 0.068 Uiso 1 1 calc R . . C56 C 0.2709(7) 0.3562(5) 0.2979(4) 0.0401(15) Uani 1 1 d U . . H56 H 0.3219 0.3612 0.2594 0.048 Uiso 1 1 calc R . . C57 C 0.4798(6) 0.8299(4) 0.3619(4) 0.0346(14) Uani 1 1 d U . . H57 H 0.4358 0.8352 0.4058 0.042 Uiso 1 1 calc R . . C58 C 0.3987(7) 0.8122(5) 0.2691(4) 0.0475(18) Uani 1 1 d U . . H58 H 0.3022 0.8052 0.2509 0.057 Uiso 1 1 calc R . . C59 C 0.4632(8) 0.8050(6) 0.2040(5) 0.062(2) Uani 1 1 d U . . H59 H 0.4112 0.7940 0.1412 0.074 Uiso 1 1 calc R . . C60 C 0.6054(8) 0.8142(6) 0.2328(4) 0.056(2) Uani 1 1 d U . . H60 H 0.6508 0.8077 0.1896 0.067 Uiso 1 1 calc R . . C61 C 0.6802(6) 0.8336(5) 0.3277(4) 0.0363(15) Uani 1 1 d U . . C62 C 0.8327(7) 0.8497(5) 0.3648(4) 0.0400(16) Uani 1 1 d U . . H62 H 0.8818 0.8451 0.3238 0.048 Uiso 1 1 calc R . . C63 C 1.0526(6) 0.8868(5) 0.4889(4) 0.0392(15) Uani 1 1 d U . . H63 H 1.0841 0.9142 0.5584 0.047 Uiso 1 1 calc R . . C64 C 1.0889(7) 0.7891(5) 0.4633(6) 0.055(2) Uani 1 1 d U . . H64A H 1.0556 0.7574 0.3954 0.083 Uiso 1 1 calc R . . H64B H 1.0445 0.7476 0.4888 0.083 Uiso 1 1 calc R . . H64C H 1.1894 0.8006 0.4895 0.083 Uiso 1 1 calc R . . C65 C 1.1290(6) 0.9628(5) 0.4620(4) 0.0365(15) Uani 1 1 d U . . C66 C 1.1470(7) 0.9388(5) 0.3751(5) 0.0436(16) Uani 1 1 d U . . H66 H 1.1184 0.8731 0.3344 0.052 Uiso 1 1 calc R . . C67 C 1.2069(7) 1.0110(6) 0.3476(5) 0.0561(19) Uani 1 1 d U . . H67 H 1.2149 0.9940 0.2883 0.067 Uiso 1 1 calc R . . C68 C 1.2535(8) 1.1064(6) 0.4086(6) 0.061(2) Uani 1 1 d U . . H68 H 1.2939 1.1547 0.3907 0.074 Uiso 1 1 calc R . . C69 C 1.2422(7) 1.1332(6) 0.4966(6) 0.062(2) Uani 1 1 d U . . H69 H 1.2754 1.1987 0.5380 0.074 Uiso 1 1 calc R . . C70 C 1.1798(7) 1.0601(5) 0.5229(5) 0.0482(18) Uani 1 1 d U . . H70 H 1.1728 1.0776 0.5824 0.058 Uiso 1 1 calc R . . C71 C 0.9803(6) 0.8437(5) 0.6968(4) 0.0366(15) Uani 1 1 d U . . H71 H 0.9491 0.7760 0.6631 0.044 Uiso 1 1 calc R . . C72 C 1.0874(6) 0.8791(5) 0.7846(4) 0.0388(15) Uani 1 1 d U . . H72 H 1.1259 0.8360 0.8097 0.047 Uiso 1 1 calc R . . C73 C 1.1356(7) 0.9778(5) 0.8341(5) 0.0457(18) Uani 1 1 d U . . H73 H 1.2078 1.0036 0.8936 0.055 Uiso 1 1 calc R . . C74 C 1.0760(7) 1.0391(5) 0.7946(4) 0.0446(16) Uani 1 1 d U . . H74 H 1.1081 1.1070 0.8271 0.054 Uiso 1 1 calc R . . C75 C 0.9677(6) 0.9991(5) 0.7061(4) 0.0341(14) Uani 1 1 d U . . C76 C 0.8935(6) 1.0589(4) 0.6627(4) 0.0320(14) Uani 1 1 d U . . H76 H 0.9205 1.1271 0.6932 0.038 Uiso 1 1 calc R . . C77 C 0.7056(6) 1.0772(4) 0.5431(4) 0.0338(14) Uani 1 1 d U . . H77 H 0.6065 1.0433 0.5263 0.041 Uiso 1 1 calc R . . C78 C 0.7326(8) 1.1807(5) 0.6121(5) 0.0481(18) Uani 1 1 d U . . H78A H 0.8262 1.2186 0.6257 0.072 Uiso 1 1 calc R . . H78B H 0.7238 1.1781 0.6699 0.072 Uiso 1 1 calc R . . H78C H 0.6650 1.2110 0.5844 0.072 Uiso 1 1 calc R . . C79 C 0.7212(6) 1.0807(4) 0.4527(4) 0.0341(14) Uani 1 1 d U . . C80 C 0.8500(7) 1.1029(5) 0.4455(5) 0.0465(17) Uani 1 1 d U . . H80 H 0.9306 1.1127 0.4969 0.056 Uiso 1 1 calc R . . C81 C 0.8646(9) 1.1114(6) 0.3640(5) 0.062(2) Uani 1 1 d U . . H81 H 0.9534 1.1258 0.3603 0.074 Uiso 1 1 calc R . . C82 C 0.7451(10) 1.0980(6) 0.2888(5) 0.069(2) Uani 1 1 d U . . H82 H 0.7527 1.1041 0.2337 0.083 Uiso 1 1 calc R . . C83 C 0.6153(9) 1.0756(6) 0.2947(5) 0.065(2) Uani 1 1 d U . . H83 H 0.5347 1.0657 0.2433 0.078 Uiso 1 1 calc R . . C84 C 0.6032(8) 1.0678(5) 0.3754(5) 0.0527(18) Uani 1 1 d U . . H84 H 0.5142 1.0535 0.3787 0.063 Uiso 1 1 calc R . . C1S C 0.2330(12) 0.0780(8) 0.1174(8) 0.103(3) Uani 1 1 d U . . H85A H 0.2590 0.0400 0.1559 0.154 Uiso 1 1 calc R . . H85B H 0.1481 0.0397 0.0635 0.154 Uiso 1 1 calc R . . H85C H 0.2173 0.1368 0.1543 0.154 Uiso 1 1 calc R . . C2S C 0.1457(14) 0.8058(8) 0.0264(14) 0.228(11) Uani 1 1 d U . . H86A H 0.1270 0.7919 -0.0398 0.341 Uiso 1 1 calc R . . H86B H 0.2433 0.8410 0.0626 0.341 Uiso 1 1 calc R . . H86C H 0.0873 0.8451 0.0466 0.341 Uiso 1 1 calc R . . C3S C 0.7686(16) 0.9083(11) 0.0351(11) 0.167(7) Uani 1 1 d U . . H87A H 0.7163 0.8400 0.0077 0.251 Uiso 1 1 calc R . . H87B H 0.8079 0.9240 -0.0081 0.251 Uiso 1 1 calc R . . H87C H 0.7068 0.9484 0.0469 0.251 Uiso 1 1 calc R . . Cl1 Cl 0.18791(16) 0.26663(12) 0.76520(11) 0.0434(4) Uani 1 1 d U . . Cl2 Cl 0.47910(16) 0.35939(11) 0.70092(10) 0.0377(4) Uani 1 1 d U . . Cl3 Cl 0.74364(14) 0.68548(10) 0.49050(10) 0.0298(3) Uani 1 1 d U . . Cl4 Cl 0.56470(15) 0.83005(10) 0.57844(10) 0.0313(3) Uani 1 1 d U . . Cl5 Cl 0.9371(2) 0.70093(15) 0.17126(14) 0.0695(5) Uani 1 1 d U . . Cl6 Cl 0.4553(3) 0.93192(18) 0.01297(18) 0.0869(7) Uani 1 1 d U . . 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 0.0330(4) 0.0268(4) 0.0279(4) 0.0105(3) 0.0086(3) 0.0100(3) Ni2 0.0245(4) 0.0269(4) 0.0282(4) 0.0096(3) 0.0099(3) 0.0061(3) Ni3 0.0255(4) 0.0270(4) 0.0278(4) 0.0109(3) 0.0091(3) 0.0070(3) N1 0.033(3) 0.026(3) 0.024(3) 0.008(2) 0.008(2) 0.012(2) N2 0.037(3) 0.026(3) 0.033(3) 0.009(2) 0.013(2) 0.012(2) N3 0.051(4) 0.033(3) 0.027(3) 0.009(3) 0.015(3) 0.016(3) N4 0.037(3) 0.034(3) 0.030(3) 0.014(3) 0.006(2) 0.005(2) N5 0.027(3) 0.026(3) 0.032(3) 0.013(2) 0.010(2) 0.009(2) N6 0.025(3) 0.027(3) 0.039(3) 0.012(2) 0.014(2) 0.009(2) N7 0.031(3) 0.030(3) 0.024(3) 0.004(2) 0.008(2) 0.000(2) N8 0.021(3) 0.028(3) 0.036(3) 0.013(2) 0.015(2) 0.008(2) N9 0.029(3) 0.024(3) 0.028(3) 0.009(2) 0.009(2) 0.006(2) N10 0.028(3) 0.033(3) 0.034(3) 0.014(2) 0.013(2) 0.010(2) N11 0.030(3) 0.030(3) 0.027(3) 0.011(2) 0.011(2) 0.008(2) N12 0.026(3) 0.030(3) 0.031(3) 0.010(2) 0.012(2) 0.005(2) O1S 0.099(5) 0.059(4) 0.084(4) 0.039(3) 0.043(4) 0.019(3) O2S 0.092(6) 0.239(12) 0.102(6) 0.016(7) 0.025(5) 0.035(6) O3S 0.288(19) 0.275(18) 0.161(11) 0.105(12) -0.021(11) -0.001(14) C1 0.041(4) 0.037(4) 0.034(3) 0.013(3) 0.011(3) 0.008(3) C2 0.059(5) 0.042(4) 0.047(4) 0.007(4) 0.025(4) 0.013(4) C3 0.068(5) 0.025(4) 0.056(4) 0.014(3) 0.033(4) 0.019(3) C4 0.049(4) 0.035(4) 0.049(4) 0.024(3) 0.019(3) 0.018(3) C5 0.025(3) 0.037(4) 0.034(3) 0.013(3) 0.006(3) 0.006(3) C6 0.037(4) 0.046(4) 0.029(3) 0.017(3) 0.010(3) 0.014(3) C7 0.046(4) 0.043(4) 0.035(3) 0.015(3) 0.019(3) 0.022(3) C8 0.035(4) 0.055(4) 0.038(4) 0.015(3) 0.013(3) 0.017(3) C9 0.035(4) 0.039(4) 0.032(3) 0.007(3) 0.019(3) 0.006(3) C10 0.061(5) 0.041(4) 0.046(4) 0.004(3) 0.034(4) 0.007(4) C11 0.056(5) 0.067(6) 0.052(5) -0.003(4) 0.030(4) -0.009(4) C12 0.035(4) 0.098(7) 0.036(4) 0.001(5) 0.010(3) 0.012(5) C13 0.041(4) 0.088(6) 0.043(4) 0.029(4) 0.022(4) 0.018(4) C14 0.040(4) 0.054(4) 0.032(3) 0.010(3) 0.020(3) 0.010(3) C15 0.059(5) 0.041(4) 0.036(4) 0.016(3) 0.017(3) 0.025(4) C16 0.078(6) 0.051(5) 0.058(5) 0.023(4) 0.021(4) 0.041(5) C17 0.109(7) 0.034(4) 0.048(5) 0.008(4) 0.022(5) 0.030(5) C18 0.080(6) 0.030(4) 0.038(4) -0.002(3) 0.015(4) 0.005(4) C19 0.053(4) 0.040(4) 0.024(3) 0.011(3) 0.010(3) 0.010(3) C20 0.044(4) 0.042(4) 0.029(3) 0.016(3) 0.006(3) 0.004(3) C21 0.034(4) 0.055(5) 0.038(4) 0.019(3) 0.005(3) 0.010(3) C22 0.044(5) 0.092(7) 0.089(6) 0.049(6) 0.017(4) 0.015(5) C23 0.025(3) 0.054(4) 0.036(4) 0.017(3) 0.003(3) 0.010(3) C24 0.040(4) 0.058(5) 0.036(4) 0.019(4) 0.004(3) 0.022(3) C25 0.050(5) 0.082(6) 0.040(4) 0.030(4) 0.012(3) 0.029(4) C26 0.057(5) 0.065(6) 0.064(5) 0.034(5) 0.010(4) 0.021(4) C27 0.060(5) 0.057(5) 0.077(6) 0.021(5) 0.019(5) 0.031(4) C28 0.053(5) 0.062(5) 0.044(4) 0.020(4) 0.020(4) 0.023(4) C29 0.036(4) 0.031(4) 0.033(3) 0.007(3) 0.012(3) 0.007(3) C30 0.061(5) 0.054(5) 0.033(4) 0.015(3) 0.019(3) 0.018(4) C31 0.050(5) 0.064(5) 0.036(4) 0.014(4) -0.001(4) 0.020(4) C32 0.030(4) 0.059(5) 0.047(4) 0.007(4) -0.001(3) 0.018(3) C33 0.033(4) 0.030(4) 0.042(4) 0.006(3) 0.009(3) 0.011(3) C34 0.029(4) 0.029(4) 0.049(4) 0.009(3) 0.014(3) 0.009(3) C35 0.037(4) 0.036(4) 0.041(4) 0.015(3) 0.020(3) 0.012(3) C36 0.067(5) 0.048(4) 0.057(4) 0.002(4) 0.043(4) -0.002(4) C37 0.028(3) 0.039(4) 0.050(4) 0.020(3) 0.020(3) 0.010(3) C38 0.026(3) 0.045(4) 0.042(4) 0.023(3) 0.011(3) 0.013(3) C39 0.047(5) 0.063(5) 0.072(5) 0.052(5) 0.015(4) 0.015(4) C40 0.030(4) 0.090(6) 0.100(6) 0.070(6) 0.016(4) 0.007(4) C41 0.033(4) 0.109(7) 0.119(7) 0.086(6) 0.040(4) 0.037(4) C42 0.046(4) 0.062(5) 0.088(5) 0.056(5) 0.041(4) 0.036(4) C43 0.053(4) 0.042(4) 0.041(4) 0.020(4) 0.020(3) 0.009(3) C44 0.074(6) 0.053(5) 0.024(4) 0.004(3) 0.010(4) -0.013(4) C45 0.090(6) 0.060(6) 0.035(4) 0.027(4) -0.008(4) -0.010(5) C46 0.067(5) 0.043(4) 0.039(4) 0.027(4) 0.003(4) -0.003(4) C47 0.027(3) 0.039(4) 0.037(4) 0.021(3) 0.010(3) 0.001(3) C48 0.028(3) 0.033(4) 0.039(3) 0.020(3) 0.014(3) 0.006(3) C49 0.033(3) 0.030(3) 0.033(3) 0.014(3) 0.012(3) 0.008(3) C50 0.037(4) 0.038(4) 0.044(4) 0.010(3) 0.015(3) 0.016(3) C51 0.028(3) 0.024(3) 0.036(3) 0.006(3) 0.010(3) 0.008(3) C52 0.030(4) 0.035(4) 0.036(3) 0.007(3) 0.009(3) 0.005(3) C53 0.030(4) 0.054(5) 0.053(4) 0.014(4) 0.014(3) 0.001(3) C54 0.032(4) 0.059(5) 0.062(5) 0.013(4) 0.005(4) 0.001(3) C55 0.049(5) 0.052(5) 0.040(4) 0.004(4) 0.000(4) -0.001(4) C56 0.041(4) 0.039(4) 0.039(4) 0.012(3) 0.016(3) 0.008(3) C57 0.033(4) 0.034(4) 0.039(4) 0.016(3) 0.012(3) 0.013(3) C58 0.035(4) 0.061(5) 0.043(4) 0.018(4) 0.006(3) 0.021(4) C59 0.053(5) 0.087(6) 0.030(4) 0.017(4) 0.000(4) 0.019(4) C60 0.046(5) 0.090(6) 0.031(4) 0.022(4) 0.014(3) 0.018(4) C61 0.030(3) 0.044(4) 0.033(3) 0.011(3) 0.009(3) 0.014(3) C62 0.043(4) 0.047(4) 0.038(4) 0.021(3) 0.018(3) 0.015(3) C63 0.032(4) 0.052(4) 0.040(4) 0.023(3) 0.016(3) 0.011(3) C64 0.045(4) 0.057(5) 0.093(6) 0.051(5) 0.037(4) 0.025(4) C65 0.033(4) 0.038(4) 0.046(4) 0.017(3) 0.021(3) 0.014(3) C66 0.040(4) 0.032(4) 0.051(4) 0.006(3) 0.019(3) 0.000(3) C67 0.049(5) 0.065(6) 0.056(5) 0.024(4) 0.028(4) 0.003(4) C68 0.043(5) 0.051(5) 0.084(6) 0.028(5) 0.020(4) -0.001(4) C69 0.035(4) 0.037(4) 0.079(6) 0.008(4) -0.004(4) -0.006(3) C70 0.028(4) 0.051(5) 0.046(4) 0.003(4) 0.002(3) 0.006(3) C71 0.033(4) 0.035(4) 0.037(3) 0.011(3) 0.012(3) 0.005(3) C72 0.038(4) 0.050(5) 0.037(4) 0.024(3) 0.013(3) 0.021(3) C73 0.030(4) 0.058(5) 0.038(4) 0.024(4) -0.005(3) 0.008(3) C74 0.040(4) 0.035(4) 0.041(4) 0.005(3) 0.007(3) 0.000(3) C75 0.029(3) 0.044(4) 0.030(3) 0.016(3) 0.013(3) 0.004(3) C76 0.036(4) 0.023(3) 0.035(3) 0.006(3) 0.016(3) 0.006(3) C77 0.028(3) 0.029(3) 0.045(4) 0.016(3) 0.012(3) 0.007(3) C78 0.055(5) 0.044(4) 0.054(4) 0.020(4) 0.025(4) 0.023(4) C79 0.035(4) 0.029(3) 0.041(4) 0.014(3) 0.013(3) 0.014(3) C80 0.042(4) 0.057(5) 0.055(4) 0.037(4) 0.020(3) 0.017(3) C81 0.064(5) 0.070(6) 0.067(5) 0.040(5) 0.034(4) 0.014(4) C82 0.093(7) 0.077(6) 0.055(5) 0.039(5) 0.032(5) 0.030(5) C83 0.064(6) 0.073(6) 0.058(5) 0.042(5) 0.007(4) 0.015(4) C84 0.049(5) 0.053(5) 0.056(4) 0.023(4) 0.013(4) 0.018(4) C1S 0.136(10) 0.089(8) 0.136(9) 0.070(7) 0.083(8) 0.051(7) C2S 0.112(11) 0.049(7) 0.38(2) 0.089(11) -0.099(12) -0.009(7) C3S 0.151(13) 0.148(13) 0.188(15) -0.012(12) 0.115(12) 0.046(11) Cl1 0.0337(9) 0.0429(10) 0.0497(9) 0.0226(8) 0.0061(7) 0.0077(7) Cl2 0.0416(9) 0.0378(9) 0.0341(8) 0.0163(7) 0.0122(7) 0.0095(7) Cl3 0.0278(8) 0.0276(8) 0.0349(8) 0.0110(7) 0.0136(7) 0.0074(6) Cl4 0.0330(9) 0.0281(8) 0.0356(8) 0.0099(7) 0.0179(7) 0.0094(7) Cl5 0.0707(14) 0.0598(13) 0.0646(12) 0.0175(11) 0.0142(10) 0.0145(10) Cl6 0.121(2) 0.0793(16) 0.1070(18) 0.0594(15) 0.0674(16) 0.0513(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 N1 2.055(5) . ? Ni1 N3 2.056(5) . ? Ni1 N2 2.109(5) . ? Ni1 N4 2.155(5) . ? Ni1 Cl2 2.4261(16) . ? Ni1 Cl1 2.4387(17) . ? Ni2 N5 2.083(5) . ? Ni2 N7 2.085(5) . ? Ni2 N6 2.110(5) . ? Ni2 N8 2.116(5) . ? Ni2 Cl3 2.4239(15) . ? Ni2 Cl4 2.4729(16) . ? Ni3 N9 2.078(5) . ? Ni3 N11 2.091(5) . ? Ni3 N10 2.109(4) . ? Ni3 N12 2.118(5) . ? Ni3 Cl4 2.4310(15) . ? Ni3 Cl3 2.4868(16) . ? N1 C1 1.329(7) . ? N1 C5 1.354(7) . ? N2 C6 1.267(8) . ? N2 C7 1.506(7) . ? N3 C15 1.342(8) . ? N3 C19 1.360(8) . ? N4 C20 1.253(8) . ? N4 C21 1.479(8) . ? N5 C29 1.333(7) . ? N5 C33 1.344(7) . ? N6 C34 1.259(7) . ? N6 C35 1.490(7) . ? N7 C43 1.333(8) . ? N7 C47 1.361(8) . ? N8 C48 1.294(7) . ? N8 C49 1.449(7) . ? N9 C57 1.328(7) . ? N9 C61 1.343(7) . ? N10 C62 1.281(7) . ? N10 C63 1.460(7) . ? N11 C71 1.326(7) . ? N11 C75 1.350(8) . ? N12 C76 1.267(7) . ? N12 C77 1.498(7) . ? O1S C1S 1.397(10) . ? O2S C2S 1.621(14) . ? O3S C3S 1.469(16) . ? C1 C2 1.367(9) . ? C2 C3 1.357(9) . ? C3 C4 1.380(9) . ? C4 C5 1.373(8) . ? C5 C6 1.455(8) . ? C7 C9 1.519(8) . ? C7 C8 1.519(9) . ? C9 C10 1.389(9) . ? C9 C14 1.391(9) . ? C10 C11 1.378(10) . ? C11 C12 1.379(11) . ? C12 C13 1.374(11) . ? C13 C14 1.391(9) . ? C15 C16 1.381(9) . ? C16 C17 1.369(12) . ? C17 C18 1.388(11) . ? C18 C19 1.356(9) . ? C19 C20 1.486(9) . ? C21 C23 1.502(9) . ? C21 C22 1.540(10) . ? C23 C28 1.377(9) . ? C23 C24 1.381(8) . ? C24 C25 1.386(10) . ? C25 C26 1.364(10) . ? C26 C27 1.389(10) . ? C27 C28 1.396(10) . ? C29 C30 1.392(8) . ? C30 C31 1.371(10) . ? C31 C32 1.382(9) . ? C32 C33 1.389(8) . ? C33 C34 1.470(9) . ? C35 C36 1.498(9) . ? C35 C37 1.521(9) . ? C37 C42 1.376(8) . ? C37 C38 1.392(9) . ? C38 C39 1.394(9) . ? C39 C40 1.346(9) . ? C40 C41 1.372(10) . ? C41 C42 1.377(10) . ? C43 C44 1.379(9) . ? C44 C45 1.375(11) . ? C45 C46 1.368(10) . ? C46 C47 1.382(8) . ? C47 C48 1.445(8) . ? C49 C51 1.516(8) . ? C49 C50 1.531(8) . ? C51 C56 1.378(8) . ? C51 C52 1.398(8) . ? C52 C53 1.380(9) . ? C53 C54 1.362(9) . ? C54 C55 1.388(10) . ? C55 C56 1.362(9) . ? C57 C58 1.380(8) . ? C58 C59 1.375(10) . ? C59 C60 1.370(10) . ? C60 C61 1.387(8) . ? C61 C62 1.457(8) . ? C63 C65 1.509(8) . ? C63 C64 1.519(9) . ? C65 C70 1.378(9) . ? C65 C66 1.395(8) . ? C66 C67 1.396(9) . ? C67 C68 1.358(10) . ? C68 C69 1.378(11) . ? C69 C70 1.404(10) . ? C71 C72 1.377(8) . ? C72 C73 1.357(9) . ? C73 C74 1.376(9) . ? C74 C75 1.387(8) . ? C75 C76 1.457(8) . ? C77 C79 1.507(8) . ? C77 C78 1.514(9) . ? C79 C80 1.364(9) . ? C79 C84 1.386(9) . ? C80 C81 1.387(9) . ? C81 C82 1.374(10) . ? C82 C83 1.366(11) . ? C83 C84 1.361(10) . ? 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 Ni1 N3 171.65(18) . . ? N1 Ni1 N2 79.07(18) . . ? N3 Ni1 N2 94.36(18) . . ? N1 Ni1 N4 96.23(19) . . ? N3 Ni1 N4 78.8(2) . . ? N2 Ni1 N4 93.04(18) . . ? N1 Ni1 Cl2 94.43(13) . . ? N3 Ni1 Cl2 91.79(14) . . ? N2 Ni1 Cl2 172.61(13) . . ? N4 Ni1 Cl2 84.13(13) . . ? N1 Ni1 Cl1 89.71(14) . . ? N3 Ni1 Cl1 95.05(16) . . ? N2 Ni1 Cl1 86.38(14) . . ? N4 Ni1 Cl1 173.82(15) . . ? Cl2 Ni1 Cl1 97.16(6) . . ? N5 Ni2 N7 171.13(19) . . ? N5 Ni2 N6 79.47(18) . . ? N7 Ni2 N6 94.00(19) . . ? N5 Ni2 N8 94.28(18) . . ? N7 Ni2 N8 79.77(19) . . ? N6 Ni2 N8 91.37(17) . . ? N5 Ni2 Cl3 91.53(13) . . ? N7 Ni2 Cl3 95.38(14) . . ? N6 Ni2 Cl3 170.06(13) . . ? N8 Ni2 Cl3 93.53(12) . . ? N5 Ni2 Cl4 95.05(13) . . ? N7 Ni2 Cl4 91.10(14) . . ? N6 Ni2 Cl4 91.53(13) . . ? N8 Ni2 Cl4 170.60(13) . . ? Cl3 Ni2 Cl4 85.01(5) . . ? N9 Ni3 N11 172.33(19) . . ? N9 Ni3 N10 80.02(18) . . ? N11 Ni3 N10 94.15(18) . . ? N9 Ni3 N12 96.48(18) . . ? N11 Ni3 N12 78.94(18) . . ? N10 Ni3 N12 94.77(18) . . ? N9 Ni3 Cl4 90.59(14) . . ? N11 Ni3 Cl4 95.75(13) . . ? N10 Ni3 Cl4 168.55(14) . . ? N12 Ni3 Cl4 92.77(13) . . ? N9 Ni3 Cl3 94.44(13) . . ? N11 Ni3 Cl3 90.47(14) . . ? N10 Ni3 Cl3 89.62(13) . . ? N12 Ni3 Cl3 168.78(13) . . ? Cl4 Ni3 Cl3 84.56(5) . . ? C1 N1 C5 118.0(5) . . ? C1 N1 Ni1 128.3(4) . . ? C5 N1 Ni1 113.7(4) . . ? C6 N2 C7 119.9(5) . . ? C6 N2 Ni1 112.8(4) . . ? C7 N2 Ni1 127.1(4) . . ? C15 N3 C19 117.1(6) . . ? C15 N3 Ni1 127.9(5) . . ? C19 N3 Ni1 115.0(4) . . ? C20 N4 C21 121.2(6) . . ? C20 N4 Ni1 111.8(4) . . ? C21 N4 Ni1 126.2(4) . . ? C29 N5 C33 118.8(5) . . ? C29 N5 Ni2 128.8(4) . . ? C33 N5 Ni2 112.4(4) . . ? C34 N6 C35 121.6(5) . . ? C34 N6 Ni2 112.5(4) . . ? C35 N6 Ni2 125.8(4) . . ? C43 N7 C47 118.5(5) . . ? C43 N7 Ni2 129.5(4) . . ? C47 N7 Ni2 112.0(4) . . ? C48 N8 C49 120.9(5) . . ? C48 N8 Ni2 111.8(4) . . ? C49 N8 Ni2 127.2(3) . . ? C57 N9 C61 117.7(5) . . ? C57 N9 Ni3 129.8(4) . . ? C61 N9 Ni3 112.4(4) . . ? C62 N10 C63 119.7(5) . . ? C62 N10 Ni3 111.0(4) . . ? C63 N10 Ni3 129.1(4) . . ? C71 N11 C75 117.6(5) . . ? C71 N11 Ni3 129.9(4) . . ? C75 N11 Ni3 112.4(4) . . ? C76 N12 C77 119.8(5) . . ? C76 N12 Ni3 112.8(4) . . ? C77 N12 Ni3 127.3(4) . . ? N1 C1 C2 122.1(6) . . ? C3 C2 C1 120.7(6) . . ? C2 C3 C4 117.9(6) . . ? C5 C4 C3 119.4(6) . . ? N1 C5 C4 121.9(5) . . ? N1 C5 C6 114.8(5) . . ? C4 C5 C6 123.3(6) . . ? N2 C6 C5 119.5(5) . . ? N2 C7 C9 110.6(5) . . ? N2 C7 C8 111.0(5) . . ? C9 C7 C8 115.3(5) . . ? C10 C9 C14 118.0(6) . . ? C10 C9 C7 120.4(6) . . ? C14 C9 C7 121.6(6) . . ? C11 C10 C9 121.4(7) . . ? C12 C11 C10 120.0(7) . . ? C13 C12 C11 119.8(7) . . ? C12 C13 C14 120.2(7) . . ? C13 C14 C9 120.6(7) . . ? N3 C15 C16 122.6(7) . . ? C17 C16 C15 119.5(7) . . ? C16 C17 C18 118.2(7) . . ? C19 C18 C17 119.6(7) . . ? C18 C19 N3 122.9(7) . . ? C18 C19 C20 123.4(7) . . ? N3 C19 C20 113.6(6) . . ? N4 C20 C19 120.8(6) . . ? N4 C21 C23 112.6(5) . . ? N4 C21 C22 115.0(6) . . ? C23 C21 C22 110.1(5) . . ? C28 C23 C24 119.3(6) . . ? C28 C23 C21 118.7(6) . . ? C24 C23 C21 122.0(6) . . ? C23 C24 C25 120.4(7) . . ? C26 C25 C24 121.0(7) . . ? C25 C26 C27 118.8(7) . . ? C26 C27 C28 120.6(7) . . ? C23 C28 C27 119.9(6) . . ? N5 C29 C30 121.4(6) . . ? C31 C30 C29 120.2(6) . . ? C30 C31 C32 118.2(6) . . ? C31 C32 C33 119.1(6) . . ? N5 C33 C32 122.1(6) . . ? N5 C33 C34 115.6(5) . . ? C32 C33 C34 122.3(6) . . ? N6 C34 C33 119.8(6) . . ? N6 C35 C36 108.9(5) . . ? N6 C35 C37 114.4(5) . . ? C36 C35 C37 113.3(5) . . ? C42 C37 C38 118.1(6) . . ? C42 C37 C35 122.5(6) . . ? C38 C37 C35 119.3(5) . . ? C37 C38 C39 120.3(6) . . ? C40 C39 C38 120.2(7) . . ? C39 C40 C41 120.3(7) . . ? C40 C41 C42 120.2(6) . . ? C41 C42 C37 120.8(7) . . ? N7 C43 C44 122.6(6) . . ? C45 C44 C43 119.0(7) . . ? C46 C45 C44 119.0(6) . . ? C45 C46 C47 120.0(7) . . ? N7 C47 C46 120.9(6) . . ? N7 C47 C48 116.5(5) . . ? C46 C47 C48 122.5(6) . . ? N8 C48 C47 119.6(5) . . ? N8 C49 C51 111.7(4) . . ? N8 C49 C50 115.6(5) . . ? C51 C49 C50 108.8(5) . . ? C56 C51 C52 118.9(5) . . ? C56 C51 C49 120.2(5) . . ? C52 C51 C49 120.8(5) . . ? C53 C52 C51 119.8(6) . . ? C54 C53 C52 120.4(6) . . ? C53 C54 C55 119.9(7) . . ? C56 C55 C54 120.0(6) . . ? C55 C56 C51 120.9(6) . . ? N9 C57 C58 123.1(6) . . ? C59 C58 C57 118.8(6) . . ? C60 C59 C58 119.1(6) . . ? C59 C60 C61 118.7(6) . . ? N9 C61 C60 122.5(6) . . ? N9 C61 C62 115.6(5) . . ? C60 C61 C62 122.0(6) . . ? N10 C62 C61 120.7(5) . . ? N10 C63 C65 113.1(5) . . ? N10 C63 C64 110.1(5) . . ? C65 C63 C64 114.5(5) . . ? C70 C65 C66 117.7(6) . . ? C70 C65 C63 120.1(6) . . ? C66 C65 C63 122.2(6) . . ? C67 C66 C65 121.7(6) . . ? C68 C67 C66 119.0(7) . . ? C67 C68 C69 121.4(7) . . ? C68 C69 C70 119.1(7) . . ? C65 C70 C69 121.1(7) . . ? N11 C71 C72 123.7(6) . . ? C73 C72 C71 118.9(6) . . ? C72 C73 C74 118.8(6) . . ? C73 C74 C75 119.7(6) . . ? N11 C75 C74 121.3(6) . . ? N11 C75 C76 116.0(5) . . ? C74 C75 C76 122.7(6) . . ? N12 C76 C75 119.6(5) . . ? N12 C77 C79 112.0(5) . . ? N12 C77 C78 114.4(5) . . ? C79 C77 C78 109.8(5) . . ? C80 C79 C84 117.7(6) . . ? C80 C79 C77 122.1(5) . . ? C84 C79 C77 120.0(6) . . ? C79 C80 C81 122.1(6) . . ? C82 C81 C80 118.6(7) . . ? C83 C82 C81 120.1(7) . . ? C84 C83 C82 120.4(7) . . ? C83 C84 C79 121.1(7) . . ? Ni2 Cl3 Ni3 95.08(5) . . ? Ni3 Cl4 Ni2 95.26(5) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.669 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.057 data_2R _database_code_depnum_ccdc_archive 'CCDC 756356' #TrackingRef 'Combined_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C192 H168 Fe4 N48 Ni6, C8 H20 N, F6 P, 31 (C H4 O), 10 (H2 O)' _chemical_formula_sum 'C231 H332 F6 Fe4 N49 Ni6 O41 P' _chemical_formula_weight 5164.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 3' _symmetry_space_group_name_Hall 'P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' _cell_length_a 19.567(5) _cell_length_b 19.567(5) _cell_length_c 35.123(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11646(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5418 _exptl_absorpt_coefficient_mu 0.665 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7321 _exptl_absorpt_correction_T_max 0.9675 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47213 _diffrn_reflns_av_R_equivalents 0.1452 _diffrn_reflns_av_sigmaI/netI 0.2183 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 23.29 _reflns_number_total 22157 _reflns_number_gt 10659 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Sum formula differs from actual formula as triethylamine H atoms have not been crystallographically assigned. Disordered solvent molecules have been removed from calculations using Squeeze. Large thermal parameters for some phenyl groups are due to strucural flexibilitya and resultant disordering. Restraints have been applied to ensure phenyl group shape is retained. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(2) _chemical_absolute_configuration rmad _refine_ls_number_reflns 22157 _refine_ls_number_parameters 1537 _refine_ls_number_restraints 172 _refine_ls_R_factor_all 0.1489 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.1976 _refine_ls_wR_factor_gt 0.1749 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.873 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni2 Ni 0.91763(8) 0.54977(8) 0.15151(4) 0.0406(4) Uani 1 1 d . . . Fe2 Fe 0.6667 0.3333 0.20883(7) 0.0324(6) Uani 1 3 d S . . Ni1 Ni 0.88307(10) 0.29865(10) -0.03657(4) 0.0647(5) Uani 1 1 d . . . Fe1 Fe 0.93897(10) 0.56755(10) 0.00792(5) 0.0541(5) Uani 1 1 d . . . C1 C 1.1532(7) 0.4241(7) -0.0201(3) 0.121(8) Uani 1 1 d G . . H1 H 1.1528 0.4579 -0.0008 0.145 Uiso 1 1 calc R . . C2 C 1.2037(6) 0.3936(9) -0.0171(3) 0.109(7) Uani 1 1 d G . . H2 H 1.2378 0.4066 0.0042 0.130 Uiso 1 1 calc R . . C3 C 1.2044(8) 0.3442(9) -0.0454(4) 0.186(12) Uani 1 1 d G . . H3 H 1.2389 0.3234 -0.0433 0.223 Uiso 1 1 calc R . . C4 C 1.1545(9) 0.3253(9) -0.0766(3) 0.159(11) Uani 1 1 d G . . H4 H 1.1549 0.2915 -0.0959 0.191 Uiso 1 1 calc R . . C5 C 1.1040(7) 0.3558(8) -0.0796(3) 0.134(8) Uani 1 1 d G . . H5 H 1.0699 0.3428 -0.1009 0.160 Uiso 1 1 calc R . . C6 C 1.1034(6) 0.4052(7) -0.0513(3) 0.089(5) Uani 1 1 d G . . C7 C 1.0538(9) 0.4439(10) -0.0592(5) 0.081(4) Uani 1 1 d . . . H7 H 1.0480 0.4641 -0.0339 0.098 Uiso 1 1 calc R . . C8 C 1.0966(10) 0.5149(11) -0.0835(6) 0.123(7) Uani 1 1 d . . . H8A H 1.0635 0.5387 -0.0877 0.184 Uiso 1 1 calc R . . H8B H 1.1090 0.4998 -0.1081 0.184 Uiso 1 1 calc R . . H8C H 1.1457 0.5531 -0.0709 0.184 Uiso 1 1 calc R . . C9 C 0.9486(11) 0.3922(12) -0.1047(7) 0.112(7) Uani 1 1 d . . . H9 H 0.9838 0.4297 -0.1226 0.135 Uiso 1 1 calc R . . N2 N 0.8206(6) 0.2906(6) -0.0857(2) 0.087(4) Uani 1 1 d G . . C10 C 0.8670(6) 0.3410(6) -0.1146(3) 0.110(7) Uani 1 1 d G . . C11 C 0.8339(9) 0.3384(8) -0.1499(3) 0.127(8) Uani 1 1 d G . . H11 H 0.8656 0.3728 -0.1697 0.152 Uiso 1 1 calc R . . C12 C 0.7544(10) 0.2855(9) -0.1564(3) 0.129(8) Uani 1 1 d G . . H12 H 0.7318 0.2837 -0.1806 0.154 Uiso 1 1 calc R . . C13 C 0.7080(6) 0.2351(8) -0.1275(4) 0.132(7) Uani 1 1 d G . . H13 H 0.6537 0.1989 -0.1319 0.158 Uiso 1 1 calc R . . C14 C 0.7411(6) 0.2377(6) -0.0921(3) 0.102(6) Uani 1 1 d G . . H14 H 0.7094 0.2032 -0.0723 0.123 Uiso 1 1 calc R . . C20 C 0.8931(18) 0.1571(13) -0.1128(7) 0.235(13) Uani 1 1 d GU . . C15 C 0.8554(12) 0.1666(16) -0.1442(10) 0.311(19) Uani 1 1 d GU . . H15 H 0.8033 0.1580 -0.1418 0.373 Uiso 1 1 calc R . . C16 C 0.894(2) 0.1889(16) -0.1791(8) 0.334(19) Uani 1 1 d GU . . H16 H 0.8681 0.1954 -0.2005 0.401 Uiso 1 1 calc R . . C17 C 0.970(2) 0.2015(15) -0.1826(6) 0.303(16) Uani 1 1 d GU . . H17 H 0.9965 0.2167 -0.2065 0.364 Uiso 1 1 calc R . . C18 C 1.0078(11) 0.1920(15) -0.1512(10) 0.318(17) Uani 1 1 d GU . . H18 H 1.0599 0.2006 -0.1537 0.382 Uiso 1 1 calc R . . C19 C 0.9693(18) 0.1697(13) -0.1163(7) 0.240(13) Uani 1 1 d GU . . H19 H 0.9951 0.1632 -0.0949 0.288 Uiso 1 1 calc R . . C21 C 0.8506(14) 0.1351(16) -0.0773(6) 0.139(8) Uani 1 1 d . . . H21 H 0.7988 0.1321 -0.0817 0.166 Uiso 1 1 calc R . . C22 C 0.8340(14) 0.0526(12) -0.0689(5) 0.147(9) Uani 1 1 d . . . H22A H 0.8129 0.0377 -0.0430 0.220 Uiso 1 1 calc R . . H22B H 0.8829 0.0507 -0.0710 0.220 Uiso 1 1 calc R . . H22C H 0.7953 0.0158 -0.0871 0.220 Uiso 1 1 calc R . . C23 C 0.9427(14) 0.1959(11) -0.0279(6) 0.135(8) Uani 1 1 d . . . H23 H 0.9556 0.1560 -0.0328 0.162 Uiso 1 1 calc R . . C24 C 0.9786(10) 0.2476(11) 0.0070(5) 0.100(6) Uani 1 1 d . . . C25 C 1.0282(9) 0.2424(10) 0.0305(4) 0.096(6) Uani 1 1 d . . . H25 H 1.0457 0.2056 0.0265 0.116 Uiso 1 1 calc R . . C26 C 1.0536(10) 0.2925(13) 0.0612(5) 0.105(6) Uani 1 1 d . . . H26 H 1.0848 0.2869 0.0803 0.126 Uiso 1 1 calc R . . C27 C 1.0340(8) 0.3513(10) 0.0646(4) 0.081(4) Uani 1 1 d . . . H27 H 1.0510 0.3864 0.0857 0.097 Uiso 1 1 calc R . . C28 C 0.9894(8) 0.3562(8) 0.0364(4) 0.061(3) Uani 1 1 d . . . H28 H 0.9800 0.3994 0.0369 0.074 Uiso 1 1 calc R . . C29 C 1.0010(6) 0.4678(4) 0.2509(2) 0.070(4) Uani 1 1 d G . . H29 H 0.9540 0.4179 0.2522 0.084 Uiso 1 1 calc R . . C30 C 1.0741(7) 0.4725(6) 0.2532(2) 0.072(4) Uani 1 1 d G . . H30 H 1.0772 0.4258 0.2560 0.087 Uiso 1 1 calc R . . C31 C 1.1429(5) 0.5455(7) 0.2513(2) 0.072(4) Uani 1 1 d G . . H31 H 1.1928 0.5487 0.2528 0.086 Uiso 1 1 calc R . . C32 C 1.1384(4) 0.6138(5) 0.2472(2) 0.079(5) Uani 1 1 d G . . H32 H 1.1854 0.6637 0.2459 0.095 Uiso 1 1 calc R . . C33 C 1.0653(5) 0.6091(4) 0.2449(2) 0.056(3) Uani 1 1 d G . . H33 H 1.0623 0.6558 0.2421 0.067 Uiso 1 1 calc R . . C34 C 0.9966(4) 0.5361(6) 0.2468(2) 0.056(3) Uani 1 1 d G . . C35 C 0.9173(7) 0.5247(8) 0.2421(3) 0.060(4) Uani 1 1 d . . . H35 H 0.8817 0.4681 0.2351 0.072 Uiso 1 1 calc R . . C36 C 0.8879(8) 0.5386(8) 0.2812(3) 0.070(4) Uani 1 1 d . . . H36A H 0.8355 0.5327 0.2781 0.106 Uiso 1 1 calc R . . H36B H 0.9248 0.5919 0.2904 0.106 Uiso 1 1 calc R . . H36C H 0.8850 0.4998 0.2998 0.106 Uiso 1 1 calc R . . C37 C 0.8993(6) 0.6306(7) 0.2152(3) 0.047(3) Uani 1 1 d . . . H37 H 0.8938 0.6451 0.2403 0.056 Uiso 1 1 calc R . . C38 C 0.8909(7) 0.6721(8) 0.1815(5) 0.064(4) Uani 1 1 d . . . C39 C 0.8764(6) 0.7341(8) 0.1861(5) 0.082(5) Uani 1 1 d . . . H39 H 0.8730 0.7529 0.2105 0.098 Uiso 1 1 calc R . . C40 C 0.8671(9) 0.7683(9) 0.1518(6) 0.096(6) Uani 1 1 d . . . H40 H 0.8599 0.8128 0.1530 0.115 Uiso 1 1 calc R . . C41 C 0.8685(8) 0.7368(8) 0.1176(4) 0.067(4) Uani 1 1 d . . . H41 H 0.8612 0.7579 0.0946 0.080 Uiso 1 1 calc R . . C42 C 0.8807(6) 0.6744(6) 0.1171(4) 0.043(3) Uani 1 1 d . . . H42 H 0.8804 0.6522 0.0930 0.052 Uiso 1 1 calc R . . C43 C 1.1523(5) 0.7639(5) 0.1865(3) 0.063(4) Uani 1 1 d G . . H43 H 1.1695 0.7264 0.1872 0.075 Uiso 1 1 calc R . . C44 C 1.1763(6) 0.8214(6) 0.2146(2) 0.110(6) Uani 1 1 d G . . H44 H 1.2100 0.8231 0.2345 0.132 Uiso 1 1 calc R . . C45 C 1.1510(7) 0.8763(5) 0.2136(3) 0.116(7) Uani 1 1 d G . . H45 H 1.1675 0.9156 0.2328 0.139 Uiso 1 1 calc R . . C46 C 1.1018(6) 0.8738(5) 0.1845(4) 0.084(5) Uani 1 1 d G . . H46 H 1.0845 0.9113 0.1838 0.101 Uiso 1 1 calc R . . C47 C 1.0777(5) 0.8163(6) 0.1564(3) 0.083(5) Uani 1 1 d G . . H47 H 1.0440 0.8146 0.1364 0.099 Uiso 1 1 calc R . . C48 C 1.1030(5) 0.7614(4) 0.1574(2) 0.055(3) Uani 1 1 d G . . C49 C 1.0814(7) 0.7009(7) 0.1249(4) 0.053(3) Uani 1 1 d . . . H49 H 1.0422 0.7064 0.1088 0.064 Uiso 1 1 calc R . . C50 C 1.1511(10) 0.7245(9) 0.0997(4) 0.092(5) Uani 1 1 d . . . H50A H 1.1360 0.6874 0.0784 0.137 Uiso 1 1 calc R . . H50B H 1.1933 0.7236 0.1143 0.137 Uiso 1 1 calc R . . H50C H 1.1697 0.7778 0.0899 0.137 Uiso 1 1 calc R . . C51 C 1.0754(6) 0.5839(6) 0.1427(3) 0.043(3) Uani 1 1 d . . . H51 H 1.1299 0.6095 0.1365 0.051 Uiso 1 1 calc R . . C52 C 1.0352(7) 0.5011(6) 0.1542(3) 0.039(3) Uani 1 1 d . . . C53 C 1.0702(7) 0.4548(7) 0.1578(3) 0.046(3) Uani 1 1 d . . . H53 H 1.1257 0.4783 0.1547 0.055 Uiso 1 1 calc R . . C54 C 1.0282(9) 0.3791(8) 0.1654(3) 0.057(3) Uani 1 1 d . . . H54 H 1.0535 0.3488 0.1686 0.069 Uiso 1 1 calc R . . C55 C 0.9487(10) 0.3442(8) 0.1685(3) 0.068(4) Uani 1 1 d . . . H55 H 0.9171 0.2889 0.1724 0.082 Uiso 1 1 calc R . . C56 C 0.9140(8) 0.3928(7) 0.1660(3) 0.053(3) Uani 1 1 d . . . H56 H 0.8588 0.3701 0.1699 0.063 Uiso 1 1 calc R . . C57 C 0.9599(8) 0.5886(7) -0.0463(4) 0.063(4) Uani 1 1 d . . . C58 C 0.8962(7) 0.4584(8) -0.0064(3) 0.048(3) Uani 1 1 d . . . C59 C 0.8424(8) 0.5637(8) -0.0020(3) 0.059(4) Uani 1 1 d . . . C60 C 0.9793(9) 0.6746(9) 0.0219(4) 0.072(4) Uani 1 1 d . . . C61 C 0.9182(6) 0.5455(6) 0.0616(4) 0.040(3) Uani 1 1 d . . . C62 C 1.0353(9) 0.5720(8) 0.0156(3) 0.061(4) Uani 1 1 d . . . C63 C 0.7514(7) 0.4167(7) 0.1787(3) 0.039(3) Uani 1 1 d . . . C64 C 0.7488(6) 0.3282(6) 0.2404(3) 0.042(3) Uani 1 1 d . . . N1 N 0.9743(7) 0.3868(8) -0.0707(3) 0.075(4) Uani 1 1 d . . . N3 N 0.8972(9) 0.2027(9) -0.0505(3) 0.098(5) Uani 1 1 d . . . N4 N 0.9568(6) 0.3025(7) 0.0070(3) 0.067(3) Uani 1 1 d . . . N5 N 0.9143(5) 0.5747(6) 0.2093(3) 0.051(3) Uani 1 1 d . . . N6 N 0.8934(5) 0.6413(5) 0.1482(3) 0.050(3) Uani 1 1 d . . . N7 N 1.0388(5) 0.6225(5) 0.1407(2) 0.038(2) Uani 1 1 d . . . N8 N 0.9567(6) 0.4689(5) 0.1582(2) 0.036(2) Uani 1 1 d . . . N9 N 0.9729(7) 0.6056(7) -0.0789(4) 0.081(4) Uani 1 1 d . . . N10 N 0.8798(6) 0.3944(6) -0.0170(3) 0.053(3) Uani 1 1 d . . . N11 N 0.7869(7) 0.5667(6) -0.0093(3) 0.071(3) Uani 1 1 d . . . N12 N 1.0074(7) 0.7399(7) 0.0333(3) 0.078(4) Uani 1 1 d . . . N13 N 0.9083(5) 0.5331(5) 0.0926(3) 0.043(2) Uani 1 1 d . . . N14 N 1.0969(8) 0.5757(7) 0.0226(3) 0.082(4) Uani 1 1 d . . . N15 N 0.8043(6) 0.4657(5) 0.1633(2) 0.039(2) Uani 1 1 d . . . N16 N 0.7940(6) 0.3214(6) 0.2583(3) 0.069(3) Uani 1 1 d . . . Ni4 Ni 0.21679(8) 0.25090(8) 0.42701(4) 0.0399(4) Uani 1 1 d . . . Fe4 Fe 0.0000 0.0000 0.36942(7) 0.0338(6) Uani 1 3 d S . . Ni3 Ni -0.03449(11) 0.21701(10) 0.61493(4) 0.0663(5) Uani 1 1 d . . . Fe3 Fe 0.23401(10) 0.27173(10) 0.57068(5) 0.0542(5) Uani 1 1 d . . . C70 C -0.1756(15) 0.2713(14) 0.6922(6) 0.254(13) Uani 1 1 d GDU . . C69 C -0.2317(16) 0.2950(19) 0.6904(8) 0.50(3) Uani 1 1 d GDU . . H69 H -0.2704 0.2752 0.6708 0.598 Uiso 1 1 calc R . . C68 C -0.231(2) 0.348(2) 0.7172(11) 0.58(3) Uani 1 1 d GDU . . H68 H -0.2695 0.3637 0.7159 0.694 Uiso 1 1 calc R . . C67 C -0.175(3) 0.3764(17) 0.7458(9) 0.57(3) Uani 1 1 d GU . . H67 H -0.1742 0.4123 0.7641 0.683 Uiso 1 1 calc R . . C66 C -0.118(2) 0.3528(18) 0.7477(8) 0.49(3) Uani 1 1 d GU . . H66 H -0.0797 0.3725 0.7672 0.593 Uiso 1 1 calc R . . C65 C -0.1189(15) 0.3002(18) 0.7209(9) 0.35(2) Uani 1 1 d GU . . H65 H -0.0806 0.2841 0.7221 0.417 Uiso 1 1 calc R . . C71 C -0.1775(16) 0.2093(18) 0.6662(8) 0.34(3) Uani 1 1 d D . . H71 H -0.1672 0.1714 0.6806 0.407 Uiso 1 1 calc R . . C72 C -0.261(2) 0.1671(11) 0.6490(6) 0.25(2) Uani 1 1 d . . . H72A H -0.2690 0.1216 0.6340 0.380 Uiso 1 1 calc R . . H72B H -0.2680 0.2038 0.6325 0.380 Uiso 1 1 calc R . . H72C H -0.3004 0.1492 0.6696 0.380 Uiso 1 1 calc R . . C73 C -0.1408(14) 0.2827(19) 0.6079(6) 0.186(14) Uani 1 1 d . . . H73 H -0.1770 0.2999 0.6142 0.223 Uiso 1 1 calc R . . C74 C -0.0968(15) 0.3063(16) 0.5762(10) 0.188(16) Uani 1 1 d . . . C75 C -0.0923(10) 0.3596(9) 0.5454(4) 0.089(5) Uani 1 1 d . . . H75 H -0.1311 0.3751 0.5459 0.106 Uiso 1 1 calc R . . C76 C -0.0433(15) 0.3871(13) 0.5183(6) 0.139(9) Uani 1 1 d . . . H76 H -0.0481 0.4198 0.4997 0.167 Uiso 1 1 calc R . . C77 C 0.0194(11) 0.3698(10) 0.5153(5) 0.097(5) Uani 1 1 d . . . H77 H 0.0572 0.3902 0.4953 0.116 Uiso 1 1 calc R . . C78 C 0.0212(8) 0.3227(9) 0.5428(4) 0.069(4) Uani 1 1 d . . . H78 H 0.0626 0.3107 0.5416 0.083 Uiso 1 1 calc R . . C79 C 0.0254(16) 0.4418(13) 0.6596(6) 0.159(10) Uani 1 1 d . . . H79 H 0.0179 0.4178 0.6839 0.191 Uiso 1 1 calc R . . C80 C -0.0098(15) 0.4866(17) 0.6490(9) 0.181(11) Uani 1 1 d . . . H80 H -0.0533 0.4793 0.6640 0.217 Uiso 1 1 calc R . . C81 C 0.011(2) 0.540(2) 0.6194(5) 0.207(17) Uani 1 1 d . . . H81 H -0.0083 0.5753 0.6159 0.248 Uiso 1 1 calc R . . C82 C 0.0581(15) 0.5354(10) 0.5987(7) 0.128(8) Uani 1 1 d . . . H82 H 0.0785 0.5731 0.5787 0.154 Uiso 1 1 calc R . . C83 C 0.0868(12) 0.4823(10) 0.5998(5) 0.113(6) Uani 1 1 d . . . H83 H 0.1163 0.4780 0.5795 0.135 Uiso 1 1 calc R . . C84 C 0.0693(11) 0.4360(11) 0.6329(4) 0.097(5) Uani 1 1 d . . . C85 C 0.1045(14) 0.3842(11) 0.6391(5) 0.114(7) Uani 1 1 d . . . H85 H 0.1211 0.3777 0.6130 0.137 Uiso 1 1 calc R . . C86 C 0.1867(12) 0.4299(12) 0.6627(5) 0.118(6) Uani 1 1 d . . . H86A H 0.2099 0.3958 0.6649 0.176 Uiso 1 1 calc R . . H86B H 0.1763 0.4429 0.6882 0.176 Uiso 1 1 calc R . . H86C H 0.2235 0.4785 0.6493 0.176 Uiso 1 1 calc R . . C87 C 0.0566(13) 0.2777(13) 0.6833(5) 0.109(7) Uani 1 1 d . . . H87 H 0.0948 0.3099 0.7017 0.130 Uiso 1 1 calc R . . C88 C 0.0041(11) 0.1970(12) 0.6917(5) 0.088(5) Uani 1 1 d . . . C89 C 0.0028(12) 0.1647(15) 0.7276(5) 0.113(7) Uani 1 1 d . . . H89 H 0.0355 0.1943 0.7483 0.136 Uiso 1 1 calc R . . C90 C -0.054(2) 0.0814(19) 0.7295(8) 0.171(13) Uani 1 1 d . . . H90 H -0.0558 0.0554 0.7527 0.205 Uiso 1 1 calc R . . C91 C -0.1001(14) 0.0400(14) 0.7040(7) 0.136(9) Uani 1 1 d . . . H91 H -0.1362 -0.0146 0.7076 0.164 Uiso 1 1 calc R . . C92 C -0.0965(10) 0.0758(11) 0.6720(5) 0.105(6) Uani 1 1 d . . . H92 H -0.1322 0.0454 0.6524 0.126 Uiso 1 1 calc R . . C93 C 0.4318(5) 0.4852(5) 0.3925(3) 0.077(4) Uani 1 1 d G . . H93 H 0.3939 0.5019 0.3922 0.093 Uiso 1 1 calc R . . C94 C 0.4876(7) 0.5085(6) 0.3636(3) 0.105(7) Uani 1 1 d G . . H94 H 0.4879 0.5412 0.3436 0.126 Uiso 1 1 calc R . . C95 C 0.5431(6) 0.4839(6) 0.3640(3) 0.122(8) Uani 1 1 d G . . H95 H 0.5813 0.4999 0.3443 0.146 Uiso 1 1 calc R . . C96 C 0.5428(5) 0.4361(6) 0.3934(3) 0.101(6) Uani 1 1 d G . . H96 H 0.5807 0.4193 0.3937 0.121 Uiso 1 1 calc R . . C97 C 0.4870(5) 0.4127(5) 0.4222(3) 0.074(4) Uani 1 1 d G . . H97 H 0.4867 0.3800 0.4423 0.089 Uiso 1 1 calc R . . C98 C 0.4315(5) 0.4373(5) 0.4218(2) 0.047(3) Uani 1 1 d G . . C99 C 0.3690(7) 0.4131(7) 0.4541(3) 0.047(3) Uani 1 1 d . . . H99 H 0.3728 0.3736 0.4707 0.057 Uiso 1 1 calc R . . C100 C 0.3906(6) 0.4861(8) 0.4779(3) 0.063(4) Uani 1 1 d . . . H10A H 0.3527 0.4721 0.4989 0.094 Uiso 1 1 calc R . . H10B H 0.3892 0.5264 0.4620 0.094 Uiso 1 1 calc R . . H10C H 0.4438 0.5068 0.4884 0.094 Uiso 1 1 calc R . . C101 C 0.2505(6) 0.4091(6) 0.4356(3) 0.037(3) Uani 1 1 d . . . H101 H 0.2766 0.4640 0.4411 0.045 Uiso 1 1 calc R . . C102 C 0.1687(7) 0.3699(7) 0.4254(3) 0.048(3) Uani 1 1 d . . . C103 C 0.1234(7) 0.4029(8) 0.4210(3) 0.049(3) Uani 1 1 d . . . H103 H 0.1478 0.4585 0.4239 0.058 Uiso 1 1 calc R . . C104 C 0.0436(7) 0.3617(8) 0.4127(3) 0.051(3) Uani 1 1 d . . . H104 H 0.0127 0.3865 0.4102 0.061 Uiso 1 1 calc R . . C105 C 0.0126(8) 0.2811(9) 0.4083(3) 0.064(4) Uani 1 1 d . . . H105 H -0.0421 0.2488 0.4031 0.076 Uiso 1 1 calc R . . C106 C 0.0588(7) 0.2469(7) 0.4114(3) 0.045(3) Uani 1 1 d . . . H106 H 0.0361 0.1918 0.4072 0.054 Uiso 1 1 calc R . . C107 C 0.1348(5) 0.3347(5) 0.3290(2) 0.063(4) Uani 1 1 d G . . H107 H 0.0850 0.2876 0.3278 0.075 Uiso 1 1 calc R . . C108 C 0.1393(5) 0.4077(7) 0.3260(2) 0.082(5) Uani 1 1 d G . . H108 H 0.0926 0.4105 0.3229 0.099 Uiso 1 1 calc R . . C109 C 0.2122(7) 0.4766(5) 0.3278(2) 0.071(4) Uani 1 1 d G . . H109 H 0.2153 0.5265 0.3258 0.085 Uiso 1 1 calc R . . C110 C 0.2806(5) 0.4724(5) 0.3324(2) 0.073(4) Uani 1 1 d G . . H110 H 0.3304 0.5195 0.3336 0.088 Uiso 1 1 calc R . . C111 C 0.2761(5) 0.3994(6) 0.3353(2) 0.067(4) Uani 1 1 d G . . H111 H 0.3228 0.3966 0.3385 0.080 Uiso 1 1 calc R . . C112 C 0.2032(6) 0.3306(4) 0.3336(2) 0.077(4) Uani 1 1 d G . . C113 C 0.1956(7) 0.2522(7) 0.3377(4) 0.059(4) Uani 1 1 d . . . H113 H 0.1398 0.2158 0.3456 0.070 Uiso 1 1 calc R . . C114 C 0.2065(9) 0.2200(8) 0.2978(3) 0.073(4) Uani 1 1 d . . . H11A H 0.1998 0.1673 0.3012 0.110 Uiso 1 1 calc R . . H11B H 0.2595 0.2557 0.2878 0.110 Uiso 1 1 calc R . . H11C H 0.1670 0.2171 0.2797 0.110 Uiso 1 1 calc R . . C115 C 0.2937(8) 0.2355(7) 0.3634(3) 0.055(4) Uani 1 1 d . . . H115 H 0.3057 0.2282 0.3380 0.066 Uiso 1 1 calc R . . C116 C 0.3399(8) 0.2253(7) 0.3962(4) 0.062(4) Uani 1 1 d . . . C117 C 0.4014(8) 0.2103(7) 0.3942(5) 0.076(5) Uani 1 1 d . . . H117 H 0.4200 0.2072 0.3697 0.091 Uiso 1 1 calc R . . C118 C 0.4369(8) 0.1998(8) 0.4247(6) 0.079(5) Uani 1 1 d . . . H118 H 0.4815 0.1928 0.4231 0.094 Uiso 1 1 calc R . . C119 C 0.4013(8) 0.2003(8) 0.4581(4) 0.071(4) Uani 1 1 d . . . H119 H 0.4199 0.1891 0.4809 0.085 Uiso 1 1 calc R . . C120 C 0.3403(6) 0.2160(6) 0.4608(4) 0.051(3) Uani 1 1 d . . . H120 H 0.3212 0.2194 0.4852 0.061 Uiso 1 1 calc R . . C121 C 0.2313(8) 0.1747(9) 0.5802(3) 0.063(4) Uani 1 1 d . . . C122 C 0.1264(8) 0.2309(8) 0.5858(3) 0.058(4) Uani 1 1 d . . . C123 C 0.2588(7) 0.2921(8) 0.6247(4) 0.065(4) Uani 1 1 d . . . C124 C 0.2087(6) 0.2493(6) 0.5156(4) 0.044(3) Uani 1 1 d . . . C125 C 0.3480(11) 0.3188(8) 0.5559(4) 0.072(4) Uani 1 1 d . . . C126 C 0.2424(7) 0.3733(10) 0.5621(3) 0.060(4) Uani 1 1 d . . . C127 C 0.0825(6) 0.0842(6) 0.4005(3) 0.042(3) Uani 1 1 d . . . C128 C -0.0791(6) -0.0852(7) 0.3379(4) 0.046(3) Uani 1 1 d . . . N17 N -0.1301(8) 0.2345(9) 0.6293(4) 0.098(4) Uani 1 1 d D . . N18 N -0.0297(8) 0.2915(6) 0.5713(3) 0.084(4) Uani 1 1 d . . . N19 N 0.0535(7) 0.3087(7) 0.6507(4) 0.075(3) Uani 1 1 d . . . N20 N -0.0452(7) 0.1538(8) 0.6647(3) 0.071(3) Uani 1 1 d . . . N21 N 0.2877(5) 0.3749(5) 0.4377(2) 0.040(2) Uani 1 1 d . . . N22 N 0.1354(5) 0.2899(5) 0.4204(2) 0.042(2) Uani 1 1 d . . . N23 N 0.2436(6) 0.2522(6) 0.3684(3) 0.048(3) Uani 1 1 d . . . N24 N 0.3075(6) 0.2267(5) 0.4293(3) 0.051(3) Uani 1 1 d . . . N25 N 0.2311(8) 0.1159(8) 0.5868(3) 0.077(4) Uani 1 1 d . . . N26 N 0.0624(7) 0.2116(6) 0.5942(3) 0.056(3) Uani 1 1 d . . . N27 N 0.2722(8) 0.3059(8) 0.6569(3) 0.092(4) Uani 1 1 d . . . N28 N 0.2005(5) 0.2420(5) 0.4839(3) 0.046(3) Uani 1 1 d . . . N29 N 0.4076(8) 0.3385(9) 0.5437(3) 0.097(5) Uani 1 1 d . . . N30 N 0.2435(8) 0.4355(8) 0.5560(4) 0.094(4) Uani 1 1 d . . . N31 N 0.1323(5) 0.1362(5) 0.4161(2) 0.038(2) Uani 1 1 d . . . N32 N -0.1241(6) -0.1362(7) 0.3205(4) 0.078(4) Uani 1 1 d . . . P1 P 0.3333 0.6667 0.4166(2) 0.083(2) Uani 1 3 d S . . F1 F 0.2838(7) 0.5898(6) 0.4405(4) 0.174(5) Uani 1 1 d . . . F2 F 0.3664(9) 0.6110(9) 0.3962(4) 0.201(6) Uani 1 1 d . . . P2 P 0.3333 0.6667 0.1621(2) 0.079(2) Uani 1 3 d S . . F3 F 0.2850(11) 0.6976(11) 0.1854(5) 0.278(10) Uani 1 1 d . . . F4 F 0.2588(6) 0.6233(7) 0.1352(3) 0.153(4) Uani 1 1 d . . . C130 C 0.7098(17) 0.3813(19) 0.0226(6) 0.055(9) Uani 0.33 1 d PDU A -1 C129 C 0.672(2) 0.3616(13) -0.0158(5) 0.021(7) Uani 0.33 1 d PDU A -1 C131 C 0.698(2) 0.3920(14) 0.0873(8) 0.107(9) Uani 0.50 1 d PDU A -2 C132 C 0.7138(13) 0.4196(9) 0.0558(7) 0.060(6) Uani 0.50 1 d PDU A -3 N33 N 0.6667 0.3333 0.0567(3) 0.027(3) Uani 1 3 d SDU . . C133 C 0.6865(11) 0.4616(10) 0.0813(5) 0.099(5) Uani 1 1 d DU . . C135 C -0.006(3) -0.0436(16) 0.5573(5) 0.067(9) Uani 0.33 1 d PDU B -4 C136 C 0.0558(15) 0.022(2) 0.4899(8) 0.122(10) Uani 0.50 1 d PDU B -5 C137 C 0.0857(9) 0.0434(16) 0.5252(8) 0.079(8) Uani 0.50 1 d PDU B -6 N34 N 0.0000 0.0000 0.5224(4) 0.037(3) Uani 1 3 d SDU . . C134 C 0.0000 0.0000 0.5927(8) 0.111(8) Uani 1 3 d SDU . . C138 C 0.1336(9) 0.0254(11) 0.4979(5) 0.105(5) Uani 1 1 d DU . . 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 Ni2 0.0404(9) 0.0324(8) 0.0415(8) 0.0007(7) 0.0002(7) 0.0127(7) Fe2 0.0289(9) 0.0289(9) 0.0393(15) 0.000 0.000 0.0145(5) Ni1 0.0632(12) 0.0741(12) 0.0581(10) -0.0128(9) 0.0015(9) 0.0354(10) Fe1 0.0535(12) 0.0537(12) 0.0502(11) 0.0079(9) 0.0159(9) 0.0231(10) C1 0.038(9) 0.19(2) 0.078(12) -0.037(12) -0.023(8) 0.011(11) C2 0.056(11) 0.18(2) 0.105(14) 0.015(13) -0.013(9) 0.074(13) C3 0.114(18) 0.19(3) 0.32(4) 0.02(3) -0.02(2) 0.13(2) C4 0.25(3) 0.33(3) 0.058(11) -0.030(14) -0.020(13) 0.27(3) C5 0.113(15) 0.22(2) 0.087(13) -0.045(14) -0.044(11) 0.101(17) C6 0.099(13) 0.088(12) 0.078(11) 0.008(9) 0.027(10) 0.047(11) C7 0.061(11) 0.100(13) 0.096(11) 0.004(10) 0.008(9) 0.050(10) C8 0.077(12) 0.104(15) 0.19(2) 0.044(14) 0.026(12) 0.047(11) C9 0.078(13) 0.119(16) 0.17(2) 0.009(14) 0.018(13) 0.076(13) N2 0.089(10) 0.080(9) 0.104(10) -0.046(8) -0.032(8) 0.050(8) C10 0.16(2) 0.170(19) 0.061(11) 0.041(12) 0.040(13) 0.133(18) C11 0.21(3) 0.20(2) 0.045(10) 0.002(12) 0.004(12) 0.15(2) C12 0.106(16) 0.136(18) 0.147(19) -0.027(15) -0.077(16) 0.063(15) C13 0.102(16) 0.151(19) 0.105(15) -0.012(14) -0.034(13) 0.035(14) C14 0.074(12) 0.095(13) 0.130(15) -0.011(11) -0.052(11) 0.035(11) C20 0.258(19) 0.22(2) 0.23(2) -0.034(16) 0.007(16) 0.120(17) C15 0.33(3) 0.33(3) 0.29(2) 0.041(18) 0.006(15) 0.176(18) C16 0.34(2) 0.35(3) 0.32(2) -0.019(18) 0.044(18) 0.185(19) C17 0.32(2) 0.32(3) 0.24(2) 0.004(17) 0.056(16) 0.142(18) C18 0.31(2) 0.34(3) 0.212(18) -0.034(17) 0.025(15) 0.095(17) C19 0.202(17) 0.23(2) 0.201(18) -0.022(16) 0.015(15) 0.044(15) C21 0.17(2) 0.19(2) 0.113(17) 0.007(17) 0.029(15) 0.13(2) C22 0.20(2) 0.098(16) 0.101(15) -0.015(12) 0.003(14) 0.042(15) C23 0.20(2) 0.133(17) 0.130(16) -0.086(14) -0.068(16) 0.131(17) C24 0.086(13) 0.093(13) 0.109(14) -0.047(11) 0.015(11) 0.035(11) C25 0.085(12) 0.128(15) 0.067(10) -0.005(10) -0.064(10) 0.047(11) C26 0.083(12) 0.145(17) 0.085(13) 0.053(13) -0.001(10) 0.054(13) C27 0.049(9) 0.089(12) 0.079(11) -0.017(9) -0.021(8) 0.016(9) C28 0.072(10) 0.049(8) 0.052(8) 0.012(7) 0.007(8) 0.022(7) C29 0.076(11) 0.084(12) 0.036(8) -0.005(7) -0.011(7) 0.030(9) C30 0.082(11) 0.083(12) 0.042(8) -0.009(7) -0.016(8) 0.034(10) C31 0.091(12) 0.114(13) 0.027(7) 0.020(8) 0.008(7) 0.064(12) C32 0.068(11) 0.130(14) 0.041(8) 0.018(8) -0.019(7) 0.049(10) C33 0.044(8) 0.047(8) 0.050(8) -0.001(6) -0.001(6) 0.003(7) C34 0.062(10) 0.068(9) 0.033(7) -0.028(6) -0.019(6) 0.029(8) C35 0.040(8) 0.056(8) 0.067(9) -0.009(7) 0.001(6) 0.011(7) C36 0.073(9) 0.094(11) 0.029(7) 0.002(7) 0.007(6) 0.031(8) C37 0.041(8) 0.036(7) 0.055(8) -0.010(6) 0.003(6) 0.013(6) C38 0.050(9) 0.041(8) 0.099(12) -0.004(8) 0.007(8) 0.020(7) C39 0.013(7) 0.050(9) 0.161(16) -0.032(10) 0.006(8) 0.000(6) C40 0.075(11) 0.062(11) 0.176(19) 0.037(12) 0.028(12) 0.053(9) C41 0.068(10) 0.066(10) 0.066(9) -0.006(8) 0.021(7) 0.032(8) C42 0.023(6) 0.031(7) 0.067(9) -0.004(6) 0.008(6) 0.006(5) C43 0.054(8) 0.059(9) 0.056(8) -0.033(7) -0.026(7) 0.014(7) C44 0.124(16) 0.069(12) 0.115(16) 0.005(11) -0.018(12) 0.031(12) C45 0.107(16) 0.106(16) 0.065(12) -0.027(10) 0.026(10) 0.000(12) C46 0.075(11) 0.026(8) 0.132(14) 0.028(9) 0.047(10) 0.010(8) C47 0.028(8) 0.043(9) 0.153(14) -0.019(9) 0.020(8) -0.001(7) C48 0.025(7) 0.024(7) 0.091(10) 0.004(6) 0.031(7) -0.006(6) C49 0.045(8) 0.041(8) 0.076(9) 0.001(7) 0.009(7) 0.024(7) C50 0.130(15) 0.098(12) 0.044(8) 0.008(8) 0.010(9) 0.056(11) C51 0.025(6) 0.032(7) 0.042(7) -0.011(5) -0.003(5) -0.007(6) C52 0.035(7) 0.036(7) 0.031(6) -0.010(5) -0.003(5) 0.006(6) C53 0.057(8) 0.044(8) 0.047(7) 0.006(6) -0.016(6) 0.032(7) C54 0.080(11) 0.058(10) 0.043(8) -0.008(7) -0.014(7) 0.041(9) C55 0.104(13) 0.043(8) 0.044(8) -0.011(6) -0.005(8) 0.027(9) C56 0.057(8) 0.046(9) 0.050(8) 0.017(6) 0.004(6) 0.022(8) C57 0.081(10) 0.049(8) 0.046(8) 0.000(7) 0.012(7) 0.022(7) C58 0.054(8) 0.057(9) 0.028(7) 0.018(6) 0.011(6) 0.025(7) C59 0.041(8) 0.080(10) 0.052(8) 0.031(7) 0.020(7) 0.027(8) C60 0.123(13) 0.051(9) 0.046(8) 0.026(7) 0.032(8) 0.046(10) C61 0.027(6) 0.031(7) 0.055(8) 0.029(6) 0.028(6) 0.010(5) C62 0.053(9) 0.079(10) 0.054(8) 0.009(7) 0.031(7) 0.034(8) C63 0.045(8) 0.029(7) 0.037(7) -0.022(6) -0.026(6) 0.015(6) C64 0.022(6) 0.029(7) 0.060(8) 0.003(6) 0.012(6) 0.002(5) N1 0.056(8) 0.124(11) 0.062(8) 0.011(7) 0.004(6) 0.057(8) N3 0.141(13) 0.146(13) 0.059(8) -0.043(8) -0.045(8) 0.111(11) N4 0.058(7) 0.069(8) 0.058(7) -0.003(6) 0.002(6) 0.019(7) N5 0.043(6) 0.047(6) 0.048(6) -0.003(5) 0.003(5) 0.013(5) N6 0.040(6) 0.037(6) 0.057(7) -0.008(5) -0.019(5) 0.008(5) N7 0.056(6) 0.034(6) 0.037(5) -0.001(4) -0.009(4) 0.032(5) N8 0.049(7) 0.033(6) 0.018(5) -0.010(4) -0.010(4) 0.013(5) N9 0.091(9) 0.089(9) 0.069(8) 0.008(7) 0.007(7) 0.050(8) N10 0.054(7) 0.036(6) 0.056(7) 0.002(5) -0.001(5) 0.013(5) N11 0.063(8) 0.045(7) 0.087(9) 0.021(6) 0.027(7) 0.013(6) N12 0.086(9) 0.045(8) 0.091(9) 0.016(7) 0.019(7) 0.023(7) N13 0.043(6) 0.028(5) 0.046(6) 0.021(5) 0.016(5) 0.009(5) N14 0.068(9) 0.075(8) 0.094(9) -0.034(7) 0.005(7) 0.029(7) N15 0.041(6) 0.027(5) 0.032(5) -0.002(4) -0.004(4) 0.002(5) N16 0.032(6) 0.074(8) 0.101(9) 0.035(6) -0.006(6) 0.026(6) Ni4 0.0298(8) 0.0372(9) 0.0437(9) -0.0009(7) -0.0028(7) 0.0099(7) Fe4 0.0319(9) 0.0319(9) 0.0376(15) 0.000 0.000 0.0160(5) Ni3 0.0771(13) 0.0639(12) 0.0593(11) -0.0044(9) 0.0137(9) 0.0363(10) Fe3 0.0567(12) 0.0548(12) 0.0485(11) -0.0160(9) -0.0051(9) 0.0260(10) C70 0.248(19) 0.28(2) 0.144(16) -0.039(15) 0.080(13) 0.060(15) C69 0.49(3) 0.52(3) 0.54(4) 0.017(19) -0.02(2) 0.29(2) C68 0.59(3) 0.57(3) 0.56(3) -0.028(19) -0.007(19) 0.28(2) C67 0.57(3) 0.59(4) 0.57(4) -0.01(2) -0.002(19) 0.30(2) C66 0.49(3) 0.51(3) 0.45(3) -0.050(19) 0.02(2) 0.23(2) C65 0.32(3) 0.37(3) 0.37(3) 0.025(18) -0.059(17) 0.185(19) C71 0.17(3) 0.34(5) 0.65(9) 0.13(5) 0.12(4) 0.23(4) C72 0.50(5) 0.065(14) 0.120(17) 0.004(12) 0.17(3) 0.09(2) C73 0.18(2) 0.34(4) 0.091(14) 0.14(2) 0.109(16) 0.18(3) C74 0.16(2) 0.17(2) 0.31(4) -0.19(3) -0.13(2) 0.14(2) C75 0.131(15) 0.099(12) 0.080(11) 0.059(10) 0.011(10) 0.091(12) C76 0.139(19) 0.17(2) 0.071(12) 0.053(13) -0.024(13) 0.050(17) C77 0.084(13) 0.100(13) 0.086(12) 0.039(10) 0.043(10) 0.031(11) C78 0.058(9) 0.093(11) 0.045(8) 0.021(8) 0.018(7) 0.028(8) C79 0.30(3) 0.19(2) 0.115(15) 0.047(14) 0.088(17) 0.22(2) C80 0.19(3) 0.23(3) 0.21(3) 0.02(2) 0.06(2) 0.17(2) C81 0.40(5) 0.24(3) 0.036(12) 0.019(15) 0.048(18) 0.20(4) C82 0.23(3) 0.044(10) 0.111(18) 0.004(11) -0.027(16) 0.066(14) C83 0.19(2) 0.071(12) 0.073(12) -0.030(10) -0.023(12) 0.062(13) C84 0.143(16) 0.125(15) 0.048(9) -0.033(10) -0.012(10) 0.085(13) C85 0.21(2) 0.079(13) 0.112(14) 0.011(11) 0.043(15) 0.115(16) C86 0.131(17) 0.130(16) 0.091(13) -0.037(11) -0.007(12) 0.065(14) C87 0.17(2) 0.139(19) 0.079(13) 0.014(12) 0.012(12) 0.129(18) C88 0.107(14) 0.096(14) 0.059(11) 0.015(11) 0.024(10) 0.049(12) C89 0.124(16) 0.19(2) 0.072(13) -0.007(14) -0.001(11) 0.111(18) C90 0.27(4) 0.15(3) 0.11(2) 0.087(19) 0.11(2) 0.12(3) C91 0.15(2) 0.084(16) 0.103(19) -0.002(15) 0.009(15) 0.008(14) C92 0.107(14) 0.071(13) 0.082(13) 0.008(10) 0.030(11) 0.002(11) C93 0.057(10) 0.042(8) 0.111(12) 0.009(8) -0.006(9) 0.008(7) C94 0.042(10) 0.172(19) 0.083(13) 0.007(11) -0.024(9) 0.041(12) C95 0.103(17) 0.068(12) 0.100(14) 0.012(10) -0.002(11) -0.028(11) C96 0.033(8) 0.074(11) 0.172(17) -0.067(12) 0.020(10) 0.009(8) C97 0.062(9) 0.080(11) 0.073(10) -0.026(8) 0.007(8) 0.030(9) C98 0.045(8) 0.043(8) 0.056(8) -0.011(6) 0.001(6) 0.024(6) C99 0.046(8) 0.043(7) 0.053(8) -0.004(6) -0.001(6) 0.022(6) C100 0.021(7) 0.084(10) 0.070(9) -0.019(8) 0.004(6) 0.017(7) C101 0.023(6) 0.034(7) 0.063(8) 0.002(5) -0.001(5) 0.021(6) C102 0.064(9) 0.047(8) 0.041(7) 0.004(6) 0.012(6) 0.033(7) C103 0.047(8) 0.083(9) 0.037(7) -0.010(6) -0.003(6) 0.048(8) C104 0.040(8) 0.061(9) 0.048(7) 0.017(6) 0.015(6) 0.023(7) C105 0.067(9) 0.088(12) 0.027(7) 0.009(7) -0.015(6) 0.032(9) C106 0.042(8) 0.052(8) 0.034(7) -0.003(6) -0.012(5) 0.019(7) C107 0.055(9) 0.068(10) 0.050(8) 0.008(7) 0.008(7) 0.019(8) C108 0.070(11) 0.101(13) 0.058(9) 0.039(9) 0.015(7) 0.029(10) C109 0.111(13) 0.059(10) 0.050(8) 0.003(7) -0.011(8) 0.047(10) C110 0.122(13) 0.073(11) 0.040(8) -0.008(7) -0.015(8) 0.060(10) C111 0.047(9) 0.044(8) 0.090(10) 0.000(7) 0.004(7) 0.007(7) C112 0.091(12) 0.112(14) 0.041(8) 0.022(8) 0.008(8) 0.061(11) C113 0.049(8) 0.042(8) 0.076(10) 0.026(7) 0.001(7) 0.017(6) C114 0.111(12) 0.064(9) 0.042(8) 0.015(7) 0.031(7) 0.041(9) C115 0.039(8) 0.056(9) 0.041(8) 0.016(6) 0.006(6) 0.003(7) C116 0.049(9) 0.047(8) 0.080(10) -0.004(7) 0.021(8) 0.016(7) C117 0.042(9) 0.051(9) 0.135(15) -0.018(9) 0.026(9) 0.022(7) C118 0.038(9) 0.049(9) 0.148(16) -0.008(10) 0.007(10) 0.021(7) C119 0.055(10) 0.058(9) 0.090(11) -0.028(8) -0.020(8) 0.020(8) C120 0.018(6) 0.022(6) 0.102(11) -0.001(6) 0.006(6) 0.003(5) C121 0.076(10) 0.079(11) 0.018(6) -0.016(7) -0.009(6) 0.027(9) C122 0.049(9) 0.082(10) 0.028(7) -0.024(6) -0.035(6) 0.022(8) C123 0.041(8) 0.088(10) 0.063(9) 0.013(8) -0.008(7) 0.031(8) C124 0.029(7) 0.034(7) 0.069(9) 0.003(6) -0.010(6) 0.014(6) C125 0.088(12) 0.060(10) 0.069(10) -0.021(8) -0.031(9) 0.039(10) C126 0.050(8) 0.085(11) 0.041(8) -0.026(7) -0.003(6) 0.031(8) C127 0.015(6) 0.021(6) 0.077(8) 0.006(6) 0.007(6) -0.002(5) C128 0.012(6) 0.042(8) 0.082(9) 0.007(7) 0.014(6) 0.013(6) N17 0.101(11) 0.120(12) 0.095(10) 0.021(9) 0.045(8) 0.073(10) N18 0.104(10) 0.057(8) 0.046(7) -0.011(6) -0.018(7) 0.006(7) N19 0.110(10) 0.050(8) 0.080(9) -0.018(7) 0.018(8) 0.051(8) N20 0.074(9) 0.093(10) 0.056(8) 0.006(7) 0.009(7) 0.049(8) N21 0.039(6) 0.031(5) 0.051(6) 0.000(4) 0.002(5) 0.018(5) N22 0.021(5) 0.039(6) 0.050(6) 0.017(5) 0.011(4) 0.002(5) N23 0.034(6) 0.048(6) 0.051(7) 0.006(5) -0.007(5) 0.011(5) N24 0.041(6) 0.038(6) 0.062(7) 0.009(5) 0.001(6) 0.012(5) N25 0.117(11) 0.074(9) 0.057(8) -0.023(6) -0.024(7) 0.060(8) N26 0.048(7) 0.043(6) 0.060(7) -0.007(5) -0.011(6) 0.010(6) N27 0.113(11) 0.106(10) 0.048(8) -0.034(7) -0.044(7) 0.047(9) N28 0.049(6) 0.046(6) 0.023(5) -0.004(5) -0.016(5) 0.009(5) N29 0.046(8) 0.166(15) 0.053(8) -0.034(8) -0.003(6) 0.033(9) N30 0.104(11) 0.062(9) 0.107(10) 0.010(8) 0.024(8) 0.034(8) N31 0.037(6) 0.026(5) 0.033(5) -0.003(4) -0.006(4) 0.002(5) N32 0.042(7) 0.043(7) 0.132(11) -0.013(7) -0.019(7) 0.008(6) P1 0.077(3) 0.077(3) 0.095(5) 0.000 0.000 0.0387(16) F1 0.149(10) 0.087(8) 0.238(14) 0.063(8) -0.007(9) 0.023(7) F2 0.216(15) 0.245(16) 0.181(12) -0.053(11) 0.031(11) 0.145(13) P2 0.074(3) 0.074(3) 0.089(5) 0.000 0.000 0.0368(15) F3 0.31(2) 0.28(2) 0.283(18) -0.059(17) 0.150(17) 0.175(17) F4 0.086(7) 0.163(11) 0.191(11) 0.008(8) -0.041(7) 0.049(7) C130 0.061(17) 0.064(17) 0.024(10) 0.014(11) -0.001(10) 0.019(12) C129 0.029(10) 0.019(12) 0.011(8) -0.004(7) 0.010(8) 0.008(9) C131 0.15(2) 0.079(13) 0.119(16) -0.066(11) -0.017(14) 0.077(14) C132 0.066(14) 0.041(8) 0.058(13) 0.017(10) 0.038(11) 0.015(9) N33 0.038(5) 0.038(5) 0.003(6) 0.000 0.000 0.019(2) C133 0.128(14) 0.100(12) 0.108(11) -0.033(9) -0.025(10) 0.086(11) C135 0.073(18) 0.051(16) 0.055(11) 0.024(9) -0.014(15) 0.015(15) C136 0.099(13) 0.15(2) 0.145(17) 0.041(16) 0.072(12) 0.082(16) C137 0.050(9) 0.095(16) 0.092(16) -0.057(13) -0.020(11) 0.036(11) N34 0.048(5) 0.048(5) 0.014(6) 0.000 0.000 0.024(3) C134 0.124(10) 0.124(10) 0.085(12) 0.000 0.000 0.062(5) C138 0.072(9) 0.123(12) 0.125(11) 0.010(9) 0.042(8) 0.054(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 Ni2 N15 2.037(10) . ? Ni2 N6 2.074(10) . ? Ni2 N8 2.086(9) . ? Ni2 N13 2.090(10) . ? Ni2 N5 2.096(9) . ? Ni2 N7 2.101(9) . ? Fe2 C63 1.955(13) 3_665 ? Fe2 C63 1.955(13) . ? Fe2 C63 1.955(13) 2_655 ? Fe2 C64 1.997(13) . ? Fe2 C64 1.997(13) 3_665 ? Fe2 C64 1.997(13) 2_655 ? Ni1 N10 2.026(11) . ? Ni1 N2 2.074(8) . ? Ni1 N4 2.078(11) . ? Ni1 N3 2.089(13) . ? Ni1 N11 2.102(14) 3_665 ? Ni1 N1 2.126(12) . ? Fe1 C62 1.863(15) . ? Fe1 C59 1.886(15) . ? Fe1 C60 1.896(16) . ? Fe1 C61 1.930(12) . ? Fe1 C58 1.931(14) . ? Fe1 C57 1.948(14) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C6 C7 1.524(16) . ? C7 N1 1.448(18) . ? C7 C8 1.48(2) . ? C9 N1 1.32(2) . ? C9 C10 1.44(2) . ? N2 C10 1.3900 . ? N2 C14 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C20 C15 1.3900 . ? C20 C19 1.3900 . ? C20 C21 1.44(2) . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C21 N3 1.50(3) . ? C21 C22 1.51(3) . ? C23 N3 1.248(19) . ? C23 C24 1.52(2) . ? C24 C25 1.32(2) . ? C24 N4 1.34(2) . ? C25 C26 1.37(2) . ? C26 C27 1.39(2) . ? C27 C28 1.354(18) . ? C28 N4 1.381(16) . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.462(14) . ? C35 N5 1.532(15) . ? C35 C36 1.564(16) . ? C37 N5 1.282(14) . ? C37 C38 1.490(17) . ? C38 N6 1.329(15) . ? C38 C39 1.386(18) . ? C39 C40 1.43(2) . ? C40 C41 1.36(2) . ? C41 C42 1.356(17) . ? C42 N6 1.354(14) . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.543(13) . ? C49 N7 1.443(13) . ? C49 C50 1.490(17) . ? C51 N7 1.277(13) . ? C51 C52 1.461(15) . ? C52 N8 1.344(13) . ? C52 C53 1.389(15) . ? C53 C54 1.311(16) . ? C54 C55 1.355(18) . ? C55 C56 1.421(18) . ? C56 N8 1.321(13) . ? C57 N9 1.185(14) . ? C58 N10 1.187(14) . ? C59 N11 1.145(14) . ? C60 N12 1.181(15) . ? C61 N13 1.111(11) . ? C62 N14 1.197(16) . ? C63 N15 1.136(12) . ? C64 N16 1.145(12) . ? N11 Ni1 2.102(14) 2_655 ? Ni4 N28 2.018(10) . ? Ni4 N31 2.051(9) . ? Ni4 N24 2.055(11) . ? Ni4 N22 2.095(9) . ? Ni4 N23 2.122(10) . ? Ni4 N21 2.142(9) . ? Fe4 C128 1.955(13) . ? Fe4 C128 1.955(13) 2 ? Fe4 C128 1.955(13) 3 ? Fe4 C127 1.963(12) 2 ? Fe4 C127 1.963(12) 3 ? Fe4 C127 1.963(12) . ? Ni3 N25 2.075(13) 2 ? Ni3 N26 2.083(12) . ? Ni3 N18 2.084(11) . ? Ni3 N20 2.090(11) . ? Ni3 N17 2.125(13) . ? Ni3 N19 2.161(12) . ? Fe3 C121 1.902(17) . ? Fe3 C122 1.917(15) . ? Fe3 C126 1.935(17) . ? Fe3 C123 1.951(15) . ? Fe3 C124 1.989(14) . ? Fe3 C125 2.010(19) . ? C70 C69 1.3900 . ? C70 C65 1.3900 . ? C70 C71 1.505(18) . ? C69 C68 1.3900 . ? C68 C67 1.3900 . ? C67 C66 1.3900 . ? C66 C65 1.3900 . ? C71 N17 1.525(19) . ? C71 C72 1.54(4) . ? C73 N17 1.30(2) . ? C73 C74 1.34(4) . ? C74 C75 1.47(4) . ? C74 N18 1.49(2) . ? C75 C76 1.26(2) . ? C76 C77 1.43(3) . ? C77 C78 1.35(2) . ? C78 N18 1.327(15) . ? C79 C84 1.31(2) . ? C79 C80 1.41(3) . ? C80 C81 1.38(3) . ? C81 C82 1.21(3) . ? C82 C83 1.41(2) . ? C83 C84 1.41(2) . ? C84 C85 1.50(2) . ? C85 N19 1.37(2) . ? C85 C86 1.62(2) . ? C87 N19 1.311(18) . ? C87 C88 1.42(2) . ? C88 N20 1.315(19) . ? C88 C89 1.41(2) . ? C89 C90 1.44(3) . ? C90 C91 1.24(3) . ? C91 C92 1.31(2) . ? C92 N20 1.367(19) . ? C93 C94 1.3900 . ? C93 C98 1.3900 . ? C94 C95 1.3900 . ? C95 C96 1.3900 . ? C96 C97 1.3900 . ? C97 C98 1.3900 . ? C98 C99 1.557(13) . ? C99 N21 1.493(14) . ? C99 C100 1.523(15) . ? C101 N21 1.212(12) . ? C101 C102 1.434(15) . ? C102 C103 1.342(15) . ? C102 N22 1.374(14) . ? C103 C104 1.383(15) . ? C104 C105 1.385(17) . ? C105 C106 1.373(17) . ? C106 N22 1.338(13) . ? C107 C108 1.3900 . ? C107 C112 1.3900 . ? C108 C109 1.3900 . ? C109 C110 1.3900 . ? C110 C111 1.3900 . ? C111 C112 1.3900 . ? C112 C113 1.471(13) . ? C113 N23 1.429(14) . ? C113 C114 1.597(17) . ? C115 N23 1.192(15) . ? C115 C116 1.537(18) . ? C116 N24 1.332(14) . ? C116 C117 1.374(18) . ? C117 C118 1.347(19) . ? C118 C119 1.368(18) . ? C119 C120 1.377(17) . ? C120 N24 1.347(14) . ? C121 N25 1.173(16) . ? C122 N26 1.150(14) . ? C123 N27 1.161(15) . ? C124 N28 1.124(12) . ? C125 N29 1.114(17) . ? C126 N30 1.226(16) . ? C127 N31 1.137(11) . ? C128 N32 1.125(13) . ? N25 Ni3 2.075(13) 3 ? P1 F1 1.564(11) 3_565 ? P1 F1 1.564(11) . ? P1 F1 1.564(11) 2_665 ? P1 F2 1.680(13) 3_565 ? P1 F2 1.680(13) 2_665 ? P1 F2 1.680(12) . ? P2 F4 1.582(11) . ? P2 F4 1.582(11) 3_565 ? P2 F4 1.582(11) 2_665 ? P2 F3 1.582(12) . ? P2 F3 1.582(12) 3_565 ? P2 F3 1.582(12) 2_665 ? C130 C129 1.493(18) . ? C130 N33 1.495(17) . ? C131 N33 1.466(16) . ? C131 C133 1.506(18) . ? C132 N33 1.465(15) . ? C132 C133 1.481(16) . ? N33 C132 1.465(15) 3_665 ? N33 C132 1.465(15) 2_655 ? N33 C131 1.466(16) 3_665 ? N33 C131 1.466(16) 2_655 ? N33 C130 1.495(17) 3_665 ? N33 C130 1.495(17) 2_655 ? C135 N34 1.463(5) . ? C135 C134 1.477(10) . ? C136 N34 1.485(17) . ? C136 C138 1.518(18) . ? C137 N34 1.456(16) . ? C137 C138 1.503(17) . ? N34 C137 1.456(16) 3 ? N34 C137 1.456(16) 2 ? N34 C135 1.463(5) 2 ? N34 C135 1.463(5) 3 ? N34 C136 1.485(17) 3 ? N34 C136 1.485(17) 2 ? C134 C135 1.477(10) 3 ? C134 C135 1.477(10) 2 ? 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 N15 Ni2 N6 94.7(4) . . ? N15 Ni2 N8 91.7(4) . . ? N6 Ni2 N8 172.1(4) . . ? N15 Ni2 N13 95.8(3) . . ? N6 Ni2 N13 92.2(4) . . ? N8 Ni2 N13 91.7(3) . . ? N15 Ni2 N5 80.9(3) . . ? N6 Ni2 N5 78.9(4) . . ? N8 Ni2 N5 97.6(4) . . ? N13 Ni2 N5 170.2(4) . . ? N15 Ni2 N7 171.1(4) . . ? N6 Ni2 N7 94.2(4) . . ? N8 Ni2 N7 79.4(3) . . ? N13 Ni2 N7 84.7(3) . . ? N5 Ni2 N7 100.0(3) . . ? C63 Fe2 C63 93.5(4) 3_665 . ? C63 Fe2 C63 93.5(4) 3_665 2_655 ? C63 Fe2 C63 93.5(4) . 2_655 ? C63 Fe2 C64 85.8(4) 3_665 . ? C63 Fe2 C64 88.5(4) . . ? C63 Fe2 C64 177.9(4) 2_655 . ? C63 Fe2 C64 88.5(4) 3_665 3_665 ? C63 Fe2 C64 177.9(4) . 3_665 ? C63 Fe2 C64 85.8(4) 2_655 3_665 ? C64 Fe2 C64 92.1(4) . 3_665 ? C63 Fe2 C64 177.9(4) 3_665 2_655 ? C63 Fe2 C64 85.8(4) . 2_655 ? C63 Fe2 C64 88.5(4) 2_655 2_655 ? C64 Fe2 C64 92.1(4) . 2_655 ? C64 Fe2 C64 92.1(4) 3_665 2_655 ? N10 Ni1 N2 93.6(4) . . ? N10 Ni1 N4 93.4(5) . . ? N2 Ni1 N4 170.8(4) . . ? N10 Ni1 N3 172.0(5) . . ? N2 Ni1 N3 94.3(4) . . ? N4 Ni1 N3 78.7(5) . . ? N10 Ni1 N11 96.9(4) . 3_665 ? N2 Ni1 N11 91.3(5) . 3_665 ? N4 Ni1 N11 93.8(4) . 3_665 ? N3 Ni1 N11 84.1(5) . 3_665 ? N10 Ni1 N1 81.0(4) . . ? N2 Ni1 N1 79.4(5) . . ? N4 Ni1 N1 95.8(4) . . ? N3 Ni1 N1 99.4(5) . . ? N11 Ni1 N1 170.3(5) 3_665 . ? C62 Fe1 C59 177.6(5) . . ? C62 Fe1 C60 93.4(6) . . ? C59 Fe1 C60 87.0(6) . . ? C62 Fe1 C61 88.0(5) . . ? C59 Fe1 C61 94.4(5) . . ? C60 Fe1 C61 85.3(5) . . ? C62 Fe1 C58 87.6(5) . . ? C59 Fe1 C58 92.1(6) . . ? C60 Fe1 C58 179.0(6) . . ? C61 Fe1 C58 94.6(4) . . ? C62 Fe1 C57 91.8(6) . . ? C59 Fe1 C57 85.9(6) . . ? C60 Fe1 C57 95.3(5) . . ? C61 Fe1 C57 179.3(5) . . ? C58 Fe1 C57 84.7(5) . . ? C2 C1 C6 120.0 . . ? C1 C2 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 C7 116.4(11) . . ? C1 C6 C7 123.1(11) . . ? N1 C7 C8 116.6(14) . . ? N1 C7 C6 111.9(13) . . ? C8 C7 C6 111.6(12) . . ? N1 C9 C10 119.7(17) . . ? C10 N2 C14 120.0 . . ? C10 N2 Ni1 113.7(7) . . ? C14 N2 Ni1 126.1(7) . . ? N2 C10 C11 120.0 . . ? N2 C10 C9 115.0(12) . . ? C11 C10 C9 125.0(12) . . ? C10 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C13 C14 N2 120.0 . . ? C15 C20 C19 120.0 . . ? C15 C20 C21 117(3) . . ? C19 C20 C21 122(3) . . ? C20 C15 C16 120.0 . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C19 120.0 . . ? C18 C19 C20 120.0 . . ? C20 C21 N3 106(2) . . ? C20 C21 C22 105.9(19) . . ? N3 C21 C22 122.0(17) . . ? N3 C23 C24 124.0(17) . . ? C25 C24 N4 127.2(16) . . ? C25 C24 C23 124.6(18) . . ? N4 C24 C23 107.9(17) . . ? C24 C25 C26 117.1(18) . . ? C25 C26 C27 120.6(15) . . ? C28 C27 C26 116.8(15) . . ? C27 C28 N4 124.1(13) . . ? C30 C29 C34 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C29 120.0 . . ? C33 C34 C35 124.0(8) . . ? C29 C34 C35 115.8(8) . . ? C34 C35 N5 111.3(9) . . ? C34 C35 C36 109.2(9) . . ? N5 C35 C36 114.5(11) . . ? N5 C37 C38 118.2(11) . . ? N6 C38 C39 124.6(15) . . ? N6 C38 C37 114.4(11) . . ? C39 C38 C37 120.9(15) . . ? C38 C39 C40 116.2(15) . . ? C41 C40 C39 119.6(14) . . ? C42 C41 C40 118.4(14) . . ? N6 C42 C41 125.1(12) . . ? C44 C43 C48 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 C49 120.5(8) . . ? C43 C48 C49 119.4(8) . . ? N7 C49 C50 120.7(10) . . ? N7 C49 C48 108.7(9) . . ? C50 C49 C48 110.1(10) . . ? N7 C51 C52 121.4(10) . . ? N8 C52 C53 120.4(10) . . ? N8 C52 C51 113.8(11) . . ? C53 C52 C51 125.5(11) . . ? C54 C53 C52 121.2(12) . . ? C53 C54 C55 120.0(13) . . ? C54 C55 C56 117.9(13) . . ? N8 C56 C55 121.6(12) . . ? N9 C57 Fe1 176.1(12) . . ? N10 C58 Fe1 171.1(11) . . ? N11 C59 Fe1 174.9(12) . . ? N12 C60 Fe1 174.1(13) . . ? N13 C61 Fe1 178.0(10) . . ? N14 C62 Fe1 176.4(11) . . ? N15 C63 Fe2 175.0(9) . . ? N16 C64 Fe2 176.7(10) . . ? C9 N1 C7 119.8(14) . . ? C9 N1 Ni1 112.1(12) . . ? C7 N1 Ni1 127.6(10) . . ? C23 N3 C21 117.1(15) . . ? C23 N3 Ni1 111.6(11) . . ? C21 N3 Ni1 130.0(12) . . ? C24 N4 C28 113.5(12) . . ? C24 N4 Ni1 117.7(11) . . ? C28 N4 Ni1 128.8(10) . . ? C37 N5 C35 121.4(10) . . ? C37 N5 Ni2 113.6(8) . . ? C35 N5 Ni2 124.4(8) . . ? C38 N6 C42 116.0(11) . . ? C38 N6 Ni2 114.7(9) . . ? C42 N6 Ni2 129.3(8) . . ? C51 N7 C49 116.9(10) . . ? C51 N7 Ni2 111.5(7) . . ? C49 N7 Ni2 130.3(7) . . ? C56 N8 C52 118.6(10) . . ? C56 N8 Ni2 127.8(9) . . ? C52 N8 Ni2 113.6(7) . . ? C58 N10 Ni1 164.8(10) . . ? C59 N11 Ni1 164.6(11) . 2_655 ? C61 N13 Ni2 160.9(9) . . ? C63 N15 Ni2 160.6(9) . . ? N28 Ni4 N31 94.9(3) . . ? N28 Ni4 N24 93.4(4) . . ? N31 Ni4 N24 94.1(4) . . ? N28 Ni4 N22 91.4(4) . . ? N31 Ni4 N22 91.9(4) . . ? N24 Ni4 N22 171.9(4) . . ? N28 Ni4 N23 171.8(4) . . ? N31 Ni4 N23 83.7(3) . . ? N24 Ni4 N23 78.7(4) . . ? N22 Ni4 N23 96.7(4) . . ? N28 Ni4 N21 84.8(3) . . ? N31 Ni4 N21 169.6(4) . . ? N24 Ni4 N21 96.2(4) . . ? N22 Ni4 N21 77.7(4) . . ? N23 Ni4 N21 98.0(3) . . ? C128 Fe4 C128 91.1(5) . 2 ? C128 Fe4 C128 91.1(5) . 3 ? C128 Fe4 C128 91.1(5) 2 3 ? C128 Fe4 C127 90.0(4) . 2 ? C128 Fe4 C127 177.6(4) 2 2 ? C128 Fe4 C127 86.8(4) 3 2 ? C128 Fe4 C127 86.8(5) . 3 ? C128 Fe4 C127 90.0(4) 2 3 ? C128 Fe4 C127 177.6(4) 3 3 ? C127 Fe4 C127 92.1(4) 2 3 ? C128 Fe4 C127 177.6(4) . . ? C128 Fe4 C127 86.8(5) 2 . ? C128 Fe4 C127 90.0(4) 3 . ? C127 Fe4 C127 92.1(4) 2 . ? C127 Fe4 C127 92.1(4) 3 . ? N25 Ni3 N26 93.8(4) 2 . ? N25 Ni3 N18 93.8(4) 2 . ? N26 Ni3 N18 93.1(5) . . ? N25 Ni3 N20 91.6(5) 2 . ? N26 Ni3 N20 95.0(4) . . ? N18 Ni3 N20 169.9(5) . . ? N25 Ni3 N17 87.3(5) 2 . ? N26 Ni3 N17 171.4(5) . . ? N18 Ni3 N17 78.3(6) . . ? N20 Ni3 N17 93.5(5) . . ? N25 Ni3 N19 169.6(5) 2 . ? N26 Ni3 N19 83.0(4) . . ? N18 Ni3 N19 96.2(5) . . ? N20 Ni3 N19 78.9(5) . . ? N17 Ni3 N19 97.4(5) . . ? C121 Fe3 C122 93.4(6) . . ? C121 Fe3 C126 176.9(6) . . ? C122 Fe3 C126 89.0(6) . . ? C121 Fe3 C123 85.0(5) . . ? C122 Fe3 C123 85.6(5) . . ? C126 Fe3 C123 93.3(5) . . ? C121 Fe3 C124 94.0(4) . . ? C122 Fe3 C124 94.5(4) . . ? C126 Fe3 C124 87.7(4) . . ? C123 Fe3 C124 179.0(5) . . ? C121 Fe3 C125 88.5(6) . . ? C122 Fe3 C125 177.6(6) . . ? C126 Fe3 C125 89.1(5) . . ? C123 Fe3 C125 93.0(5) . . ? C124 Fe3 C125 86.9(5) . . ? C69 C70 C65 120.0 . . ? C69 C70 C71 122(2) . . ? C65 C70 C71 118(2) . . ? C68 C69 C70 120.0 . . ? C69 C68 C67 120.0 . . ? C66 C67 C68 120.0 . . ? C65 C66 C67 120.0 . . ? C66 C65 C70 120.0 . . ? C70 C71 N17 119(2) . . ? C70 C71 C72 105.1(14) . . ? N17 C71 C72 98.8(19) . . ? N17 C73 C74 115(2) . . ? C73 C74 C75 130.8(19) . . ? C73 C74 N18 120(3) . . ? C75 C74 N18 108(3) . . ? C76 C75 C74 128(2) . . ? C75 C76 C77 120.8(17) . . ? C78 C77 C76 115.3(14) . . ? N18 C78 C77 125.9(15) . . ? C84 C79 C80 114.2(19) . . ? C81 C80 C79 128(2) . . ? C82 C81 C80 110(3) . . ? C81 C82 C83 129(3) . . ? C84 C83 C82 116.2(18) . . ? C79 C84 C83 119.4(18) . . ? C79 C84 C85 119.8(17) . . ? C83 C84 C85 120.6(16) . . ? N19 C85 C84 116.1(18) . . ? N19 C85 C86 115.4(15) . . ? C84 C85 C86 111.5(15) . . ? N19 C87 C88 121.4(19) . . ? N20 C88 C89 121.0(18) . . ? N20 C88 C87 117.2(16) . . ? C89 C88 C87 122(2) . . ? C88 C89 C90 112.3(19) . . ? C91 C90 C89 127(2) . . ? C90 C91 C92 116(2) . . ? C91 C92 N20 125.0(18) . . ? C94 C93 C98 120.0 . . ? C93 C94 C95 120.0 . . ? C94 C95 C96 120.0 . . ? C97 C96 C95 120.0 . . ? C98 C97 C96 120.0 . . ? C97 C98 C93 120.0 . . ? C97 C98 C99 121.1(8) . . ? C93 C98 C99 118.9(8) . . ? N21 C99 C100 114.1(9) . . ? N21 C99 C98 110.4(8) . . ? C100 C99 C98 107.9(9) . . ? N21 C101 C102 122.6(11) . . ? C103 C102 N22 119.0(12) . . ? C103 C102 C101 127.0(12) . . ? N22 C102 C101 114.1(10) . . ? C102 C103 C104 124.6(13) . . ? C103 C104 C105 114.3(12) . . ? C106 C105 C104 121.7(13) . . ? N22 C106 C105 121.0(12) . . ? C108 C107 C112 120.0 . . ? C109 C108 C107 120.0 . . ? C108 C109 C110 120.0 . . ? C111 C110 C109 120.0 . . ? C110 C111 C112 120.0 . . ? C111 C112 C107 120.0 . . ? C111 C112 C113 121.7(8) . . ? C107 C112 C113 118.3(8) . . ? N23 C113 C112 110.5(10) . . ? N23 C113 C114 116.4(11) . . ? C112 C113 C114 111.2(9) . . ? N23 C115 C116 122.8(12) . . ? N24 C116 C117 121.7(14) . . ? N24 C116 C115 109.6(11) . . ? C117 C116 C115 128.6(14) . . ? C118 C117 C116 124.5(15) . . ? C117 C118 C119 112.2(14) . . ? C118 C119 C120 124.1(15) . . ? N24 C120 C119 120.9(13) . . ? N25 C121 Fe3 178.2(12) . . ? N26 C122 Fe3 175.1(13) . . ? N27 C123 Fe3 177.4(13) . . ? N28 C124 Fe3 174.1(10) . . ? N29 C125 Fe3 170.8(13) . . ? N30 C126 Fe3 176.4(12) . . ? N31 C127 Fe4 175.0(10) . . ? N32 C128 Fe4 177.4(12) . . ? C73 N17 C71 115.6(16) . . ? C73 N17 Ni3 117.0(13) . . ? C71 N17 Ni3 126.3(12) . . ? C78 N18 C74 122(2) . . ? C78 N18 Ni3 129.7(12) . . ? C74 N18 Ni3 108.4(17) . . ? C87 N19 C85 125.6(17) . . ? C87 N19 Ni3 109.0(12) . . ? C85 N19 Ni3 124.8(12) . . ? C88 N20 C92 118.3(14) . . ? C88 N20 Ni3 113.5(11) . . ? C92 N20 Ni3 128.2(12) . . ? C101 N21 C99 122.0(10) . . ? C101 N21 Ni4 112.7(8) . . ? C99 N21 Ni4 124.0(7) . . ? C106 N22 C102 119.3(10) . . ? C106 N22 Ni4 127.8(8) . . ? C102 N22 Ni4 112.8(7) . . ? C115 N23 C113 121.3(11) . . ? C115 N23 Ni4 111.9(9) . . ? C113 N23 Ni4 124.9(9) . . ? C116 N24 C120 116.4(11) . . ? C116 N24 Ni4 116.5(9) . . ? C120 N24 Ni4 127.0(8) . . ? C121 N25 Ni3 160.2(11) . 3 ? C122 N26 Ni3 160.2(10) . . ? C124 N28 Ni4 164.6(9) . . ? C127 N31 Ni4 158.5(9) . . ? F1 P1 F1 93.9(8) 3_565 . ? F1 P1 F1 93.9(8) 3_565 2_665 ? F1 P1 F1 93.9(8) . 2_665 ? F1 P1 F2 81.9(8) 3_565 3_565 ? F1 P1 F2 80.5(7) . 3_565 ? F1 P1 F2 172.8(9) 2_665 3_565 ? F1 P1 F2 80.5(7) 3_565 2_665 ? F1 P1 F2 172.8(9) . 2_665 ? F1 P1 F2 81.9(8) 2_665 2_665 ? F2 P1 F2 103.1(7) 3_565 2_665 ? F1 P1 F2 172.8(9) 3_565 . ? F1 P1 F2 81.9(8) . . ? F1 P1 F2 80.5(7) 2_665 . ? F2 P1 F2 103.1(7) 3_565 . ? F2 P1 F2 103.1(7) 2_665 . ? F4 P2 F4 88.0(7) . 3_565 ? F4 P2 F4 88.0(7) . 2_665 ? F4 P2 F4 88.0(7) 3_565 2_665 ? F4 P2 F3 86.9(9) . . ? F4 P2 F3 89.1(9) 3_565 . ? F4 P2 F3 174.3(10) 2_665 . ? F4 P2 F3 174.3(10) . 3_565 ? F4 P2 F3 86.9(9) 3_565 3_565 ? F4 P2 F3 89.1(9) 2_665 3_565 ? F3 P2 F3 95.6(11) . 3_565 ? F4 P2 F3 89.1(9) . 2_665 ? F4 P2 F3 174.3(10) 3_565 2_665 ? F4 P2 F3 86.9(9) 2_665 2_665 ? F3 P2 F3 95.6(11) . 2_665 ? F3 P2 F3 95.6(11) 3_565 2_665 ? C129 C130 N33 121(2) . . ? N33 C131 C133 114.1(16) . . ? N33 C132 C133 115.6(14) . . ? C132 N33 C132 119.96(8) 3_665 . ? C132 N33 C132 119.96(8) 3_665 2_655 ? C132 N33 C132 119.96(8) . 2_655 ? C132 N33 C131 48.4(14) 3_665 3_665 ? C132 N33 C131 111(2) . 3_665 ? C132 N33 C131 111.0(12) 2_655 3_665 ? C132 N33 C131 111.0(12) 3_665 . ? C132 N33 C131 48.4(14) . . ? C132 N33 C131 111(2) 2_655 . ? C131 N33 C131 72(2) 3_665 . ? C132 N33 C131 111(2) 3_665 2_655 ? C132 N33 C131 111.0(12) . 2_655 ? C132 N33 C131 48.4(14) 2_655 2_655 ? C131 N33 C131 72(2) 3_665 2_655 ? C131 N33 C131 72(2) . 2_655 ? C132 N33 C130 55.1(15) 3_665 3_665 ? C132 N33 C130 117.0(16) . 3_665 ? C132 N33 C130 94(2) 2_655 3_665 ? C131 N33 C130 102.2(18) 3_665 3_665 ? C131 N33 C130 155(2) . 3_665 ? C131 N33 C130 130.1(17) 2_655 3_665 ? C132 N33 C130 94(2) 3_665 . ? C132 N33 C130 55.1(15) . . ? C132 N33 C130 117.0(16) 2_655 . ? C131 N33 C130 130.1(16) 3_665 . ? C131 N33 C130 102.2(18) . . ? C131 N33 C130 155(2) 2_655 . ? C130 N33 C130 62.4(17) 3_665 . ? C132 N33 C130 117.0(16) 3_665 2_655 ? C132 N33 C130 94(2) . 2_655 ? C132 N33 C130 55.1(15) 2_655 2_655 ? C131 N33 C130 155(2) 3_665 2_655 ? C131 N33 C130 130.1(16) . 2_655 ? C131 N33 C130 102.2(18) 2_655 2_655 ? C130 N33 C130 62.4(17) 3_665 2_655 ? C130 N33 C130 62.4(17) . 2_655 ? C132 C133 C131 47.5(14) . . ? N34 C135 C134 114(2) . . ? N34 C136 C138 116.5(17) . . ? N34 C137 C138 119.4(15) . . ? C137 N34 C137 119.5(3) 3 . ? C137 N34 C137 119.5(3) 3 2 ? C137 N34 C137 119.5(3) . 2 ? C137 N34 C135 111.7(18) 3 2 ? C137 N34 C135 55.7(14) . 2 ? C137 N34 C135 91(2) 2 2 ? C137 N34 C135 55.7(14) 3 . ? C137 N34 C135 91(2) . . ? C137 N34 C135 111.7(18) 2 . ? C135 N34 C135 56.4(18) 2 . ? C137 N34 C135 91(2) 3 3 ? C137 N34 C135 111.7(19) . 3 ? C137 N34 C135 55.7(14) 2 3 ? C135 N34 C135 56.4(18) 2 3 ? C135 N34 C135 56.4(18) . 3 ? C137 N34 C136 107(2) 3 . ? C137 N34 C136 54.4(15) . . ? C137 N34 C136 116.1(15) 2 . ? C135 N34 C136 109.7(18) 2 . ? C135 N34 C136 131(2) . . ? C135 N34 C136 160(3) 3 . ? C137 N34 C136 54.4(15) 3 3 ? C137 N34 C136 116.1(15) . 3 ? C137 N34 C136 107(2) 2 3 ? C135 N34 C136 160(2) 2 3 ? C135 N34 C136 109.7(17) . 3 ? C135 N34 C136 131(2) 3 3 ? C136 N34 C136 67.5(19) . 3 ? C137 N34 C136 116.1(15) 3 2 ? C137 N34 C136 108(2) . 2 ? C137 N34 C136 54.4(15) 2 2 ? C135 N34 C136 131(2) 2 2 ? C135 N34 C136 160(2) . 2 ? C135 N34 C136 109.7(17) 3 2 ? C136 N34 C136 67.5(19) . 2 ? C136 N34 C136 67.5(19) 3 2 ? C135 C134 C135 55.8(17) . 3 ? C135 C134 C135 55.8(17) . 2 ? C135 C134 C135 55.8(17) 3 2 ? C137 C138 C136 52.8(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.468 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.084 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.011 -0.010 -0.158 2188 447 ' Corresponds to 20 (CH3OH) and 12 (H2O) ' 2 -0.081 0.252 0.290 71 21 ' Corresponds to 3 (H2O) ' 3 0.333 0.081 0.290 71 21 ' Corresponds to 3 (H2O) ' 4 0.333 0.667 0.290 33 6 ' Corresponds to 1 (H2O) ' 5 0.667 0.333 0.482 367 101 ' Corresponds to 6 (CH3OH) ' 6 0.748 0.667 0.290 72 21 ' Corresponds to 3 (H2O) ' _platon_squeeze_details ; ; data_2S _database_code_depnum_ccdc_archive 'CCDC 756357' #TrackingRef 'Combined_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C192 H168 Fe4 N48 Ni6, C8 H20 N, F6 P, 33 (C H4 O), 10 (H2 O)' _chemical_formula_sum 'C233 H340 F6 Fe4 N49 Ni6 O43 P' _chemical_formula_weight 5228.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 3' _symmetry_space_group_name_Hall 'P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' _cell_length_a 19.574(3) _cell_length_b 19.574(3) _cell_length_c 35.075(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11638(4) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5532 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6864 _exptl_absorpt_correction_T_max 0.9604 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47355 _diffrn_reflns_av_R_equivalents 0.1456 _diffrn_reflns_av_sigmaI/netI 0.2626 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 23.30 _reflns_number_total 21372 _reflns_number_gt 8303 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Sum formula differs from actual formula as triethylamine H atoms have not been crystallographically assigned. Disordered solvent molecules have been removed from calculations using Squeeze. Large thermal parameters for some phenyl groups are due to strucural flexibilitya and resultant disordering. Restraints have been applied to ensure phenyl group shape is retained ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.057(17) _chemical_absolute_configuration rmad _refine_ls_number_reflns 21372 _refine_ls_number_parameters 1531 _refine_ls_number_restraints 246 _refine_ls_R_factor_all 0.1577 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1556 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 0.775 _refine_ls_restrained_S_all 0.780 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.03347(9) 0.25068(8) 0.28848(4) 0.0457(4) Uani 1 1 d . . . Fe1 Fe 0.0000 0.0000 0.23059(7) 0.0373(7) Uani 1 3 d S . . Ni2 Ni 0.25147(10) 0.21749(10) 0.47684(5) 0.0681(5) Uani 1 1 d . . . Fe2 Fe 0.03746(11) 0.27145(10) 0.43264(5) 0.0603(5) Uani 1 1 d . . . C1 C 0.1234(5) 0.3980(6) 0.1963(2) 0.071(4) Uani 1 1 d G . . H1 H 0.0736 0.3946 0.1996 0.085 Uiso 1 1 calc R . . C2 C 0.1914(7) 0.4713(5) 0.1934(2) 0.061(4) Uani 1 1 d G . . H2 H 0.1882 0.5180 0.1947 0.073 Uiso 1 1 calc R . . C3 C 0.2642(5) 0.4762(5) 0.1886(2) 0.076(4) Uani 1 1 d G . . H3 H 0.3107 0.5263 0.1866 0.091 Uiso 1 1 calc R . . C4 C 0.2690(5) 0.4078(7) 0.1867(2) 0.094(6) Uani 1 1 d G . . H4 H 0.3188 0.4111 0.1834 0.113 Uiso 1 1 calc R . . C5 C 0.2010(7) 0.3344(5) 0.1895(2) 0.056(4) Uani 1 1 d G . . H5 H 0.2042 0.2877 0.1882 0.067 Uiso 1 1 calc R . . C6 C 0.1282(5) 0.3295(5) 0.1944(2) 0.056(3) Uani 1 1 d G . . C7 C 0.0557(7) 0.2516(7) 0.1967(4) 0.050(3) Uani 1 1 d . . . H7 H 0.0739 0.2141 0.2045 0.060 Uiso 1 1 calc R . . C8 C 0.0139(7) 0.2205(6) 0.1591(3) 0.057(3) Uani 1 1 d . . . H8A H -0.0338 0.1693 0.1631 0.086 Uiso 1 1 calc R . . H8B H 0.0490 0.2144 0.1413 0.086 Uiso 1 1 calc R . . H8C H -0.0008 0.2578 0.1485 0.086 Uiso 1 1 calc R . . C9 C -0.0673(9) 0.2312(7) 0.2256(4) 0.061(4) Uani 1 1 d . . . H9 H -0.0902 0.2208 0.2009 0.074 Uiso 1 1 calc R . . C10 C -0.1153(8) 0.2245(7) 0.2575(4) 0.053(3) Uani 1 1 d . . . C11 C -0.1884(8) 0.2134(7) 0.2553(5) 0.076(4) Uani 1 1 d . . . H11 H -0.2079 0.2139 0.2306 0.091 Uiso 1 1 calc R . . C12 C -0.2369(8) 0.2017(7) 0.2847(5) 0.070(4) Uani 1 1 d . . . H12 H -0.2887 0.1935 0.2818 0.084 Uiso 1 1 calc R . . C13 C -0.2037(9) 0.2029(7) 0.3197(4) 0.071(4) Uani 1 1 d . . . H13 H -0.2341 0.1934 0.3423 0.086 Uiso 1 1 calc R . . C14 C -0.1253(7) 0.2180(6) 0.3226(4) 0.055(4) Uani 1 1 d . . . H14 H -0.1029 0.2230 0.3472 0.066 Uiso 1 1 calc R . . C15 C -0.0741(8) 0.4106(7) 0.2844(4) 0.066(4) Uani 1 1 d . . . H15 H -0.1076 0.3773 0.3040 0.079 Uiso 1 1 calc R . . C16 C -0.1035(10) 0.4402(10) 0.2528(6) 0.100(7) Uani 1 1 d . . . H16 H -0.1575 0.4260 0.2514 0.120 Uiso 1 1 calc R . . C17 C -0.0504(18) 0.4886(9) 0.2257(5) 0.137(11) Uani 1 1 d . . . H17 H -0.0702 0.5059 0.2054 0.165 Uiso 1 1 calc R . . C18 C 0.0277(13) 0.5135(14) 0.2255(6) 0.138(10) Uani 1 1 d . . . H18 H 0.0625 0.5487 0.2067 0.166 Uiso 1 1 calc R . . C19 C 0.0529(8) 0.4843(7) 0.2542(4) 0.071(4) Uani 1 1 d . . . H19 H 0.1071 0.4989 0.2541 0.085 Uiso 1 1 calc R . . C20 C 0.0072(8) 0.4358(7) 0.2830(3) 0.053(3) Uani 1 1 d . . . C21 C 0.0450(6) 0.4130(6) 0.3147(3) 0.041(3) Uani 1 1 d . . . H21 H 0.0008 0.3744 0.3311 0.049 Uiso 1 1 calc R . . C22 C 0.0965(7) 0.4895(7) 0.3407(3) 0.069(4) Uani 1 1 d . . . H22A H 0.1203 0.4755 0.3617 0.103 Uiso 1 1 calc R . . H22B H 0.0625 0.5084 0.3510 0.103 Uiso 1 1 calc R . . H22C H 0.1383 0.5310 0.3252 0.103 Uiso 1 1 calc R . . C23 C 0.1560(8) 0.4080(6) 0.2969(3) 0.049(3) Uani 1 1 d . . . H23 H 0.1841 0.4628 0.3026 0.058 Uiso 1 1 calc R . . C24 C 0.2001(7) 0.3684(7) 0.2865(3) 0.045(3) Uani 1 1 d . . . C25 C 0.2813(7) 0.4055(7) 0.2827(3) 0.042(3) Uani 1 1 d . . . H25 H 0.3116 0.4612 0.2855 0.050 Uiso 1 1 calc R . . C26 C 0.3179(8) 0.3659(8) 0.2752(4) 0.063(4) Uani 1 1 d . . . H26 H 0.3737 0.3911 0.2731 0.075 Uiso 1 1 calc R . . C27 C 0.2687(10) 0.2834(10) 0.2705(3) 0.074(4) Uani 1 1 d . . . H27 H 0.2919 0.2520 0.2645 0.089 Uiso 1 1 calc R . . C28 C 0.1875(7) 0.2474(7) 0.2744(3) 0.050(3) Uani 1 1 d . . . H28 H 0.1557 0.1916 0.2729 0.060 Uiso 1 1 calc R . . C34 C 0.4376(17) 0.2665(9) 0.5534(7) 0.214(9) Uani 1 1 d GDU . . C29 C 0.4101(10) 0.2963(15) 0.5817(9) 0.316(16) Uani 1 1 d GU . . H29 H 0.3550 0.2759 0.5848 0.379 Uiso 1 1 calc R . . C30 C 0.463(2) 0.3561(16) 0.6056(6) 0.375(17) Uani 1 1 d GU . . H30 H 0.4444 0.3765 0.6249 0.450 Uiso 1 1 calc R . . C31 C 0.5438(19) 0.3860(10) 0.6011(7) 0.371(18) Uani 1 1 d GU . . H31 H 0.5800 0.4268 0.6174 0.445 Uiso 1 1 calc R . . C32 C 0.5713(10) 0.3561(16) 0.5728(9) 0.366(18) Uani 1 1 d GU . . H32 H 0.6264 0.3765 0.5698 0.439 Uiso 1 1 calc R . . C33 C 0.518(2) 0.2963(16) 0.5490(6) 0.309(15) Uani 1 1 d GU . . H33 H 0.5371 0.2759 0.5297 0.370 Uiso 1 1 calc R . . C35 C 0.3825(10) 0.1956(10) 0.5272(5) 0.143(6) Uani 1 1 d DU . . H35 H 0.3351 0.1532 0.5406 0.172 Uiso 1 1 calc R . . C36 C 0.4344(11) 0.1678(10) 0.5102(5) 0.163(8) Uani 1 1 d DU . . H36A H 0.4018 0.1173 0.4973 0.244 Uiso 1 1 calc R . . H36B H 0.4650 0.1610 0.5305 0.244 Uiso 1 1 calc R . . H36C H 0.4704 0.2069 0.4918 0.244 Uiso 1 1 calc R . . C37 C 0.4120(10) 0.2744(9) 0.4670(5) 0.108(5) Uani 1 1 d DU . . H37 H 0.4632 0.2809 0.4697 0.130 Uiso 1 1 calc R . . C38 C 0.4025(11) 0.3132(9) 0.4352(5) 0.097(5) Uani 1 1 d U . . C39 C 0.4553(11) 0.3573(10) 0.4082(5) 0.100(6) Uani 1 1 d . . . H39 H 0.5081 0.3675 0.4090 0.120 Uiso 1 1 calc R . . C40 C 0.4320(13) 0.3842(11) 0.3823(6) 0.125(7) Uani 1 1 d . . . H40 H 0.4720 0.4196 0.3653 0.151 Uiso 1 1 calc R . . C41 C 0.3535(14) 0.3699(10) 0.3739(5) 0.111(7) Uani 1 1 d . . . H41 H 0.3387 0.3899 0.3527 0.133 Uiso 1 1 calc R . . C42 C 0.3080(11) 0.3260(11) 0.4000(5) 0.100(6) Uani 1 1 d . . . H42 H 0.2550 0.3145 0.3974 0.120 Uiso 1 1 calc R . . C43 C 0.3988(8) 0.4861(7) 0.4595(3) 0.121(7) Uani 1 1 d G . . H43 H 0.3654 0.4844 0.4394 0.145 Uiso 1 1 calc R . . C44 C 0.4799(9) 0.5358(6) 0.4569(3) 0.154(9) Uani 1 1 d G . . H44 H 0.5019 0.5682 0.4350 0.185 Uiso 1 1 calc R . . C45 C 0.5287(6) 0.5382(7) 0.4862(5) 0.134(7) Uani 1 1 d G . . H45 H 0.5842 0.5722 0.4844 0.160 Uiso 1 1 calc R . . C46 C 0.4964(8) 0.4908(9) 0.5182(4) 0.199(13) Uani 1 1 d G . . H46 H 0.5298 0.4924 0.5383 0.239 Uiso 1 1 calc R . . C47 C 0.4153(9) 0.4411(7) 0.5209(3) 0.169(10) Uani 1 1 d G . . H47 H 0.3933 0.4087 0.5427 0.203 Uiso 1 1 calc R . . C48 C 0.3665(6) 0.4387(6) 0.4915(3) 0.089(5) Uani 1 1 d G . . C49 C 0.2770(10) 0.3893(9) 0.4984(5) 0.095(5) Uani 1 1 d . . . H49 H 0.2525 0.3828 0.4727 0.114 Uiso 1 1 calc R . . C50 C 0.2429(10) 0.4300(10) 0.5226(5) 0.123(6) Uani 1 1 d . . . H50A H 0.1854 0.3965 0.5240 0.185 Uiso 1 1 calc R . . H50B H 0.2563 0.4808 0.5111 0.185 Uiso 1 1 calc R . . H50C H 0.2651 0.4387 0.5484 0.185 Uiso 1 1 calc R . . C51 C 0.2204(9) 0.2794(10) 0.5426(5) 0.095(5) Uani 1 1 d . . . H51 H 0.2122 0.3136 0.5587 0.114 Uiso 1 1 calc R . . C52 C 0.1914(6) 0.1988(5) 0.5571(4) 0.095(5) Uani 1 1 d G . . C53 C 0.1605(7) 0.1645(9) 0.5923(3) 0.125(7) Uani 1 1 d G . . H53 H 0.1572 0.1954 0.6123 0.150 Uiso 1 1 calc R . . C54 C 0.1345(6) 0.0850(9) 0.5982(3) 0.175(11) Uani 1 1 d G . . H54 H 0.1134 0.0616 0.6222 0.210 Uiso 1 1 calc R . . C55 C 0.1394(7) 0.0398(6) 0.5689(4) 0.139(7) Uani 1 1 d G . . H55 H 0.1216 -0.0146 0.5729 0.167 Uiso 1 1 calc R . . C56 C 0.1703(6) 0.0740(7) 0.5337(3) 0.116(6) Uani 1 1 d G . . H56 H 0.1737 0.0431 0.5137 0.139 Uiso 1 1 calc R . . N15 N 0.1963(5) 0.1536(7) 0.5278(3) 0.090(4) Uani 1 1 d G . . C57 C 0.0016(7) 0.0840(8) 0.2620(3) 0.054(4) Uani 1 1 d . . . C58 C -0.0784(6) 0.0038(6) 0.2000(3) 0.048(3) Uani 1 1 d . . . C59 C 0.0420(7) 0.2499(7) 0.3775(4) 0.053(4) Uani 1 1 d . . . C60 C -0.0328(10) 0.3206(8) 0.4153(5) 0.088(6) Uani 1 1 d . . . C61 C 0.0348(9) 0.2925(8) 0.4862(4) 0.085(5) Uani 1 1 d . . . C62 C 0.1027(8) 0.2297(7) 0.4466(3) 0.052(4) Uani 1 1 d . . . C63 C 0.1322(8) 0.3760(10) 0.4238(4) 0.069(4) Uani 1 1 d . . . C64 C 0.2312(9) 0.0568(10) 0.4424(4) 0.081(5) Uani 1 1 d . . . N1 N 0.0047(7) 0.2503(6) 0.2288(3) 0.055(3) Uani 1 1 d . . . N2 N -0.0788(6) 0.2260(5) 0.2900(3) 0.057(3) Uani 1 1 d . . . N3 N 0.0810(5) 0.3708(5) 0.2984(2) 0.042(3) Uani 1 1 d . . . N4 N 0.1547(5) 0.2910(6) 0.2803(2) 0.039(2) Uani 1 1 d . . . N5 N 0.0416(6) 0.2421(6) 0.3468(3) 0.059(3) Uani 1 1 d . . . N6 N 0.0035(5) 0.1370(6) 0.2780(3) 0.045(3) Uani 1 1 d . . . N7 N -0.0719(9) 0.3395(9) 0.4060(4) 0.103(6) Uani 1 1 d . . . N8 N 0.1913(7) 0.4342(7) 0.4174(3) 0.088(4) Uani 1 1 d . . . N9 N 0.0346(7) 0.3048(7) 0.5187(3) 0.086(4) Uani 1 1 d . . . N10 N -0.1247(6) 0.0109(6) 0.1828(3) 0.065(3) Uani 1 1 d . . . N11 N 0.1473(7) 0.2106(5) 0.4565(3) 0.061(3) Uani 1 1 d . . . N12 N 0.3625(7) 0.2319(8) 0.4926(4) 0.112(4) Uani 1 1 d DU . . N13 N 0.3204(7) 0.2924(6) 0.4311(4) 0.079(4) Uani 1 1 d . . . N14 N 0.2561(7) 0.3096(7) 0.5103(3) 0.081(4) Uani 1 1 d . . . N16 N 0.2324(7) 0.1170(8) 0.4500(4) 0.092(4) Uani 1 1 d . . . Ni3 Ni 0.63305(8) 0.55014(8) 1.01254(4) 0.0442(4) Uani 1 1 d . . . Ni4 Ni 0.41546(10) 0.29959(10) 0.82388(5) 0.0690(5) Uani 1 1 d . . . Fe3 Fe 0.6667 0.3333 1.07013(8) 0.0375(7) Uani 1 3 d S . . Fe4 Fe 0.62885(10) 0.56767(10) 0.86830(5) 0.0590(5) Uani 1 1 d . . . C65 C 0.7397(8) 0.8176(8) 1.0172(4) 0.074(4) Uani 1 1 d . . . H65 H 0.7721 0.8182 0.9969 0.089 Uiso 1 1 calc R . . C66 C 0.7709(10) 0.8732(8) 1.0477(6) 0.095(6) Uani 1 1 d . . . H66 H 0.8262 0.9085 1.0491 0.114 Uiso 1 1 calc R . . C67 C 0.7222(15) 0.8764(11) 1.0753(5) 0.106(7) Uani 1 1 d . . . H67 H 0.7423 0.9172 1.0939 0.127 Uiso 1 1 calc R . . C68 C 0.6467(12) 0.8211(10) 1.0751(5) 0.109(7) Uani 1 1 d . . . H68 H 0.6146 0.8218 1.0953 0.131 Uiso 1 1 calc R . . C69 C 0.6117(10) 0.7640(9) 1.0488(4) 0.083(5) Uani 1 1 d . . . H69 H 0.5572 0.7259 1.0501 0.099 Uiso 1 1 calc R . . C70 C 0.6604(7) 0.7632(6) 1.0186(4) 0.052(4) Uani 1 1 d . . . C71 C 0.6232(6) 0.7015(6) 0.9865(3) 0.045(3) Uani 1 1 d . . . H71 H 0.6674 0.7059 0.9703 0.054 Uiso 1 1 calc R . . C72 C 0.5724(9) 0.7228(8) 0.9610(4) 0.097(5) Uani 1 1 d . . . H72A H 0.5498 0.6846 0.9401 0.145 Uiso 1 1 calc R . . H72B H 0.6053 0.7759 0.9505 0.145 Uiso 1 1 calc R . . H72C H 0.5297 0.7214 0.9763 0.145 Uiso 1 1 calc R . . C73 C 0.5069(7) 0.5824(7) 1.0037(3) 0.042(3) Uani 1 1 d . . . H73 H 0.4769 0.6069 0.9975 0.050 Uiso 1 1 calc R . . C74 C 0.4669(8) 0.5002(7) 1.0152(3) 0.047(3) Uani 1 1 d . . . C75 C 0.3880(8) 0.4582(7) 1.0190(3) 0.058(4) Uani 1 1 d . . . H75 H 0.3576 0.4834 1.0161 0.069 Uiso 1 1 calc R . . C76 C 0.3520(8) 0.3800(9) 1.0269(3) 0.061(4) Uani 1 1 d . . . H76 H 0.2966 0.3507 1.0306 0.074 Uiso 1 1 calc R . . C77 C 0.3975(8) 0.3423(8) 1.0294(3) 0.065(4) Uani 1 1 d . . . H77 H 0.3746 0.2870 1.0329 0.078 Uiso 1 1 calc R . . C78 C 0.4782(8) 0.3927(8) 1.0265(3) 0.058(4) Uani 1 1 d . . . H78 H 0.5114 0.3708 1.0301 0.070 Uiso 1 1 calc R . . C79 C 0.5444(6) 0.6102(5) 1.1049(2) 0.067(4) Uani 1 1 d G . . H79 H 0.5942 0.6568 1.1021 0.080 Uiso 1 1 calc R . . C80 C 0.4762(8) 0.6153(6) 1.1070(2) 0.084(5) Uani 1 1 d G . . H80 H 0.4794 0.6653 1.1057 0.101 Uiso 1 1 calc R . . C81 C 0.4033(6) 0.5472(8) 1.1112(2) 0.085(5) Uani 1 1 d G . . H81 H 0.3566 0.5507 1.1127 0.102 Uiso 1 1 calc R . . C82 C 0.3986(5) 0.4741(6) 1.1132(2) 0.081(5) Uani 1 1 d G . . H82 H 0.3487 0.4275 1.1161 0.097 Uiso 1 1 calc R . . C83 C 0.4668(7) 0.4690(5) 1.1111(2) 0.074(4) Uani 1 1 d G . . H83 H 0.4636 0.4190 1.1125 0.089 Uiso 1 1 calc R . . C84 C 0.5397(6) 0.5371(7) 1.1069(2) 0.064(4) Uani 1 1 d G . . C85 C 0.6074(7) 0.5253(7) 1.1046(4) 0.057(4) Uani 1 1 d . . . H85 H 0.5880 0.4691 1.0975 0.069 Uiso 1 1 calc R . . C86 C 0.6519(6) 0.5421(6) 1.1411(3) 0.055(3) Uani 1 1 d . . . H86A H 0.6963 0.5329 1.1378 0.083 Uiso 1 1 calc R . . H86B H 0.6168 0.5072 1.1611 0.083 Uiso 1 1 calc R . . H86C H 0.6717 0.5972 1.1484 0.083 Uiso 1 1 calc R . . C87 C 0.7309(8) 0.6300(7) 1.0771(4) 0.055(4) Uani 1 1 d . . . H87 H 0.7527 0.6440 1.1020 0.066 Uiso 1 1 calc R . . C88 C 0.7826(7) 0.6720(8) 1.0440(5) 0.060(4) Uani 1 1 d . . . C89 C 0.8577(9) 0.7358(9) 1.0469(5) 0.073(4) Uani 1 1 d . . . H89 H 0.8790 0.7571 1.0712 0.088 Uiso 1 1 calc R . . C90 C 0.9034(9) 0.7697(8) 1.0138(6) 0.092(5) Uani 1 1 d . . . H90 H 0.9556 0.8134 1.0148 0.110 Uiso 1 1 calc R . . C91 C 0.8690(9) 0.7370(8) 0.9815(4) 0.065(4) Uani 1 1 d . . . H91 H 0.8988 0.7577 0.9588 0.078 Uiso 1 1 calc R . . C92 C 0.7945(8) 0.6761(7) 0.9780(4) 0.047(3) Uani 1 1 d . . . H92 H 0.7731 0.6576 0.9533 0.057 Uiso 1 1 calc R . . C93 C 0.2729(9) 0.4274(6) 0.8391(3) 0.149(9) Uani 1 1 d G . . H93 H 0.3087 0.4638 0.8571 0.179 Uiso 1 1 calc R . . C94 C 0.1921(10) 0.3956(9) 0.8441(3) 0.121(7) Uani 1 1 d G . . H94 H 0.1728 0.4103 0.8656 0.146 Uiso 1 1 calc R . . C95 C 0.1396(6) 0.3423(9) 0.8177(5) 0.187(11) Uani 1 1 d G . . H95 H 0.0844 0.3206 0.8211 0.224 Uiso 1 1 calc R . . C96 C 0.1678(8) 0.3208(8) 0.7862(4) 0.238(16) Uani 1 1 d G . . H96 H 0.1319 0.2843 0.7681 0.285 Uiso 1 1 calc R . . C97 C 0.2485(9) 0.3525(8) 0.7812(3) 0.138(8) Uani 1 1 d G . . H97 H 0.2678 0.3378 0.7597 0.166 Uiso 1 1 calc R . . C98 C 0.3011(6) 0.4058(7) 0.8076(4) 0.106(6) Uani 1 1 d G . . C99 C 0.3900(8) 0.4455(10) 0.8056(5) 0.096(6) Uani 1 1 d . . . H99 H 0.4125 0.4648 0.8316 0.116 Uiso 1 1 calc R . . C100 C 0.4207(10) 0.5189(9) 0.7775(4) 0.118(6) Uani 1 1 d . . . H10A H 0.4784 0.5457 0.7759 0.178 Uiso 1 1 calc R . . H10B H 0.4047 0.5557 0.7872 0.178 Uiso 1 1 calc R . . H10C H 0.3980 0.5005 0.7521 0.178 Uiso 1 1 calc R . . C101 C 0.4392(10) 0.3947(10) 0.7624(7) 0.109(7) Uani 1 1 d . . . H101 H 0.4424 0.4350 0.7462 0.130 Uiso 1 1 calc R . . N29 N 0.4683(4) 0.2895(6) 0.7754(2) 0.073(3) Uani 1 1 d GU . . C102 C 0.4728(5) 0.3420(5) 0.7475(3) 0.087(5) Uani 1 1 d GU . . C103 C 0.5044(6) 0.3423(7) 0.7119(3) 0.111(6) Uani 1 1 d GU . . H103 H 0.5075 0.3781 0.6928 0.133 Uiso 1 1 calc R . . C104 C 0.5313(6) 0.2900(8) 0.7043(3) 0.184(13) Uani 1 1 d GU . . H104 H 0.5529 0.2902 0.6800 0.220 Uiso 1 1 calc R . . C105 C 0.5267(6) 0.2376(7) 0.7323(4) 0.149(9) Uani 1 1 d GU . . H105 H 0.5452 0.2019 0.7271 0.179 Uiso 1 1 calc R . . C106 C 0.4952(5) 0.2373(5) 0.7678(3) 0.092(5) Uani 1 1 d GU . . H106 H 0.4921 0.2014 0.7869 0.110 Uiso 1 1 calc R . . C112 C 0.2782(14) 0.1597(12) 0.7494(5) 0.233(13) Uani 1 1 d GU . . C111 C 0.2331(13) 0.1956(14) 0.7438(7) 0.347(19) Uani 1 1 d GU . . H111 H 0.2082 0.2048 0.7648 0.416 Uiso 1 1 calc R . . C110 C 0.2243(12) 0.2179(12) 0.7073(10) 0.39(2) Uani 1 1 d GU . . H110 H 0.1935 0.2424 0.7034 0.470 Uiso 1 1 calc R . . C109 C 0.2607(15) 0.2044(13) 0.6765(6) 0.304(15) Uani 1 1 d GU . . H109 H 0.2547 0.2196 0.6516 0.365 Uiso 1 1 calc R . . C108 C 0.3058(12) 0.1685(13) 0.6821(6) 0.312(16) Uani 1 1 d GU . . H108 H 0.3306 0.1592 0.6611 0.375 Uiso 1 1 calc R . . C107 C 0.3145(10) 0.1461(10) 0.7186(9) 0.233(12) Uani 1 1 d GU . . H107 H 0.3453 0.1216 0.7225 0.279 Uiso 1 1 calc R . . C113 C 0.2810(13) 0.131(2) 0.7834(6) 0.215(17) Uani 1 1 d . . . H113 H 0.3292 0.1254 0.7833 0.258 Uiso 1 1 calc R . . C114 C 0.2203(13) 0.0597(13) 0.7930(6) 0.159(9) Uani 1 1 d . . . H11A H 0.2303 0.0443 0.8180 0.239 Uiso 1 1 calc R . . H11B H 0.2149 0.0207 0.7739 0.239 Uiso 1 1 calc R . . H11C H 0.1716 0.0622 0.7939 0.239 Uiso 1 1 calc R . . C115 C 0.2480(11) 0.1920(10) 0.8342(6) 0.138(8) Uani 1 1 d . . . H115 H 0.1966 0.1476 0.8314 0.166 Uiso 1 1 calc R . . N31 N 0.3460(6) 0.3036(6) 0.8677(2) 0.067(3) Uani 1 1 d G . . C116 C 0.2674(6) 0.2441(5) 0.8662(3) 0.117(6) Uani 1 1 d G . . C117 C 0.2152(4) 0.2386(6) 0.8944(4) 0.113(7) Uani 1 1 d G . . H117 H 0.1615 0.1979 0.8934 0.136 Uiso 1 1 calc R . . C118 C 0.2414(7) 0.2926(8) 0.9242(3) 0.128(8) Uani 1 1 d G . . H118 H 0.2057 0.2889 0.9435 0.154 Uiso 1 1 calc R . . C119 C 0.3199(8) 0.3522(6) 0.9257(2) 0.093(5) Uani 1 1 d G . . H119 H 0.3378 0.3892 0.9461 0.112 Uiso 1 1 calc R . . C120 C 0.3722(5) 0.3577(5) 0.8975(3) 0.068(4) Uani 1 1 d G . . H120 H 0.4258 0.3984 0.8985 0.082 Uiso 1 1 calc R . . C121 C 0.6645(6) 0.4115(6) 1.0399(3) 0.036(3) Uani 1 1 d U . . C122 C 0.5859(7) 0.3284(6) 1.1008(4) 0.049(3) Uani 1 1 d U . . C123 C 0.6263(6) 0.5424(7) 0.9222(4) 0.043(3) Uani 1 1 d . . . C124 C 0.6910(9) 0.6720(10) 0.8826(4) 0.084(5) Uani 1 1 d . . . C125 C 0.6307(9) 0.5898(9) 0.8146(5) 0.083(5) Uani 1 1 d . . . C126 C 0.5592(8) 0.4549(9) 0.8521(4) 0.063(4) Uani 1 1 d . . . C127 C 0.5383(9) 0.5731(7) 0.8763(3) 0.061(4) Uani 1 1 d . . . C128 C 0.4351(8) 0.1574(9) 0.8593(4) 0.069(5) Uani 1 1 d . . . N17 N 0.5820(6) 0.6222(5) 1.0017(2) 0.039(2) Uani 1 1 d . . . N18 N 0.5123(5) 0.4688(5) 1.0189(2) 0.042(2) Uani 1 1 d . . . N19 N 0.6584(7) 0.5757(6) 1.0738(3) 0.060(3) Uani 1 1 d . . . N20 N 0.7495(6) 0.6407(6) 1.0099(3) 0.055(3) Uani 1 1 d . . . N21 N 0.6252(6) 0.5334(6) 0.9537(3) 0.060(3) Uani 1 1 d . . . N22 N 0.6623(5) 0.4660(5) 1.0229(3) 0.047(3) Uani 1 1 d . . . N23 N 0.7333(7) 0.7385(7) 0.8936(3) 0.082(4) Uani 1 1 d . . . N24 N 0.4790(8) 0.5768(7) 0.8838(4) 0.108(5) Uani 1 1 d . . . N25 N 0.6312(8) 0.6031(7) 0.7836(4) 0.100(4) Uani 1 1 d . . . N26 N 0.5295(7) 0.3193(6) 1.1191(3) 0.079(4) Uani 1 1 d . . . N27 N 0.5132(7) 0.3894(7) 0.8433(3) 0.062(3) Uani 1 1 d . . . N28 N 0.4095(7) 0.3869(10) 0.7934(4) 0.110(6) Uani 1 1 d . . . N30 N 0.3023(8) 0.2072(9) 0.8091(4) 0.113(5) Uani 1 1 d . . . N32 N 0.4315(6) 0.2139(7) 0.8512(3) 0.086(4) Uani 1 1 d . . . C129 C 0.655(4) 0.3073(15) 0.8431(7) 0.040(12) Uani 0.33 1 d PDU A -1 C130 C 0.6182(17) 0.2955(19) 0.8809(7) 0.056(9) Uani 0.33 1 d PDU A -1 C131 C 0.5784(15) 0.2796(16) 0.9191(9) 0.074(7) Uani 0.50 1 d PU A -2 C132 C 0.6105(14) 0.310(2) 0.9505(9) 0.113(10) Uani 0.50 1 d PDU A -3 N33 N 0.6667 0.3333 0.9172(4) 0.036(3) Uani 1 3 d SDU . . C133 C 0.5342(8) 0.3077(9) 0.9420(5) 0.095(5) Uani 1 1 d DU . . C134 C 0.001(4) -0.022(3) 0.4546(9) 0.050(14) Uani 0.33 1 d PDU B -4 C135 C 0.0463(17) 0.009(2) 0.4190(7) 0.059(9) Uani 0.33 1 d PDU B -4 C136 C 0.0583(14) 0.0280(16) 0.3519(7) 0.114(10) Uani 0.50 1 d PDU B -5 C137 C 0.0852(9) 0.0424(14) 0.3850(7) 0.076(8) Uani 0.50 1 d PDU B -6 C138 C 0.1298(8) 0.1102(8) 0.3585(4) 0.087(4) Uani 1 1 d DU . . N34 N 0.0000 0.0000 0.3833(4) 0.032(3) Uani 1 3 d SDU . . P1 P 0.3333 0.6667 0.2789(3) 0.085(2) Uani 1 3 d S . . F1 F 0.4086(5) 0.7139(6) 0.3036(3) 0.149(4) Uani 1 1 d . . . F2 F 0.3784(5) 0.7393(5) -0.0057(3) 0.139(4) Uani 1 1 d . . . P2 P 0.3333 0.6667 0.0218(2) 0.081(2) Uani 1 3 d S . . F3 F 0.4159(6) 0.6953(7) 0.0443(4) 0.192(5) Uani 1 1 d . . . F4 F 0.3848(7) 0.6366(7) 0.2569(4) 0.211(6) 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 Ni1 0.0560(11) 0.0471(10) 0.0427(11) -0.0001(8) 0.0009(8) 0.0323(9) Fe1 0.0374(11) 0.0374(11) 0.0369(19) 0.000 0.000 0.0187(5) Ni2 0.0695(12) 0.0698(12) 0.0531(12) -0.0010(10) -0.0169(9) 0.0259(10) Fe2 0.0733(14) 0.0668(13) 0.0466(13) -0.0155(10) -0.0083(10) 0.0393(12) C1 0.051(9) 0.063(10) 0.095(12) -0.006(8) -0.012(8) 0.026(9) C2 0.078(10) 0.063(10) 0.042(9) -0.010(7) 0.009(7) 0.036(9) C3 0.094(12) 0.110(13) 0.029(9) 0.010(8) 0.018(8) 0.055(10) C4 0.186(18) 0.152(16) 0.031(9) 0.039(9) 0.041(9) 0.149(17) C5 0.080(10) 0.052(9) 0.039(9) 0.022(6) 0.012(7) 0.036(8) C6 0.080(11) 0.085(12) 0.018(7) 0.007(6) 0.000(6) 0.053(10) C7 0.052(8) 0.043(8) 0.067(10) 0.011(7) 0.014(7) 0.032(7) C8 0.073(9) 0.049(8) 0.029(8) -0.007(6) -0.005(6) 0.015(7) C9 0.086(11) 0.070(10) 0.050(10) 0.004(7) -0.024(9) 0.056(9) C10 0.050(9) 0.076(10) 0.041(9) 0.016(7) 0.025(8) 0.039(8) C11 0.048(10) 0.076(10) 0.097(14) 0.010(9) -0.003(9) 0.025(9) C12 0.047(10) 0.061(9) 0.106(14) -0.022(9) -0.023(10) 0.029(8) C13 0.082(12) 0.059(9) 0.090(13) -0.027(8) 0.014(9) 0.048(9) C14 0.060(9) 0.041(8) 0.080(11) -0.005(7) -0.019(8) 0.037(7) C15 0.067(10) 0.061(9) 0.070(11) -0.014(7) -0.007(8) 0.033(8) C16 0.112(14) 0.116(14) 0.132(16) -0.076(13) -0.098(13) 0.101(13) C17 0.32(3) 0.049(12) 0.057(13) 0.016(9) 0.012(18) 0.098(17) C18 0.18(2) 0.21(2) 0.106(19) 0.002(15) 0.058(16) 0.16(2) C19 0.075(10) 0.059(9) 0.101(13) 0.042(9) 0.018(9) 0.050(8) C20 0.050(9) 0.047(8) 0.048(9) 0.003(7) -0.011(7) 0.015(7) C21 0.026(7) 0.046(8) 0.055(9) 0.000(6) -0.007(6) 0.021(6) C22 0.087(10) 0.090(11) 0.041(9) 0.006(8) 0.001(7) 0.054(9) C23 0.070(10) 0.031(7) 0.054(9) 0.007(6) 0.006(7) 0.033(8) C24 0.050(9) 0.044(8) 0.034(8) 0.008(6) 0.008(6) 0.017(7) C25 0.045(8) 0.067(9) 0.027(7) -0.004(6) 0.006(6) 0.038(8) C26 0.053(9) 0.060(10) 0.075(11) 0.014(8) -0.010(8) 0.028(9) C27 0.103(13) 0.134(15) 0.024(8) 0.021(9) 0.014(8) 0.088(12) C28 0.042(9) 0.050(8) 0.054(9) 0.025(7) 0.000(6) 0.020(7) C34 0.281(17) 0.242(16) 0.176(17) -0.021(12) -0.060(13) 0.173(13) C29 0.28(2) 0.34(2) 0.35(2) -0.033(16) 0.049(15) 0.179(16) C30 0.39(2) 0.39(2) 0.34(2) -0.029(17) 0.000(18) 0.195(17) C31 0.39(2) 0.40(3) 0.32(3) 0.027(17) -0.013(17) 0.194(18) C32 0.39(2) 0.33(2) 0.32(2) -0.003(16) -0.015(17) 0.135(17) C33 0.290(18) 0.32(2) 0.27(2) 0.003(16) 0.023(17) 0.116(16) C35 0.117(9) 0.147(10) 0.167(11) 0.065(7) -0.006(8) 0.067(7) C36 0.190(11) 0.138(11) 0.152(12) -0.001(8) -0.028(8) 0.076(8) C37 0.088(8) 0.132(10) 0.099(9) 0.024(7) -0.019(6) 0.051(7) C38 0.089(13) 0.067(11) 0.107(15) 0.012(9) -0.019(12) 0.020(10) C39 0.131(16) 0.116(14) 0.076(13) 0.060(11) 0.037(12) 0.081(13) C40 0.14(2) 0.134(18) 0.097(18) 0.015(14) 0.041(15) 0.066(16) C41 0.18(2) 0.102(14) 0.035(11) 0.034(9) 0.014(12) 0.063(15) C42 0.170(19) 0.125(15) 0.066(13) -0.021(11) -0.050(13) 0.120(15) C43 0.153(17) 0.075(11) 0.044(11) 0.014(9) -0.033(10) -0.012(11) C44 0.128(17) 0.071(12) 0.121(19) 0.003(11) 0.031(14) -0.056(12) C45 0.109(15) 0.17(2) 0.084(16) 0.016(14) -0.001(13) 0.036(14) C46 0.104(18) 0.22(2) 0.19(3) 0.13(2) -0.029(16) 0.015(16) C47 0.088(14) 0.22(2) 0.109(16) 0.094(15) -0.014(13) 0.010(14) C48 0.114(15) 0.073(11) 0.051(11) -0.022(9) -0.026(11) 0.025(11) C49 0.106(14) 0.075(12) 0.082(13) 0.015(10) -0.045(10) 0.028(11) C50 0.120(15) 0.126(15) 0.122(17) -0.027(12) -0.027(12) 0.059(13) C51 0.080(12) 0.085(13) 0.126(17) -0.054(12) -0.055(11) 0.047(11) C52 0.121(14) 0.084(14) 0.074(14) -0.012(11) -0.022(11) 0.046(11) C53 0.092(12) 0.22(2) 0.024(10) -0.012(11) 0.000(8) 0.051(14) C54 0.27(3) 0.046(12) 0.123(19) 0.048(13) 0.030(17) 0.017(14) C55 0.171(18) 0.130(17) 0.091(16) 0.047(14) -0.012(14) 0.057(15) C56 0.212(19) 0.107(15) 0.080(14) 0.013(11) -0.034(13) 0.118(14) N15 0.064(8) 0.073(9) 0.101(11) 0.034(8) -0.018(7) 0.009(7) C57 0.069(9) 0.076(10) 0.041(9) 0.038(8) 0.007(7) 0.055(9) C58 0.011(6) 0.048(8) 0.064(9) -0.002(7) -0.013(6) 0.000(6) C59 0.065(9) 0.055(8) 0.048(10) -0.003(8) 0.017(8) 0.037(7) C60 0.114(15) 0.050(10) 0.070(13) -0.024(8) 0.044(11) 0.018(10) C61 0.111(12) 0.065(10) 0.050(11) -0.002(9) 0.026(10) 0.023(9) C62 0.104(11) 0.064(9) 0.021(8) -0.013(6) 0.006(7) 0.066(9) C63 0.060(10) 0.120(13) 0.047(9) -0.044(9) -0.017(8) 0.059(10) C64 0.111(12) 0.119(15) 0.027(9) 0.033(9) -0.002(8) 0.067(12) N1 0.077(8) 0.068(7) 0.026(7) 0.007(5) 0.008(6) 0.041(7) N2 0.077(8) 0.059(7) 0.033(7) 0.020(5) 0.020(6) 0.034(6) N3 0.018(5) 0.060(7) 0.046(7) 0.011(5) 0.014(5) 0.016(5) N4 0.067(7) 0.039(7) 0.036(6) 0.010(5) 0.007(5) 0.045(6) N5 0.071(8) 0.082(8) 0.034(7) -0.001(6) 0.026(6) 0.046(7) N6 0.060(7) 0.047(7) 0.031(7) 0.009(5) 0.003(5) 0.030(6) N7 0.144(13) 0.145(14) 0.091(11) -0.033(9) -0.036(9) 0.125(12) N8 0.070(9) 0.073(9) 0.078(10) -0.004(7) -0.011(8) 0.003(7) N9 0.125(10) 0.091(9) 0.043(8) -0.028(7) -0.011(8) 0.054(8) N10 0.053(7) 0.079(8) 0.053(8) 0.012(6) 0.001(6) 0.025(7) N11 0.096(9) 0.031(6) 0.052(8) -0.011(5) 0.003(6) 0.029(6) N12 0.086(7) 0.132(8) 0.087(8) 0.013(6) -0.012(6) 0.031(6) N13 0.075(9) 0.038(7) 0.105(11) -0.025(7) -0.003(8) 0.014(7) N14 0.078(9) 0.056(9) 0.049(9) -0.003(7) -0.013(7) -0.011(7) N16 0.081(9) 0.096(11) 0.098(11) 0.029(9) 0.000(7) 0.044(9) Ni3 0.0537(10) 0.0409(9) 0.0375(10) -0.0005(8) -0.0012(8) 0.0233(8) Ni4 0.0713(12) 0.0856(13) 0.0593(12) -0.0166(10) -0.0166(10) 0.0462(11) Fe3 0.0364(11) 0.0364(11) 0.0398(19) 0.000 0.000 0.0182(5) Fe4 0.0753(14) 0.0594(13) 0.0495(13) 0.0058(10) -0.0078(10) 0.0390(11) C65 0.072(11) 0.040(8) 0.103(13) -0.002(9) -0.050(9) 0.023(8) C66 0.094(13) 0.034(9) 0.165(19) -0.018(11) -0.070(13) 0.038(9) C67 0.18(2) 0.087(15) 0.096(16) -0.035(12) -0.060(15) 0.098(16) C68 0.154(19) 0.059(12) 0.080(15) -0.009(10) -0.018(13) 0.027(12) C69 0.135(14) 0.094(12) 0.061(11) -0.017(10) 0.000(11) 0.089(12) C70 0.043(8) 0.023(7) 0.085(11) 0.002(7) -0.033(8) 0.014(7) C71 0.039(7) 0.035(8) 0.062(9) -0.001(7) -0.006(6) 0.019(6) C72 0.150(14) 0.078(11) 0.068(11) -0.006(8) -0.033(10) 0.061(11) C73 0.026(7) 0.043(8) 0.049(8) 0.001(6) -0.008(6) 0.012(6) C74 0.061(9) 0.044(9) 0.044(9) 0.007(6) 0.012(7) 0.034(8) C75 0.060(10) 0.038(9) 0.042(9) 0.002(6) 0.001(7) -0.001(7) C76 0.057(9) 0.084(11) 0.021(8) -0.028(7) -0.001(6) 0.019(9) C77 0.066(10) 0.058(9) 0.054(10) -0.001(7) -0.003(8) 0.018(9) C78 0.054(9) 0.048(9) 0.057(9) 0.004(7) 0.021(7) 0.013(8) C79 0.089(11) 0.085(11) 0.049(9) 0.011(8) 0.011(8) 0.060(10) C80 0.100(12) 0.123(14) 0.037(9) 0.013(8) 0.024(9) 0.061(13) C81 0.119(15) 0.128(14) 0.039(10) 0.022(9) 0.021(9) 0.085(13) C82 0.140(15) 0.082(12) 0.039(9) -0.030(8) -0.003(9) 0.070(11) C83 0.134(14) 0.070(11) 0.013(8) -0.010(7) 0.001(8) 0.047(12) C84 0.047(9) 0.079(11) 0.035(8) 0.003(7) 0.005(6) 0.010(9) C85 0.051(9) 0.061(9) 0.056(10) 0.015(8) 0.020(8) 0.025(7) C86 0.071(9) 0.073(9) 0.020(8) 0.008(6) 0.002(6) 0.034(7) C87 0.045(9) 0.061(9) 0.063(11) -0.026(8) -0.024(8) 0.030(8) C88 0.024(8) 0.049(9) 0.105(14) -0.028(9) -0.022(9) 0.017(7) C89 0.064(11) 0.079(11) 0.100(14) -0.031(10) -0.025(10) 0.054(10) C90 0.075(12) 0.047(10) 0.130(18) 0.005(11) -0.002(12) 0.013(9) C91 0.083(12) 0.048(9) 0.063(11) -0.012(8) -0.015(9) 0.032(9) C92 0.066(10) 0.050(9) 0.044(9) -0.017(7) -0.025(8) 0.043(8) C93 0.26(3) 0.30(3) 0.038(11) 0.002(13) 0.015(13) 0.25(2) C94 0.148(18) 0.23(2) 0.080(15) -0.013(13) 0.010(13) 0.161(18) C95 0.16(2) 0.34(4) 0.075(17) 0.04(2) 0.022(16) 0.14(2) C96 0.065(14) 0.47(4) 0.036(13) -0.039(17) -0.025(10) 0.026(19) C97 0.116(16) 0.26(2) 0.083(14) -0.050(15) -0.026(13) 0.127(17) C98 0.103(15) 0.146(16) 0.082(14) 0.001(11) -0.036(12) 0.072(13) C99 0.061(11) 0.133(15) 0.125(16) -0.027(12) 0.000(10) 0.072(11) C100 0.162(17) 0.117(14) 0.110(15) 0.020(12) -0.022(12) 0.095(13) C101 0.068(13) 0.118(15) 0.16(2) -0.071(15) -0.096(13) 0.065(12) N29 0.054(7) 0.092(9) 0.089(10) -0.032(8) -0.027(6) 0.048(7) C102 0.034(8) 0.121(14) 0.035(10) -0.002(10) -0.001(7) -0.015(9) C103 0.061(11) 0.157(16) 0.100(16) -0.049(12) -0.025(10) 0.044(11) C104 0.098(15) 0.21(2) 0.20(3) -0.10(2) 0.072(15) 0.045(16) C105 0.110(16) 0.19(2) 0.13(2) -0.038(16) 0.035(14) 0.066(15) C106 0.060(10) 0.106(13) 0.093(14) -0.018(10) 0.008(9) 0.029(10) C112 0.25(2) 0.196(18) 0.22(2) -0.043(16) -0.028(15) 0.090(15) C111 0.35(2) 0.38(3) 0.37(3) -0.008(18) -0.053(18) 0.225(19) C110 0.43(3) 0.40(3) 0.33(2) 0.014(17) 0.031(17) 0.196(19) C109 0.32(2) 0.34(2) 0.23(2) 0.056(16) -0.033(16) 0.150(17) C108 0.29(2) 0.33(2) 0.27(2) 0.062(17) -0.052(17) 0.124(16) C107 0.221(18) 0.233(19) 0.217(18) 0.032(15) 0.001(14) 0.094(14) C113 0.095(17) 0.41(5) 0.065(16) -0.09(2) -0.017(14) 0.07(2) C114 0.15(2) 0.20(3) 0.13(2) -0.028(16) -0.060(17) 0.084(19) C115 0.094(14) 0.120(15) 0.121(17) -0.062(13) 0.007(13) -0.006(12) N31 0.104(10) 0.076(8) 0.056(8) -0.003(6) -0.003(7) 0.071(8) C116 0.083(13) 0.154(18) 0.125(18) -0.026(14) -0.041(13) 0.068(14) C117 0.097(12) 0.158(16) 0.142(17) 0.051(14) 0.089(12) 0.106(13) C118 0.27(3) 0.163(18) 0.049(11) 0.012(11) 0.060(14) 0.18(2) C119 0.117(14) 0.105(13) 0.077(13) 0.035(10) 0.007(11) 0.071(12) C120 0.107(12) 0.075(10) 0.049(10) 0.002(8) 0.006(9) 0.066(9) C121 0.024(5) 0.020(5) 0.039(6) -0.022(5) 0.004(5) -0.007(5) C122 0.064(7) 0.046(6) 0.064(7) 0.001(5) -0.014(6) 0.047(6) C123 0.046(8) 0.057(8) 0.041(9) 0.014(7) 0.005(7) 0.037(7) C124 0.104(13) 0.081(12) 0.037(10) -0.014(8) 0.008(8) 0.024(10) C125 0.111(13) 0.102(12) 0.052(11) 0.023(10) -0.014(10) 0.064(10) C126 0.074(11) 0.089(12) 0.044(10) 0.040(9) 0.026(8) 0.055(10) C127 0.111(12) 0.075(10) 0.035(8) -0.005(7) -0.034(8) 0.077(10) C128 0.090(11) 0.090(12) 0.052(10) -0.007(8) -0.033(7) 0.063(10) N17 0.048(7) 0.026(6) 0.044(7) -0.001(5) 0.000(5) 0.020(5) N18 0.069(7) 0.032(6) 0.028(6) 0.000(4) 0.009(5) 0.028(6) N19 0.071(8) 0.049(7) 0.082(9) -0.037(6) -0.035(7) 0.047(7) N20 0.069(8) 0.073(8) 0.035(7) -0.016(6) -0.001(6) 0.044(7) N21 0.064(7) 0.077(8) 0.030(7) 0.035(6) 0.023(6) 0.029(6) N22 0.058(7) 0.017(5) 0.053(7) -0.013(5) 0.005(5) 0.009(5) N23 0.115(11) 0.091(10) 0.048(9) 0.004(7) 0.009(7) 0.057(9) N24 0.127(12) 0.066(8) 0.136(13) -0.037(8) -0.088(10) 0.052(9) N25 0.121(11) 0.080(9) 0.082(11) 0.018(9) 0.007(9) 0.038(8) N26 0.101(9) 0.070(8) 0.097(10) 0.012(6) 0.000(8) 0.067(8) N27 0.079(9) 0.074(8) 0.051(8) 0.010(7) -0.002(6) 0.052(8) N28 0.055(9) 0.193(16) 0.069(11) -0.028(11) 0.009(8) 0.052(9) N30 0.094(10) 0.198(15) 0.059(10) -0.061(10) -0.012(8) 0.082(11) N32 0.068(8) 0.093(10) 0.075(10) -0.053(8) -0.026(7) 0.025(8) C129 0.062(19) 0.008(18) 0.025(12) 0.007(11) -0.018(15) -0.001(14) C130 0.048(17) 0.054(18) 0.052(13) -0.016(14) -0.013(10) 0.014(12) C131 0.051(9) 0.070(15) 0.083(17) -0.020(12) -0.001(11) 0.018(9) C132 0.084(13) 0.17(2) 0.104(17) -0.008(15) 0.041(11) 0.078(16) N33 0.040(5) 0.040(5) 0.027(8) 0.000 0.000 0.020(3) C133 0.068(8) 0.115(11) 0.116(11) 0.023(8) 0.036(8) 0.055(8) C134 0.046(17) 0.06(2) 0.054(14) -0.004(13) -0.005(15) 0.036(15) C135 0.048(16) 0.058(17) 0.054(14) 0.009(15) -0.020(9) 0.013(15) C136 0.087(15) 0.116(14) 0.077(15) 0.021(15) 0.037(11) 0.004(10) C137 0.052(9) 0.087(14) 0.062(15) 0.006(11) -0.017(12) 0.013(10) C138 0.072(8) 0.084(8) 0.099(10) 0.011(7) 0.018(7) 0.034(7) N34 0.042(5) 0.042(5) 0.011(7) 0.000 0.000 0.021(3) P1 0.071(3) 0.071(3) 0.115(7) 0.000 0.000 0.0354(16) F1 0.093(7) 0.146(9) 0.197(11) 0.028(8) -0.032(7) 0.050(7) F2 0.125(8) 0.099(7) 0.179(11) 0.039(7) 0.002(7) 0.047(6) P2 0.077(3) 0.077(3) 0.091(6) 0.000 0.000 0.0383(16) F3 0.141(9) 0.189(11) 0.202(13) 0.006(9) -0.073(9) 0.049(9) F4 0.220(13) 0.211(12) 0.213(14) -0.046(10) 0.089(10) 0.116(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 N2 2.001(11) . ? Ni1 N6 2.031(10) . ? Ni1 N5 2.063(11) . ? Ni1 N3 2.081(9) . ? Ni1 N4 2.113(9) . ? Ni1 N1 2.168(9) . ? Fe1 C58 1.904(12) 3 ? Fe1 C58 1.904(12) . ? Fe1 C58 1.904(12) 2 ? Fe1 C57 1.967(15) . ? Fe1 C57 1.967(15) 3 ? Fe1 C57 1.967(15) 2 ? Ni2 N16 2.040(14) . ? Ni2 N11 2.101(12) . ? Ni2 N14 2.114(12) . ? Ni2 N12 2.120(12) . ? Ni2 N13 2.137(12) . ? Ni2 N15 2.140(8) . ? Fe2 C62 1.893(13) . ? Fe2 C64 1.904(18) 2 ? Fe2 C61 1.929(15) . ? Fe2 C63 1.983(17) . ? Fe2 C59 1.991(14) . ? Fe2 C60 2.12(2) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C6 C7 1.478(12) . ? C7 N1 1.496(13) . ? C7 C8 1.510(14) . ? C9 N1 1.269(13) . ? C9 C10 1.424(16) . ? C10 N2 1.337(14) . ? C10 C11 1.338(16) . ? C11 C12 1.341(17) . ? C12 C13 1.385(17) . ? C13 C14 1.413(15) . ? C14 N2 1.421(14) . ? C15 C20 1.412(15) . ? C15 C16 1.493(19) . ? C16 C17 1.38(2) . ? C17 C18 1.35(3) . ? C18 C19 1.37(2) . ? C19 C20 1.368(15) . ? C20 C21 1.520(14) . ? C21 N3 1.444(12) . ? C21 C22 1.606(14) . ? C23 N3 1.273(12) . ? C23 C24 1.465(15) . ? C24 N4 1.337(12) . ? C24 C25 1.385(14) . ? C25 C26 1.318(14) . ? C26 C27 1.417(16) . ? C27 C28 1.387(15) . ? C28 N4 1.315(12) . ? C34 C29 1.3900 . ? C34 C33 1.3900 . ? C34 C35 1.561(15) . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C35 C36 1.494(15) . ? C35 N12 1.554(14) . ? C37 N12 1.277(17) . ? C37 C38 1.412(19) . ? C38 C39 1.348(19) . ? C38 N13 1.454(17) . ? C39 C40 1.25(2) . ? C40 C41 1.45(2) . ? C41 C42 1.27(2) . ? C42 N13 1.356(16) . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.539(17) . ? C49 N14 1.462(17) . ? C49 C50 1.528(19) . ? C51 N14 1.307(18) . ? C51 C52 1.474(18) . ? C52 C53 1.3900 . ? C52 N15 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 N15 1.3900 . ? C57 N6 1.163(12) . ? C58 N10 1.152(11) . ? C59 N5 1.088(12) . ? C60 N7 1.056(18) . ? C61 N9 1.165(15) . ? C62 N11 1.160(13) . ? C63 N8 1.169(15) . ? C64 N16 1.197(16) . ? C64 Fe2 1.904(18) 3 ? Ni3 N22 2.028(9) . ? Ni3 N20 2.075(11) . ? Ni3 N21 2.082(10) . ? Ni3 N18 2.100(9) . ? Ni3 N17 2.133(8) . ? Ni3 N19 2.206(10) . ? Ni4 N27 1.961(12) . ? Ni4 N29 2.049(8) . ? Ni4 N28 2.068(18) . ? Ni4 N31 2.080(7) . ? Ni4 N32 2.089(14) . ? Ni4 N30 2.107(13) . ? Fe3 C122 1.874(13) 2_655 ? Fe3 C122 1.874(14) 3_665 ? Fe3 C122 1.874(13) . ? Fe3 C121 1.880(12) 3_665 ? Fe3 C121 1.880(13) 2_655 ? Fe3 C121 1.880(12) . ? Fe4 C124 1.849(16) . ? Fe4 C127 1.850(15) . ? Fe4 C128 1.882(15) 3_665 ? Fe4 C125 1.929(16) . ? Fe4 C123 1.947(13) . ? Fe4 C126 2.011(17) . ? C65 C70 1.375(15) . ? C65 C66 1.428(19) . ? C66 C67 1.38(2) . ? C67 C68 1.33(2) . ? C68 C69 1.345(18) . ? C69 C70 1.429(16) . ? C70 C71 1.543(15) . ? C71 N17 1.445(12) . ? C71 C72 1.541(15) . ? C73 N17 1.275(11) . ? C73 C74 1.452(15) . ? C74 N18 1.315(12) . ? C74 C75 1.344(15) . ? C75 C76 1.355(15) . ? C76 C77 1.414(16) . ? C77 C78 1.386(15) . ? C78 N18 1.319(13) . ? C79 C80 1.3900 . ? C79 C84 1.3900 . ? C80 C81 1.3900 . ? C81 C82 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.455(13) . ? C85 N19 1.465(14) . ? C85 C86 1.491(14) . ? C87 N19 1.285(14) . ? C87 C88 1.487(17) . ? C88 N20 1.354(15) . ? C88 C89 1.376(17) . ? C89 C90 1.412(18) . ? C90 C91 1.307(18) . ? C91 C92 1.351(15) . ? C92 N20 1.379(14) . ? C93 C94 1.3900 . ? C93 C98 1.3900 . ? C94 C95 1.3900 . ? C95 C96 1.3900 . ? C96 C97 1.3900 . ? C97 C98 1.3900 . ? C98 C99 1.512(15) . ? C99 N28 1.444(19) . ? C99 C100 1.590(19) . ? C101 N28 1.20(2) . ? C101 C102 1.566(18) . ? N29 C102 1.3900 . ? N29 C106 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C105 C106 1.3900 . ? C112 C113 1.33(3) . ? C112 C111 1.3900 . ? C112 C107 1.3900 . ? C111 C110 1.3900 . ? C110 C109 1.3900 . ? C109 C108 1.3900 . ? C108 C107 1.3900 . ? C113 C114 1.35(3) . ? C113 N30 1.61(3) . ? C115 N30 1.294(18) . ? C115 C116 1.434(18) . ? N31 C116 1.3900 . ? N31 C120 1.3900 . ? C116 C117 1.3900 . ? C117 C118 1.3900 . ? C118 C119 1.3900 . ? C119 C120 1.3900 . ? C121 N22 1.242(12) . ? C122 N26 1.212(13) . ? C123 N21 1.119(11) . ? C124 N23 1.204(14) . ? C125 N25 1.117(15) . ? C126 N27 1.182(14) . ? C127 N24 1.226(16) . ? C128 N32 1.178(14) . ? C128 Fe4 1.882(14) 2_655 ? C129 C130 1.47(2) . ? C130 N33 1.541(17) . ? C131 C133 1.47(3) . ? C131 N33 1.51(2) . ? C132 C133 1.502(17) . ? C132 N33 1.51(3) . ? N33 C131 1.51(2) 2_655 ? N33 C131 1.51(2) 3_665 ? N33 C132 1.51(3) 2_655 ? N33 C132 1.51(3) 3_665 ? N33 C130 1.541(18) 2_655 ? N33 C130 1.541(18) 3_665 ? C134 C135 1.47(2) . ? C135 N34 1.504(17) . ? C136 N34 1.479(17) . ? C136 C138 1.533(17) . ? C137 N34 1.445(16) . ? C137 C138 1.493(17) . ? N34 C137 1.445(16) 2 ? N34 C137 1.445(16) 3 ? N34 C136 1.479(17) 2 ? N34 C136 1.479(17) 3 ? N34 C135 1.504(17) 2 ? N34 C135 1.504(17) 3 ? P1 F1 1.552(10) 2_665 ? P1 F1 1.552(10) . ? P1 F1 1.552(10) 3_565 ? P1 F4 1.597(10) 2_665 ? P1 F4 1.597(10) 3_565 ? P1 F4 1.597(10) . ? F2 P2 1.574(10) . ? P2 F2 1.574(10) 2_665 ? P2 F2 1.574(10) 3_565 ? P2 F3 1.626(10) 2_665 ? P2 F3 1.626(10) . ? P2 F3 1.626(10) 3_565 ? 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 N2 Ni1 N6 93.4(4) . . ? N2 Ni1 N5 94.2(4) . . ? N6 Ni1 N5 94.8(4) . . ? N2 Ni1 N3 94.8(4) . . ? N6 Ni1 N3 171.7(4) . . ? N5 Ni1 N3 85.2(4) . . ? N2 Ni1 N4 170.6(4) . . ? N6 Ni1 N4 92.3(4) . . ? N5 Ni1 N4 92.7(4) . . ? N3 Ni1 N4 79.4(3) . . ? N2 Ni1 N1 76.8(4) . . ? N6 Ni1 N1 83.6(4) . . ? N5 Ni1 N1 170.8(4) . . ? N3 Ni1 N1 97.7(3) . . ? N4 Ni1 N1 96.4(4) . . ? C58 Fe1 C58 91.3(5) 3 . ? C58 Fe1 C58 91.3(5) 3 2 ? C58 Fe1 C58 91.3(5) . 2 ? C58 Fe1 C57 89.3(5) 3 . ? C58 Fe1 C57 87.7(5) . . ? C58 Fe1 C57 178.8(5) 2 . ? C58 Fe1 C57 87.7(5) 3 3 ? C58 Fe1 C57 178.8(5) . 3 ? C58 Fe1 C57 89.3(5) 2 3 ? C57 Fe1 C57 91.6(4) . 3 ? C58 Fe1 C57 178.8(5) 3 2 ? C58 Fe1 C57 89.3(5) . 2 ? C58 Fe1 C57 87.7(5) 2 2 ? C57 Fe1 C57 91.6(4) . 2 ? C57 Fe1 C57 91.6(4) 3 2 ? N16 Ni2 N11 94.4(4) . . ? N16 Ni2 N14 170.9(5) . . ? N11 Ni2 N14 82.5(4) . . ? N16 Ni2 N12 85.9(5) . . ? N11 Ni2 N12 174.2(5) . . ? N14 Ni2 N12 98.0(5) . . ? N16 Ni2 N13 93.7(4) . . ? N11 Ni2 N13 92.8(5) . . ? N14 Ni2 N13 95.1(4) . . ? N12 Ni2 N13 81.4(6) . . ? N16 Ni2 N15 91.5(5) . . ? N11 Ni2 N15 93.3(4) . . ? N14 Ni2 N15 80.2(5) . . ? N12 Ni2 N15 92.5(4) . . ? N13 Ni2 N15 171.7(4) . . ? C62 Fe2 C64 92.8(6) . 2 ? C62 Fe2 C61 86.3(6) . . ? C64 Fe2 C61 85.5(6) 2 . ? C62 Fe2 C63 90.1(5) . . ? C64 Fe2 C63 176.4(6) 2 . ? C61 Fe2 C63 92.5(5) . . ? C62 Fe2 C59 92.8(5) . . ? C64 Fe2 C59 95.0(5) 2 . ? C61 Fe2 C59 179.0(6) . . ? C63 Fe2 C59 87.0(5) . . ? C62 Fe2 C60 177.9(6) . . ? C64 Fe2 C60 88.8(6) 2 . ? C61 Fe2 C60 95.1(6) . . ? C63 Fe2 C60 88.3(5) . . ? C59 Fe2 C60 85.7(5) . . ? C2 C1 C6 120.0 . . ? C3 C2 C1 120.0 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 C7 120.0(8) . . ? C1 C6 C7 120.0(8) . . ? C6 C7 N1 110.3(9) . . ? C6 C7 C8 114.5(9) . . ? N1 C7 C8 115.3(10) . . ? N1 C9 C10 122.9(12) . . ? N2 C10 C11 124.7(12) . . ? N2 C10 C9 110.3(12) . . ? C11 C10 C9 124.9(14) . . ? C10 C11 C12 126.2(15) . . ? C11 C12 C13 113.2(14) . . ? C12 C13 C14 121.1(13) . . ? C13 C14 N2 122.4(12) . . ? C20 C15 C16 115.2(13) . . ? C17 C16 C15 118.3(16) . . ? C18 C17 C16 125(2) . . ? C17 C18 C19 115(2) . . ? C18 C19 C20 125.9(15) . . ? C19 C20 C15 120.0(12) . . ? C19 C20 C21 119.8(12) . . ? C15 C20 C21 120.1(11) . . ? N3 C21 C20 109.1(10) . . ? N3 C21 C22 119.9(8) . . ? C20 C21 C22 108.3(9) . . ? N3 C23 C24 121.7(11) . . ? N4 C24 C25 121.1(11) . . ? N4 C24 C23 114.0(11) . . ? C25 C24 C23 124.9(12) . . ? C26 C25 C24 122.0(12) . . ? C25 C26 C27 115.8(13) . . ? C28 C27 C26 121.3(13) . . ? N4 C28 C27 119.6(12) . . ? C29 C34 C33 120.0 . . ? C29 C34 C35 124(3) . . ? C33 C34 C35 116(3) . . ? C34 C29 C30 120.0 . . ? C31 C30 C29 120.0 . . ? C32 C31 C30 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C36 C35 C34 105.4(19) . . ? C36 C35 N12 103.1(14) . . ? C34 C35 N12 105.9(13) . . ? N12 C37 C38 130.0(16) . . ? C39 C38 C37 129.3(18) . . ? C39 C38 N13 119.6(15) . . ? C37 C38 N13 110.7(16) . . ? C40 C39 C38 117.3(19) . . ? C39 C40 C41 130(2) . . ? C42 C41 C40 107.6(18) . . ? C41 C42 N13 132.4(18) . . ? C44 C43 C48 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C47 C46 C45 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 C49 116.9(11) . . ? C43 C48 C49 122.7(11) . . ? N14 C49 C48 109.8(13) . . ? N14 C49 C50 115.8(15) . . ? C48 C49 C50 114.6(13) . . ? N14 C51 C52 128.0(15) . . ? C53 C52 N15 120.0 . . ? C53 C52 C51 131.7(12) . . ? N15 C52 C51 108.3(12) . . ? C54 C53 C52 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? N15 C56 C55 120.0 . . ? C56 N15 C52 120.0 . . ? C56 N15 Ni2 125.1(8) . . ? C52 N15 Ni2 114.8(8) . . ? N6 C57 Fe1 174.6(10) . . ? N10 C58 Fe1 175.2(11) . . ? N5 C59 Fe2 173.7(12) . . ? N7 C60 Fe2 174.5(17) . . ? N9 C61 Fe2 178.5(15) . . ? N11 C62 Fe2 174.0(12) . . ? N8 C63 Fe2 174.1(13) . . ? N16 C64 Fe2 176.5(15) . 3 ? C9 N1 C7 125.0(11) . . ? C9 N1 Ni1 109.4(8) . . ? C7 N1 Ni1 123.8(8) . . ? C10 N2 C14 112.1(11) . . ? C10 N2 Ni1 119.6(8) . . ? C14 N2 Ni1 127.9(9) . . ? C23 N3 C21 116.3(10) . . ? C23 N3 Ni1 112.0(8) . . ? C21 N3 Ni1 130.0(7) . . ? C28 N4 C24 119.9(10) . . ? C28 N4 Ni1 126.9(8) . . ? C24 N4 Ni1 112.8(7) . . ? C59 N5 Ni1 164.9(11) . . ? C57 N6 Ni1 158.0(10) . . ? C62 N11 Ni2 160.5(10) . . ? C37 N12 C35 124.4(14) . . ? C37 N12 Ni2 107.3(11) . . ? C35 N12 Ni2 128.2(10) . . ? C42 N13 C38 112.7(13) . . ? C42 N13 Ni2 137.0(13) . . ? C38 N13 Ni2 110.3(11) . . ? C51 N14 C49 122.1(14) . . ? C51 N14 Ni2 108.0(10) . . ? C49 N14 Ni2 128.4(11) . . ? C64 N16 Ni2 163.1(13) . . ? N22 Ni3 N20 93.8(3) . . ? N22 Ni3 N21 94.4(4) . . ? N20 Ni3 N21 93.1(4) . . ? N22 Ni3 N18 91.9(4) . . ? N20 Ni3 N18 172.6(4) . . ? N21 Ni3 N18 91.2(3) . . ? N22 Ni3 N17 170.2(4) . . ? N20 Ni3 N17 96.0(4) . . ? N21 Ni3 N17 84.6(4) . . ? N18 Ni3 N17 78.4(4) . . ? N22 Ni3 N19 83.6(3) . . ? N20 Ni3 N19 79.8(5) . . ? N21 Ni3 N19 172.4(4) . . ? N18 Ni3 N19 96.2(4) . . ? N17 Ni3 N19 98.7(3) . . ? N27 Ni4 N29 93.5(4) . . ? N27 Ni4 N28 82.6(5) . . ? N29 Ni4 N28 83.7(5) . . ? N27 Ni4 N31 94.2(4) . . ? N29 Ni4 N31 170.9(4) . . ? N28 Ni4 N31 92.4(5) . . ? N27 Ni4 N32 95.1(4) . . ? N29 Ni4 N32 91.0(5) . . ? N28 Ni4 N32 174.1(5) . . ? N31 Ni4 N32 93.2(4) . . ? N27 Ni4 N30 171.9(5) . . ? N29 Ni4 N30 94.4(4) . . ? N28 Ni4 N30 96.5(6) . . ? N31 Ni4 N30 77.7(5) . . ? N32 Ni4 N30 86.5(5) . . ? C122 Fe3 C122 90.4(5) 2_655 3_665 ? C122 Fe3 C122 90.4(5) 2_655 . ? C122 Fe3 C122 90.4(5) 3_665 . ? C122 Fe3 C121 88.1(4) 2_655 3_665 ? C122 Fe3 C121 90.2(4) 3_665 3_665 ? C122 Fe3 C121 178.4(4) . 3_665 ? C122 Fe3 C121 90.2(4) 2_655 2_655 ? C122 Fe3 C121 178.4(4) 3_665 2_655 ? C122 Fe3 C121 88.1(5) . 2_655 ? C121 Fe3 C121 91.3(4) 3_665 2_655 ? C122 Fe3 C121 178.4(5) 2_655 . ? C122 Fe3 C121 88.1(5) 3_665 . ? C122 Fe3 C121 90.2(4) . . ? C121 Fe3 C121 91.3(4) 3_665 . ? C121 Fe3 C121 91.3(4) 2_655 . ? C124 Fe4 C127 90.9(6) . . ? C124 Fe4 C128 88.0(7) . 3_665 ? C127 Fe4 C128 178.3(6) . 3_665 ? C124 Fe4 C125 95.1(6) . . ? C127 Fe4 C125 92.6(6) . . ? C128 Fe4 C125 86.2(6) 3_665 . ? C124 Fe4 C123 86.3(5) . . ? C127 Fe4 C123 87.9(5) . . ? C128 Fe4 C123 93.3(5) 3_665 . ? C125 Fe4 C123 178.5(6) . . ? C124 Fe4 C126 178.4(6) . . ? C127 Fe4 C126 87.8(5) . . ? C128 Fe4 C126 93.2(6) 3_665 . ? C125 Fe4 C126 84.1(6) . . ? C123 Fe4 C126 94.5(5) . . ? C70 C65 C66 116.8(15) . . ? C67 C66 C65 121.1(16) . . ? C68 C67 C66 118.1(18) . . ? C67 C68 C69 125(2) . . ? C68 C69 C70 117.0(17) . . ? C65 C70 C69 121.2(13) . . ? C65 C70 C71 119.3(13) . . ? C69 C70 C71 119.5(12) . . ? N17 C71 C72 114.5(9) . . ? N17 C71 C70 111.3(9) . . ? C72 C71 C70 109.0(9) . . ? N17 C73 C74 120.8(11) . . ? N18 C74 C75 122.8(12) . . ? N18 C74 C73 115.4(12) . . ? C75 C74 C73 121.6(12) . . ? C74 C75 C76 120.0(14) . . ? C75 C76 C77 119.6(13) . . ? C78 C77 C76 114.5(13) . . ? N18 C78 C77 124.8(13) . . ? C80 C79 C84 120.0 . . ? C79 C80 C81 120.0 . . ? C82 C81 C80 120.0 . . ? C81 C82 C83 120.0 . . ? C84 C83 C82 120.0 . . ? C83 C84 C79 120.0 . . ? C83 C84 C85 115.7(10) . . ? C79 C84 C85 124.3(10) . . ? C84 C85 N19 107.7(10) . . ? C84 C85 C86 113.1(10) . . ? N19 C85 C86 111.0(10) . . ? N19 C87 C88 123.6(12) . . ? N20 C88 C89 121.8(15) . . ? N20 C88 C87 113.5(11) . . ? C89 C88 C87 124.7(14) . . ? C88 C89 C90 120.3(15) . . ? C91 C90 C89 115.5(15) . . ? C90 C91 C92 125.2(15) . . ? C91 C92 N20 120.3(12) . . ? C94 C93 C98 120.0 . . ? C95 C94 C93 120.0 . . ? C94 C95 C96 120.0 . . ? C97 C96 C95 120.0 . . ? C96 C97 C98 120.0 . . ? C97 C98 C93 120.0 . . ? C97 C98 C99 125.7(12) . . ? C93 C98 C99 114.3(12) . . ? N28 C99 C98 107.4(13) . . ? N28 C99 C100 113.8(14) . . ? C98 C99 C100 108.2(12) . . ? N28 C101 C102 124(2) . . ? C102 N29 C106 120.0 . . ? C102 N29 Ni4 111.3(7) . . ? C106 N29 Ni4 128.6(7) . . ? N29 C102 C103 120.0 . . ? N29 C102 C101 110.9(12) . . ? C103 C102 C101 129.1(12) . . ? C104 C103 C102 120.0 . . ? C105 C104 C103 120.0 . . ? C104 C105 C106 120.0 . . ? C105 C106 N29 120.0 . . ? C113 C112 C111 121(3) . . ? C113 C112 C107 119(3) . . ? C111 C112 C107 120.0 . . ? C112 C111 C110 120.0 . . ? C109 C110 C111 120.0 . . ? C110 C109 C108 120.0 . . ? C109 C108 C107 120.0 . . ? C108 C107 C112 120.0 . . ? C112 C113 C114 117(2) . . ? C112 C113 N30 99(3) . . ? C114 C113 N30 120(2) . . ? N30 C115 C116 118.2(14) . . ? C116 N31 C120 120.0 . . ? C116 N31 Ni4 114.2(7) . . ? C120 N31 Ni4 125.8(7) . . ? C117 C116 N31 120.0 . . ? C117 C116 C115 125.5(11) . . ? N31 C116 C115 114.5(11) . . ? C116 C117 C118 120.0 . . ? C119 C118 C117 120.0 . . ? C120 C119 C118 120.0 . . ? C119 C120 N31 120.0 . . ? N22 C121 Fe3 174.4(9) . . ? N26 C122 Fe3 174.6(11) . . ? N21 C123 Fe4 174.6(11) . . ? N23 C124 Fe4 176.1(14) . . ? N25 C125 Fe4 179.0(17) . . ? N27 C126 Fe4 174.7(12) . . ? N24 C127 Fe4 176.2(11) . . ? N32 C128 Fe4 173.8(13) . 2_655 ? C73 N17 C71 122.1(9) . . ? C73 N17 Ni3 111.3(7) . . ? C71 N17 Ni3 125.5(7) . . ? C74 N18 C78 118.0(11) . . ? C74 N18 Ni3 113.7(8) . . ? C78 N18 Ni3 128.3(9) . . ? C87 N19 C85 126.2(11) . . ? C87 N19 Ni3 107.7(9) . . ? C85 N19 Ni3 124.4(8) . . ? C88 N20 C92 116.7(12) . . ? C88 N20 Ni3 114.9(9) . . ? C92 N20 Ni3 128.2(9) . . ? C123 N21 Ni3 163.8(11) . . ? C121 N22 Ni3 158.2(8) . . ? C126 N27 Ni4 159.3(11) . . ? C101 N28 C99 118.0(19) . . ? C101 N28 Ni4 110.4(15) . . ? C99 N28 Ni4 130.5(11) . . ? C115 N30 C113 111.4(16) . . ? C115 N30 Ni4 114.9(11) . . ? C113 N30 Ni4 127.4(11) . . ? C128 N32 Ni4 165.7(11) . . ? C129 C130 N33 122(3) . . ? C133 C131 N33 116.4(19) . . ? C133 C132 N33 115(2) . . ? C131 N33 C131 119.8(2) 2_655 . ? C131 N33 C131 119.8(2) 2_655 3_665 ? C131 N33 C131 119.8(2) . 3_665 ? C131 N33 C132 49.4(14) 2_655 2_655 ? C131 N33 C132 99(2) . 2_655 ? C131 N33 C132 113.3(17) 3_665 2_655 ? C131 N33 C132 99(2) 2_655 3_665 ? C131 N33 C132 113.3(17) . 3_665 ? C131 N33 C132 49.4(14) 3_665 3_665 ? C132 N33 C132 66.6(17) 2_655 3_665 ? C131 N33 C132 113.3(17) 2_655 . ? C131 N33 C132 49.4(14) . . ? C131 N33 C132 99(2) 3_665 . ? C132 N33 C132 66.6(17) 2_655 . ? C132 N33 C132 66.6(17) 3_665 . ? C131 N33 C130 59.0(14) 2_655 2_655 ? C131 N33 C130 113.7(19) . 2_655 ? C131 N33 C130 103(2) 3_665 2_655 ? C132 N33 C130 108.3(16) 2_655 2_655 ? C132 N33 C130 132.9(18) 3_665 2_655 ? C132 N33 C130 158(2) . 2_655 ? C131 N33 C130 103(2) 2_655 . ? C131 N33 C130 59.0(14) . . ? C131 N33 C130 113.7(19) 3_665 . ? C132 N33 C130 132.9(18) 2_655 . ? C132 N33 C130 158(2) 3_665 . ? C132 N33 C130 108.3(16) . . ? C130 N33 C130 58(2) 2_655 . ? C131 N33 C130 113.7(19) 2_655 3_665 ? C131 N33 C130 103(2) . 3_665 ? C131 N33 C130 59.0(14) 3_665 3_665 ? C132 N33 C130 158(2) 2_655 3_665 ? C132 N33 C130 108.3(16) 3_665 3_665 ? C132 N33 C130 132.9(17) . 3_665 ? C130 N33 C130 58(2) 2_655 3_665 ? C130 N33 C130 58(2) . 3_665 ? C131 C133 C132 50.1(14) . . ? C134 C135 N34 117(3) . . ? N34 C136 C138 114.1(16) . . ? N34 C137 C138 118.7(15) . . ? C137 C138 C136 48.6(13) . . ? C137 N34 C137 119.83(17) . 2 ? C137 N34 C137 119.83(17) . 3 ? C137 N34 C137 119.83(17) 2 3 ? C137 N34 C136 110.6(14) . 2 ? C137 N34 C136 50.4(14) 2 2 ? C137 N34 C136 112(2) 3 2 ? C137 N34 C136 50.4(14) . . ? C137 N34 C136 112(2) 2 . ? C137 N34 C136 110.6(14) 3 . ? C136 N34 C136 70.7(19) 2 . ? C137 N34 C136 112(2) . 3 ? C137 N34 C136 110.6(14) 2 3 ? C137 N34 C136 50.4(14) 3 3 ? C136 N34 C136 70.7(19) 2 3 ? C136 N34 C136 70.7(19) . 3 ? C137 N34 C135 56.2(14) . . ? C137 N34 C135 112.3(19) 2 . ? C137 N34 C135 94(2) 3 . ? C136 N34 C135 153(2) 2 . ? C136 N34 C135 105.6(18) . . ? C136 N34 C135 134.4(18) 3 . ? C137 N34 C135 94(2) . 2 ? C137 N34 C135 56.2(14) 2 2 ? C137 N34 C135 112.3(19) 3 2 ? C136 N34 C135 105.6(18) 2 2 ? C136 N34 C135 134.4(18) . 2 ? C136 N34 C135 153(2) 3 2 ? C135 N34 C135 57(2) . 2 ? C137 N34 C135 112.3(19) . 3 ? C137 N34 C135 94(2) 2 3 ? C137 N34 C135 56.2(14) 3 3 ? C136 N34 C135 134.4(18) 2 3 ? C136 N34 C135 153(2) . 3 ? C136 N34 C135 105.6(18) 3 3 ? C135 N34 C135 57(2) . 3 ? C135 N34 C135 57(2) 2 3 ? F1 P1 F1 92.0(7) 2_665 . ? F1 P1 F1 92.0(7) 2_665 3_565 ? F1 P1 F1 92.0(7) . 3_565 ? F1 P1 F4 84.4(7) 2_665 2_665 ? F1 P1 F4 84.7(6) . 2_665 ? F1 P1 F4 175.1(9) 3_565 2_665 ? F1 P1 F4 84.7(6) 2_665 3_565 ? F1 P1 F4 175.1(9) . 3_565 ? F1 P1 F4 84.4(7) 3_565 3_565 ? F4 P1 F4 98.6(8) 2_665 3_565 ? F1 P1 F4 175.1(9) 2_665 . ? F1 P1 F4 84.4(7) . . ? F1 P1 F4 84.7(6) 3_565 . ? F4 P1 F4 98.6(8) 2_665 . ? F4 P1 F4 98.6(8) 3_565 . ? F2 P2 F2 86.4(7) 2_665 . ? F2 P2 F2 86.4(7) 2_665 3_565 ? F2 P2 F2 86.4(7) . 3_565 ? F2 P2 F3 88.5(6) 2_665 2_665 ? F2 P2 F3 86.1(6) . 2_665 ? F2 P2 F3 171.1(8) 3_565 2_665 ? F2 P2 F3 171.1(8) 2_665 . ? F2 P2 F3 88.5(6) . . ? F2 P2 F3 86.1(6) 3_565 . ? F3 P2 F3 98.4(7) 2_665 . ? F2 P2 F3 86.1(6) 2_665 3_565 ? F2 P2 F3 171.1(8) . 3_565 ? F2 P2 F3 88.5(6) 3_565 3_565 ? F3 P2 F3 98.4(7) 2_665 3_565 ? F3 P2 F3 98.4(7) . 3_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.363 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.070 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.017 -0.013 -0.294 2165 491 ' Corresponds to 22 (CH3OH) and 12 (H2O) ' 2 -0.084 0.665 0.151 68 23 ' Corresponds to 3 (H2O) ' 3 0.334 0.251 0.151 68 23 ' Corresponds to 3 (H2O) ' 4 0.333 0.667 0.151 34 7 ' Corresponds to 1 (H2O) ' 5 0.667 0.333 0.348 375 106 ' Corresponds to 6 (CH3OH) ' 6 0.667 0.333 0.636 7 2 ' ' 7 0.749 0.083 0.151 68 23 ' Corresponds to 3 (H2O) ' _platon_squeeze_details ; ;