# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Shie-Ming Peng' 'Chien-Lan Chiu' 'Hasan Hasanov' 'Shao-An Hua' 'Gin-Chen Huang' 'Rayyat H Ismayilov' 'Gene-Hsiang Lee' 'Isiah Po-Chun Liu' 'Chen-Yu Yeh' _publ_contact_author_name 'Shie-Ming Peng' _publ_contact_author_email SMPENG@NTU.EDU.TW _publ_section_title ; Probing the electronic communication of linear heptanickel and nonanickel string complexes by utilizing two redox-active [Ni2(napy)4]3+ moieties ; # Attachment 'compound 2.cif' data_ic11159 _database_code_depnum_ccdc_archive 'CCDC 753222' #TrackingRef 'compound 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H72 Cl20 N28 Ni7 O2' _chemical_formula_weight 2721.75 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.0614(3) _cell_length_b 16.6227(3) _cell_length_c 21.0026(4) _cell_angle_alpha 70.9557(10) _cell_angle_beta 77.1020(10) _cell_angle_gamma 84.3794(10) _cell_volume 5164.79(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 1.830 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.664 _exptl_absorpt_correction_T_max 0.927 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64820 _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18148 _reflns_number_gt 10704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(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^)+(0.1292P)^2^+16.7017P] 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_number_reflns 18148 _refine_ls_number_parameters 1346 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1246 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.2445 _refine_ls_wR_factor_gt 0.2065 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _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 0.20645(6) 0.37615(5) -0.23323(4) 0.0226(2) Uani 1 1 d . . . Ni2 Ni 0.21421(5) 0.33158(5) -0.11757(4) 0.0179(2) Uani 1 1 d . . . Ni3 Ni 0.22157(5) 0.28703(5) -0.00221(4) 0.0165(2) Uani 1 1 d . . . Ni4 Ni 0.23156(5) 0.24283(5) 0.11100(4) 0.0192(2) Uani 1 1 d . . . Ni5 Ni 0.24185(5) 0.19881(5) 0.22452(4) 0.0150(2) Uani 1 1 d . . . Ni6 Ni 0.24877(5) 0.15237(5) 0.34035(4) 0.0161(2) Uani 1 1 d . . . Ni7 Ni 0.25503(5) 0.10620(5) 0.45665(4) 0.0204(2) Uani 1 1 d . . . Cl1 Cl 0.19655(14) 0.42154(12) -0.35162(9) 0.0345(5) Uani 1 1 d . . . Cl2 Cl 0.26282(12) 0.05505(11) 0.57918(9) 0.0297(4) Uani 1 1 d . . . N1 N 0.2120(4) 0.5018(3) -0.2269(3) 0.0235(13) Uani 1 1 d . . . N2 N 0.1869(3) 0.4489(3) -0.1073(3) 0.0192(12) Uani 1 1 d . . . N3 N 0.1624(3) 0.3874(3) 0.0102(3) 0.0191(12) Uani 1 1 d . . . N4 N 0.1398(4) 0.3204(3) 0.1283(3) 0.0214(13) Uani 1 1 d . . . N5 N 0.1293(4) 0.2438(3) 0.2441(3) 0.0232(13) Uani 1 1 d . . . N6 N 0.1193(4) 0.1701(4) 0.3594(3) 0.0235(13) Uani 1 1 d . . . N7 N 0.1192(4) 0.1015(4) 0.4746(3) 0.0245(14) Uani 1 1 d . . . N8 N 0.2030(4) 0.2429(4) -0.2187(3) 0.0252(14) Uani 1 1 d . . . N9 N 0.2442(4) 0.2094(3) -0.1138(3) 0.0208(13) Uani 1 1 d . . . N10 N 0.2830(4) 0.1864(3) -0.0109(3) 0.0218(13) Uani 1 1 d . . . N11 N 0.3237(4) 0.1671(4) 0.0935(3) 0.0258(14) Uani 1 1 d . . . N12 N 0.3543(4) 0.1543(4) 0.1999(3) 0.0244(13) Uani 1 1 d . . . N13 N 0.3763(3) 0.1407(4) 0.3080(3) 0.0222(13) Uani 1 1 d . . . N14 N 0.3876(4) 0.1242(4) 0.4188(3) 0.0285(14) Uani 1 1 d . . . N15 N 0.3431(4) 0.3685(4) -0.2512(3) 0.0284(14) Uani 1 1 d . . . N16 N 0.3397(4) 0.3578(3) -0.1380(3) 0.0242(13) Uani 1 1 d . . . N17 N 0.3259(3) 0.3438(3) -0.0232(3) 0.0204(13) Uani 1 1 d . . . N18 N 0.3096(4) 0.3312(4) 0.0927(3) 0.0234(13) Uani 1 1 d . . . N19 N 0.2864(4) 0.3064(3) 0.2111(3) 0.0215(13) Uani 1 1 d . . . N20 N 0.2607(4) 0.2774(3) 0.3287(3) 0.0219(13) Uani 1 1 d . . . N21 N 0.2394(4) 0.2367(4) 0.4474(3) 0.0289(14) Uani 1 1 d . . . N22 N 0.0720(4) 0.3774(4) -0.1954(3) 0.0261(14) Uani 1 1 d . . . N23 N 0.0881(4) 0.3041(3) -0.0840(3) 0.0201(13) Uani 1 1 d . . . N24 N 0.1162(4) 0.2306(3) 0.0231(3) 0.0204(13) Uani 1 1 d . . . N25 N 0.1495(4) 0.1578(3) 0.1300(3) 0.0220(13) Uani 1 1 d . . . N26 N 0.1948(4) 0.0941(3) 0.2330(3) 0.0220(13) Uani 1 1 d . . . N27 N 0.2352(4) 0.0333(4) 0.3380(3) 0.0253(14) Uani 1 1 d . . . N28 N 0.2683(3) -0.0191(3) 0.4454(3) 0.0214(13) Uani 1 1 d . . . C1 C 0.2229(5) 0.5686(4) -0.2842(4) 0.0300(18) Uani 1 1 d . . . H1A H 0.2318 0.5580 -0.3271 0.036 Uiso 1 1 calc R . . C2 C 0.2220(5) 0.6531(5) -0.2852(4) 0.036(2) Uani 1 1 d . . . H2A H 0.2290 0.6985 -0.3274 0.043 Uiso 1 1 calc R . . C3 C 0.2110(5) 0.6689(5) -0.2240(4) 0.0357(19) Uani 1 1 d . . . H3A H 0.2116 0.7258 -0.2235 0.043 Uiso 1 1 calc R . . C4 C 0.1987(5) 0.6017(4) -0.1620(4) 0.0271(17) Uani 1 1 d . . . C5 C 0.1999(4) 0.5183(4) -0.1657(3) 0.0224(16) Uani 1 1 d . . . C6 C 0.1872(5) 0.6124(5) -0.0966(3) 0.0274(17) Uani 1 1 d . . . H6A H 0.1891 0.6675 -0.0926 0.033 Uiso 1 1 calc R . . C7 C 0.1733(5) 0.5438(4) -0.0399(4) 0.0281(17) Uani 1 1 d . . . H7A H 0.1645 0.5507 0.0043 0.034 Uiso 1 1 calc R . . C8 C 0.1718(4) 0.4607(4) -0.0456(3) 0.0196(15) Uani 1 1 d . . . C9 C 0.1180(4) 0.3862(4) 0.0742(3) 0.0188(15) Uani 1 1 d . . . C10 C 0.0520(4) 0.4423(4) 0.0880(3) 0.0226(16) Uani 1 1 d . . . H10A H 0.0336 0.4861 0.0513 0.027 Uiso 1 1 calc R . . C11 C 0.0134(4) 0.4341(4) 0.1551(4) 0.0234(16) Uani 1 1 d . . . H11A H -0.0314 0.4731 0.1643 0.028 Uiso 1 1 calc R . . C12 C 0.0379(4) 0.3707(4) 0.2096(4) 0.0240(16) Uani 1 1 d . . . H12A H 0.0135 0.3679 0.2558 0.029 Uiso 1 1 calc R . . C13 C 0.0996(4) 0.3110(4) 0.1945(3) 0.0222(16) Uani 1 1 d . . . C14 C 0.0785(4) 0.2084(4) 0.3072(3) 0.0211(15) Uani 1 1 d . . . C15 C -0.0122(5) 0.2046(5) 0.3176(4) 0.0289(17) Uani 1 1 d . . . H15A H -0.0403 0.2273 0.2799 0.035 Uiso 1 1 calc R . . C16 C -0.0585(5) 0.1677(5) 0.3828(4) 0.0302(18) Uani 1 1 d . . . H16A H -0.1187 0.1639 0.3904 0.036 Uiso 1 1 calc R . . C17 C -0.0159(4) 0.1357(4) 0.4383(3) 0.0242(16) Uani 1 1 d . . . C18 C 0.0729(4) 0.1355(4) 0.4244(3) 0.0200(15) Uani 1 1 d . . . C19 C -0.0599(5) 0.1017(5) 0.5065(4) 0.0323(18) Uani 1 1 d . . . H19A H -0.1205 0.1018 0.5173 0.039 Uiso 1 1 calc R . . C20 C -0.0143(5) 0.0688(5) 0.5567(4) 0.0358(19) Uani 1 1 d . . . H20A H -0.0422 0.0463 0.6035 0.043 Uiso 1 1 calc R . . C21 C 0.0748(5) 0.0687(5) 0.5380(4) 0.0325(18) Uani 1 1 d . . . H21A H 0.1059 0.0431 0.5734 0.039 Uiso 1 1 calc R . . C22 C 0.1829(5) 0.2175(4) -0.2670(4) 0.0274(17) Uani 1 1 d . . . H22A H 0.1653 0.2597 -0.3049 0.033 Uiso 1 1 calc R . . C23 C 0.1860(5) 0.1319(5) -0.2653(4) 0.036(2) Uani 1 1 d . . . H23A H 0.1700 0.1172 -0.3010 0.044 Uiso 1 1 calc R . . C24 C 0.2120(5) 0.0710(5) -0.2125(4) 0.0314(18) Uani 1 1 d . . . H24A H 0.2152 0.0129 -0.2107 0.038 Uiso 1 1 calc R . . C25 C 0.2344(5) 0.0947(4) -0.1596(4) 0.0273(17) Uani 1 1 d . . . C26 C 0.2270(4) 0.1815(4) -0.1644(3) 0.0221(16) Uani 1 1 d . . . C27 C 0.2621(5) 0.0369(4) -0.1016(4) 0.0282(17) Uani 1 1 d . . . H27A H 0.2677 -0.0222 -0.0967 0.034 Uiso 1 1 calc R . . C28 C 0.2806(5) 0.0651(4) -0.0534(4) 0.0276(17) Uani 1 1 d . . . H28A H 0.2998 0.0261 -0.0148 0.033 Uiso 1 1 calc R . . C29 C 0.2714(4) 0.1537(4) -0.0600(3) 0.0204(15) Uani 1 1 d . . . C30 C 0.3404(4) 0.1487(4) 0.0332(3) 0.0241(16) Uani 1 1 d . . . C31 C 0.4132(5) 0.1033(5) 0.0149(4) 0.0315(18) Uani 1 1 d . . . H31A H 0.4288 0.0979 -0.0299 0.038 Uiso 1 1 calc R . . C32 C 0.4629(5) 0.0656(5) 0.0635(4) 0.0311(18) Uani 1 1 d . . . H32A H 0.5119 0.0321 0.0523 0.037 Uiso 1 1 calc R . . C33 C 0.4428(5) 0.0759(5) 0.1270(4) 0.0306(18) Uani 1 1 d . . . H33A H 0.4738 0.0454 0.1615 0.037 Uiso 1 1 calc R . . C34 C 0.3751(4) 0.1327(4) 0.1407(4) 0.0265(17) Uani 1 1 d . . . C35 C 0.4115(4) 0.1476(4) 0.2420(4) 0.0248(16) Uani 1 1 d . . . C36 C 0.5014(5) 0.1549(5) 0.2179(4) 0.0336(19) Uani 1 1 d . . . H36A H 0.5252 0.1613 0.1709 0.040 Uiso 1 1 calc R . . C37 C 0.5535(5) 0.1528(5) 0.2610(4) 0.037(2) Uani 1 1 d . . . H37A H 0.6134 0.1582 0.2442 0.045 Uiso 1 1 calc R . . C38 C 0.5181(5) 0.1423(5) 0.3317(4) 0.0307(18) Uani 1 1 d . . . C39 C 0.4286(5) 0.1360(5) 0.3526(4) 0.0266(17) Uani 1 1 d . . . C40 C 0.5662(5) 0.1385(7) 0.3796(4) 0.057(3) Uani 1 1 d . . . H40A H 0.6267 0.1411 0.3673 0.068 Uiso 1 1 calc R . . C41 C 0.5238(6) 0.1309(8) 0.4455(5) 0.075(4) Uani 1 1 d . . . H41A H 0.5546 0.1308 0.4792 0.090 Uiso 1 1 calc R . . C42 C 0.4355(6) 0.1232(7) 0.4628(4) 0.054(3) Uani 1 1 d . . . H42A H 0.4079 0.1169 0.5091 0.065 Uiso 1 1 calc R . . C43 C 0.3891(5) 0.3747(5) -0.3133(4) 0.0351(19) Uani 1 1 d . . . H43A H 0.3596 0.3747 -0.3479 0.042 Uiso 1 1 calc R . . C44 C 0.4759(6) 0.3810(6) -0.3311(4) 0.047(2) Uani 1 1 d . . . H44A H 0.5045 0.3839 -0.3765 0.057 Uiso 1 1 calc R . . C45 C 0.5224(6) 0.3831(6) -0.2843(4) 0.044(2) Uani 1 1 d . . . H45A H 0.5826 0.3892 -0.2966 0.052 Uiso 1 1 calc R . . C46 C 0.4764(5) 0.3760(5) -0.2166(4) 0.0336(19) Uani 1 1 d . . . C47 C 0.3872(5) 0.3671(4) -0.2023(4) 0.0269(17) Uani 1 1 d . . . C48 C 0.5162(5) 0.3728(5) -0.1623(4) 0.0338(19) Uani 1 1 d . . . H48A H 0.5765 0.3760 -0.1698 0.041 Uiso 1 1 calc R . . C49 C 0.4667(5) 0.3650(5) -0.0990(4) 0.0302(18) Uani 1 1 d . . . H49A H 0.4927 0.3647 -0.0624 0.036 Uiso 1 1 calc R . . C50 C 0.3783(5) 0.3577(4) -0.0869(3) 0.0237(16) Uani 1 1 d . . . C51 C 0.3447(4) 0.3739(4) 0.0258(3) 0.0224(16) Uani 1 1 d . . . C52 C 0.3880(5) 0.4475(5) 0.0117(4) 0.0322(18) Uani 1 1 d . . . H52A H 0.4060 0.4822 -0.0345 0.039 Uiso 1 1 calc R . . C53 C 0.4048(5) 0.4704(5) 0.0644(4) 0.0342(19) Uani 1 1 d . . . H53A H 0.4346 0.5212 0.0542 0.041 Uiso 1 1 calc R . . C54 C 0.3792(5) 0.4213(5) 0.1316(4) 0.0300(18) Uani 1 1 d . . . H54A H 0.3985 0.4321 0.1675 0.036 Uiso 1 1 calc R . . C55 C 0.3244(5) 0.3552(4) 0.1457(3) 0.0255(16) Uani 1 1 d . . . C56 C 0.2704(4) 0.3370(4) 0.2663(3) 0.0231(16) Uani 1 1 d . . . C57 C 0.2581(5) 0.4250(4) 0.2608(4) 0.0296(18) Uani 1 1 d . . . H57A H 0.2613 0.4663 0.2168 0.036 Uiso 1 1 calc R . . C58 C 0.2421(5) 0.4506(5) 0.3175(4) 0.0312(18) Uani 1 1 d . . . H58A H 0.2334 0.5092 0.3136 0.037 Uiso 1 1 calc R . . C59 C 0.2385(5) 0.3879(4) 0.3829(3) 0.0245(16) Uani 1 1 d . . . C60 C 0.2463(4) 0.3007(4) 0.3868(4) 0.0226(16) Uani 1 1 d . . . C61 C 0.2235(6) 0.4081(5) 0.4446(4) 0.039(2) Uani 1 1 d . . . H61A H 0.2190 0.4659 0.4437 0.047 Uiso 1 1 calc R . . C62 C 0.2153(6) 0.3440(5) 0.5054(4) 0.048(2) Uani 1 1 d . . . H62A H 0.2041 0.3562 0.5477 0.058 Uiso 1 1 calc R . . C63 C 0.2238(6) 0.2602(5) 0.5045(4) 0.039(2) Uani 1 1 d . . . H63A H 0.2181 0.2164 0.5475 0.047 Uiso 1 1 calc R . . C64 C 0.0198(5) 0.4137(5) -0.2386(4) 0.0327(19) Uani 1 1 d . . . H64A H 0.0452 0.4415 -0.2852 0.039 Uiso 1 1 calc R . . C65 C -0.0688(6) 0.4142(6) -0.2210(4) 0.043(2) Uani 1 1 d . . . H65A H -0.1024 0.4420 -0.2543 0.052 Uiso 1 1 calc R . . C66 C -0.1062(5) 0.3735(5) -0.1543(4) 0.0357(19) Uani 1 1 d . . . H66A H -0.1667 0.3710 -0.1410 0.043 Uiso 1 1 calc R . . C67 C -0.0558(5) 0.3356(5) -0.1055(4) 0.0266(17) Uani 1 1 d . . . C68 C 0.0342(5) 0.3386(4) -0.1278(3) 0.0218(16) Uani 1 1 d . . . C69 C -0.0876(5) 0.2935(4) -0.0345(4) 0.0254(16) Uani 1 1 d . . . H69A H -0.1475 0.2897 -0.0172 0.030 Uiso 1 1 calc R . . C70 C -0.0332(4) 0.2590(4) 0.0082(4) 0.0230(16) Uani 1 1 d . . . H70A H -0.0548 0.2319 0.0557 0.028 Uiso 1 1 calc R . . C71 C 0.0567(4) 0.2630(4) -0.0178(3) 0.0201(15) Uani 1 1 d . . . C72 C 0.0981(4) 0.1639(4) 0.0842(3) 0.0197(15) Uani 1 1 d . . . C73 C 0.0384(5) 0.1025(4) 0.0987(4) 0.0259(17) Uani 1 1 d . . . H73A H 0.0073 0.1023 0.0652 0.031 Uiso 1 1 calc R . . C74 C 0.0245(5) 0.0413(5) 0.1631(4) 0.0290(17) Uani 1 1 d . . . H74A H -0.0189 0.0010 0.1747 0.035 Uiso 1 1 calc R . . C75 C 0.0728(5) 0.0382(4) 0.2104(4) 0.0277(17) Uani 1 1 d . . . H75A H 0.0607 -0.0014 0.2555 0.033 Uiso 1 1 calc R . . C76 C 0.1395(4) 0.0938(4) 0.1911(3) 0.0220(16) Uani 1 1 d . . . C77 C 0.2128(4) 0.0217(4) 0.2831(3) 0.0229(16) Uani 1 1 d . . . C78 C 0.2149(5) -0.0607(5) 0.2763(4) 0.0302(18) Uani 1 1 d . . . H78A H 0.2006 -0.0674 0.2368 0.036 Uiso 1 1 calc R . . C79 C 0.2372(5) -0.1300(5) 0.3259(4) 0.0326(18) Uani 1 1 d . . . H79A H 0.2393 -0.1851 0.3212 0.039 Uiso 1 1 calc R . . C80 C 0.2577(5) -0.1189(4) 0.3858(3) 0.0250(16) Uani 1 1 d . . . C81 C 0.2547(4) -0.0352(4) 0.3891(3) 0.0196(15) Uani 1 1 d . . . C82 C 0.2787(5) -0.1868(5) 0.4408(4) 0.0282(17) Uani 1 1 d . . . H82A H 0.2832 -0.2434 0.4390 0.034 Uiso 1 1 calc R . . C83 C 0.2924(5) -0.1701(5) 0.4964(4) 0.0307(18) Uani 1 1 d . . . H83A H 0.3060 -0.2151 0.5345 0.037 Uiso 1 1 calc R . . C84 C 0.2861(4) -0.0858(4) 0.4971(4) 0.0254(17) Uani 1 1 d . . . H84A H 0.2951 -0.0753 0.5369 0.031 Uiso 1 1 calc R . . Cl3 Cl 0.78628(14) 0.15718(12) 0.13791(11) 0.0423(5) Uani 1 1 d . . . Cl4 Cl 0.24719(18) 0.64349(14) 0.36619(13) 0.0590(7) Uani 1 1 d . . . O1 O 0.7848(4) 0.1257(3) 0.3014(3) 0.066(2) Uani 1 1 d D . . H1B H 0.7633 0.0756 0.3300 0.099 Uiso 1 1 d D . . H1C H 0.8350 0.1138 0.2763 0.099 Uiso 1 1 d D . . O2 O 0.2692(4) 0.6583(4) 0.2134(3) 0.074(2) Uani 1 1 d D . . H2B H 0.2692 0.6781 0.2486 0.111 Uiso 1 1 d D . . H2C H 0.2905 0.6991 0.1743 0.111 Uiso 1 1 d D . . C85 C 0.6319(10) 0.2459(15) 0.0312(7) 0.229(15) Uani 1 1 d . . . H85A H 0.6764 0.2197 0.0582 0.274 Uiso 1 1 calc R . . H85B H 0.5965 0.2000 0.0318 0.274 Uiso 1 1 calc R . . Cl5 Cl 0.6775(2) 0.2982(3) -0.0496(2) 0.1263(15) Uani 1 1 d . . . Cl6 Cl 0.5648(3) 0.3210(2) 0.06949(16) 0.0979(11) Uani 1 1 d . . . C86 C 0.1027(6) 0.9210(6) 0.0350(5) 0.053(2) Uani 1 1 d . . . H86A H 0.1173 0.8973 -0.0038 0.063 Uiso 1 1 calc R . . H86B H 0.1068 0.9837 0.0156 0.063 Uiso 1 1 calc R . . Cl7 Cl 0.17592(18) 0.88212(19) 0.08785(17) 0.0866(10) Uani 1 1 d . . . Cl8 Cl -0.00402(14) 0.89517(14) 0.07899(12) 0.0474(6) Uani 1 1 d . . . C87 C 0.0383(8) 0.7144(8) 0.3359(5) 0.080(4) Uani 1 1 d . . . H87A H 0.0005 0.6703 0.3367 0.096 Uiso 1 1 calc R . . H87B H 0.0934 0.6865 0.3457 0.096 Uiso 1 1 calc R . . Cl9 Cl 0.0555(2) 0.7910(2) 0.25469(19) 0.1026(12) Uani 1 1 d . . . Cl10 Cl -0.0069(3) 0.7597(3) 0.3963(2) 0.1375(17) Uani 1 1 d . . . C88 C 0.4237(6) 0.8401(7) 0.2129(5) 0.066(3) Uani 1 1 d . . . H88A H 0.4095 0.7833 0.2468 0.080 Uiso 1 1 calc R . . H88B H 0.4012 0.8836 0.2357 0.080 Uiso 1 1 calc R . . Cl11 Cl 0.37499(19) 0.8550(2) 0.14342(17) 0.0840(9) Uani 1 1 d . . . Cl12 Cl 0.53583(16) 0.84753(17) 0.18629(13) 0.0628(7) Uani 1 1 d . . . C89 C 0.4190(7) 0.1161(9) 0.6594(6) 0.083(4) Uani 1 1 d . . . H89A H 0.3964 0.1178 0.7069 0.100 Uiso 1 1 calc R . . H89B H 0.3824 0.0784 0.6501 0.100 Uiso 1 1 calc R . . Cl13 Cl 0.4130(3) 0.2191(3) 0.6014(3) 0.1450(19) Uani 1 1 d . . . Cl14 Cl 0.52103(19) 0.0744(2) 0.65379(16) 0.0804(9) Uani 1 1 d . . . C90 C 0.5535(8) 0.3898(9) 0.2996(7) 0.104(5) Uani 1 1 d . . . H90A H 0.5913 0.3434 0.3217 0.124 Uiso 1 1 calc R . . H90B H 0.5693 0.4429 0.3050 0.124 Uiso 1 1 calc R . . Cl15 Cl 0.4523(2) 0.3684(3) 0.3419(3) 0.1405(18) Uani 1 1 d . . . Cl16 Cl 0.5730(3) 0.4011(3) 0.2134(2) 0.1142(13) Uani 1 1 d . . . C91 C 0.3396(7) 0.5489(7) 0.5092(5) 0.073(3) Uani 1 1 d . . . H91A H 0.2881 0.5259 0.5443 0.087 Uiso 1 1 calc R . . H91B H 0.3206 0.5836 0.4666 0.087 Uiso 1 1 calc R . . Cl17 Cl 0.3897(2) 0.6149(2) 0.53800(19) 0.1026(11) Uani 1 1 d . . . Cl18 Cl 0.4029(2) 0.4650(2) 0.49301(17) 0.0957(10) Uani 1 1 d . . . C92 C 0.0735(6) 0.5838(8) 0.5474(6) 0.093(4) Uani 1 1 d D . . H92A H 0.1179 0.5377 0.5510 0.112 Uiso 0.50 1 calc PR A 1 H92B H 0.0746 0.6079 0.4974 0.112 Uiso 0.50 1 calc PR A 1 H92C H 0.0987 0.5259 0.5641 0.112 Uiso 0.50 1 d PR A 2 H92D H 0.0682 0.5963 0.4990 0.112 Uiso 0.50 1 d PR A 2 Cl19 Cl 0.1261(5) 0.6608(3) 0.5597(3) 0.204(3) Uani 1 1 d D B . Cl1A Cl -0.0185(4) 0.5247(6) 0.5744(4) 0.114(3) Uani 0.50 1 d P B 1 Cl1B Cl -0.0276(5) 0.6005(7) 0.6029(5) 0.145(3) Uiso 0.50 1 d PD B 2 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 0.0341(6) 0.0189(5) 0.0150(5) -0.0038(4) -0.0088(4) 0.0022(4) Ni2 0.0242(5) 0.0141(5) 0.0147(5) -0.0029(3) -0.0062(4) 0.0019(4) Ni3 0.0185(5) 0.0140(5) 0.0160(5) -0.0034(3) -0.0043(4) 0.0009(4) Ni4 0.0206(5) 0.0174(5) 0.0188(5) -0.0040(4) -0.0049(4) 0.0003(4) Ni5 0.0157(5) 0.0140(4) 0.0140(5) -0.0023(3) -0.0038(4) -0.0003(3) Ni6 0.0166(5) 0.0167(5) 0.0137(5) -0.0023(3) -0.0035(4) -0.0018(4) Ni7 0.0225(5) 0.0230(5) 0.0146(5) -0.0034(4) -0.0044(4) -0.0028(4) Cl1 0.0589(13) 0.0277(10) 0.0187(9) -0.0062(7) -0.0151(9) 0.0037(9) Cl2 0.0354(11) 0.0330(10) 0.0200(9) -0.0054(8) -0.0078(8) -0.0026(8) N1 0.032(4) 0.019(3) 0.018(3) -0.001(2) -0.010(3) 0.002(3) N2 0.022(3) 0.017(3) 0.018(3) -0.003(2) -0.005(2) -0.004(2) N3 0.022(3) 0.017(3) 0.016(3) -0.001(2) -0.008(3) 0.002(2) N4 0.023(3) 0.019(3) 0.023(3) -0.007(2) -0.007(3) 0.004(2) N5 0.023(3) 0.020(3) 0.028(3) -0.008(3) -0.008(3) 0.004(3) N6 0.022(3) 0.025(3) 0.023(3) -0.006(3) -0.007(3) -0.002(3) N7 0.027(3) 0.023(3) 0.017(3) -0.001(2) 0.000(3) -0.001(3) N8 0.039(4) 0.022(3) 0.014(3) -0.006(2) -0.007(3) 0.002(3) N9 0.024(3) 0.022(3) 0.017(3) -0.006(2) -0.005(3) 0.000(2) N10 0.027(3) 0.016(3) 0.020(3) -0.001(2) -0.007(3) 0.001(2) N11 0.027(3) 0.023(3) 0.026(3) -0.006(3) -0.007(3) 0.002(3) N12 0.025(3) 0.023(3) 0.024(3) -0.006(3) -0.005(3) -0.001(3) N13 0.017(3) 0.028(3) 0.016(3) -0.001(2) -0.003(3) -0.003(3) N14 0.021(3) 0.042(4) 0.023(3) -0.008(3) -0.006(3) -0.007(3) N15 0.039(4) 0.027(3) 0.016(3) -0.002(3) -0.006(3) 0.000(3) N16 0.030(3) 0.021(3) 0.019(3) -0.003(2) -0.004(3) -0.003(3) N17 0.021(3) 0.021(3) 0.019(3) -0.006(2) -0.007(3) 0.001(2) N18 0.024(3) 0.022(3) 0.024(3) -0.004(3) -0.010(3) 0.001(3) N19 0.026(3) 0.022(3) 0.018(3) -0.005(2) -0.007(3) -0.002(3) N20 0.027(3) 0.020(3) 0.019(3) -0.004(2) -0.008(3) 0.000(3) N21 0.037(4) 0.036(4) 0.016(3) -0.009(3) -0.005(3) -0.010(3) N22 0.031(4) 0.027(3) 0.023(3) -0.009(3) -0.009(3) 0.001(3) N23 0.025(3) 0.017(3) 0.019(3) -0.005(2) -0.007(3) -0.001(2) N24 0.025(3) 0.019(3) 0.018(3) -0.006(2) -0.007(3) 0.000(2) N25 0.026(3) 0.022(3) 0.019(3) -0.006(2) -0.008(3) -0.002(3) N26 0.025(3) 0.017(3) 0.019(3) 0.002(2) -0.004(3) -0.004(2) N27 0.032(4) 0.021(3) 0.024(3) -0.006(3) -0.009(3) 0.001(3) N28 0.020(3) 0.022(3) 0.020(3) -0.003(2) -0.006(3) 0.001(2) C1 0.044(5) 0.025(4) 0.020(4) -0.005(3) -0.006(4) -0.003(3) C2 0.058(6) 0.025(4) 0.018(4) 0.004(3) -0.008(4) -0.010(4) C3 0.053(5) 0.016(4) 0.035(5) -0.002(3) -0.008(4) -0.008(4) C4 0.036(4) 0.016(4) 0.029(4) -0.004(3) -0.009(3) -0.002(3) C5 0.025(4) 0.025(4) 0.018(4) -0.006(3) -0.006(3) 0.002(3) C6 0.037(5) 0.021(4) 0.022(4) -0.006(3) -0.003(3) -0.002(3) C7 0.033(4) 0.028(4) 0.021(4) -0.006(3) -0.006(3) 0.003(3) C8 0.025(4) 0.017(4) 0.019(4) -0.007(3) -0.007(3) -0.002(3) C9 0.021(4) 0.018(4) 0.019(4) -0.005(3) -0.009(3) -0.001(3) C10 0.025(4) 0.021(4) 0.022(4) -0.004(3) -0.011(3) 0.002(3) C11 0.022(4) 0.019(4) 0.029(4) -0.011(3) -0.004(3) 0.006(3) C12 0.024(4) 0.026(4) 0.022(4) -0.012(3) 0.001(3) 0.002(3) C13 0.023(4) 0.024(4) 0.021(4) -0.004(3) -0.010(3) -0.004(3) C14 0.025(4) 0.020(4) 0.018(4) -0.006(3) -0.005(3) 0.002(3) C15 0.027(4) 0.030(4) 0.030(4) -0.005(3) -0.010(4) -0.006(3) C16 0.016(4) 0.038(5) 0.030(4) -0.003(3) 0.003(3) -0.007(3) C17 0.027(4) 0.024(4) 0.019(4) -0.007(3) 0.001(3) -0.003(3) C18 0.026(4) 0.020(4) 0.013(4) -0.004(3) 0.000(3) -0.007(3) C19 0.025(4) 0.034(4) 0.030(5) -0.006(3) 0.008(4) -0.006(3) C20 0.035(5) 0.042(5) 0.022(4) -0.002(4) -0.001(4) -0.005(4) C21 0.029(4) 0.038(5) 0.025(4) -0.001(3) -0.006(4) -0.004(4) C22 0.042(5) 0.020(4) 0.023(4) -0.009(3) -0.011(4) 0.003(3) C23 0.053(5) 0.034(5) 0.026(4) -0.013(4) -0.009(4) -0.007(4) C24 0.047(5) 0.019(4) 0.032(4) -0.013(3) -0.007(4) -0.003(3) C25 0.035(4) 0.020(4) 0.024(4) -0.008(3) 0.000(3) -0.001(3) C26 0.025(4) 0.025(4) 0.016(4) -0.009(3) -0.001(3) 0.004(3) C27 0.039(5) 0.017(4) 0.027(4) -0.006(3) -0.007(4) 0.004(3) C28 0.037(5) 0.023(4) 0.021(4) -0.003(3) -0.009(3) 0.000(3) C29 0.020(4) 0.021(4) 0.016(4) -0.003(3) -0.001(3) 0.000(3) C30 0.024(4) 0.028(4) 0.021(4) -0.007(3) -0.007(3) 0.001(3) C31 0.034(5) 0.039(5) 0.022(4) -0.014(3) -0.006(4) 0.014(4) C32 0.031(4) 0.030(4) 0.030(4) -0.012(3) -0.005(4) 0.016(3) C33 0.038(5) 0.028(4) 0.027(4) -0.009(3) -0.016(4) 0.014(3) C34 0.025(4) 0.025(4) 0.027(4) -0.006(3) -0.005(3) 0.005(3) C35 0.022(4) 0.020(4) 0.031(4) -0.004(3) -0.010(3) 0.001(3) C36 0.028(4) 0.036(5) 0.029(4) -0.002(3) -0.005(4) 0.004(4) C37 0.018(4) 0.051(5) 0.038(5) -0.011(4) -0.003(4) 0.005(4) C38 0.023(4) 0.046(5) 0.021(4) -0.003(3) -0.008(3) -0.003(3) C39 0.026(4) 0.029(4) 0.022(4) -0.002(3) -0.007(3) -0.004(3) C40 0.019(4) 0.109(9) 0.036(5) -0.012(5) -0.005(4) -0.013(5) C41 0.025(5) 0.167(12) 0.035(6) -0.026(7) -0.015(4) -0.014(6) C42 0.037(5) 0.093(8) 0.029(5) -0.010(5) -0.012(4) -0.015(5) C43 0.040(5) 0.043(5) 0.022(4) -0.012(4) -0.005(4) 0.004(4) C44 0.050(6) 0.058(6) 0.026(5) -0.011(4) 0.008(4) -0.010(5) C45 0.037(5) 0.060(6) 0.026(5) -0.010(4) 0.005(4) -0.008(4) C46 0.041(5) 0.034(5) 0.023(4) -0.007(3) -0.001(4) -0.006(4) C47 0.030(4) 0.025(4) 0.019(4) -0.002(3) 0.003(3) -0.005(3) C48 0.022(4) 0.046(5) 0.029(5) -0.008(4) 0.002(4) -0.010(4) C49 0.026(4) 0.036(5) 0.030(4) -0.012(3) -0.006(4) -0.002(3) C50 0.032(4) 0.020(4) 0.016(4) -0.003(3) -0.002(3) -0.003(3) C51 0.025(4) 0.023(4) 0.014(4) 0.001(3) -0.003(3) 0.001(3) C52 0.032(4) 0.031(4) 0.027(4) -0.004(3) 0.001(4) -0.007(4) C53 0.036(5) 0.035(5) 0.034(5) -0.006(4) -0.015(4) -0.006(4) C54 0.029(4) 0.040(5) 0.024(4) -0.010(3) -0.004(3) -0.012(4) C55 0.029(4) 0.026(4) 0.020(4) -0.004(3) -0.007(3) -0.001(3) C56 0.020(4) 0.024(4) 0.023(4) -0.004(3) -0.005(3) -0.004(3) C57 0.047(5) 0.020(4) 0.022(4) -0.004(3) -0.012(4) 0.000(3) C58 0.042(5) 0.022(4) 0.035(5) -0.009(3) -0.018(4) 0.002(3) C59 0.029(4) 0.026(4) 0.020(4) -0.008(3) -0.007(3) -0.002(3) C60 0.019(4) 0.025(4) 0.027(4) -0.011(3) -0.007(3) 0.000(3) C61 0.058(6) 0.032(5) 0.031(5) -0.014(4) -0.009(4) -0.001(4) C62 0.083(7) 0.036(5) 0.027(5) -0.009(4) -0.008(5) -0.017(5) C63 0.061(6) 0.032(5) 0.024(4) -0.010(3) -0.006(4) -0.003(4) C64 0.039(5) 0.038(5) 0.023(4) -0.008(3) -0.014(4) -0.001(4) C65 0.045(6) 0.052(6) 0.036(5) -0.010(4) -0.025(4) 0.004(4) C66 0.032(5) 0.039(5) 0.040(5) -0.012(4) -0.018(4) 0.002(4) C67 0.031(4) 0.029(4) 0.025(4) -0.012(3) -0.011(3) 0.001(3) C68 0.034(4) 0.017(4) 0.016(4) -0.004(3) -0.008(3) -0.002(3) C69 0.021(4) 0.028(4) 0.027(4) -0.007(3) -0.006(3) 0.000(3) C70 0.025(4) 0.025(4) 0.020(4) -0.008(3) -0.002(3) -0.004(3) C71 0.026(4) 0.014(3) 0.023(4) -0.007(3) -0.010(3) 0.001(3) C72 0.025(4) 0.017(4) 0.018(4) -0.007(3) -0.005(3) 0.001(3) C73 0.032(4) 0.024(4) 0.024(4) -0.002(3) -0.015(3) -0.004(3) C74 0.033(4) 0.026(4) 0.030(4) -0.007(3) -0.010(4) -0.010(3) C75 0.031(4) 0.022(4) 0.025(4) -0.001(3) -0.006(3) -0.004(3) C76 0.029(4) 0.021(4) 0.017(4) -0.005(3) -0.006(3) -0.001(3) C77 0.022(4) 0.026(4) 0.018(4) -0.003(3) -0.003(3) -0.002(3) C78 0.037(5) 0.031(4) 0.026(4) -0.010(3) -0.012(4) -0.004(3) C79 0.043(5) 0.020(4) 0.029(4) -0.001(3) -0.005(4) -0.005(3) C80 0.030(4) 0.024(4) 0.020(4) -0.004(3) -0.007(3) 0.000(3) C81 0.020(4) 0.020(4) 0.016(4) -0.004(3) -0.003(3) 0.002(3) C82 0.032(4) 0.022(4) 0.025(4) -0.001(3) -0.005(3) 0.004(3) C83 0.036(5) 0.026(4) 0.026(4) 0.002(3) -0.015(4) 0.001(3) C84 0.027(4) 0.030(4) 0.021(4) -0.004(3) -0.014(3) 0.004(3) Cl3 0.0498(13) 0.0222(10) 0.0491(13) -0.0019(9) -0.0105(10) -0.0047(9) Cl4 0.0848(19) 0.0341(12) 0.0671(16) -0.0186(11) -0.0354(14) 0.0120(12) O1 0.085(5) 0.039(4) 0.063(4) 0.002(3) -0.012(4) -0.014(3) O2 0.058(5) 0.086(5) 0.069(5) -0.005(4) -0.021(4) -0.010(4) C85 0.085(11) 0.35(3) 0.084(11) 0.091(14) 0.026(9) 0.121(15) Cl5 0.078(2) 0.199(5) 0.091(3) -0.036(3) -0.020(2) 0.021(3) Cl6 0.140(3) 0.0648(19) 0.0651(19) -0.0032(15) -0.004(2) 0.0101(19) C86 0.055(6) 0.042(5) 0.065(6) -0.014(5) -0.023(5) 0.000(4) Cl7 0.0575(17) 0.080(2) 0.103(2) 0.0126(17) -0.0383(17) -0.0050(15) Cl8 0.0467(13) 0.0441(13) 0.0577(14) -0.0215(11) -0.0128(11) -0.0059(10) C87 0.096(9) 0.080(8) 0.070(8) -0.030(6) -0.027(7) 0.017(7) Cl9 0.112(3) 0.076(2) 0.105(3) 0.0058(19) -0.039(2) -0.0139(19) Cl10 0.161(4) 0.152(4) 0.113(3) -0.078(3) -0.016(3) 0.034(3) C88 0.057(7) 0.067(7) 0.070(7) -0.019(6) -0.009(6) 0.003(5) Cl11 0.0706(19) 0.087(2) 0.103(2) -0.0338(19) -0.0252(18) -0.0147(16) Cl12 0.0469(15) 0.0738(18) 0.0602(16) -0.0176(13) -0.0035(12) 0.0047(13) C89 0.057(7) 0.138(12) 0.068(8) -0.046(8) -0.011(6) -0.015(7) Cl13 0.190(5) 0.095(3) 0.207(5) -0.093(3) -0.107(4) 0.042(3) Cl14 0.0631(18) 0.088(2) 0.089(2) -0.0355(18) -0.0008(16) -0.0048(16) C90 0.081(9) 0.083(9) 0.130(13) -0.009(9) -0.012(9) -0.024(7) Cl15 0.060(2) 0.164(4) 0.216(5) -0.104(4) 0.008(3) -0.023(2) Cl16 0.107(3) 0.127(3) 0.126(3) -0.043(3) -0.064(3) 0.021(2) C91 0.065(7) 0.075(8) 0.058(7) 0.004(6) -0.001(6) -0.017(6) Cl17 0.108(3) 0.086(2) 0.107(3) -0.016(2) -0.036(2) 0.009(2) Cl18 0.096(2) 0.107(3) 0.076(2) -0.0143(19) -0.0152(19) -0.018(2) C92 0.075(9) 0.094(10) 0.079(9) 0.023(7) -0.030(7) 0.004(7) Cl19 0.421(10) 0.078(3) 0.167(5) -0.064(3) -0.168(6) 0.077(4) Cl1A 0.063(4) 0.154(7) 0.100(5) 0.011(5) -0.043(4) -0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 N22 2.128(6) . ? Ni1 N8 2.139(6) . ? Ni1 N15 2.140(6) . ? Ni1 N1 2.148(6) . ? Ni1 Ni2 2.3255(11) . ? Ni1 Cl1 2.3888(18) . ? Ni2 N9 2.021(6) . ? Ni2 N16 2.025(6) . ? Ni2 N2 2.027(5) . ? Ni2 N23 2.036(6) . ? Ni2 Ni3 2.3178(11) . ? Ni3 N17 1.898(6) . ? Ni3 N10 1.898(5) . ? Ni3 N24 1.900(6) . ? Ni3 N3 1.901(5) . ? Ni3 Ni4 2.2860(11) . ? Ni4 N11 1.899(6) . ? Ni4 N18 1.912(6) . ? Ni4 N25 1.912(6) . ? Ni4 N4 1.914(5) . ? Ni4 Ni5 2.2936(11) . ? Ni5 N5 1.898(6) . ? Ni5 N19 1.903(6) . ? Ni5 N26 1.904(5) . ? Ni5 N12 1.910(6) . ? Ni5 Ni6 2.3249(11) . ? Ni6 N13 2.021(5) . ? Ni6 N27 2.030(6) . ? Ni6 N20 2.036(5) . ? Ni6 N6 2.038(6) . ? Ni6 Ni7 2.3317(11) . ? Ni7 N21 2.108(6) . ? Ni7 N14 2.114(6) . ? Ni7 N7 2.134(6) . ? Ni7 N28 2.157(6) . ? Ni7 Cl2 2.4608(18) . ? N1 C1 1.336(8) . ? N1 C5 1.369(8) . ? N2 C8 1.338(8) . ? N2 C5 1.374(8) . ? N3 C9 1.370(8) . ? N3 C8 1.381(8) . ? N4 C13 1.360(9) . ? N4 C9 1.379(8) . ? N5 C14 1.368(9) . ? N5 C13 1.384(8) . ? N6 C14 1.350(8) . ? N6 C18 1.366(8) . ? N7 C21 1.326(9) . ? N7 C18 1.365(8) . ? N8 C22 1.328(8) . ? N8 C26 1.361(8) . ? N9 C29 1.336(8) . ? N9 C26 1.377(8) . ? N10 C29 1.366(8) . ? N10 C30 1.410(8) . ? N11 C30 1.361(9) . ? N11 C34 1.376(9) . ? N12 C34 1.366(9) . ? N12 C35 1.385(9) . ? N13 C35 1.346(9) . ? N13 C39 1.371(9) . ? N14 C42 1.323(9) . ? N14 C39 1.358(9) . ? N15 C43 1.326(9) . ? N15 C47 1.365(9) . ? N16 C50 1.353(9) . ? N16 C47 1.363(9) . ? N17 C50 1.373(9) . ? N17 C51 1.380(8) . ? N18 C51 1.368(8) . ? N18 C55 1.370(9) . ? N19 C56 1.378(9) . ? N19 C55 1.384(9) . ? N20 C56 1.348(8) . ? N20 C60 1.362(8) . ? N21 C63 1.343(9) . ? N21 C60 1.358(9) . ? N22 C64 1.331(9) . ? N22 C68 1.378(9) . ? N23 C71 1.338(8) . ? N23 C68 1.355(8) . ? N24 C71 1.381(8) . ? N24 C72 1.388(8) . ? N25 C76 1.362(8) . ? N25 C72 1.375(8) . ? N26 C77 1.371(8) . ? N26 C76 1.386(8) . ? N27 C81 1.353(8) . ? N27 C77 1.357(8) . ? N28 C84 1.333(8) . ? N28 C81 1.360(8) . ? C1 C2 1.397(10) . ? C2 C3 1.364(10) . ? C3 C4 1.401(10) . ? C4 C6 1.411(10) . ? C4 C5 1.411(10) . ? C6 C7 1.347(9) . ? C7 C8 1.428(9) . ? C9 C10 1.386(9) . ? C10 C11 1.376(9) . ? C11 C12 1.382(9) . ? C12 C13 1.393(9) . ? C14 C15 1.429(10) . ? C15 C16 1.374(10) . ? C16 C17 1.411(10) . ? C17 C18 1.390(10) . ? C17 C19 1.402(10) . ? C19 C20 1.357(10) . ? C20 C21 1.396(10) . ? C22 C23 1.409(10) . ? C23 C24 1.350(10) . ? C24 C25 1.418(10) . ? C25 C26 1.408(10) . ? C25 C27 1.415(10) . ? C27 C28 1.344(10) . ? C28 C29 1.430(10) . ? C30 C31 1.379(10) . ? C31 C32 1.386(10) . ? C32 C33 1.363(10) . ? C33 C34 1.412(10) . ? C35 C36 1.423(10) . ? C36 C37 1.354(11) . ? C37 C38 1.426(10) . ? C38 C40 1.382(11) . ? C38 C39 1.410(10) . ? C40 C41 1.369(12) . ? C41 C42 1.391(12) . ? C43 C44 1.366(12) . ? C44 C45 1.372(12) . ? C45 C46 1.421(11) . ? C46 C47 1.408(10) . ? C46 C48 1.411(10) . ? C48 C49 1.361(10) . ? C49 C50 1.396(10) . ? C51 C52 1.380(10) . ? C52 C53 1.368(10) . ? C53 C54 1.373(10) . ? C54 C55 1.389(10) . ? C56 C57 1.426(10) . ? C57 C58 1.355(10) . ? C58 C59 1.420(10) . ? C59 C61 1.406(10) . ? C59 C60 1.418(10) . ? C61 C62 1.360(11) . ? C62 C63 1.392(11) . ? C64 C65 1.388(11) . ? C65 C66 1.367(11) . ? C66 C67 1.398(10) . ? C67 C68 1.416(10) . ? C67 C69 1.422(10) . ? C69 C70 1.347(9) . ? C70 C71 1.425(9) . ? C72 C73 1.383(9) . ? C73 C74 1.388(9) . ? C74 C75 1.377(10) . ? C75 C76 1.386(10) . ? C77 C78 1.418(10) . ? C78 C79 1.359(10) . ? C79 C80 1.439(10) . ? C80 C82 1.404(9) . ? C80 C81 1.411(10) . ? C82 C83 1.351(10) . ? C83 C84 1.401(10) . ? C85 Cl5 1.667(13) . ? C85 Cl6 1.84(2) . ? C86 Cl7 1.732(9) . ? C86 Cl8 1.777(10) . ? C87 Cl10 1.676(11) . ? C87 Cl9 1.746(11) . ? C88 Cl11 1.743(10) . ? C88 Cl12 1.766(10) . ? C89 Cl14 1.710(11) . ? C89 Cl13 1.756(13) . ? C90 Cl15 1.679(13) . ? C90 Cl16 1.716(15) . ? C91 Cl18 1.725(12) . ? C91 Cl17 1.743(12) . ? C92 Cl19 1.715(14) . ? C92 Cl1A 1.737(13) . ? C92 Cl1B 1.832(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 N22 Ni1 N8 89.3(2) . . ? N22 Ni1 N15 169.1(2) . . ? N8 Ni1 N15 90.2(2) . . ? N22 Ni1 N1 89.9(2) . . ? N8 Ni1 N1 168.7(2) . . ? N15 Ni1 N1 88.4(2) . . ? N22 Ni1 Ni2 84.48(15) . . ? N8 Ni1 Ni2 84.21(15) . . ? N15 Ni1 Ni2 84.67(15) . . ? N1 Ni1 Ni2 84.47(14) . . ? N22 Ni1 Cl1 94.80(16) . . ? N8 Ni1 Cl1 95.61(15) . . ? N15 Ni1 Cl1 96.05(16) . . ? N1 Ni1 Cl1 95.72(15) . . ? Ni2 Ni1 Cl1 179.26(7) . . ? N9 Ni2 N16 90.6(2) . . ? N9 Ni2 N2 171.8(2) . . ? N16 Ni2 N2 88.1(2) . . ? N9 Ni2 N23 90.7(2) . . ? N16 Ni2 N23 172.5(2) . . ? N2 Ni2 N23 89.6(2) . . ? N9 Ni2 Ni3 85.96(15) . . ? N16 Ni2 Ni3 86.79(16) . . ? N2 Ni2 Ni3 85.86(15) . . ? N23 Ni2 Ni3 85.90(15) . . ? N9 Ni2 Ni1 94.03(15) . . ? N16 Ni2 Ni1 93.37(16) . . ? N2 Ni2 Ni1 94.16(15) . . ? N23 Ni2 Ni1 93.95(15) . . ? Ni3 Ni2 Ni1 179.85(6) . . ? N17 Ni3 N10 90.1(2) . . ? N17 Ni3 N24 177.3(2) . . ? N10 Ni3 N24 90.9(2) . . ? N17 Ni3 N3 88.7(2) . . ? N10 Ni3 N3 177.2(2) . . ? N24 Ni3 N3 90.2(2) . . ? N17 Ni3 Ni4 88.25(16) . . ? N10 Ni3 Ni4 88.41(16) . . ? N24 Ni3 Ni4 89.25(16) . . ? N3 Ni3 Ni4 89.06(16) . . ? N17 Ni3 Ni2 90.88(16) . . ? N10 Ni3 Ni2 90.95(17) . . ? N24 Ni3 Ni2 91.63(16) . . ? N3 Ni3 Ni2 91.56(16) . . ? Ni4 Ni3 Ni2 178.92(5) . . ? N11 Ni4 N18 90.6(2) . . ? N11 Ni4 N25 91.8(2) . . ? N18 Ni4 N25 177.5(2) . . ? N11 Ni4 N4 179.2(2) . . ? N18 Ni4 N4 88.6(2) . . ? N25 Ni4 N4 89.0(2) . . ? N11 Ni4 Ni3 90.61(17) . . ? N18 Ni4 Ni3 90.35(17) . . ? N25 Ni4 Ni3 89.60(16) . . ? N4 Ni4 Ni3 89.37(17) . . ? N11 Ni4 Ni5 89.40(17) . . ? N18 Ni4 Ni5 89.48(17) . . ? N25 Ni4 Ni5 90.58(16) . . ? N4 Ni4 Ni5 90.62(17) . . ? Ni3 Ni4 Ni5 179.83(6) . . ? N5 Ni5 N19 89.8(2) . . ? N5 Ni5 N26 89.1(2) . . ? N19 Ni5 N26 176.6(2) . . ? N5 Ni5 N12 176.9(2) . . ? N19 Ni5 N12 90.8(2) . . ? N26 Ni5 N12 90.2(2) . . ? N5 Ni5 Ni4 87.51(17) . . ? N19 Ni5 Ni4 89.27(16) . . ? N26 Ni5 Ni4 87.49(16) . . ? N12 Ni5 Ni4 89.42(17) . . ? N5 Ni5 Ni6 91.50(17) . . ? N19 Ni5 Ni6 91.94(16) . . ? N26 Ni5 Ni6 91.28(16) . . ? N12 Ni5 Ni6 91.55(17) . . ? Ni4 Ni5 Ni6 178.44(5) . . ? N13 Ni6 N27 89.6(2) . . ? N13 Ni6 N20 90.2(2) . . ? N27 Ni6 N20 172.0(2) . . ? N13 Ni6 N6 172.3(2) . . ? N27 Ni6 N6 90.2(2) . . ? N20 Ni6 N6 88.9(2) . . ? N13 Ni6 Ni5 86.09(16) . . ? N27 Ni6 Ni5 86.35(16) . . ? N20 Ni6 Ni5 85.65(15) . . ? N6 Ni6 Ni5 86.25(16) . . ? N13 Ni6 Ni7 94.19(16) . . ? N27 Ni6 Ni7 93.79(16) . . ? N20 Ni6 Ni7 94.21(15) . . ? N6 Ni6 Ni7 93.48(16) . . ? Ni5 Ni6 Ni7 179.69(5) . . ? N21 Ni7 N14 88.9(2) . . ? N21 Ni7 N7 87.6(2) . . ? N14 Ni7 N7 168.8(2) . . ? N21 Ni7 N28 168.8(2) . . ? N14 Ni7 N28 90.5(2) . . ? N7 Ni7 N28 90.8(2) . . ? N21 Ni7 Ni6 84.32(15) . . ? N14 Ni7 Ni6 83.80(16) . . ? N7 Ni7 Ni6 85.22(15) . . ? N28 Ni7 Ni6 84.49(15) . . ? N21 Ni7 Cl2 96.65(16) . . ? N14 Ni7 Cl2 95.88(16) . . ? N7 Ni7 Cl2 95.14(15) . . ? N28 Ni7 Cl2 94.54(15) . . ? Ni6 Ni7 Cl2 178.97(6) . . ? C1 N1 C5 117.1(6) . . ? C1 N1 Ni1 119.9(5) . . ? C5 N1 Ni1 122.9(4) . . ? C8 N2 C5 119.3(6) . . ? C8 N2 Ni2 121.4(4) . . ? C5 N2 Ni2 118.2(4) . . ? C9 N3 C8 122.6(5) . . ? C9 N3 Ni3 119.6(4) . . ? C8 N3 Ni3 117.7(4) . . ? C13 N4 C9 121.5(6) . . ? C13 N4 Ni4 118.8(4) . . ? C9 N4 Ni4 119.7(4) . . ? C14 N5 C13 121.1(6) . . ? C14 N5 Ni5 119.0(4) . . ? C13 N5 Ni5 119.9(5) . . ? C14 N6 C18 119.6(6) . . ? C14 N6 Ni6 120.4(5) . . ? C18 N6 Ni6 119.7(4) . . ? C21 N7 C18 116.2(6) . . ? C21 N7 Ni7 120.0(5) . . ? C18 N7 Ni7 123.7(4) . . ? C22 N8 C26 117.0(6) . . ? C22 N8 Ni1 119.5(4) . . ? C26 N8 Ni1 123.3(4) . . ? C29 N9 C26 119.7(6) . . ? C29 N9 Ni2 121.4(4) . . ? C26 N9 Ni2 118.6(4) . . ? C29 N10 C30 122.3(6) . . ? C29 N10 Ni3 119.2(4) . . ? C30 N10 Ni3 118.4(4) . . ? C30 N11 C34 120.0(6) . . ? C30 N11 Ni4 119.8(5) . . ? C34 N11 Ni4 120.2(5) . . ? C34 N12 C35 123.3(6) . . ? C34 N12 Ni5 118.5(5) . . ? C35 N12 Ni5 118.2(5) . . ? C35 N13 C39 119.2(6) . . ? C35 N13 Ni6 121.8(4) . . ? C39 N13 Ni6 118.6(5) . . ? C42 N14 C39 116.6(7) . . ? C42 N14 Ni7 118.1(5) . . ? C39 N14 Ni7 125.3(5) . . ? C43 N15 C47 116.5(7) . . ? C43 N15 Ni1 120.8(5) . . ? C47 N15 Ni1 122.3(5) . . ? C50 N16 C47 119.8(6) . . ? C50 N16 Ni2 120.5(5) . . ? C47 N16 Ni2 119.3(5) . . ? C50 N17 C51 121.7(6) . . ? C50 N17 Ni3 120.1(4) . . ? C51 N17 Ni3 118.1(4) . . ? C51 N18 C55 121.1(6) . . ? C51 N18 Ni4 118.6(5) . . ? C55 N18 Ni4 120.1(5) . . ? C56 N19 C55 122.0(6) . . ? C56 N19 Ni5 117.8(4) . . ? C55 N19 Ni5 119.7(4) . . ? C56 N20 C60 120.4(6) . . ? C56 N20 Ni6 121.3(5) . . ? C60 N20 Ni6 117.6(4) . . ? C63 N21 C60 116.1(6) . . ? C63 N21 Ni7 119.3(5) . . ? C60 N21 Ni7 124.6(5) . . ? C64 N22 C68 116.6(6) . . ? C64 N22 Ni1 119.9(5) . . ? C68 N22 Ni1 123.3(5) . . ? C71 N23 C68 119.9(6) . . ? C71 N23 Ni2 120.9(4) . . ? C68 N23 Ni2 118.6(4) . . ? C71 N24 C72 122.0(6) . . ? C71 N24 Ni3 117.7(4) . . ? C72 N24 Ni3 120.1(4) . . ? C76 N25 C72 120.5(6) . . ? C76 N25 Ni4 119.0(4) . . ? C72 N25 Ni4 120.4(4) . . ? C77 N26 C76 121.5(6) . . ? C77 N26 Ni5 119.2(4) . . ? C76 N26 Ni5 119.2(4) . . ? C81 N27 C77 119.4(6) . . ? C81 N27 Ni6 119.8(4) . . ? C77 N27 Ni6 120.6(4) . . ? C84 N28 C81 117.2(6) . . ? C84 N28 Ni7 119.5(5) . . ? C81 N28 Ni7 123.2(4) . . ? N1 C1 C2 124.1(7) . . ? C3 C2 C1 118.3(7) . . ? C2 C3 C4 120.3(7) . . ? C3 C4 C6 123.9(7) . . ? C3 C4 C5 117.6(7) . . ? C6 C4 C5 118.4(6) . . ? N1 C5 N2 116.2(6) . . ? N1 C5 C4 122.4(6) . . ? N2 C5 C4 121.4(6) . . ? C7 C6 C4 119.3(7) . . ? C6 C7 C8 120.5(7) . . ? N2 C8 N3 115.5(6) . . ? N2 C8 C7 120.9(6) . . ? N3 C8 C7 123.4(6) . . ? N3 C9 N4 115.5(6) . . ? N3 C9 C10 125.6(6) . . ? N4 C9 C10 118.8(6) . . ? C11 C10 C9 119.4(6) . . ? C10 C11 C12 121.8(6) . . ? C11 C12 C13 117.8(6) . . ? N4 C13 N5 115.7(6) . . ? N4 C13 C12 120.4(6) . . ? N5 C13 C12 123.7(6) . . ? N6 C14 N5 116.2(6) . . ? N6 C14 C15 120.6(6) . . ? N5 C14 C15 123.0(6) . . ? C16 C15 C14 119.3(7) . . ? C15 C16 C17 119.6(7) . . ? C18 C17 C19 119.1(7) . . ? C18 C17 C16 118.5(6) . . ? C19 C17 C16 122.3(7) . . ? N7 C18 N6 115.7(6) . . ? N7 C18 C17 122.3(6) . . ? N6 C18 C17 122.0(6) . . ? C20 C19 C17 118.9(7) . . ? C19 C20 C21 118.3(7) . . ? N7 C21 C20 125.1(7) . . ? N8 C22 C23 124.0(7) . . ? C24 C23 C22 119.1(7) . . ? C23 C24 C25 119.1(7) . . ? C26 C25 C27 117.7(6) . . ? C26 C25 C24 117.9(6) . . ? C27 C25 C24 124.4(7) . . ? N8 C26 N9 115.7(6) . . ? N8 C26 C25 122.8(6) . . ? N9 C26 C25 121.5(6) . . ? C28 C27 C25 120.2(7) . . ? C27 C28 C29 120.2(6) . . ? N9 C29 N10 115.6(6) . . ? N9 C29 C28 120.7(6) . . ? N10 C29 C28 123.5(6) . . ? N11 C30 C31 121.2(6) . . ? N11 C30 N10 115.2(6) . . ? C31 C30 N10 123.3(6) . . ? C30 C31 C32 118.4(7) . . ? C33 C32 C31 121.2(7) . . ? C32 C33 C34 119.0(7) . . ? N12 C34 N11 116.5(6) . . ? N12 C34 C33 124.2(6) . . ? N11 C34 C33 119.3(6) . . ? N13 C35 N12 115.6(6) . . ? N13 C35 C36 120.5(6) . . ? N12 C35 C36 123.7(7) . . ? C37 C36 C35 120.8(7) . . ? C36 C37 C38 119.7(7) . . ? C40 C38 C39 119.2(7) . . ? C40 C38 C37 123.8(7) . . ? C39 C38 C37 117.0(6) . . ? N14 C39 N13 114.9(6) . . ? N14 C39 C38 122.4(6) . . ? N13 C39 C38 122.7(6) . . ? C41 C40 C38 117.9(8) . . ? C40 C41 C42 119.7(8) . . ? N14 C42 C41 124.1(8) . . ? N15 C43 C44 124.4(8) . . ? C43 C44 C45 121.0(8) . . ? C44 C45 C46 117.0(8) . . ? C47 C46 C48 118.5(7) . . ? C47 C46 C45 118.2(7) . . ? C48 C46 C45 123.2(7) . . ? N16 C47 N15 116.1(6) . . ? N16 C47 C46 121.1(7) . . ? N15 C47 C46 122.9(6) . . ? C49 C48 C46 118.9(7) . . ? C48 C49 C50 121.0(7) . . ? N16 C50 N17 115.6(6) . . ? N16 C50 C49 120.7(6) . . ? N17 C50 C49 123.6(6) . . ? N18 C51 N17 116.1(6) . . ? N18 C51 C52 118.7(6) . . ? N17 C51 C52 124.9(6) . . ? C53 C52 C51 120.0(7) . . ? C52 C53 C54 121.0(7) . . ? C53 C54 C55 118.2(7) . . ? N18 C55 N19 115.7(6) . . ? N18 C55 C54 119.6(6) . . ? N19 C55 C54 124.6(6) . . ? N20 C56 N19 115.5(6) . . ? N20 C56 C57 120.1(6) . . ? N19 C56 C57 124.2(6) . . ? C58 C57 C56 121.0(7) . . ? C57 C58 C59 118.6(7) . . ? C61 C59 C60 118.2(6) . . ? C61 C59 C58 122.9(7) . . ? C60 C59 C58 118.8(6) . . ? N21 C60 N20 116.6(6) . . ? N21 C60 C59 122.7(6) . . ? N20 C60 C59 120.8(6) . . ? C62 C61 C59 119.2(8) . . ? C61 C62 C63 118.8(8) . . ? N21 C63 C62 125.0(7) . . ? N22 C64 C65 125.4(7) . . ? C66 C65 C64 117.9(7) . . ? C65 C66 C67 120.2(8) . . ? C66 C67 C68 118.2(7) . . ? C66 C67 C69 125.1(7) . . ? C68 C67 C69 116.8(6) . . ? N23 C68 N22 116.0(6) . . ? N23 C68 C67 122.3(6) . . ? N22 C68 C67 121.7(6) . . ? C70 C69 C67 120.3(7) . . ? C69 C70 C71 120.1(6) . . ? N23 C71 N24 116.0(6) . . ? N23 C71 C70 120.6(6) . . ? N24 C71 C70 123.3(6) . . ? N25 C72 C73 119.9(6) . . ? N25 C72 N24 114.8(6) . . ? C73 C72 N24 125.1(6) . . ? C72 C73 C74 118.9(6) . . ? C75 C74 C73 120.8(7) . . ? C74 C75 C76 118.8(6) . . ? N25 C76 N26 115.4(6) . . ? N25 C76 C75 120.3(6) . . ? N26 C76 C75 124.0(6) . . ? N27 C77 N26 116.1(6) . . ? N27 C77 C78 121.0(6) . . ? N26 C77 C78 122.8(6) . . ? C79 C78 C77 120.4(7) . . ? C78 C79 C80 119.1(7) . . ? C82 C80 C81 119.0(6) . . ? C82 C80 C79 123.4(7) . . ? C81 C80 C79 117.6(6) . . ? N27 C81 N28 116.0(6) . . ? N27 C81 C80 122.3(6) . . ? N28 C81 C80 121.6(6) . . ? C83 C82 C80 118.9(7) . . ? C82 C83 C84 119.1(6) . . ? N28 C84 C83 124.1(6) . . ? Cl5 C85 Cl6 108.9(11) . . ? Cl7 C86 Cl8 112.6(5) . . ? Cl10 C87 Cl9 110.3(7) . . ? Cl11 C88 Cl12 111.4(6) . . ? Cl14 C89 Cl13 112.5(7) . . ? Cl15 C90 Cl16 115.5(8) . . ? Cl18 C91 Cl17 114.4(6) . . ? Cl19 C92 Cl1A 145.3(8) . . ? Cl19 C92 Cl1B 94.8(7) . . ? Cl1A C92 Cl1B 51.2(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.759 _refine_diff_density_min -1.540 _refine_diff_density_rms 0.194 # Attachment 'compound 3.cif' data_ic13246 _database_code_depnum_ccdc_archive 'CCDC 753223' #TrackingRef 'compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C124 H108 Cl2 F12 N42 Ni9 O5 P2' _chemical_formula_weight 3155.75 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.3842(3) _cell_length_b 20.5272(4) _cell_length_c 21.7735(4) _cell_angle_alpha 107.5094(10) _cell_angle_beta 91.1126(12) _cell_angle_gamma 103.7607(10) _cell_volume 6750.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3220 _exptl_absorpt_coefficient_mu 1.375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90057 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 23421 _reflns_number_gt 12641 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(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^)+(0.1020P)^2^+66.0230P] 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_number_reflns 23421 _refine_ls_number_parameters 1526 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1567 _refine_ls_R_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.3004 _refine_ls_wR_factor_gt 0.2494 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 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 0.98454(8) 1.18751(6) 0.45128(5) 0.0434(3) Uani 1 1 d . . . Ni2 Ni 0.94583(7) 1.26576(6) 0.54005(5) 0.0375(3) Uani 1 1 d . . . Ni3 Ni 0.90689(7) 1.34334(6) 0.62781(5) 0.0352(3) Uani 1 1 d . . . Ni4 Ni 0.86705(7) 1.42021(5) 0.71361(5) 0.0329(3) Uani 1 1 d . . . Ni5 Ni 0.82824(7) 1.49638(6) 0.79808(5) 0.0345(3) Uani 1 1 d . . . Ni6 Ni 0.78989(7) 1.57334(5) 0.88199(5) 0.0322(3) Uani 1 1 d . . . Ni7 Ni 0.75139(7) 1.65140(6) 0.96760(5) 0.0340(3) Uani 1 1 d . . . Ni8 Ni 0.71602(7) 1.73167(6) 1.05536(5) 0.0370(3) Uani 1 1 d . . . Ni9 Ni 0.68109(8) 1.81300(6) 1.14346(5) 0.0444(3) Uani 1 1 d . . . Cl1 Cl 1.02421(18) 1.10646(13) 0.36044(12) 0.0578(7) Uani 1 1 d . . . Cl2 Cl 0.64669(18) 1.89645(14) 1.23606(12) 0.0607(7) Uani 1 1 d . . . N1 N 1.0362(5) 1.1527(4) 0.5228(4) 0.0460(19) Uani 1 1 d . . . N2 N 1.0265(5) 1.2522(4) 0.6044(3) 0.0394(17) Uani 1 1 d . . . N3 N 1.0061(5) 1.3512(4) 0.6802(3) 0.0382(17) Uani 1 1 d . . . N4 N 0.9819(4) 1.4531(4) 0.7520(3) 0.0348(16) Uani 1 1 d . . . N5 N 0.9425(4) 1.5504(4) 0.8191(3) 0.0348(16) Uani 1 1 d . . . N6 N 0.8915(5) 1.6425(4) 0.8829(3) 0.0373(17) Uani 1 1 d . . . N7 N 0.8289(5) 1.7250(4) 0.9473(3) 0.0409(18) Uani 1 1 d . . . N8 N 0.7657(5) 1.8061(4) 1.0130(4) 0.0438(19) Uani 1 1 d . . . N9 N 0.6992(5) 1.8807(4) 1.0845(4) 0.053(2) Uani 1 1 d . . . N10 N 1.0987(5) 1.2699(4) 0.4676(4) 0.0466(19) Uani 1 1 d . . . N11 N 1.0372(5) 1.3501(4) 0.5362(3) 0.0383(17) Uani 1 1 d . . . N12 N 0.9660(5) 1.4226(4) 0.6038(3) 0.0404(18) Uani 1 1 d . . . N13 N 0.8894(5) 1.4914(4) 0.6718(3) 0.0374(17) Uani 1 1 d . . . N14 N 0.8102(5) 1.5510(4) 0.7447(3) 0.0400(18) Uani 1 1 d . . . N15 N 0.7333(5) 1.6062(4) 0.8240(3) 0.0362(17) Uani 1 1 d . . . N16 N 0.6649(5) 1.6574(4) 0.9112(3) 0.0404(18) Uani 1 1 d . . . N17 N 0.6053(5) 1.7109(4) 1.0013(3) 0.0397(17) Uani 1 1 d . . . N18 N 0.5562(5) 1.7682(4) 1.0967(4) 0.0464(19) Uani 1 1 d . . . N19 N 0.9272(5) 1.2390(4) 0.3976(3) 0.048(2) Uani 1 1 d . . . N20 N 0.8633(5) 1.2901(4) 0.4865(3) 0.0432(19) Uani 1 1 d . . . N21 N 0.8062(5) 1.3391(4) 0.5798(3) 0.0392(17) Uani 1 1 d . . . N22 N 0.7520(4) 1.3886(4) 0.6759(3) 0.0371(17) Uani 1 1 d . . . N23 N 0.7140(5) 1.4434(4) 0.7771(3) 0.0383(17) Uani 1 1 d . . . N24 N 0.6881(4) 1.5028(3) 0.8799(3) 0.0348(16) Uani 1 1 d . . . N25 N 0.6761(4) 1.5731(4) 0.9839(3) 0.0369(17) Uani 1 1 d . . . N26 N 0.6707(5) 1.6473(4) 1.0868(3) 0.0395(17) Uani 1 1 d . . . N27 N 0.6668(5) 1.7284(4) 1.1858(3) 0.0458(19) Uani 1 1 d . . . N28 N 0.8629(5) 1.1216(4) 0.4514(4) 0.0459(19) Uani 1 1 d . . . N29 N 0.8501(5) 1.1912(4) 0.5552(3) 0.0407(18) Uani 1 1 d . . . N30 N 0.8458(5) 1.2677(4) 0.6557(3) 0.0384(17) Uani 1 1 d . . . N31 N 0.8428(4) 1.3496(4) 0.7559(3) 0.0363(17) Uani 1 1 d . . . N32 N 0.8445(5) 1.4406(4) 0.8507(3) 0.0370(17) Uani 1 1 d . . . N33 N 0.8442(4) 1.5379(4) 0.9393(3) 0.0358(16) Uani 1 1 d . . . N34 N 0.8391(5) 1.6413(4) 1.0198(3) 0.0404(18) Uani 1 1 d . . . N35 N 0.8310(5) 1.7425(4) 1.0981(3) 0.0404(18) Uani 1 1 d . . . N36 N 0.8141(5) 1.8453(4) 1.1722(3) 0.0465(19) Uani 1 1 d . . . C1 C 1.0604(7) 1.0932(5) 0.5054(5) 0.054(3) Uani 1 1 d . . . H1 H 1.0448 1.0632 0.4620 0.064 Uiso 1 1 calc R . . C2 C 1.1067(8) 1.0711(6) 0.5454(5) 0.063(3) Uani 1 1 d . . . H2 H 1.1214 1.0273 0.5298 0.075 Uiso 1 1 calc R . . C3 C 1.1309(7) 1.1137(6) 0.6080(5) 0.058(3) Uani 1 1 d . . . H3 H 1.1649 1.1010 0.6360 0.070 Uiso 1 1 calc R . . C4 C 1.1048(7) 1.1767(5) 0.6302(5) 0.052(3) Uani 1 1 d . . . C5 C 1.0554(6) 1.1936(5) 0.5860(4) 0.039(2) Uani 1 1 d . . . C6 C 1.1230(6) 1.2232(5) 0.6946(5) 0.051(3) Uani 1 1 d . . . H6 H 1.1556 1.2134 0.7256 0.062 Uiso 1 1 calc R . . C7 C 1.0932(6) 1.2821(5) 0.7114(4) 0.048(2) Uani 1 1 d . . . H7 H 1.1059 1.3139 0.7543 0.058 Uiso 1 1 calc R . . C8 C 1.0433(6) 1.2962(5) 0.6652(4) 0.041(2) Uani 1 1 d . . . C9 C 1.0393(6) 1.4147(5) 0.7295(4) 0.039(2) Uani 1 1 d . . . C10 C 1.1230(6) 1.4414(5) 0.7514(4) 0.047(2) Uani 1 1 d . . . H10 H 1.1635 1.4165 0.7338 0.057 Uiso 1 1 calc R . . C11 C 1.1469(6) 1.5052(5) 0.7993(5) 0.051(3) Uani 1 1 d . . . H11 H 1.2048 1.5234 0.8155 0.061 Uiso 1 1 calc R . . C12 C 1.0914(6) 1.5440(5) 0.8251(4) 0.044(2) Uani 1 1 d . . . H12 H 1.1098 1.5871 0.8596 0.052 Uiso 1 1 calc R . . C13 C 1.0062(6) 1.5184(5) 0.7991(4) 0.039(2) Uani 1 1 d . . . C14 C 0.9568(6) 1.6222(5) 0.8484(4) 0.041(2) Uani 1 1 d . . . C15 C 1.0252(6) 1.6728(5) 0.8428(4) 0.049(2) Uani 1 1 d . . . H15 H 1.0677 1.6599 0.8161 0.059 Uiso 1 1 calc R . . C16 C 1.0316(7) 1.7433(6) 0.8769(5) 0.062(3) Uani 1 1 d . . . H16 H 1.0801 1.7783 0.8747 0.074 Uiso 1 1 calc R . . C17 C 0.9700(7) 1.7633(5) 0.9135(5) 0.057(3) Uani 1 1 d . . . H17 H 0.9767 1.8113 0.9385 0.069 Uiso 1 1 calc R . . C18 C 0.8966(6) 1.7117(5) 0.9137(4) 0.046(2) Uani 1 1 d . . . C19 C 0.8093(6) 1.7902(5) 0.9619(4) 0.044(2) Uani 1 1 d . . . C20 C 0.8266(8) 1.8341(5) 0.9215(5) 0.061(3) Uani 1 1 d . . . H20 H 0.8571 1.8218 0.8849 0.073 Uiso 1 1 calc R . . C21 C 0.7989(9) 1.8935(6) 0.9360(6) 0.077(4) Uani 1 1 d . . . H21 H 0.8084 1.9223 0.9085 0.092 Uiso 1 1 calc R . . C22 C 0.7558(8) 1.9133(6) 0.9915(6) 0.068(3) Uani 1 1 d . . . C23 C 0.7414(7) 1.8672(5) 1.0295(5) 0.051(3) Uani 1 1 d . . . C24 C 0.7273(10) 1.9750(7) 1.0120(7) 0.087(4) Uani 1 1 d . . . H24 H 0.7383 2.0085 0.9891 0.104 Uiso 1 1 calc R . . C25 C 0.6834(9) 1.9863(7) 1.0656(7) 0.086(4) Uani 1 1 d . . . H25 H 0.6611 2.0265 1.0789 0.103 Uiso 1 1 calc R . . C26 C 0.6718(8) 1.9388(6) 1.1003(6) 0.072(3) Uani 1 1 d . . . H26 H 0.6423 1.9485 1.1378 0.086 Uiso 1 1 calc R . . C27 C 1.1642(7) 1.2563(6) 0.4362(5) 0.064(3) Uani 1 1 d . . . H27 H 1.1595 1.2094 0.4092 0.077 Uiso 1 1 calc R . . C28 C 1.2404(8) 1.3075(7) 0.4406(6) 0.079(4) Uani 1 1 d . . . H28 H 1.2858 1.2947 0.4175 0.095 Uiso 1 1 calc R . . C29 C 1.2488(7) 1.3757(6) 0.4785(6) 0.068(3) Uani 1 1 d . . . H29 H 1.2995 1.4111 0.4818 0.082 Uiso 1 1 calc R . . C30 C 1.1810(7) 1.3920(5) 0.5124(5) 0.053(3) Uani 1 1 d . . . C31 C 1.1063(6) 1.3377(5) 0.5058(4) 0.046(2) Uani 1 1 d . . . C32 C 1.1815(7) 1.4608(6) 0.5541(5) 0.060(3) Uani 1 1 d . . . H32 H 1.2312 1.4983 0.5620 0.072 Uiso 1 1 calc R . . C33 C 1.1115(7) 1.4725(5) 0.5825(5) 0.050(2) Uani 1 1 d . . . H33 H 1.1118 1.5188 0.6089 0.060 Uiso 1 1 calc R . . C34 C 1.0381(6) 1.4170(5) 0.5734(4) 0.042(2) Uani 1 1 d . . . C35 C 0.9418(6) 1.4852(5) 0.6228(4) 0.041(2) Uani 1 1 d . . . C36 C 0.9609(7) 1.5375(5) 0.5936(4) 0.048(2) Uani 1 1 d . . . H36 H 0.9939 1.5325 0.5579 0.058 Uiso 1 1 calc R . . C37 C 0.9316(6) 1.5966(5) 0.6169(4) 0.048(2) Uani 1 1 d . . . H37 H 0.9465 1.6332 0.5978 0.058 Uiso 1 1 calc R . . C38 C 0.8818(6) 1.6043(5) 0.6665(4) 0.048(2) Uani 1 1 d . . . H38 H 0.8633 1.6463 0.6826 0.057 Uiso 1 1 calc R . . C39 C 0.8584(6) 1.5498(5) 0.6935(4) 0.039(2) Uani 1 1 d . . . C40 C 0.7530(6) 1.5914(5) 0.7610(4) 0.043(2) Uani 1 1 d . . . C41 C 0.7094(7) 1.6123(6) 0.7178(4) 0.053(3) Uani 1 1 d . . . H41 H 0.7182 1.5990 0.6732 0.063 Uiso 1 1 calc R . . C42 C 0.6538(7) 1.6521(6) 0.7403(5) 0.055(3) Uani 1 1 d . . . H42 H 0.6260 1.6681 0.7112 0.066 Uiso 1 1 calc R . . C43 C 0.6370(7) 1.6696(6) 0.8045(5) 0.053(3) Uani 1 1 d . . . H43 H 0.5996 1.6986 0.8199 0.064 Uiso 1 1 calc R . . C44 C 0.6764(6) 1.6436(5) 0.8461(4) 0.042(2) Uani 1 1 d . . . C45 C 0.5937(6) 1.6745(5) 0.9379(4) 0.042(2) Uani 1 1 d . . . C46 C 0.5123(6) 1.6499(5) 0.9036(5) 0.048(2) Uani 1 1 d . . . H46 H 0.5052 1.6236 0.8589 0.058 Uiso 1 1 calc R . . C47 C 0.4443(7) 1.6640(5) 0.9348(5) 0.054(3) Uani 1 1 d . . . H47 H 0.3895 1.6468 0.9121 0.064 Uiso 1 1 calc R . . C48 C 0.4554(6) 1.7044(5) 1.0013(5) 0.048(2) Uani 1 1 d . . . C49 C 0.5382(6) 1.7277(5) 1.0324(4) 0.044(2) Uani 1 1 d . . . C50 C 0.3902(7) 1.7220(6) 1.0373(5) 0.062(3) Uani 1 1 d . . . H50 H 0.3336 1.7065 1.0178 0.075 Uiso 1 1 calc R . . C51 C 0.4082(7) 1.7621(6) 1.1015(6) 0.069(3) Uani 1 1 d . . . H51 H 0.3646 1.7747 1.1270 0.083 Uiso 1 1 calc R . . C52 C 0.4919(7) 1.7839(5) 1.1282(5) 0.054(3) Uani 1 1 d . . . H52 H 0.5036 1.8123 1.1723 0.065 Uiso 1 1 calc R . . C53 C 0.9401(7) 1.2292(5) 0.3346(5) 0.057(3) Uani 1 1 d . . . H53 H 0.9782 1.2018 0.3165 0.068 Uiso 1 1 calc R . . C54 C 0.9013(8) 1.2564(7) 0.2949(5) 0.071(3) Uani 1 1 d . . . H54 H 0.9127 1.2477 0.2510 0.085 Uiso 1 1 calc R . . C55 C 0.8460(8) 1.2966(6) 0.3197(5) 0.067(3) Uani 1 1 d . . . H55 H 0.8197 1.3167 0.2933 0.080 Uiso 1 1 calc R . . C56 C 0.8289(7) 1.3075(6) 0.3846(4) 0.055(3) Uani 1 1 d . . . C57 C 0.8726(6) 1.2792(5) 0.4222(4) 0.045(2) Uani 1 1 d . . . C58 C 0.7718(7) 1.3456(6) 0.4145(5) 0.057(3) Uani 1 1 d . . . H58 H 0.7408 1.3647 0.3902 0.068 Uiso 1 1 calc R . . C59 C 0.7609(7) 1.3552(5) 0.4782(4) 0.049(2) Uani 1 1 d . . . H59 H 0.7223 1.3809 0.4985 0.058 Uiso 1 1 calc R . . C60 C 0.8080(6) 1.3264(5) 0.5139(4) 0.044(2) Uani 1 1 d . . . C61 C 0.7360(6) 1.3507(5) 0.6107(4) 0.042(2) Uani 1 1 d . . . C62 C 0.6539(6) 1.3226(5) 0.5842(4) 0.050(2) Uani 1 1 d . . . H62 H 0.6416 1.2922 0.5407 0.060 Uiso 1 1 calc R . . C63 C 0.5885(7) 1.3384(6) 0.6210(5) 0.057(3) Uani 1 1 d . . . H63 H 0.5318 1.3209 0.6019 0.069 Uiso 1 1 calc R . . C64 C 0.6058(6) 1.3791(6) 0.6847(4) 0.052(3) Uani 1 1 d . . . H64 H 0.5614 1.3914 0.7093 0.063 Uiso 1 1 calc R . . C65 C 0.6883(6) 1.4022(5) 0.7129(4) 0.038(2) Uani 1 1 d . . . C66 C 0.6626(5) 1.4448(5) 0.8270(4) 0.037(2) Uani 1 1 d . . . C67 C 0.5944(6) 1.3901(5) 0.8281(4) 0.043(2) Uani 1 1 d . . . H67 H 0.5778 1.3482 0.7921 0.052 Uiso 1 1 calc R . . C68 C 0.5513(6) 1.3979(5) 0.8822(4) 0.045(2) Uani 1 1 d . . . H68 H 0.5043 1.3609 0.8832 0.054 Uiso 1 1 calc R . . C69 C 0.5745(6) 1.4575(5) 0.9347(4) 0.041(2) Uani 1 1 d . . . H69 H 0.5424 1.4630 0.9709 0.049 Uiso 1 1 calc R . . C70 C 0.6449(6) 1.5094(5) 0.9342(4) 0.038(2) Uani 1 1 d . . . C71 C 0.6643(6) 1.5807(5) 1.0482(4) 0.042(2) Uani 1 1 d . . . C72 C 0.6520(6) 1.5237(5) 1.0745(4) 0.043(2) Uani 1 1 d . . . H72 H 0.6487 1.4771 1.0472 0.052 Uiso 1 1 calc R . . C73 C 0.6449(6) 1.5365(5) 1.1393(4) 0.050(2) Uani 1 1 d . . . H73 H 0.6369 1.4987 1.1571 0.059 Uiso 1 1 calc R . . C74 C 0.6495(6) 1.6059(5) 1.1799(4) 0.046(2) Uani 1 1 d . . . C75 C 0.6627(6) 1.6601(5) 1.1505(4) 0.043(2) Uani 1 1 d . . . C76 C 0.6396(7) 1.6236(6) 1.2460(5) 0.062(3) Uani 1 1 d . . . H76 H 0.6306 1.5882 1.2667 0.074 Uiso 1 1 calc R . . C77 C 0.6428(8) 1.6905(6) 1.2801(5) 0.065(3) Uani 1 1 d . . . H77 H 0.6360 1.7028 1.3250 0.078 Uiso 1 1 calc R . . C78 C 0.6564(7) 1.7420(6) 1.2490(5) 0.060(3) Uani 1 1 d . . . H78 H 0.6583 1.7892 1.2740 0.072 Uiso 1 1 calc R . . C79 C 0.8280(7) 1.0664(5) 0.4001(5) 0.054(3) Uani 1 1 d . . . H79 H 0.8583 1.0587 0.3629 0.065 Uiso 1 1 calc R . . C80 C 0.7523(8) 1.0200(6) 0.3970(5) 0.066(3) Uani 1 1 d . . . H80 H 0.7308 0.9823 0.3581 0.079 Uiso 1 1 calc R . . C81 C 0.7071(8) 1.0272(6) 0.4494(5) 0.066(3) Uani 1 1 d . . . H81 H 0.6553 0.9940 0.4486 0.079 Uiso 1 1 calc R . . C82 C 0.7396(7) 1.0855(5) 0.5046(5) 0.054(3) Uani 1 1 d . . . C83 C 0.8171(7) 1.1321(5) 0.5042(4) 0.047(2) Uani 1 1 d . . . C84 C 0.6972(7) 1.1007(6) 0.5627(5) 0.064(3) Uani 1 1 d . . . H84 H 0.6444 1.0705 0.5653 0.076 Uiso 1 1 calc R . . C85 C 0.7332(6) 1.1579(5) 0.6132(5) 0.051(2) Uani 1 1 d . . . H85 H 0.7065 1.1671 0.6522 0.061 Uiso 1 1 calc R . . C86 C 0.8103(6) 1.2045(5) 0.6092(4) 0.041(2) Uani 1 1 d . . . C87 C 0.8322(6) 1.2802(5) 0.7208(4) 0.039(2) Uani 1 1 d . . . C88 C 0.8129(6) 1.2279(5) 0.7499(4) 0.043(2) Uani 1 1 d . . . H88 H 0.8115 1.1803 0.7267 0.051 Uiso 1 1 calc R . . C89 C 0.7957(6) 1.2471(5) 0.8142(4) 0.045(2) Uani 1 1 d . . . H89 H 0.7778 1.2114 0.8341 0.054 Uiso 1 1 calc R . . C90 C 0.8039(6) 1.3151(5) 0.8491(4) 0.044(2) Uani 1 1 d . . . H90 H 0.7911 1.3270 0.8928 0.053 Uiso 1 1 calc R . . C91 C 0.8318(5) 1.3693(5) 0.8203(4) 0.037(2) Uani 1 1 d . . . C92 C 0.8591(5) 1.4726(5) 0.9166(4) 0.038(2) Uani 1 1 d . . . C93 C 0.8923(6) 1.4449(5) 0.9609(4) 0.046(2) Uani 1 1 d . . . H93 H 0.9061 1.4007 0.9464 0.056 Uiso 1 1 calc R . . C94 C 0.9040(6) 1.4830(6) 1.0243(4) 0.053(3) Uani 1 1 d . . . H94 H 0.9241 1.4638 1.0544 0.063 Uiso 1 1 calc R . . C95 C 0.8878(6) 1.5490(5) 1.0476(4) 0.045(2) Uani 1 1 d . . . H95 H 0.8953 1.5742 1.0926 0.053 Uiso 1 1 calc R . . C96 C 0.8606(6) 1.5767(5) 1.0032(4) 0.040(2) Uani 1 1 d . . . C97 C 0.8775(6) 1.6968(5) 1.0728(4) 0.042(2) Uani 1 1 d . . . C98 C 0.9627(7) 1.7098(5) 1.0962(5) 0.055(3) Uani 1 1 d . . . H98 H 0.9942 1.6763 1.0785 0.066 Uiso 1 1 calc R . . C99 C 0.9992(7) 1.7706(6) 1.1442(5) 0.059(3) Uani 1 1 d . . . H99 H 1.0568 1.7801 1.1597 0.071 Uiso 1 1 calc R . . C100 C 0.9520(6) 1.8199(5) 1.1713(5) 0.053(3) Uani 1 1 d . . . C101 C 0.8669(6) 1.8026(5) 1.1473(4) 0.046(2) Uani 1 1 d . . . C102 C 0.9844(8) 1.8842(6) 1.2200(5) 0.066(3) Uani 1 1 d . . . H102 H 1.0416 1.8971 1.2376 0.079 Uiso 1 1 calc R . . C103 C 0.9334(7) 1.9286(6) 1.2425(5) 0.064(3) Uani 1 1 d . . . H103 H 0.9553 1.9736 1.2740 0.077 Uiso 1 1 calc R . . C104 C 0.8488(7) 1.9061(5) 1.2182(5) 0.054(3) Uani 1 1 d . . . H104 H 0.8133 1.9362 1.2356 0.064 Uiso 1 1 calc R . . P1 P 0.3600(3) 1.5858(3) 0.7216(2) 0.1058(15) Uani 1 1 d . . . F1 F 0.4423(8) 1.5580(7) 0.7325(6) 0.174(5) Uiso 1 1 d . . . F2 F 0.2718(6) 1.5974(5) 0.7111(5) 0.130(3) Uiso 1 1 d . . . F3 F 0.3717(6) 1.5757(5) 0.6484(5) 0.132(3) Uiso 1 1 d . . . F4 F 0.3466(6) 1.5932(5) 0.7941(4) 0.115(3) Uiso 1 1 d . . . F5 F 0.3109(7) 1.5044(6) 0.7038(5) 0.143(4) Uiso 1 1 d . . . F6 F 0.4210(9) 1.6555(8) 0.7417(7) 0.189(5) Uiso 1 1 d . . . P2 P 0.7539(8) 1.0418(7) -0.1850(6) 0.230(4) Uiso 1 1 d . . . F7 F 0.7548(12) 1.0674(10) -0.2487(9) 0.250 Uiso 1 1 d . . . F8 F 0.7560(13) 1.0173(11) -0.1212(10) 0.275(9) Uiso 1 1 d . . . F9 F 0.8315(13) 1.1058(10) -0.1511(9) 0.253(8) Uiso 1 1 d . . . F10 F 0.6853(12) 0.9742(10) -0.2283(9) 0.250 Uiso 1 1 d . . . F11 F 0.8244(12) 0.9941(10) -0.2203(9) 0.250 Uiso 1 1 d . . . F12 F 0.6919(12) 1.0900(10) -0.1507(9) 0.248(7) Uiso 1 1 d . . . O1 O 0.4258(11) 1.1902(9) 0.5985(8) 0.190(6) Uiso 1 1 d D . . C105 C 0.3285(16) 1.2020(13) 0.5222(12) 0.190(10) Uiso 1 1 d D . . H10A H 0.3074 1.1874 0.4764 0.285 Uiso 1 1 calc R . . H10B H 0.3559 1.2528 0.5370 0.285 Uiso 1 1 calc R . . H10C H 0.2813 1.1922 0.5478 0.285 Uiso 1 1 calc R . . C106 C 0.390(2) 1.1629(16) 0.5302(12) 0.250 Uiso 1 1 d D . . H10D H 0.4351 1.1692 0.5015 0.300 Uiso 1 1 calc R . . H10E H 0.3615 1.1119 0.5185 0.300 Uiso 1 1 calc R . . C107 C 0.4761(16) 1.1481(12) 0.6183(11) 0.191(10) Uiso 1 1 d D . . H10F H 0.5121 1.1326 0.5836 0.229 Uiso 1 1 calc R . . H10G H 0.4375 1.1053 0.6232 0.229 Uiso 1 1 calc R . . C108 C 0.5301(12) 1.1869(11) 0.6793(9) 0.153(8) Uiso 1 1 d D . . H10H H 0.5463 1.1532 0.6977 0.230 Uiso 1 1 calc R . . H10I H 0.4990 1.2151 0.7099 0.230 Uiso 1 1 calc R . . H10J H 0.5809 1.2181 0.6709 0.230 Uiso 1 1 calc R . . N37 N 0.9021(10) 1.0768(8) 0.6242(7) 0.129(5) Uiso 1 1 d D . . C109 C 0.8545(10) 1.0325(8) 0.6253(8) 0.098(5) Uiso 1 1 d D . . C110 C 0.7896(12) 0.9706(10) 0.6222(10) 0.150(7) Uiso 1 1 d D . . H11A H 0.8146 0.9307 0.6170 0.226 Uiso 1 1 calc R . . H11B H 0.7480 0.9599 0.5852 0.226 Uiso 1 1 calc R . . H11C H 0.7617 0.9790 0.6622 0.226 Uiso 1 1 calc R . . N38 N 0.6332(17) 1.4772(15) 0.5370(13) 0.236(11) Uiso 1 1 d D . . C111 C 0.5746(18) 1.4752(16) 0.5611(14) 0.198(11) Uiso 1 1 d D . . C112 C 0.5004(16) 1.4783(14) 0.5984(13) 0.203(11) Uiso 1 1 d D . . H11D H 0.4606 1.4314 0.5856 0.305 Uiso 1 1 calc R . . H11E H 0.4728 1.5123 0.5895 0.305 Uiso 1 1 calc R . . H11F H 0.5187 1.4930 0.6447 0.305 Uiso 1 1 calc R . . N39 N 0.869(2) 1.7878(17) 0.7574(16) 0.275(14) Uiso 1 1 d D . . C113 C 0.840(3) 1.832(2) 0.752(2) 0.30(2) Uiso 1 1 d D . . C114 C 0.754(2) 1.836(2) 0.7268(19) 0.32(2) Uiso 1 1 d D . . H11G H 0.7626 1.8701 0.7031 0.473 Uiso 1 1 calc R . . H11H H 0.7215 1.8502 0.7633 0.473 Uiso 1 1 calc R . . H11I H 0.7239 1.7890 0.6978 0.473 Uiso 1 1 calc R . . N40 N 0.8353(14) 1.2949(12) 0.0086(11) 0.186(8) Uiso 1 1 d D . . C115 C 0.8354(18) 1.2389(14) -0.0075(14) 0.191(11) Uiso 1 1 d D . . C116 C 0.819(2) 1.1596(15) -0.0172(15) 0.250 Uiso 1 1 d D . . H11J H 0.8418 1.1525 0.0214 0.375 Uiso 1 1 calc R . . H11K H 0.8455 1.1374 -0.0549 0.375 Uiso 1 1 calc R . . H11L H 0.7575 1.1382 -0.0243 0.375 Uiso 1 1 calc R . . N41 N 1.0614(18) 1.9320(15) 0.8464(13) 0.250 Uiso 1 1 d D . . C117 C 1.035(2) 1.9725(17) 0.8896(16) 0.250 Uiso 1 1 d D . . C118 C 1.007(2) 2.0377(16) 0.9274(15) 0.250 Uiso 1 1 d D . . H11P H 0.9861 2.0317 0.9677 0.375 Uiso 1 1 calc R . . H11Q H 0.9619 2.0442 0.9013 0.375 Uiso 1 1 calc R . . H11R H 1.0551 2.0794 0.9374 0.375 Uiso 1 1 calc R . . O2 O 0.5118(14) 1.1141(11) 0.0746(10) 0.250 Uiso 1 1 d D . . C119 C 0.558(2) 1.0765(16) -0.0323(12) 0.250 Uiso 1 1 d D . . H11M H 0.5666 1.0907 -0.0713 0.375 Uiso 1 1 calc R . . H11N H 0.5141 1.0322 -0.0425 0.375 Uiso 1 1 calc R . . H11O H 0.6112 1.0696 -0.0168 0.375 Uiso 1 1 calc R . . C120 C 0.533(2) 1.1319(14) 0.0181(13) 0.250 Uiso 1 1 d D . . H12A H 0.5800 1.1754 0.0302 0.300 Uiso 1 1 calc R . . H12B H 0.4839 1.1427 -0.0001 0.300 Uiso 1 1 calc R . . C121 C 0.469(2) 1.1644(15) 0.1143(13) 0.250 Uiso 1 1 d D . . H12C H 0.4175 1.1637 0.0898 0.300 Uiso 1 1 calc R . . H12D H 0.5070 1.2128 0.1269 0.300 Uiso 1 1 calc R . . C122 C 0.4477(19) 1.1435(16) 0.1733(12) 0.250 Uiso 1 1 d D . . H12E H 0.4102 1.1709 0.1969 0.375 Uiso 1 1 calc R . . H12F H 0.4995 1.1528 0.2013 0.375 Uiso 1 1 calc R . . H12G H 0.4192 1.0930 0.1603 0.375 Uiso 1 1 calc R . . N42 N 0.5177(18) 0.9316(15) 0.5724(12) 0.250 Uiso 1 1 d D . . C123 C 0.526(2) 0.9827(15) 0.6174(14) 0.250 Uiso 1 1 d D . . C124 C 0.527(2) 1.0032(15) 0.6901(13) 0.250 Uiso 1 1 d D . . H12H H 0.5409 1.0548 0.7084 0.375 Uiso 1 1 calc R . . H12I H 0.5697 0.9853 0.7074 0.375 Uiso 1 1 calc R . . H12J H 0.4714 0.9829 0.7016 0.375 Uiso 1 1 calc R . . O3 O 0.5121(13) 1.7146(11) 0.6040(10) 0.250 Uiso 1 1 d . . . H3A H 0.5142 1.6757 0.5771 0.375 Uiso 1 1 d R . . H3B H 0.4693 1.7252 0.5962 0.375 Uiso 1 1 d R . . O4 O 0.7212(13) 1.2248(11) 0.1424(10) 0.250 Uiso 1 1 d . . . H4A H 0.6752 1.1949 0.1320 0.375 Uiso 1 1 d R . . H4B H 0.7296 1.2440 0.1044 0.375 Uiso 1 1 d R . . O5 O 0.6792(13) 1.1106(11) 0.2665(10) 0.250 Uiso 1 1 d . . . H5A H 0.6714 1.1290 0.3059 0.375 Uiso 1 1 d R . . H5B H 0.7263 1.1371 0.2681 0.375 Uiso 1 1 d 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 0.0586(8) 0.0400(7) 0.0300(6) 0.0052(5) 0.0041(5) 0.0171(6) Ni2 0.0489(7) 0.0357(6) 0.0262(6) 0.0062(5) 0.0019(5) 0.0124(5) Ni3 0.0451(7) 0.0357(6) 0.0234(5) 0.0070(5) 0.0012(5) 0.0109(5) Ni4 0.0406(7) 0.0339(6) 0.0236(5) 0.0079(5) 0.0007(5) 0.0102(5) Ni5 0.0423(7) 0.0368(6) 0.0251(5) 0.0093(5) 0.0016(5) 0.0119(5) Ni6 0.0390(6) 0.0338(6) 0.0246(5) 0.0091(5) 0.0010(5) 0.0108(5) Ni7 0.0415(7) 0.0338(6) 0.0265(6) 0.0079(5) 0.0017(5) 0.0116(5) Ni8 0.0444(7) 0.0370(6) 0.0281(6) 0.0064(5) 0.0030(5) 0.0127(5) Ni9 0.0543(8) 0.0422(7) 0.0335(6) 0.0037(5) 0.0056(5) 0.0166(6) Cl1 0.0796(19) 0.0480(14) 0.0425(13) 0.0034(11) 0.0087(13) 0.0236(14) Cl2 0.0720(18) 0.0572(16) 0.0466(14) 0.0019(12) 0.0125(13) 0.0226(14) N1 0.059(5) 0.044(5) 0.037(4) 0.013(4) 0.009(4) 0.018(4) N2 0.048(5) 0.039(4) 0.030(4) 0.007(3) 0.007(3) 0.013(4) N3 0.048(5) 0.039(4) 0.025(4) 0.008(3) 0.002(3) 0.010(4) N4 0.042(4) 0.037(4) 0.021(3) 0.005(3) 0.000(3) 0.010(3) N5 0.042(4) 0.038(4) 0.024(3) 0.007(3) 0.003(3) 0.011(3) N6 0.046(4) 0.036(4) 0.028(4) 0.010(3) 0.001(3) 0.006(3) N7 0.049(5) 0.038(4) 0.032(4) 0.006(3) 0.005(3) 0.010(4) N8 0.052(5) 0.037(4) 0.038(4) 0.005(3) 0.005(4) 0.012(4) N9 0.065(6) 0.049(5) 0.043(5) 0.008(4) 0.012(4) 0.023(4) N10 0.057(5) 0.048(5) 0.036(4) 0.011(4) 0.007(4) 0.018(4) N11 0.050(5) 0.036(4) 0.028(4) 0.009(3) 0.005(3) 0.013(4) N12 0.055(5) 0.039(4) 0.027(4) 0.008(3) 0.004(3) 0.013(4) N13 0.051(5) 0.043(4) 0.019(3) 0.010(3) -0.001(3) 0.013(4) N14 0.054(5) 0.037(4) 0.030(4) 0.011(3) -0.001(3) 0.012(4) N15 0.049(5) 0.037(4) 0.026(4) 0.011(3) 0.002(3) 0.015(4) N16 0.050(5) 0.040(4) 0.033(4) 0.011(3) -0.004(3) 0.016(4) N17 0.047(5) 0.035(4) 0.036(4) 0.007(3) 0.002(3) 0.015(4) N18 0.055(5) 0.044(5) 0.041(4) 0.011(4) 0.006(4) 0.018(4) N19 0.068(6) 0.045(5) 0.028(4) 0.007(3) 0.003(4) 0.016(4) N20 0.059(5) 0.041(4) 0.027(4) 0.004(3) 0.000(4) 0.018(4) N21 0.050(5) 0.042(4) 0.024(4) 0.004(3) -0.002(3) 0.017(4) N22 0.036(4) 0.039(4) 0.036(4) 0.012(3) -0.001(3) 0.010(3) N23 0.043(4) 0.035(4) 0.034(4) 0.009(3) 0.000(3) 0.007(3) N24 0.042(4) 0.031(4) 0.030(4) 0.009(3) -0.001(3) 0.009(3) N25 0.041(4) 0.038(4) 0.033(4) 0.012(3) 0.006(3) 0.011(3) N26 0.047(5) 0.041(4) 0.032(4) 0.012(3) 0.009(3) 0.013(4) N27 0.057(5) 0.047(5) 0.032(4) 0.006(4) 0.004(4) 0.019(4) N28 0.059(5) 0.041(4) 0.036(4) 0.005(4) 0.002(4) 0.019(4) N29 0.051(5) 0.035(4) 0.032(4) 0.006(3) 0.000(3) 0.010(4) N30 0.050(5) 0.038(4) 0.028(4) 0.010(3) 0.004(3) 0.012(4) N31 0.041(4) 0.043(4) 0.028(4) 0.012(3) 0.004(3) 0.015(3) N32 0.047(4) 0.040(4) 0.024(4) 0.007(3) 0.001(3) 0.015(4) N33 0.042(4) 0.038(4) 0.029(4) 0.013(3) 0.002(3) 0.012(3) N34 0.049(5) 0.042(4) 0.029(4) 0.007(3) 0.001(3) 0.015(4) N35 0.046(5) 0.046(5) 0.026(4) 0.005(3) 0.001(3) 0.016(4) N36 0.056(5) 0.047(5) 0.033(4) 0.005(4) 0.004(4) 0.015(4) C1 0.069(7) 0.052(6) 0.041(5) 0.013(5) 0.007(5) 0.021(6) C2 0.090(9) 0.049(6) 0.055(7) 0.015(5) 0.011(6) 0.031(6) C3 0.082(8) 0.060(7) 0.048(6) 0.023(5) 0.008(5) 0.040(6) C4 0.060(7) 0.056(6) 0.047(6) 0.020(5) 0.009(5) 0.022(5) C5 0.040(5) 0.037(5) 0.042(5) 0.012(4) 0.003(4) 0.014(4) C6 0.057(6) 0.059(7) 0.043(6) 0.017(5) 0.000(5) 0.023(5) C7 0.056(6) 0.055(6) 0.035(5) 0.012(5) 0.002(4) 0.018(5) C8 0.046(6) 0.044(5) 0.037(5) 0.013(4) 0.008(4) 0.017(5) C9 0.043(5) 0.045(5) 0.031(5) 0.015(4) 0.005(4) 0.013(4) C10 0.046(6) 0.052(6) 0.037(5) 0.004(5) -0.001(4) 0.014(5) C11 0.043(6) 0.060(7) 0.043(6) 0.013(5) -0.001(5) 0.005(5) C12 0.041(5) 0.048(6) 0.032(5) 0.005(4) 0.001(4) 0.003(5) C13 0.046(6) 0.044(5) 0.027(4) 0.014(4) 0.004(4) 0.010(4) C14 0.050(6) 0.049(6) 0.022(4) 0.008(4) 0.003(4) 0.012(5) C15 0.049(6) 0.055(6) 0.041(5) 0.013(5) 0.013(5) 0.010(5) C16 0.061(7) 0.053(7) 0.063(7) 0.012(6) 0.014(6) 0.006(6) C17 0.061(7) 0.044(6) 0.055(6) 0.006(5) 0.018(5) 0.005(5) C18 0.060(6) 0.047(6) 0.027(5) 0.006(4) 0.007(4) 0.014(5) C19 0.054(6) 0.036(5) 0.039(5) 0.009(4) 0.001(4) 0.008(5) C20 0.091(9) 0.048(6) 0.055(6) 0.023(5) 0.030(6) 0.028(6) C21 0.119(11) 0.055(7) 0.073(8) 0.035(6) 0.039(8) 0.034(7) C22 0.104(10) 0.043(6) 0.063(7) 0.014(6) 0.022(7) 0.031(6) C23 0.067(7) 0.035(5) 0.048(6) 0.007(5) -0.001(5) 0.015(5) C24 0.136(13) 0.064(8) 0.088(10) 0.041(7) 0.038(9) 0.054(9) C25 0.122(12) 0.067(8) 0.086(9) 0.024(7) 0.033(9) 0.058(8) C26 0.106(10) 0.057(7) 0.067(8) 0.018(6) 0.025(7) 0.046(7) C27 0.059(7) 0.066(7) 0.061(7) 0.006(6) 0.007(6) 0.021(6) C28 0.074(9) 0.070(8) 0.090(9) 0.011(7) 0.038(7) 0.030(7) C29 0.051(7) 0.071(8) 0.080(8) 0.023(7) 0.020(6) 0.013(6) C30 0.058(7) 0.054(6) 0.047(6) 0.012(5) 0.011(5) 0.018(6) C31 0.056(6) 0.056(6) 0.036(5) 0.020(5) 0.003(5) 0.023(5) C32 0.055(7) 0.065(7) 0.061(7) 0.026(6) 0.015(5) 0.010(6) C33 0.062(7) 0.042(6) 0.043(5) 0.008(4) 0.002(5) 0.014(5) C34 0.049(6) 0.050(6) 0.028(4) 0.013(4) 0.000(4) 0.013(5) C35 0.051(6) 0.041(5) 0.029(5) 0.007(4) -0.003(4) 0.014(4) C36 0.069(7) 0.050(6) 0.028(5) 0.016(4) 0.009(4) 0.014(5) C37 0.061(6) 0.047(6) 0.043(5) 0.027(5) 0.008(5) 0.008(5) C38 0.064(7) 0.045(6) 0.042(5) 0.020(5) 0.007(5) 0.020(5) C39 0.053(6) 0.040(5) 0.020(4) 0.002(4) 0.001(4) 0.014(5) C40 0.050(6) 0.046(6) 0.032(5) 0.009(4) -0.001(4) 0.016(5) C41 0.066(7) 0.068(7) 0.032(5) 0.022(5) -0.002(5) 0.026(6) C42 0.070(7) 0.067(7) 0.041(6) 0.022(5) 0.002(5) 0.035(6) C43 0.062(7) 0.067(7) 0.043(6) 0.021(5) 0.002(5) 0.033(6) C44 0.057(6) 0.038(5) 0.033(5) 0.010(4) 0.000(4) 0.015(5) C45 0.053(6) 0.046(5) 0.041(5) 0.023(4) 0.007(4) 0.023(5) C46 0.051(6) 0.048(6) 0.042(5) 0.011(5) -0.007(5) 0.012(5) C47 0.049(6) 0.061(7) 0.051(6) 0.015(5) -0.002(5) 0.020(5) C48 0.042(6) 0.055(6) 0.049(6) 0.013(5) 0.000(5) 0.018(5) C49 0.054(6) 0.039(5) 0.040(5) 0.010(4) 0.005(5) 0.019(5) C50 0.045(6) 0.076(8) 0.061(7) 0.013(6) 0.000(5) 0.016(6) C51 0.060(8) 0.081(8) 0.066(8) 0.015(7) 0.024(6) 0.029(7) C52 0.055(7) 0.058(7) 0.047(6) 0.007(5) 0.010(5) 0.023(5) C53 0.079(8) 0.052(6) 0.039(6) 0.010(5) 0.011(5) 0.021(6) C54 0.107(10) 0.087(9) 0.029(5) 0.018(6) 0.010(6) 0.044(8) C55 0.103(10) 0.068(7) 0.036(6) 0.020(5) -0.001(6) 0.032(7) C56 0.081(8) 0.061(7) 0.029(5) 0.012(5) 0.003(5) 0.029(6) C57 0.059(6) 0.048(6) 0.026(5) 0.006(4) 0.001(4) 0.015(5) C58 0.073(7) 0.061(7) 0.040(6) 0.014(5) -0.002(5) 0.027(6) C59 0.066(7) 0.049(6) 0.033(5) 0.012(4) 0.006(5) 0.020(5) C60 0.057(6) 0.040(5) 0.028(5) 0.005(4) -0.005(4) 0.005(5) C61 0.053(6) 0.044(5) 0.028(5) 0.007(4) 0.000(4) 0.018(5) C62 0.058(7) 0.055(6) 0.029(5) 0.001(4) 0.000(5) 0.017(5) C63 0.052(6) 0.068(7) 0.042(6) 0.007(5) -0.011(5) 0.012(6) C64 0.052(6) 0.069(7) 0.034(5) 0.012(5) 0.005(5) 0.018(5) C65 0.042(5) 0.038(5) 0.034(5) 0.009(4) 0.002(4) 0.013(4) C66 0.036(5) 0.045(5) 0.034(5) 0.013(4) 0.003(4) 0.017(4) C67 0.046(6) 0.043(5) 0.036(5) 0.011(4) -0.001(4) 0.007(5) C68 0.046(6) 0.042(5) 0.045(5) 0.016(5) 0.006(4) 0.006(4) C69 0.036(5) 0.046(6) 0.039(5) 0.014(4) 0.007(4) 0.009(4) C70 0.045(5) 0.041(5) 0.027(4) 0.005(4) 0.004(4) 0.017(4) C71 0.042(5) 0.052(6) 0.033(5) 0.015(4) 0.003(4) 0.013(5) C72 0.062(6) 0.035(5) 0.038(5) 0.013(4) 0.007(4) 0.018(5) C73 0.054(6) 0.059(6) 0.042(5) 0.023(5) 0.008(5) 0.016(5) C74 0.055(6) 0.045(6) 0.039(5) 0.016(5) 0.006(4) 0.012(5) C75 0.049(6) 0.051(6) 0.036(5) 0.017(5) 0.011(4) 0.017(5) C76 0.086(8) 0.071(8) 0.038(6) 0.027(6) 0.014(5) 0.024(7) C77 0.090(9) 0.074(8) 0.033(5) 0.017(6) 0.010(5) 0.021(7) C78 0.073(8) 0.065(7) 0.038(6) 0.007(5) 0.010(5) 0.022(6) C79 0.069(7) 0.046(6) 0.036(5) -0.001(5) -0.005(5) 0.014(6) C80 0.079(9) 0.060(7) 0.042(6) -0.005(5) -0.009(6) 0.018(7) C81 0.066(7) 0.054(7) 0.057(7) -0.002(6) -0.003(6) 0.006(6) C82 0.058(7) 0.041(6) 0.050(6) 0.001(5) 0.004(5) 0.007(5) C83 0.063(7) 0.035(5) 0.039(5) 0.005(4) -0.002(5) 0.017(5) C84 0.058(7) 0.048(6) 0.062(7) -0.001(5) 0.005(6) -0.005(5) C85 0.051(6) 0.053(6) 0.040(5) 0.006(5) 0.002(5) 0.009(5) C86 0.048(6) 0.035(5) 0.037(5) 0.006(4) -0.001(4) 0.014(4) C87 0.041(5) 0.040(5) 0.036(5) 0.011(4) 0.004(4) 0.011(4) C88 0.048(6) 0.038(5) 0.043(5) 0.015(4) 0.006(4) 0.011(4) C89 0.053(6) 0.045(6) 0.045(5) 0.022(5) 0.012(5) 0.013(5) C90 0.053(6) 0.053(6) 0.034(5) 0.019(5) 0.011(4) 0.019(5) C91 0.032(5) 0.047(5) 0.034(5) 0.015(4) 0.002(4) 0.014(4) C92 0.039(5) 0.043(5) 0.031(5) 0.011(4) 0.003(4) 0.010(4) C93 0.064(7) 0.051(6) 0.032(5) 0.014(4) 0.001(4) 0.029(5) C94 0.064(7) 0.065(7) 0.036(5) 0.021(5) -0.004(5) 0.022(6) C95 0.056(6) 0.055(6) 0.022(4) 0.006(4) 0.001(4) 0.021(5) C96 0.044(5) 0.050(6) 0.025(4) 0.006(4) 0.007(4) 0.018(5) C97 0.049(6) 0.051(6) 0.027(5) 0.013(4) 0.002(4) 0.015(5) C98 0.057(7) 0.056(6) 0.045(6) -0.001(5) -0.003(5) 0.024(5) C99 0.054(6) 0.068(7) 0.046(6) 0.002(5) -0.007(5) 0.020(6) C100 0.051(6) 0.051(6) 0.049(6) 0.008(5) 0.000(5) 0.009(5) C101 0.054(6) 0.046(6) 0.032(5) 0.005(4) 0.001(4) 0.010(5) C102 0.064(7) 0.065(7) 0.051(6) -0.005(6) -0.002(6) 0.012(6) C103 0.071(8) 0.054(7) 0.049(6) -0.002(5) -0.007(6) 0.006(6) C104 0.070(7) 0.037(5) 0.044(6) -0.002(5) 0.007(5) 0.015(5) P1 0.077(3) 0.165(5) 0.076(2) 0.065(3) -0.011(2) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 N28 2.126(8) . ? Ni1 N19 2.129(8) . ? Ni1 N1 2.135(8) . ? Ni1 N10 2.143(8) . ? Ni1 Ni2 2.3199(16) . ? Ni1 Cl1 2.385(3) . ? Ni2 N20 2.011(7) . ? Ni2 N29 2.024(7) . ? Ni2 N11 2.026(7) . ? Ni2 N2 2.031(7) . ? Ni2 Ni3 2.3009(15) . ? Ni3 N21 1.905(7) . ? Ni3 N12 1.909(7) . ? Ni3 N30 1.907(7) . ? Ni3 N3 1.914(7) . ? Ni3 Ni4 2.2736(15) . ? Ni4 N31 1.911(7) . ? Ni4 N13 1.912(7) . ? Ni4 N4 1.922(7) . ? Ni4 N22 1.920(7) . ? Ni4 Ni5 2.2405(15) . ? Ni5 N23 1.896(7) . ? Ni5 N14 1.903(7) . ? Ni5 N5 1.902(7) . ? Ni5 N32 1.902(7) . ? Ni5 Ni6 2.2380(15) . ? Ni6 N6 1.909(7) . ? Ni6 N15 1.918(7) . ? Ni6 N33 1.921(7) . ? Ni6 N24 1.920(7) . ? Ni6 Ni7 2.2738(15) . ? Ni7 N7 1.898(7) . ? Ni7 N34 1.903(7) . ? Ni7 N16 1.906(7) . ? Ni7 N25 1.911(7) . ? Ni7 Ni8 2.3032(15) . ? Ni8 N35 2.019(7) . ? Ni8 N17 2.026(7) . ? Ni8 N26 2.035(7) . ? Ni8 N8 2.032(8) . ? Ni8 Ni9 2.3161(16) . ? Ni9 N18 2.128(8) . ? Ni9 N9 2.136(8) . ? Ni9 N36 2.143(8) . ? Ni9 N27 2.168(8) . ? Ni9 Cl2 2.396(3) . ? N1 C1 1.324(12) . ? N1 C5 1.363(11) . ? N2 C8 1.338(11) . ? N2 C5 1.349(11) . ? N3 C8 1.367(11) . ? N3 C9 1.395(11) . ? N4 C9 1.372(11) . ? N4 C13 1.381(11) . ? N5 C13 1.372(11) . ? N5 C14 1.377(11) . ? N6 C18 1.357(11) . ? N6 C14 1.392(11) . ? N7 C18 1.376(12) . ? N7 C19 1.395(11) . ? N8 C19 1.333(12) . ? N8 C23 1.354(12) . ? N9 C26 1.325(12) . ? N9 C23 1.382(12) . ? N10 C27 1.324(13) . ? N10 C31 1.364(12) . ? N11 C31 1.360(12) . ? N11 C34 1.364(11) . ? N12 C34 1.378(12) . ? N12 C35 1.380(11) . ? N13 C39 1.370(11) . ? N13 C35 1.377(11) . ? N14 C39 1.377(11) . ? N14 C40 1.379(11) . ? N15 C44 1.350(11) . ? N15 C40 1.375(11) . ? N16 C44 1.386(11) . ? N16 C45 1.385(11) . ? N17 C45 1.342(11) . ? N17 C49 1.362(12) . ? N18 C52 1.319(12) . ? N18 C49 1.380(11) . ? N19 C53 1.355(12) . ? N19 C57 1.368(12) . ? N20 C60 1.343(12) . ? N20 C57 1.368(11) . ? N21 C61 1.377(11) . ? N21 C60 1.382(11) . ? N22 C65 1.361(11) . ? N22 C61 1.382(11) . ? N23 C66 1.387(11) . ? N23 C65 1.392(11) . ? N24 C66 1.356(11) . ? N24 C70 1.379(11) . ? N25 C71 1.383(11) . ? N25 C70 1.396(11) . ? N26 C75 1.348(11) . ? N26 C71 1.349(11) . ? N27 C78 1.342(12) . ? N27 C75 1.366(11) . ? N28 C79 1.328(11) . ? N28 C83 1.376(12) . ? N29 C86 1.343(11) . ? N29 C83 1.361(11) . ? N30 C86 1.368(11) . ? N30 C87 1.395(11) . ? N31 C91 1.366(10) . ? N31 C87 1.366(11) . ? N32 C91 1.375(11) . ? N32 C92 1.375(10) . ? N33 C96 1.363(10) . ? N33 C92 1.365(11) . ? N34 C97 1.365(11) . ? N34 C96 1.398(11) . ? N35 C97 1.344(11) . ? N35 C101 1.360(11) . ? N36 C104 1.331(12) . ? N36 C101 1.379(12) . ? C1 C2 1.385(14) . ? C2 C3 1.369(14) . ? C3 C4 1.408(13) . ? C4 C6 1.418(13) . ? C4 C5 1.416(13) . ? C6 C7 1.362(13) . ? C7 C8 1.421(12) . ? C9 C10 1.367(13) . ? C10 C11 1.369(13) . ? C11 C12 1.368(13) . ? C12 C13 1.410(12) . ? C14 C15 1.370(13) . ? C15 C16 1.391(14) . ? C16 C17 1.362(14) . ? C17 C18 1.402(14) . ? C19 C20 1.427(13) . ? C20 C21 1.354(14) . ? C21 C22 1.413(15) . ? C22 C24 1.404(15) . ? C22 C23 1.418(14) . ? C24 C25 1.372(17) . ? C25 C26 1.384(16) . ? C27 C28 1.408(16) . ? C28 C29 1.367(16) . ? C29 C30 1.396(14) . ? C30 C31 1.418(14) . ? C30 C32 1.429(14) . ? C32 C33 1.350(14) . ? C33 C34 1.411(13) . ? C35 C36 1.384(12) . ? C36 C37 1.368(13) . ? C37 C38 1.361(13) . ? C38 C39 1.394(12) . ? C40 C41 1.393(12) . ? C41 C42 1.366(13) . ? C42 C43 1.387(13) . ? C43 C44 1.398(12) . ? C45 C46 1.416(13) . ? C46 C47 1.360(14) . ? C47 C48 1.419(13) . ? C48 C50 1.390(14) . ? C48 C49 1.411(13) . ? C50 C51 1.375(15) . ? C51 C52 1.393(15) . ? C53 C54 1.379(14) . ? C54 C55 1.378(15) . ? C55 C56 1.408(13) . ? C56 C58 1.405(14) . ? C56 C57 1.407(13) . ? C58 C59 1.361(13) . ? C59 C60 1.423(13) . ? C61 C62 1.370(13) . ? C62 C63 1.392(14) . ? C63 C64 1.369(13) . ? C64 C65 1.386(13) . ? C66 C67 1.389(12) . ? C67 C68 1.373(12) . ? C68 C69 1.367(13) . ? C69 C70 1.373(12) . ? C71 C72 1.427(12) . ? C72 C73 1.367(12) . ? C73 C74 1.415(13) . ? C74 C76 1.397(13) . ? C74 C75 1.421(13) . ? C76 C77 1.337(15) . ? C77 C78 1.396(15) . ? C79 C80 1.359(15) . ? C80 C81 1.363(15) . ? C81 C82 1.402(14) . ? C82 C83 1.398(14) . ? C82 C84 1.443(14) . ? C84 C85 1.343(13) . ? C85 C86 1.414(13) . ? C87 C88 1.381(12) . ? C88 C89 1.390(12) . ? C89 C90 1.348(13) . ? C90 C91 1.423(12) . ? C92 C93 1.418(12) . ? C93 C94 1.350(13) . ? C94 C95 1.388(13) . ? C95 C96 1.373(12) . ? C97 C98 1.412(13) . ? C98 C99 1.359(14) . ? C99 C100 1.415(14) . ? C100 C102 1.396(14) . ? C100 C101 1.403(14) . ? C102 C103 1.370(15) . ? C103 C104 1.391(15) . ? P1 F6 1.472(15) . ? P1 F2 1.543(11) . ? P1 F4 1.564(10) . ? P1 F3 1.566(11) . ? P1 F5 1.596(12) . ? P1 F1 1.624(14) . ? P2 F9 1.57(2) . ? P2 F10 1.583(19) . ? P2 F8 1.62(2) . ? P2 F12 1.622(19) . ? P2 F7 1.623(19) . ? P2 F11 1.733(19) . ? O1 C107 1.469(16) . ? O1 C106 1.479(17) . ? C105 C106 1.463(18) . ? C107 C108 1.471(16) . ? N37 C109 1.054(14) . ? C109 C110 1.433(15) . ? N38 C111 1.101(18) . ? C111 C112 1.477(17) . ? N39 C113 1.154(19) . ? C113 C114 1.519(19) . ? N40 C115 1.097(17) . ? C115 C116 1.532(18) . ? N41 C117 1.219(18) . ? C117 C118 1.521(18) . ? O2 C120 1.411(17) . ? O2 C121 1.459(17) . ? C119 C120 1.470(17) . ? C121 C122 1.496(17) . ? N42 C123 1.179(17) . ? C123 C124 1.508(17) . ? 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 N28 Ni1 N19 88.5(3) . . ? N28 Ni1 N1 91.1(3) . . ? N19 Ni1 N1 167.6(3) . . ? N28 Ni1 N10 167.8(3) . . ? N19 Ni1 N10 89.3(3) . . ? N1 Ni1 N10 88.4(3) . . ? N28 Ni1 Ni2 84.0(2) . . ? N19 Ni1 Ni2 83.9(2) . . ? N1 Ni1 Ni2 83.7(2) . . ? N10 Ni1 Ni2 83.8(2) . . ? N28 Ni1 Cl1 95.8(2) . . ? N19 Ni1 Cl1 96.4(2) . . ? N1 Ni1 Cl1 96.0(2) . . ? N10 Ni1 Cl1 96.4(2) . . ? Ni2 Ni1 Cl1 179.59(9) . . ? N20 Ni2 N29 89.3(3) . . ? N20 Ni2 N11 90.4(3) . . ? N29 Ni2 N11 171.8(3) . . ? N20 Ni2 N2 172.1(3) . . ? N29 Ni2 N2 91.4(3) . . ? N11 Ni2 N2 87.8(3) . . ? N20 Ni2 Ni3 86.0(2) . . ? N29 Ni2 Ni3 85.8(2) . . ? N11 Ni2 Ni3 86.0(2) . . ? N2 Ni2 Ni3 86.3(2) . . ? N20 Ni2 Ni1 93.8(2) . . ? N29 Ni2 Ni1 94.1(2) . . ? N11 Ni2 Ni1 94.1(2) . . ? N2 Ni2 Ni1 94.0(2) . . ? Ni3 Ni2 Ni1 179.74(7) . . ? N21 Ni3 N12 90.5(3) . . ? N21 Ni3 N30 89.2(3) . . ? N12 Ni3 N30 176.8(3) . . ? N21 Ni3 N3 176.7(3) . . ? N12 Ni3 N3 89.4(3) . . ? N30 Ni3 N3 90.6(3) . . ? N21 Ni3 Ni4 87.5(2) . . ? N12 Ni3 Ni4 88.1(2) . . ? N30 Ni3 Ni4 88.7(2) . . ? N3 Ni3 Ni4 89.2(2) . . ? N21 Ni3 Ni2 91.7(2) . . ? N12 Ni3 Ni2 91.7(2) . . ? N30 Ni3 Ni2 91.5(2) . . ? N3 Ni3 Ni2 91.6(2) . . ? Ni4 Ni3 Ni2 179.21(7) . . ? N31 Ni4 N13 178.9(3) . . ? N31 Ni4 N4 91.5(3) . . ? N13 Ni4 N4 89.2(3) . . ? N31 Ni4 N22 88.9(3) . . ? N13 Ni4 N22 90.3(3) . . ? N4 Ni4 N22 179.2(3) . . ? N31 Ni4 Ni5 89.9(2) . . ? N13 Ni4 Ni5 89.2(2) . . ? N4 Ni4 Ni5 90.3(2) . . ? N22 Ni4 Ni5 88.9(2) . . ? N31 Ni4 Ni3 90.3(2) . . ? N13 Ni4 Ni3 90.5(2) . . ? N4 Ni4 Ni3 89.5(2) . . ? N22 Ni4 Ni3 91.2(2) . . ? Ni5 Ni4 Ni3 179.73(8) . . ? N23 Ni5 N14 89.8(3) . . ? N23 Ni5 N5 179.4(3) . . ? N14 Ni5 N5 89.7(3) . . ? N23 Ni5 N32 89.3(3) . . ? N14 Ni5 N32 179.0(3) . . ? N5 Ni5 N32 91.2(3) . . ? N23 Ni5 Ni6 89.5(2) . . ? N14 Ni5 Ni6 89.4(2) . . ? N5 Ni5 Ni6 90.2(2) . . ? N32 Ni5 Ni6 90.9(2) . . ? N23 Ni5 Ni4 90.8(2) . . ? N14 Ni5 Ni4 90.1(2) . . ? N5 Ni5 Ni4 89.6(2) . . ? N32 Ni5 Ni4 89.7(2) . . ? Ni6 Ni5 Ni4 179.41(7) . . ? N6 Ni6 N15 89.8(3) . . ? N6 Ni6 N33 91.7(3) . . ? N15 Ni6 N33 178.4(3) . . ? N6 Ni6 N24 179.1(3) . . ? N15 Ni6 N24 90.1(3) . . ? N33 Ni6 N24 88.3(3) . . ? N6 Ni6 Ni5 89.6(2) . . ? N15 Ni6 Ni5 90.5(2) . . ? N33 Ni6 Ni5 88.9(2) . . ? N24 Ni6 Ni5 89.5(2) . . ? N6 Ni6 Ni7 90.3(2) . . ? N15 Ni6 Ni7 89.8(2) . . ? N33 Ni6 Ni7 90.8(2) . . ? N24 Ni6 Ni7 90.5(2) . . ? Ni5 Ni6 Ni7 179.69(7) . . ? N7 Ni7 N34 90.1(3) . . ? N7 Ni7 N16 90.1(3) . . ? N34 Ni7 N16 176.7(3) . . ? N7 Ni7 N25 176.3(3) . . ? N34 Ni7 N25 89.3(3) . . ? N16 Ni7 N25 90.3(3) . . ? N7 Ni7 Ni6 88.0(2) . . ? N34 Ni7 Ni6 87.7(2) . . ? N16 Ni7 Ni6 88.9(2) . . ? N25 Ni7 Ni6 88.3(2) . . ? N7 Ni7 Ni8 91.1(2) . . ? N34 Ni7 Ni8 91.1(2) . . ? N16 Ni7 Ni8 92.3(2) . . ? N25 Ni7 Ni8 92.5(2) . . ? Ni6 Ni7 Ni8 178.51(7) . . ? N35 Ni8 N17 171.7(3) . . ? N35 Ni8 N26 88.7(3) . . ? N17 Ni8 N26 90.8(3) . . ? N35 Ni8 N8 90.8(3) . . ? N17 Ni8 N8 88.5(3) . . ? N26 Ni8 N8 171.9(3) . . ? N35 Ni8 Ni7 86.2(2) . . ? N17 Ni8 Ni7 85.5(2) . . ? N26 Ni8 Ni7 85.4(2) . . ? N8 Ni8 Ni7 86.5(2) . . ? N35 Ni8 Ni9 93.6(2) . . ? N17 Ni8 Ni9 94.6(2) . . ? N26 Ni8 Ni9 94.9(2) . . ? N8 Ni8 Ni9 93.2(2) . . ? Ni7 Ni8 Ni9 179.61(8) . . ? N18 Ni9 N9 87.6(3) . . ? N18 Ni9 N36 168.1(3) . . ? N9 Ni9 N36 89.5(3) . . ? N18 Ni9 N27 90.0(3) . . ? N9 Ni9 N27 168.4(3) . . ? N36 Ni9 N27 90.5(3) . . ? N18 Ni9 Ni8 83.9(2) . . ? N9 Ni9 Ni8 85.1(2) . . ? N36 Ni9 Ni8 84.4(2) . . ? N27 Ni9 Ni8 83.4(2) . . ? N18 Ni9 Cl2 96.9(2) . . ? N9 Ni9 Cl2 95.8(2) . . ? N36 Ni9 Cl2 94.9(2) . . ? N27 Ni9 Cl2 95.8(2) . . ? Ni8 Ni9 Cl2 178.82(10) . . ? C1 N1 C5 116.9(8) . . ? C1 N1 Ni1 120.1(6) . . ? C5 N1 Ni1 122.5(6) . . ? C8 N2 C5 121.1(8) . . ? C8 N2 Ni2 120.8(6) . . ? C5 N2 Ni2 117.8(6) . . ? C8 N3 C9 123.5(8) . . ? C8 N3 Ni3 118.5(6) . . ? C9 N3 Ni3 117.9(6) . . ? C9 N4 C13 121.3(7) . . ? C9 N4 Ni4 120.3(6) . . ? C13 N4 Ni4 118.3(6) . . ? C13 N5 C14 122.8(8) . . ? C13 N5 Ni5 119.5(6) . . ? C14 N5 Ni5 117.4(6) . . ? C18 N6 C14 120.8(8) . . ? C18 N6 Ni6 119.2(6) . . ? C14 N6 Ni6 119.9(6) . . ? C18 N7 C19 122.0(8) . . ? C18 N7 Ni7 120.6(6) . . ? C19 N7 Ni7 117.1(6) . . ? C19 N8 C23 119.8(8) . . ? C19 N8 Ni8 120.2(6) . . ? C23 N8 Ni8 118.9(6) . . ? C26 N9 C23 117.1(9) . . ? C26 N9 Ni9 120.8(7) . . ? C23 N9 Ni9 122.0(6) . . ? C27 N10 C31 117.3(9) . . ? C27 N10 Ni1 119.1(7) . . ? C31 N10 Ni1 123.4(7) . . ? C31 N11 C34 119.7(8) . . ? C31 N11 Ni2 118.0(6) . . ? C34 N11 Ni2 121.0(6) . . ? C34 N12 C35 122.0(8) . . ? C34 N12 Ni3 117.1(6) . . ? C35 N12 Ni3 120.4(6) . . ? C39 N13 C35 120.9(7) . . ? C39 N13 Ni4 120.2(6) . . ? C35 N13 Ni4 118.8(6) . . ? C39 N14 C40 124.0(7) . . ? C39 N14 Ni5 117.3(6) . . ? C40 N14 Ni5 118.6(6) . . ? C44 N15 C40 122.1(7) . . ? C44 N15 Ni6 119.4(5) . . ? C40 N15 Ni6 118.5(6) . . ? C44 N16 C45 124.0(7) . . ? C44 N16 Ni7 118.2(6) . . ? C45 N16 Ni7 117.8(6) . . ? C45 N17 C49 119.3(8) . . ? C45 N17 Ni8 122.3(6) . . ? C49 N17 Ni8 118.0(6) . . ? C52 N18 C49 116.7(9) . . ? C52 N18 Ni9 119.5(7) . . ? C49 N18 Ni9 123.5(6) . . ? C53 N19 C57 116.5(8) . . ? C53 N19 Ni1 120.0(7) . . ? C57 N19 Ni1 123.5(6) . . ? C60 N20 C57 118.9(8) . . ? C60 N20 Ni2 121.6(6) . . ? C57 N20 Ni2 118.7(6) . . ? C61 N21 C60 122.1(8) . . ? C61 N21 Ni3 120.6(5) . . ? C60 N21 Ni3 117.3(6) . . ? C65 N22 C61 121.4(8) . . ? C65 N22 Ni4 120.5(6) . . ? C61 N22 Ni4 118.1(6) . . ? C66 N23 C65 124.0(7) . . ? C66 N23 Ni5 118.0(6) . . ? C65 N23 Ni5 117.9(6) . . ? C66 N24 C70 120.6(7) . . ? C66 N24 Ni6 120.0(6) . . ? C70 N24 Ni6 119.3(6) . . ? C71 N25 C70 123.0(7) . . ? C71 N25 Ni7 115.8(6) . . ? C70 N25 Ni7 120.7(6) . . ? C75 N26 C71 120.1(8) . . ? C75 N26 Ni8 117.6(6) . . ? C71 N26 Ni8 121.1(6) . . ? C78 N27 C75 117.4(8) . . ? C78 N27 Ni9 119.3(7) . . ? C75 N27 Ni9 123.2(6) . . ? C79 N28 C83 116.3(9) . . ? C79 N28 Ni1 121.0(7) . . ? C83 N28 Ni1 122.7(6) . . ? C86 N29 C83 120.2(8) . . ? C86 N29 Ni2 121.3(6) . . ? C83 N29 Ni2 117.4(6) . . ? C86 N30 C87 122.6(7) . . ? C86 N30 Ni3 117.6(6) . . ? C87 N30 Ni3 119.5(6) . . ? C91 N31 C87 121.1(7) . . ? C91 N31 Ni4 119.1(6) . . ? C87 N31 Ni4 119.7(5) . . ? C91 N32 C92 124.5(7) . . ? C91 N32 Ni5 117.0(5) . . ? C92 N32 Ni5 118.2(6) . . ? C96 N33 C92 121.6(7) . . ? C96 N33 Ni6 118.5(6) . . ? C92 N33 Ni6 119.6(5) . . ? C97 N34 C96 122.4(7) . . ? C97 N34 Ni7 118.9(6) . . ? C96 N34 Ni7 118.7(6) . . ? C97 N35 C101 119.3(8) . . ? C97 N35 Ni8 121.0(6) . . ? C101 N35 Ni8 118.9(6) . . ? C104 N36 C101 116.8(9) . . ? C104 N36 Ni9 121.0(7) . . ? C101 N36 Ni9 122.1(6) . . ? N1 C1 C2 125.2(9) . . ? C3 C2 C1 118.5(10) . . ? C2 C3 C4 119.1(10) . . ? C3 C4 C6 123.9(9) . . ? C3 C4 C5 118.1(9) . . ? C6 C4 C5 118.0(9) . . ? N2 C5 N1 116.7(8) . . ? N2 C5 C4 121.2(8) . . ? N1 C5 C4 122.1(8) . . ? C7 C6 C4 119.2(9) . . ? C6 C7 C8 120.4(9) . . ? N2 C8 N3 116.5(8) . . ? N2 C8 C7 120.1(8) . . ? N3 C8 C7 123.2(8) . . ? C10 C9 N4 120.7(8) . . ? C10 C9 N3 124.4(8) . . ? N4 C9 N3 114.7(8) . . ? C11 C10 C9 118.1(9) . . ? C10 C11 C12 123.2(9) . . ? C11 C12 C13 118.3(9) . . ? N5 C13 N4 115.7(8) . . ? N5 C13 C12 125.9(8) . . ? N4 C13 C12 118.2(8) . . ? C15 C14 N5 125.8(9) . . ? C15 C14 N6 119.7(8) . . ? N5 C14 N6 114.4(8) . . ? C14 C15 C16 118.9(9) . . ? C17 C16 C15 121.7(10) . . ? C16 C17 C18 118.7(10) . . ? N6 C18 N7 115.3(8) . . ? N6 C18 C17 119.9(9) . . ? N7 C18 C17 124.7(9) . . ? N8 C19 N7 115.7(8) . . ? N8 C19 C20 121.3(9) . . ? N7 C19 C20 122.7(8) . . ? C21 C20 C19 119.1(10) . . ? C20 C21 C22 120.8(10) . . ? C24 C22 C21 125.2(11) . . ? C24 C22 C23 117.9(10) . . ? C21 C22 C23 116.9(10) . . ? N8 C23 N9 116.0(9) . . ? N8 C23 C22 122.0(9) . . ? N9 C23 C22 122.0(9) . . ? C25 C24 C22 119.0(11) . . ? C24 C25 C26 119.7(11) . . ? N9 C26 C25 124.1(11) . . ? N10 C27 C28 123.7(11) . . ? C29 C28 C27 119.5(11) . . ? C28 C29 C30 118.4(11) . . ? C29 C30 C31 119.0(10) . . ? C29 C30 C32 124.2(10) . . ? C31 C30 C32 116.8(9) . . ? N11 C31 N10 115.8(9) . . ? N11 C31 C30 122.2(9) . . ? N10 C31 C30 122.0(9) . . ? C33 C32 C30 120.2(10) . . ? C32 C33 C34 120.8(10) . . ? N11 C34 N12 114.5(8) . . ? N11 C34 C33 120.2(9) . . ? N12 C34 C33 125.0(9) . . ? N13 C35 N12 115.1(8) . . ? N13 C35 C36 119.5(8) . . ? N12 C35 C36 125.2(8) . . ? C37 C36 C35 119.1(9) . . ? C38 C37 C36 121.9(9) . . ? C37 C38 C39 119.0(9) . . ? N13 C39 N14 115.0(7) . . ? N13 C39 C38 119.4(8) . . ? N14 C39 C38 125.4(8) . . ? N15 C40 N14 115.7(7) . . ? N15 C40 C41 118.8(8) . . ? N14 C40 C41 125.2(8) . . ? C42 C41 C40 119.2(9) . . ? C41 C42 C43 121.6(9) . . ? C42 C43 C44 118.3(9) . . ? N15 C44 N16 116.4(7) . . ? N15 C44 C43 119.6(8) . . ? N16 C44 C43 123.9(9) . . ? N17 C45 N16 115.1(8) . . ? N17 C45 C46 121.2(9) . . ? N16 C45 C46 123.4(8) . . ? C47 C46 C45 119.9(9) . . ? C46 C47 C48 119.9(9) . . ? C50 C48 C49 118.4(9) . . ? C50 C48 C47 124.3(10) . . ? C49 C48 C47 117.3(9) . . ? N17 C49 N18 115.7(8) . . ? N17 C49 C48 122.2(8) . . ? N18 C49 C48 122.1(9) . . ? C51 C50 C48 119.4(10) . . ? C50 C51 C52 118.5(10) . . ? N18 C52 C51 124.9(10) . . ? N19 C53 C54 124.0(10) . . ? C53 C54 C55 119.4(10) . . ? C54 C55 C56 119.1(10) . . ? C55 C56 C58 124.2(10) . . ? C55 C56 C57 117.9(10) . . ? C58 C56 C57 117.9(9) . . ? N19 C57 N20 115.0(8) . . ? N19 C57 C56 123.1(8) . . ? N20 C57 C56 122.0(9) . . ? C59 C58 C56 120.3(9) . . ? C58 C59 C60 119.1(9) . . ? N20 C60 N21 115.4(8) . . ? N20 C60 C59 121.7(8) . . ? N21 C60 C59 122.6(9) . . ? C62 C61 N21 125.8(8) . . ? C62 C61 N22 118.9(8) . . ? N21 C61 N22 115.0(8) . . ? C61 C62 C63 119.9(9) . . ? C64 C63 C62 120.2(10) . . ? C63 C64 C65 119.7(10) . . ? N22 C65 C64 119.5(8) . . ? N22 C65 N23 115.1(8) . . ? C64 C65 N23 125.2(8) . . ? N24 C66 N23 114.6(8) . . ? N24 C66 C67 120.1(8) . . ? N23 C66 C67 125.1(8) . . ? C68 C67 C66 118.6(9) . . ? C69 C68 C67 121.6(9) . . ? C68 C69 C70 119.1(8) . . ? C69 C70 N24 120.0(8) . . ? C69 C70 N25 125.6(8) . . ? N24 C70 N25 114.3(8) . . ? N26 C71 N25 115.9(8) . . ? N26 C71 C72 120.7(8) . . ? N25 C71 C72 123.3(8) . . ? C73 C72 C71 119.6(9) . . ? C72 C73 C74 120.2(9) . . ? C76 C74 C73 124.4(9) . . ? C76 C74 C75 118.5(9) . . ? C73 C74 C75 117.1(8) . . ? N26 C75 N27 116.5(8) . . ? N26 C75 C74 122.3(9) . . ? N27 C75 C74 121.2(8) . . ? C77 C76 C74 120.0(10) . . ? C76 C77 C78 119.3(10) . . ? N27 C78 C77 123.6(10) . . ? N28 C79 C80 124.9(10) . . ? C79 C80 C81 120.2(10) . . ? C80 C81 C82 117.7(11) . . ? C83 C82 C81 119.2(10) . . ? C83 C82 C84 117.3(9) . . ? C81 C82 C84 123.5(10) . . ? N29 C83 N28 116.4(9) . . ? N29 C83 C82 121.9(9) . . ? N28 C83 C82 121.7(8) . . ? C85 C84 C82 119.3(10) . . ? C84 C85 C86 120.9(10) . . ? N29 C86 N30 115.4(8) . . ? N29 C86 C85 120.3(8) . . ? N30 C86 C85 124.1(8) . . ? N31 C87 C88 120.9(8) . . ? N31 C87 N30 115.1(7) . . ? C88 C87 N30 123.9(8) . . ? C87 C88 C89 118.0(9) . . ? C90 C89 C88 121.5(9) . . ? C89 C90 C91 119.9(8) . . ? N31 C91 N32 115.9(7) . . ? N31 C91 C90 118.1(8) . . ? N32 C91 C90 125.8(8) . . ? N33 C92 N32 116.0(7) . . ? N33 C92 C93 118.6(8) . . ? N32 C92 C93 125.2(8) . . ? C94 C93 C92 118.3(9) . . ? C93 C94 C95 122.9(9) . . ? C96 C95 C94 117.7(8) . . ? N33 C96 C95 120.6(8) . . ? N33 C96 N34 115.2(7) . . ? C95 C96 N34 123.8(8) . . ? N35 C97 N34 115.4(8) . . ? N35 C97 C98 121.5(8) . . ? N34 C97 C98 122.8(9) . . ? C99 C98 C97 119.3(10) . . ? C98 C99 C100 120.4(10) . . ? C102 C100 C101 118.2(10) . . ? C102 C100 C99 124.5(10) . . ? C101 C100 C99 117.3(9) . . ? N35 C101 N36 115.7(8) . . ? N35 C101 C100 122.2(9) . . ? N36 C101 C100 122.1(8) . . ? C103 C102 C100 119.9(11) . . ? C102 C103 C104 118.3(10) . . ? N36 C104 C103 124.6(10) . . ? F6 P1 F2 107.6(8) . . ? F6 P1 F4 90.0(7) . . ? F2 P1 F4 90.1(6) . . ? F6 P1 F3 91.9(7) . . ? F2 P1 F3 89.7(6) . . ? F4 P1 F3 178.1(6) . . ? F6 P1 F5 167.5(8) . . ? F2 P1 F5 84.8(6) . . ? F4 P1 F5 88.1(6) . . ? F3 P1 F5 90.0(6) . . ? F6 P1 F1 83.6(7) . . ? F2 P1 F1 168.5(7) . . ? F4 P1 F1 87.0(6) . . ? F3 P1 F1 92.9(7) . . ? F5 P1 F1 84.0(7) . . ? F9 P2 F10 170.7(14) . . ? F9 P2 F8 88.3(12) . . ? F10 P2 F8 96.8(12) . . ? F9 P2 F12 88.7(11) . . ? F10 P2 F12 99.3(12) . . ? F8 P2 F12 87.8(12) . . ? F9 P2 F7 90.3(12) . . ? F10 P2 F7 84.5(11) . . ? F8 P2 F7 178.3(14) . . ? F12 P2 F7 93.0(11) . . ? F9 P2 F11 88.5(11) . . ? F10 P2 F11 83.5(11) . . ? F8 P2 F11 92.6(11) . . ? F12 P2 F11 177.1(13) . . ? F7 P2 F11 86.6(11) . . ? C107 O1 C106 115.7(19) . . ? C105 C106 O1 108(2) . . ? O1 C107 C108 113.2(16) . . ? N37 C109 C110 176(2) . . ? N38 C111 C112 175(4) . . ? N39 C113 C114 136(5) . . ? N40 C115 C116 165(4) . . ? N41 C117 C118 160(4) . . ? C120 O2 C121 109.5(16) . . ? O2 C120 C119 114.3(18) . . ? O2 C121 C122 107.8(17) . . ? N42 C123 C124 139(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.775 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.229 # Attachment 'compound 4.cif' data_ic11654 _database_code_depnum_ccdc_archive 'CCDC 753224' #TrackingRef 'compound 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H71 Cl2 F24 N34 Ni7 O0.50 P4' _chemical_formula_weight 2770.62 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' 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.9092(5) _cell_length_b 18.0424(6) _cell_length_c 20.6044(6) _cell_angle_alpha 105.4324(16) _cell_angle_beta 99.9320(15) _cell_angle_gamma 110.0693(15) _cell_volume 5444.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2790 _exptl_absorpt_coefficient_mu 1.398 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.600 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62038 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19047 _reflns_number_gt 11785 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(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^)+(0.1419P)^2^+29.8450P] 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_number_reflns 19047 _refine_ls_number_parameters 1423 _refine_ls_number_restraints 77 _refine_ls_R_factor_all 0.1300 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.2940 _refine_ls_wR_factor_gt 0.2473 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 1.45510(7) 2.16111(8) 0.20163(6) 0.0464(4) Uani 1 1 d . . . Ni2 Ni 1.33358(6) 2.05958(7) 0.21984(5) 0.0358(3) Uani 1 1 d . . . Ni3 Ni 1.21853(6) 1.96320(7) 0.23758(5) 0.0340(3) Uani 1 1 d . . . Ni4 Ni 1.10639(6) 1.86892(7) 0.25789(5) 0.0299(3) Uani 1 1 d . . . Ni5 Ni 0.99407(7) 1.77507(7) 0.27869(5) 0.0337(3) Uani 1 1 d . . . Ni6 Ni 0.87948(7) 1.68127(7) 0.29931(5) 0.0331(3) Uani 1 1 d . . . Ni7 Ni 0.75838(8) 1.58304(7) 0.32173(6) 0.0411(3) Uani 1 1 d . . . Cl1 Cl 1.57176(15) 2.25712(18) 0.18229(13) 0.0622(8) Uani 1 1 d . . . Cl2 Cl 0.64094(17) 1.49135(16) 0.34432(15) 0.0585(7) Uani 1 1 d . . . N1 N 1.3878(5) 2.0887(5) 0.0960(4) 0.053(2) Uani 1 1 d . . . N2 N 1.2616(4) 2.0229(5) 0.1248(4) 0.0411(19) Uani 1 1 d . . . N3 N 1.1404(4) 1.9616(5) 0.1595(3) 0.0360(17) Uani 1 1 d . . . N4 N 1.0254(4) 1.8952(4) 0.1998(3) 0.0316(15) Uani 1 1 d . . . N5 N 0.9208(4) 1.8263(4) 0.2484(3) 0.0342(16) Uani 1 1 d . . . N6 N 0.8258(5) 1.7605(4) 0.3029(4) 0.0370(16) Uani 1 1 d . . . N7 N 0.7336(5) 1.6899(5) 0.3587(4) 0.052(2) Uani 1 1 d . . . N8 N 1.4942(5) 2.2126(5) 0.3118(4) 0.048(2) Uani 1 1 d . . . N9 N 1.3968(4) 2.0895(5) 0.3169(4) 0.0379(17) Uani 1 1 d . . . N10 N 1.2953(4) 1.9642(4) 0.3154(3) 0.0345(16) Uani 1 1 d . . . N11 N 1.1882(4) 1.8425(4) 0.3150(3) 0.0327(16) Uani 1 1 d . . . N12 N 1.0677(4) 1.7236(4) 0.3080(4) 0.0360(16) Uani 1 1 d . . . N13 N 0.9437(5) 1.6100(5) 0.2954(4) 0.0373(17) Uani 1 1 d . . . N14 N 0.8153(5) 1.4997(5) 0.2846(4) 0.0405(17) Uani 1 1 d . . . N15 N 1.3755(5) 2.2279(5) 0.2014(4) 0.051(2) Uani 1 1 d . . . N16 N 1.2852(4) 2.1409(5) 0.2484(4) 0.0396(18) Uani 1 1 d . . . N17 N 1.2003(4) 2.0518(4) 0.2957(3) 0.0350(16) Uani 1 1 d . . . N18 N 1.1149(4) 1.9570(4) 0.3390(3) 0.0326(16) Uani 1 1 d . . . N19 N 1.0278(4) 1.8504(4) 0.3721(3) 0.0346(16) Uani 1 1 d . . . N20 N 0.9408(5) 1.7392(5) 0.3983(4) 0.0409(18) Uani 1 1 d . . . N21 N 0.8485(6) 1.6246(5) 0.4208(4) 0.054(2) Uani 1 1 d . . . N22 N 1.5100(4) 2.0754(5) 0.2087(4) 0.047(2) Uani 1 1 d . . . N23 N 1.3740(4) 1.9709(5) 0.1931(3) 0.0388(18) Uani 1 1 d . . . N24 N 1.2357(4) 1.8730(5) 0.1794(3) 0.0350(16) Uani 1 1 d . . . N25 N 1.0984(4) 1.7811(4) 0.1774(3) 0.0329(16) Uani 1 1 d . . . N26 N 0.9625(4) 1.7004(4) 0.1855(3) 0.0337(16) Uani 1 1 d . . . N27 N 0.8276(4) 1.6296(4) 0.1991(3) 0.0331(16) Uani 1 1 d . . . N28 N 0.6942(4) 1.5590(5) 0.2170(4) 0.0430(18) Uani 1 1 d . . . C1 C 1.4281(7) 2.0990(8) 0.0472(5) 0.074(4) Uani 1 1 d . . . H1A H 1.4898 2.1319 0.0622 0.089 Uiso 1 1 calc R . . C2 C 1.3853(7) 2.0644(10) -0.0247(5) 0.096(5) Uani 1 1 d . . . H2A H 1.4176 2.0739 -0.0572 0.115 Uiso 1 1 calc R . . C3 C 1.2971(7) 2.0168(8) -0.0481(5) 0.074(4) Uani 1 1 d . . . H3A H 1.2664 1.9945 -0.0968 0.089 Uiso 1 1 calc R . . C4 C 1.2525(6) 2.0014(7) 0.0018(5) 0.052(3) Uani 1 1 d . . . C5 C 1.3000(6) 2.0371(6) 0.0731(5) 0.047(2) Uani 1 1 d . . . C6 C 1.1611(6) 1.9502(6) -0.0165(5) 0.049(3) Uani 1 1 d . . . H6A H 1.1274 1.9235 -0.0647 0.059 Uiso 1 1 calc R . . C7 C 1.1220(6) 1.9393(6) 0.0342(4) 0.041(2) Uani 1 1 d . . . H7A H 1.0604 1.9066 0.0217 0.049 Uiso 1 1 calc R . . C8 C 1.1733(5) 1.9770(6) 0.1068(4) 0.038(2) Uani 1 1 d . . . C9 C 1.0520(5) 1.9374(5) 0.1562(4) 0.0344(19) Uani 1 1 d . . . C10 C 0.9957(6) 1.9617(6) 0.1188(5) 0.041(2) Uani 1 1 d . . . H10A H 1.0160 1.9975 0.0933 0.050 Uiso 1 1 calc R . . C11 C 0.9090(6) 1.9321(6) 0.1195(5) 0.043(2) Uani 1 1 d . . . H11A H 0.8683 1.9452 0.0918 0.051 Uiso 1 1 calc R . . C12 C 0.8803(6) 1.8842(6) 0.1596(5) 0.042(2) Uani 1 1 d . . . H12A H 0.8199 1.8614 0.1576 0.050 Uiso 1 1 calc R . . C13 C 0.9409(5) 1.8700(5) 0.2027(4) 0.0342(19) Uani 1 1 d . . . C14 C 0.8559(5) 1.8255(6) 0.2795(4) 0.040(2) Uani 1 1 d . . . C15 C 0.8276(6) 1.8925(6) 0.2934(5) 0.043(2) Uani 1 1 d . . . H15A H 0.8496 1.9370 0.2761 0.052 Uiso 1 1 calc R . . C16 C 0.7700(7) 1.8929(7) 0.3309(5) 0.052(3) Uani 1 1 d . . . H16A H 0.7519 1.9380 0.3412 0.063 Uiso 1 1 calc R . . C17 C 0.7358(7) 1.8231(6) 0.3553(6) 0.052(3) Uani 1 1 d . . . C18 C 0.7633(6) 1.7581(6) 0.3388(5) 0.046(2) Uani 1 1 d . . . C19 C 0.6782(8) 1.8217(7) 0.3980(6) 0.067(3) Uani 1 1 d . . . H19A H 0.6582 1.8654 0.4099 0.080 Uiso 1 1 calc R . . C20 C 0.6522(9) 1.7555(8) 0.4213(7) 0.082(4) Uani 1 1 d . . . H20A H 0.6157 1.7535 0.4515 0.098 Uiso 1 1 calc R . . C21 C 0.6801(8) 1.6912(8) 0.4001(6) 0.069(3) Uani 1 1 d . . . H21A H 0.6600 1.6450 0.4158 0.083 Uiso 1 1 calc R . . C22 C 1.5584(7) 2.2892(7) 0.3446(5) 0.061(3) Uani 1 1 d . . . H22A H 1.5799 2.3219 0.3171 0.073 Uiso 1 1 calc R . . C23 C 1.5957(7) 2.3239(7) 0.4174(5) 0.070(4) Uani 1 1 d . . . H23A H 1.6392 2.3800 0.4391 0.084 Uiso 1 1 calc R . . C24 C 1.5689(6) 2.2761(7) 0.4566(5) 0.060(3) Uani 1 1 d . . . H24A H 1.5958 2.2977 0.5061 0.072 Uiso 1 1 calc R . . C25 C 1.5029(6) 2.1967(6) 0.4253(5) 0.045(2) Uani 1 1 d . . . C26 C 1.4651(5) 2.1657(6) 0.3514(5) 0.042(2) Uani 1 1 d . . . C27 C 1.4689(6) 2.1418(6) 0.4617(4) 0.042(2) Uani 1 1 d . . . H27A H 1.4925 2.1602 0.5113 0.050 Uiso 1 1 calc R . . C28 C 1.4042(5) 2.0647(6) 0.4273(4) 0.037(2) Uani 1 1 d . . . H28A H 1.3834 2.0282 0.4522 0.044 Uiso 1 1 calc R . . C29 C 1.3667(5) 2.0380(6) 0.3530(4) 0.036(2) Uani 1 1 d . . . C30 C 1.2746(5) 1.8935(6) 0.3358(4) 0.035(2) Uani 1 1 d . . . C31 C 1.3368(6) 1.8728(6) 0.3715(5) 0.042(2) Uani 1 1 d . . . H31A H 1.3980 1.9061 0.3826 0.051 Uiso 1 1 calc R . . C32 C 1.3070(6) 1.8025(6) 0.3904(5) 0.052(3) Uani 1 1 d . . . H32A H 1.3483 1.7883 0.4162 0.062 Uiso 1 1 calc R . . C33 C 1.2182(6) 1.7525(6) 0.3723(5) 0.047(2) Uani 1 1 d . . . H33A H 1.1980 1.7062 0.3878 0.056 Uiso 1 1 calc R . . C34 C 1.1589(5) 1.7710(6) 0.3311(4) 0.037(2) Uani 1 1 d . . . C35 C 1.0294(5) 1.6412(6) 0.2969(4) 0.038(2) Uani 1 1 d . . . C36 C 1.0719(6) 1.5849(6) 0.2819(5) 0.051(2) Uani 1 1 d . . . H36A H 1.1313 1.6065 0.2809 0.061 Uiso 1 1 calc R . . C37 C 1.0292(6) 1.5018(7) 0.2693(6) 0.057(3) Uani 1 1 d . . . H37A H 1.0584 1.4652 0.2599 0.068 Uiso 1 1 calc R . . C38 C 0.9404(6) 1.4696(6) 0.2700(6) 0.052(3) Uani 1 1 d . . . C39 C 0.8990(6) 1.5257(5) 0.2835(5) 0.040(2) Uani 1 1 d . . . C40 C 0.8917(7) 1.3845(7) 0.2585(7) 0.068(3) Uani 1 1 d . . . H40A H 0.9184 1.3456 0.2522 0.082 Uiso 1 1 calc R . . C41 C 0.8053(7) 1.3586(7) 0.2566(7) 0.066(3) Uani 1 1 d . . . H41A H 0.7701 1.3006 0.2460 0.079 Uiso 1 1 calc R . . C42 C 0.7692(6) 1.4169(6) 0.2700(5) 0.052(3) Uani 1 1 d . . . H42A H 0.7090 1.3978 0.2689 0.062 Uiso 1 1 calc R . . C43 C 1.3981(7) 2.2959(7) 0.1820(6) 0.062(3) Uani 1 1 d . . . H43A H 1.4444 2.3069 0.1607 0.075 Uiso 1 1 calc R . . C44 C 1.3575(8) 2.3501(8) 0.1914(7) 0.083(4) Uani 1 1 d . . . H44A H 1.3762 2.3974 0.1768 0.099 Uiso 1 1 calc R . . C45 C 1.2897(8) 2.3369(7) 0.2218(6) 0.064(3) Uani 1 1 d . . . H45A H 1.2618 2.3747 0.2288 0.077 Uiso 1 1 calc R . . C46 C 1.2634(6) 2.2663(6) 0.2418(5) 0.051(3) Uani 1 1 d . . . C47 C 1.3064(6) 2.2127(6) 0.2305(5) 0.045(2) Uani 1 1 d . . . C48 C 1.1942(7) 2.2457(7) 0.2721(5) 0.054(3) Uani 1 1 d . . . H48A H 1.1621 2.2798 0.2788 0.065 Uiso 1 1 calc R . . C49 C 1.1732(6) 2.1761(6) 0.2919(5) 0.048(2) Uani 1 1 d . . . H49A H 1.1265 2.1620 0.3125 0.057 Uiso 1 1 calc R . . C50 C 1.2211(5) 2.1254(6) 0.2817(4) 0.039(2) Uani 1 1 d . . . C51 C 1.1609(6) 2.0392(6) 0.3480(4) 0.038(2) Uani 1 1 d . . . C52 C 1.1703(6) 2.1037(6) 0.4075(5) 0.044(2) Uani 1 1 d . . . H52A H 1.2042 2.1609 0.4145 0.053 Uiso 1 1 calc R . . C53 C 1.1290(7) 2.0825(6) 0.4566(5) 0.055(3) Uani 1 1 d . . . H53A H 1.1334 2.1255 0.4973 0.066 Uiso 1 1 calc R . . C54 C 1.0812(7) 1.9984(6) 0.4463(5) 0.053(3) Uani 1 1 d . . . H54A H 1.0519 1.9841 0.4795 0.063 Uiso 1 1 calc R . . C55 C 1.0761(5) 1.9360(6) 0.3886(4) 0.038(2) Uani 1 1 d . . . C56 C 1.0109(6) 1.8149(5) 0.4211(4) 0.040(2) Uani 1 1 d . . . C57 C 1.0666(7) 1.8494(6) 0.4915(5) 0.053(3) Uani 1 1 d . . . H57A H 1.1169 1.9012 0.5062 0.064 Uiso 1 1 calc R . . C58 C 1.0491(8) 1.8095(7) 0.5384(5) 0.066(3) Uani 1 1 d . . . H58A H 1.0872 1.8325 0.5850 0.080 Uiso 1 1 calc R . . C59 C 0.9729(9) 1.7329(7) 0.5161(5) 0.069(4) Uani 1 1 d . . . C60 C 0.9219(7) 1.6995(6) 0.4469(5) 0.049(2) Uani 1 1 d . . . C61 C 0.9507(11) 1.6873(9) 0.5623(6) 0.109(6) Uani 1 1 d . . . H61A H 0.9849 1.7087 0.6101 0.131 Uiso 1 1 calc R . . C62 C 0.8787(11) 1.6124(9) 0.5354(6) 0.112(6) Uani 1 1 d . . . H62A H 0.8627 1.5797 0.5641 0.134 Uiso 1 1 calc R . . C63 C 0.8287(9) 1.5837(8) 0.4653(6) 0.079(4) Uani 1 1 d . . . H63A H 0.7777 1.5322 0.4482 0.094 Uiso 1 1 calc R . . C64 C 1.5967(6) 2.1006(8) 0.2189(5) 0.056(3) Uani 1 1 d . . . H64A H 1.6314 2.1583 0.2283 0.067 Uiso 1 1 calc R . . C65 C 1.6386(6) 2.0453(8) 0.2165(5) 0.059(3) Uani 1 1 d . . . H65A H 1.7006 2.0661 0.2247 0.071 Uiso 1 1 calc R . . C66 C 1.5896(6) 1.9602(8) 0.2020(5) 0.059(3) Uani 1 1 d . . . H66A H 1.6165 1.9215 0.1985 0.070 Uiso 1 1 calc R . . C67 C 1.4988(6) 1.9339(7) 0.1929(5) 0.049(3) Uani 1 1 d . . . C68 C 1.4616(5) 1.9931(7) 0.1981(4) 0.045(2) Uani 1 1 d . . . C69 C 1.4412(6) 1.8495(7) 0.1804(5) 0.056(3) Uani 1 1 d . . . H69A H 1.4640 1.8077 0.1770 0.067 Uiso 1 1 calc R . . C70 C 1.3557(6) 1.8282(7) 0.1734(5) 0.052(3) Uani 1 1 d . . . H70A H 1.3183 1.7712 0.1646 0.062 Uiso 1 1 calc R . . C71 C 1.3198(5) 1.8891(6) 0.1791(4) 0.042(2) Uani 1 1 d . . . C72 C 1.1674(5) 1.7935(6) 0.1485(4) 0.040(2) Uani 1 1 d . . . C73 C 1.1615(6) 1.7319(7) 0.0899(5) 0.052(3) Uani 1 1 d . . . H73A H 1.2054 1.7427 0.0663 0.063 Uiso 1 1 calc R . . C74 C 1.0913(6) 1.6538(7) 0.0651(5) 0.057(3) Uani 1 1 d . . . H74A H 1.0884 1.6094 0.0262 0.068 Uiso 1 1 calc R . . C75 C 1.0247(6) 1.6412(6) 0.0981(5) 0.046(2) Uani 1 1 d . . . H75A H 0.9779 1.5871 0.0834 0.055 Uiso 1 1 calc R . . C76 C 1.0264(5) 1.7055(6) 0.1508(4) 0.037(2) Uani 1 1 d . . . C77 C 0.8762(5) 1.6486(6) 0.1552(4) 0.038(2) Uani 1 1 d . . . C78 C 0.8353(6) 1.6192(6) 0.0808(4) 0.044(2) Uani 1 1 d . . . H78A H 0.8700 1.6332 0.0507 0.053 Uiso 1 1 calc R . . C79 C 0.7483(6) 1.5720(7) 0.0534(5) 0.052(3) Uani 1 1 d . . . H79A H 0.7210 1.5551 0.0045 0.062 Uiso 1 1 calc R . . C80 C 0.6978(6) 1.5476(6) 0.0983(5) 0.045(2) Uani 1 1 d . . . C81 C 0.7380(5) 1.5788(6) 0.1710(5) 0.040(2) Uani 1 1 d . . . C82 C 0.6064(6) 1.4959(7) 0.0730(6) 0.060(3) Uani 1 1 d . . . H82A H 0.5764 1.4743 0.0241 0.072 Uiso 1 1 calc R . . C83 C 0.5620(7) 1.4775(8) 0.1202(6) 0.065(3) Uani 1 1 d . . . H83A H 0.5008 1.4425 0.1044 0.078 Uiso 1 1 calc R . . C84 C 0.6070(6) 1.5105(7) 0.1911(6) 0.055(3) Uani 1 1 d . . . H84A H 0.5749 1.4983 0.2232 0.066 Uiso 1 1 calc R . . P1 P 1.91507(16) 2.15356(18) 0.24139(12) 0.0484(6) Uani 1 1 d D . . F1 F 1.8590(4) 2.1736(4) 0.1836(3) 0.0749(19) Uani 1 1 d D . . F2 F 1.9709(4) 2.1340(4) 0.2985(3) 0.0652(16) Uani 1 1 d D . . F3 F 1.8674(4) 2.1841(4) 0.2956(3) 0.0664(17) Uani 1 1 d D . . F4 F 1.8408(4) 2.0604(4) 0.2134(3) 0.0642(16) Uani 1 1 d D . . F5 F 1.9632(4) 2.1241(4) 0.1865(3) 0.0657(17) Uani 1 1 d D . . F6 F 1.9880(4) 2.2477(4) 0.2682(3) 0.0598(15) Uani 1 1 d D . . P2 P 1.6425(2) 2.0439(2) 0.41151(15) 0.0637(8) Uani 1 1 d . . . F7 F 1.5795(5) 2.0632(5) 0.3587(3) 0.091(2) Uani 1 1 d . . . F8 F 1.7067(4) 2.0230(4) 0.4646(3) 0.0683(17) Uani 1 1 d . . . F9 F 1.5718(5) 2.0219(6) 0.4521(4) 0.098(3) Uani 1 1 d . . . F10 F 1.7168(5) 2.0660(5) 0.3726(4) 0.085(2) Uani 1 1 d . . . F11 F 1.6830(7) 2.1383(5) 0.4614(4) 0.111(3) Uani 1 1 d . . . F12 F 1.6040(5) 1.9501(5) 0.3603(4) 0.091(2) Uani 1 1 d . . . P3 P 1.3985(2) 1.2720(3) -0.1030(3) 0.0917(12) Uani 1 1 d . . . F13 F 1.4774(5) 1.2529(7) -0.0715(6) 0.132(4) Uani 1 1 d . . . F14 F 1.3182(6) 1.2828(6) -0.1377(6) 0.134(4) Uani 1 1 d . . . F15 F 1.3329(5) 1.1828(6) -0.1031(5) 0.112(3) Uani 1 1 d . . . F16 F 1.4666(8) 1.3590(6) -0.0984(8) 0.163(5) Uani 1 1 d . . . F17 F 1.3945(7) 1.3176(10) -0.0334(6) 0.166(5) Uani 1 1 d . . . F18 F 1.4041(7) 1.2252(6) -0.1784(5) 0.127(3) Uani 1 1 d . . . P4 P 1.2239(5) 1.5201(5) 0.1458(3) 0.0748(18) Uani 0.50 1 d PD A 1 F19 F 1.2395(14) 1.5539(13) 0.0870(10) 0.150 Uiso 0.50 1 d PD A 1 F20 F 1.3137(9) 1.5323(13) 0.1944(7) 0.150 Uiso 0.50 1 d PD A 1 F21 F 1.1744(12) 1.4606(10) 0.1810(8) 0.150 Uiso 0.50 1 d PD A 1 F22 F 1.1283(10) 1.5054(12) 0.1104(10) 0.133(7) Uiso 0.50 1 d PD A 1 F23 F 1.2330(13) 1.6091(9) 0.1904(10) 0.136(7) Uiso 0.50 1 d PD A 1 F24 F 1.2222(12) 1.4350(9) 0.1011(9) 0.123(6) Uiso 0.50 1 d PD A 1 P5 P 1.2922(5) 1.5423(4) 0.3576(3) 0.0706(17) Uani 0.50 1 d PD B 2 F25 F 1.2585(10) 1.5688(9) 0.2978(6) 0.120 Uiso 0.50 1 d PD B 2 F26 F 1.2272(11) 1.4524(9) 0.3389(9) 0.120 Uiso 0.50 1 d PD B 2 F27 F 1.3399(11) 1.5449(11) 0.4288(8) 0.115(6) Uiso 0.50 1 d PD B 2 F28 F 1.3634(11) 1.6360(9) 0.3759(9) 0.119(6) Uiso 0.50 1 d PD B 2 F29 F 1.3521(9) 1.5142(9) 0.3151(7) 0.087(4) Uiso 0.50 1 d PD B 2 F30 F 1.2335(11) 1.5716(11) 0.3969(9) 0.120 Uiso 0.50 1 d PD B 2 N29 N 1.1417(9) 1.1385(9) 0.0759(7) 0.107(4) Uiso 1 1 d . . . C85 C 1.1800(10) 1.1855(10) 0.0530(8) 0.090(4) Uiso 1 1 d . . . C86 C 1.2270(11) 1.2475(11) 0.0255(9) 0.112(5) Uiso 1 1 d . . . H86A H 1.2538 1.3034 0.0625 0.168 Uiso 1 1 calc R . . H86B H 1.1860 1.2478 -0.0142 0.168 Uiso 1 1 calc R . . H86C H 1.2731 1.2335 0.0096 0.168 Uiso 1 1 calc R . . N30 N 1.3625(11) 1.2890(11) 0.4277(9) 0.133(5) Uiso 1 1 d . . . C87 C 1.3926(12) 1.3523(13) 0.4247(10) 0.114(5) Uiso 1 1 d . . . C88 C 1.4454(15) 1.4257(15) 0.4034(13) 0.163(8) Uiso 1 1 d . . . H88A H 1.4234 1.4698 0.4141 0.245 Uiso 1 1 calc R . . H88B H 1.4387 1.4050 0.3529 0.245 Uiso 1 1 calc R . . H88C H 1.5078 1.4488 0.4298 0.245 Uiso 1 1 calc R . . N31 N 1.0360(14) 1.2489(13) -0.0128(13) 0.172(8) Uiso 1 1 d . . . C89 C 1.0304(18) 1.2736(18) 0.0423(17) 0.174(10) Uiso 1 1 d . . . C90 C 0.999(2) 1.294(2) 0.1031(19) 0.256(16) Uiso 1 1 d . . . H90A H 1.0211 1.2726 0.1379 0.385 Uiso 1 1 calc R . . H90B H 0.9342 1.2679 0.0883 0.385 Uiso 1 1 calc R . . H90C H 1.0193 1.3553 0.1241 0.385 Uiso 1 1 calc R . . N32 N 0.8429(14) 1.4266(13) 0.0911(11) 0.173(7) Uiso 1 1 d . . . C91 C 0.7639(13) 1.3766(12) 0.0617(10) 0.112(5) Uiso 1 1 d . . . C92 C 0.675(2) 1.334(2) 0.0209(17) 0.235(14) Uiso 1 1 d . . . H92A H 0.6566 1.2746 0.0172 0.352 Uiso 1 1 d R . . H92B H 0.6667 1.3370 -0.0263 0.352 Uiso 1 1 d R . . H92C H 0.6385 1.3573 0.0444 0.352 Uiso 1 1 d R . . N33 N 0.6097(14) 1.1058(14) -0.0276(11) 0.192(9) Uiso 1 1 d D . . C93 C 0.6639(14) 1.1615(13) 0.0166(10) 0.131(6) Uiso 1 1 d D . . C94 C 0.7287(16) 1.2013(16) 0.0909(11) 0.200 Uiso 1 1 d D . . H94A H 0.7284 1.1569 0.1100 0.300 Uiso 1 1 calc R . . H94B H 0.7111 1.2406 0.1214 0.300 Uiso 1 1 calc R . . H94C H 0.7881 1.2316 0.0887 0.300 Uiso 1 1 calc R . . N34 N 1.442(3) 1.689(3) 0.368(2) 0.200 Uiso 0.50 1 d PD C 1 C95 C 1.466(4) 1.687(3) 0.320(3) 0.200 Uiso 0.50 1 d PD C 1 C96 C 1.490(3) 1.667(3) 0.252(2) 0.200 Uiso 0.50 1 d PD C 1 H96A H 1.5094 1.6205 0.2475 0.300 Uiso 0.50 1 calc PR C 1 H96B H 1.5387 1.7169 0.2533 0.300 Uiso 0.50 1 calc PR C 1 H96C H 1.4394 1.6503 0.2125 0.300 Uiso 0.50 1 calc PR C 1 N35 N 1.059(2) 1.598(2) 0.4492(18) 0.159(13) Uiso 0.50 1 d PD D 1 C97 C 1.120(3) 1.637(3) 0.4950(19) 0.156(16) Uiso 0.50 1 d PD D 1 C98 C 1.192(2) 1.687(2) 0.5643(18) 0.133(13) Uiso 0.50 1 d PD D 1 H98A H 1.2489 1.6934 0.5563 0.200 Uiso 0.50 1 calc PR D 1 H98B H 1.1815 1.6560 0.5969 0.200 Uiso 0.50 1 calc PR D 1 H98C H 1.1915 1.7422 0.5844 0.200 Uiso 0.50 1 calc PR D 1 O1 O 1.3593(19) 1.5160(18) 0.1333(16) 0.165(11) Uiso 0.50 1 d PD E 2 H1 H 1.3070 1.4944 0.1299 0.247 Uiso 0.50 1 d P F 2 H1' H 1.3891 1.5722 0.1330 0.247 Uiso 0.50 1 d P G 2 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 0.0281(6) 0.0617(8) 0.0324(6) 0.0266(6) 0.0029(5) -0.0059(6) Ni2 0.0239(5) 0.0489(7) 0.0233(6) 0.0188(5) 0.0023(4) -0.0004(5) Ni3 0.0257(5) 0.0450(7) 0.0240(6) 0.0166(5) 0.0048(4) 0.0038(5) Ni4 0.0245(5) 0.0381(6) 0.0207(5) 0.0125(5) 0.0046(4) 0.0047(5) Ni5 0.0310(6) 0.0386(7) 0.0260(6) 0.0134(5) 0.0090(5) 0.0062(5) Ni6 0.0337(6) 0.0342(6) 0.0278(6) 0.0125(5) 0.0125(5) 0.0070(5) Ni7 0.0427(7) 0.0373(7) 0.0437(7) 0.0191(5) 0.0227(5) 0.0082(5) Cl1 0.0341(12) 0.0765(18) 0.0501(15) 0.0367(14) 0.0037(11) -0.0138(12) Cl2 0.0595(15) 0.0487(15) 0.0744(18) 0.0330(13) 0.0404(14) 0.0119(12) N1 0.034(4) 0.071(6) 0.033(4) 0.027(4) 0.008(3) -0.009(4) N2 0.028(4) 0.052(5) 0.027(4) 0.020(3) 0.003(3) -0.005(3) N3 0.026(3) 0.050(5) 0.022(3) 0.019(3) 0.003(3) 0.002(3) N4 0.030(3) 0.037(4) 0.022(3) 0.013(3) 0.008(3) 0.006(3) N5 0.032(4) 0.040(4) 0.030(4) 0.017(3) 0.011(3) 0.009(3) N6 0.039(4) 0.037(4) 0.039(4) 0.018(3) 0.020(3) 0.012(3) N7 0.057(5) 0.052(5) 0.057(5) 0.026(4) 0.036(4) 0.020(4) N8 0.034(4) 0.059(5) 0.035(4) 0.026(4) 0.002(3) -0.001(4) N9 0.023(3) 0.051(5) 0.031(4) 0.024(4) 0.003(3) 0.002(3) N10 0.029(4) 0.044(4) 0.024(3) 0.019(3) 0.005(3) 0.003(3) N11 0.027(3) 0.039(4) 0.023(3) 0.013(3) 0.006(3) 0.003(3) N12 0.033(4) 0.039(4) 0.031(4) 0.016(3) 0.008(3) 0.006(3) N13 0.037(4) 0.043(4) 0.032(4) 0.015(3) 0.013(3) 0.014(3) N14 0.038(4) 0.036(4) 0.041(4) 0.016(3) 0.010(3) 0.006(3) N15 0.037(4) 0.059(5) 0.040(4) 0.029(4) 0.000(3) -0.006(4) N16 0.028(4) 0.050(5) 0.029(4) 0.022(3) 0.002(3) -0.001(3) N17 0.031(4) 0.043(4) 0.030(4) 0.018(3) 0.011(3) 0.008(3) N18 0.031(4) 0.035(4) 0.022(3) 0.011(3) 0.006(3) 0.002(3) N19 0.036(4) 0.035(4) 0.020(3) 0.009(3) 0.007(3) 0.002(3) N20 0.050(4) 0.040(4) 0.025(4) 0.012(3) 0.013(3) 0.008(4) N21 0.072(6) 0.047(5) 0.039(4) 0.025(4) 0.023(4) 0.009(4) N22 0.024(4) 0.073(6) 0.033(4) 0.025(4) 0.007(3) 0.002(4) N23 0.025(3) 0.057(5) 0.028(4) 0.021(4) 0.007(3) 0.005(3) N24 0.024(3) 0.046(4) 0.028(4) 0.014(3) 0.011(3) 0.005(3) N25 0.025(3) 0.045(4) 0.028(4) 0.018(3) 0.011(3) 0.009(3) N26 0.029(4) 0.042(4) 0.027(4) 0.015(3) 0.011(3) 0.008(3) N27 0.028(3) 0.037(4) 0.024(3) 0.008(3) 0.008(3) 0.004(3) N28 0.030(4) 0.042(5) 0.049(5) 0.018(4) 0.016(3) 0.003(3) C1 0.044(6) 0.108(10) 0.028(5) 0.026(6) 0.006(4) -0.016(6) C2 0.054(7) 0.150(13) 0.032(6) 0.041(7) 0.012(5) -0.023(8) C3 0.063(7) 0.095(9) 0.029(5) 0.029(6) 0.006(5) -0.010(6) C4 0.037(5) 0.076(7) 0.027(5) 0.025(5) 0.008(4) -0.003(5) C5 0.036(5) 0.064(6) 0.030(5) 0.028(5) 0.008(4) 0.000(4) C6 0.040(5) 0.061(6) 0.027(5) 0.020(5) 0.000(4) -0.001(5) C7 0.033(5) 0.053(6) 0.019(4) 0.011(4) -0.001(3) 0.004(4) C8 0.027(4) 0.045(5) 0.033(5) 0.020(4) 0.005(4) 0.001(4) C9 0.027(4) 0.043(5) 0.025(4) 0.015(4) 0.003(3) 0.005(4) C10 0.036(5) 0.049(6) 0.037(5) 0.024(4) 0.010(4) 0.009(4) C11 0.033(5) 0.057(6) 0.038(5) 0.025(5) 0.006(4) 0.015(4) C12 0.030(4) 0.054(6) 0.038(5) 0.020(4) 0.009(4) 0.010(4) C13 0.030(4) 0.036(5) 0.027(4) 0.013(4) 0.007(3) 0.001(4) C14 0.027(4) 0.046(5) 0.033(5) 0.014(4) 0.008(4) 0.001(4) C15 0.047(5) 0.045(6) 0.043(5) 0.021(4) 0.021(4) 0.019(5) C16 0.057(6) 0.052(6) 0.058(6) 0.023(5) 0.030(5) 0.025(5) C17 0.060(6) 0.050(6) 0.063(7) 0.026(5) 0.037(5) 0.027(5) C18 0.049(5) 0.047(6) 0.048(6) 0.022(5) 0.029(5) 0.015(5) C19 0.084(8) 0.066(8) 0.087(8) 0.038(7) 0.063(7) 0.045(7) C20 0.117(11) 0.081(9) 0.105(10) 0.060(8) 0.093(9) 0.057(8) C21 0.086(8) 0.070(8) 0.084(8) 0.046(7) 0.066(7) 0.036(7) C22 0.051(6) 0.058(7) 0.049(6) 0.032(5) 0.000(5) -0.008(5) C23 0.061(7) 0.063(7) 0.043(6) 0.023(6) -0.009(5) -0.017(6) C24 0.046(6) 0.064(7) 0.035(5) 0.018(5) -0.015(4) -0.007(5) C25 0.040(5) 0.050(6) 0.032(5) 0.020(4) 0.002(4) 0.002(4) C26 0.027(4) 0.048(6) 0.037(5) 0.021(4) 0.003(4) -0.002(4) C27 0.040(5) 0.051(6) 0.025(4) 0.016(4) 0.002(4) 0.010(4) C28 0.029(4) 0.048(5) 0.021(4) 0.014(4) 0.000(3) 0.002(4) C29 0.023(4) 0.045(5) 0.033(5) 0.019(4) 0.008(3) 0.003(4) C30 0.026(4) 0.046(5) 0.025(4) 0.013(4) 0.004(3) 0.004(4) C31 0.034(5) 0.046(6) 0.039(5) 0.019(4) 0.002(4) 0.008(4) C32 0.038(5) 0.061(7) 0.048(6) 0.025(5) 0.000(4) 0.013(5) C33 0.046(5) 0.048(6) 0.040(5) 0.025(5) 0.004(4) 0.009(5) C34 0.030(4) 0.047(5) 0.025(4) 0.016(4) 0.002(3) 0.004(4) C35 0.031(4) 0.038(5) 0.033(5) 0.009(4) 0.009(4) 0.001(4) C36 0.035(5) 0.050(6) 0.060(6) 0.017(5) 0.016(5) 0.010(5) C37 0.042(6) 0.049(6) 0.077(8) 0.020(6) 0.017(5) 0.017(5) C38 0.035(5) 0.040(6) 0.071(7) 0.016(5) 0.012(5) 0.008(4) C39 0.039(5) 0.033(5) 0.039(5) 0.012(4) 0.009(4) 0.004(4) C40 0.054(7) 0.038(6) 0.104(10) 0.022(6) 0.022(6) 0.011(5) C41 0.046(6) 0.041(6) 0.100(9) 0.024(6) 0.021(6) 0.007(5) C42 0.036(5) 0.048(6) 0.060(6) 0.021(5) 0.009(5) 0.005(5) C43 0.048(6) 0.064(7) 0.061(7) 0.040(6) 0.004(5) -0.002(6) C44 0.063(8) 0.073(9) 0.094(10) 0.061(8) 0.002(7) -0.005(7) C45 0.066(7) 0.051(7) 0.063(7) 0.031(6) 0.010(6) 0.006(6) C46 0.049(6) 0.047(6) 0.042(5) 0.023(5) -0.001(4) 0.006(5) C47 0.037(5) 0.047(6) 0.035(5) 0.023(4) -0.001(4) -0.004(4) C48 0.051(6) 0.052(6) 0.054(6) 0.028(5) 0.008(5) 0.013(5) C49 0.045(5) 0.057(6) 0.041(5) 0.024(5) 0.014(4) 0.015(5) C50 0.030(4) 0.049(6) 0.029(4) 0.019(4) 0.006(4) 0.002(4) C51 0.040(5) 0.050(6) 0.023(4) 0.015(4) 0.011(4) 0.014(4) C52 0.050(5) 0.034(5) 0.032(5) 0.010(4) 0.009(4) 0.002(4) C53 0.076(7) 0.048(6) 0.035(5) 0.012(5) 0.027(5) 0.015(5) C54 0.061(6) 0.051(6) 0.038(5) 0.014(5) 0.025(5) 0.010(5) C55 0.035(5) 0.050(6) 0.028(4) 0.019(4) 0.011(4) 0.009(4) C56 0.050(5) 0.035(5) 0.026(4) 0.009(4) 0.016(4) 0.007(4) C57 0.063(6) 0.044(6) 0.030(5) 0.013(4) 0.010(4) -0.001(5) C58 0.093(8) 0.046(6) 0.026(5) 0.011(5) 0.010(5) -0.006(6) C59 0.103(9) 0.048(6) 0.024(5) 0.011(5) 0.017(5) -0.003(6) C60 0.059(6) 0.046(6) 0.030(5) 0.015(4) 0.017(4) 0.005(5) C61 0.158(14) 0.084(10) 0.036(6) 0.037(7) 0.010(8) -0.011(10) C62 0.157(14) 0.077(9) 0.036(6) 0.031(6) 0.013(8) -0.029(9) C63 0.099(9) 0.062(8) 0.044(6) 0.030(6) 0.015(6) -0.008(7) C64 0.030(5) 0.088(8) 0.035(5) 0.025(5) 0.010(4) 0.003(5) C65 0.026(5) 0.096(9) 0.033(5) 0.023(6) 0.009(4) -0.001(6) C66 0.040(5) 0.093(9) 0.039(6) 0.024(6) 0.018(4) 0.018(6) C67 0.032(5) 0.078(7) 0.033(5) 0.024(5) 0.012(4) 0.014(5) C68 0.025(4) 0.075(7) 0.024(4) 0.021(4) 0.006(3) 0.004(5) C69 0.038(5) 0.078(8) 0.055(6) 0.023(6) 0.022(5) 0.023(5) C70 0.037(5) 0.067(7) 0.046(6) 0.022(5) 0.014(4) 0.013(5) C71 0.031(5) 0.061(6) 0.023(4) 0.015(4) 0.004(4) 0.009(4) C72 0.032(4) 0.053(6) 0.030(5) 0.018(4) 0.010(4) 0.006(4) C73 0.038(5) 0.070(7) 0.039(5) 0.016(5) 0.018(4) 0.011(5) C74 0.046(6) 0.058(7) 0.044(6) -0.001(5) 0.021(5) 0.006(5) C75 0.036(5) 0.042(5) 0.039(5) 0.005(4) 0.010(4) 0.000(4) C76 0.035(5) 0.043(5) 0.023(4) 0.011(4) 0.007(3) 0.006(4) C77 0.034(5) 0.042(5) 0.030(4) 0.013(4) 0.010(4) 0.005(4) C78 0.034(5) 0.055(6) 0.027(5) 0.012(4) 0.005(4) 0.005(4) C79 0.034(5) 0.068(7) 0.031(5) 0.014(5) 0.001(4) 0.002(5) C80 0.028(4) 0.051(6) 0.040(5) 0.013(4) 0.003(4) 0.006(4) C81 0.031(4) 0.040(5) 0.039(5) 0.011(4) 0.011(4) 0.004(4) C82 0.037(5) 0.062(7) 0.061(7) 0.019(6) 0.006(5) 0.003(5) C83 0.034(5) 0.078(8) 0.070(8) 0.033(7) 0.012(5) 0.005(5) C84 0.046(6) 0.056(7) 0.065(7) 0.030(6) 0.025(5) 0.013(5) P1 0.0399(13) 0.0617(17) 0.0318(13) 0.0086(12) 0.0051(10) 0.0155(12) F1 0.072(4) 0.096(5) 0.052(4) 0.024(4) 0.003(3) 0.038(4) F2 0.050(3) 0.089(5) 0.055(4) 0.032(3) 0.008(3) 0.025(3) F3 0.053(3) 0.085(5) 0.050(3) 0.010(3) 0.021(3) 0.023(3) F4 0.043(3) 0.063(4) 0.064(4) 0.007(3) 0.006(3) 0.011(3) F5 0.058(4) 0.085(5) 0.047(3) 0.012(3) 0.019(3) 0.028(3) F6 0.058(3) 0.063(4) 0.051(3) 0.019(3) 0.016(3) 0.016(3) P2 0.081(2) 0.092(2) 0.0436(16) 0.0363(17) 0.0258(15) 0.0510(19) F7 0.123(6) 0.149(7) 0.053(4) 0.058(4) 0.038(4) 0.093(6) F8 0.072(4) 0.098(5) 0.056(4) 0.044(4) 0.019(3) 0.046(4) F9 0.087(5) 0.195(9) 0.070(5) 0.084(6) 0.044(4) 0.085(6) F10 0.096(5) 0.115(6) 0.063(4) 0.049(4) 0.038(4) 0.046(5) F11 0.185(9) 0.107(7) 0.059(5) 0.028(5) 0.031(5) 0.084(7) F12 0.093(5) 0.090(6) 0.081(5) 0.032(4) 0.005(4) 0.034(4) P3 0.057(2) 0.078(3) 0.110(3) 0.008(2) 0.005(2) 0.0206(19) F13 0.070(5) 0.171(10) 0.153(9) 0.051(8) 0.026(5) 0.054(6) F14 0.091(6) 0.093(6) 0.175(10) 0.021(6) -0.017(6) 0.034(5) F15 0.071(5) 0.114(7) 0.155(8) 0.061(6) 0.031(5) 0.034(5) F16 0.135(9) 0.083(7) 0.224(13) 0.027(8) 0.047(9) 0.016(6) F17 0.116(8) 0.287(16) 0.105(8) 0.066(9) 0.048(6) 0.090(9) F18 0.153(9) 0.117(7) 0.105(7) 0.030(6) 0.039(6) 0.054(7) P4 0.099(5) 0.083(5) 0.062(4) 0.036(4) 0.033(4) 0.048(4) P5 0.087(5) 0.076(4) 0.039(3) 0.005(3) 0.008(3) 0.039(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 N22 2.082(9) . ? Ni1 N1 2.086(8) . ? Ni1 N15 2.092(9) . ? Ni1 N8 2.096(7) . ? Ni1 Cl1 2.312(2) . ? Ni1 Ni2 2.4015(13) . ? Ni2 N2 1.922(7) . ? Ni2 N16 1.923(8) . ? Ni2 N9 1.930(7) . ? Ni2 N23 1.934(8) . ? Ni2 Ni3 2.2812(13) . ? Ni3 N10 1.873(6) . ? Ni3 N17 1.879(7) . ? Ni3 N3 1.885(6) . ? Ni3 N24 1.891(7) . ? Ni3 Ni4 2.2591(13) . ? Ni4 N25 1.911(7) . ? Ni4 N18 1.920(7) . ? Ni4 N11 1.926(7) . ? Ni4 N4 1.927(7) . ? Ni4 Ni5 2.2622(13) . ? Ni5 N26 1.887(7) . ? Ni5 N19 1.891(6) . ? Ni5 N5 1.899(7) . ? Ni5 N12 1.899(7) . ? Ni5 Ni6 2.2838(13) . ? Ni6 N27 1.921(6) . ? Ni6 N20 1.929(7) . ? Ni6 N6 1.931(7) . ? Ni6 N13 1.942(7) . ? Ni6 Ni7 2.4122(14) . ? Ni7 N7 2.087(8) . ? Ni7 N21 2.092(8) . ? Ni7 N28 2.097(8) . ? Ni7 N14 2.100(8) . ? Ni7 Cl2 2.317(2) . ? N1 C1 1.327(11) . ? N1 C5 1.367(11) . ? N2 C8 1.360(10) . ? N2 C5 1.375(10) . ? N3 C8 1.351(10) . ? N3 C9 1.390(10) . ? N4 C13 1.360(10) . ? N4 C9 1.363(10) . ? N5 C14 1.361(10) . ? N5 C13 1.394(10) . ? N6 C14 1.358(11) . ? N6 C18 1.386(11) . ? N7 C21 1.348(12) . ? N7 C18 1.360(12) . ? N8 C22 1.329(12) . ? N8 C26 1.357(11) . ? N9 C26 1.355(11) . ? N9 C29 1.359(10) . ? N10 C29 1.362(10) . ? N10 C30 1.399(11) . ? N11 C30 1.347(10) . ? N11 C34 1.366(11) . ? N12 C35 1.337(11) . ? N12 C34 1.401(10) . ? N13 C35 1.353(10) . ? N13 C39 1.377(11) . ? N14 C39 1.335(11) . ? N14 C42 1.345(12) . ? N15 C43 1.344(13) . ? N15 C47 1.382(12) . ? N16 C50 1.368(10) . ? N16 C47 1.388(11) . ? N17 C50 1.374(11) . ? N17 C51 1.389(10) . ? N18 C51 1.361(11) . ? N18 C55 1.372(10) . ? N19 C56 1.352(10) . ? N19 C55 1.388(11) . ? N20 C56 1.358(11) . ? N20 C60 1.399(11) . ? N21 C63 1.340(12) . ? N21 C60 1.374(12) . ? N22 C64 1.336(11) . ? N22 C68 1.361(12) . ? N23 C71 1.361(11) . ? N23 C68 1.374(10) . ? N24 C71 1.351(10) . ? N24 C72 1.386(11) . ? N25 C76 1.369(10) . ? N25 C72 1.378(10) . ? N26 C77 1.353(10) . ? N26 C76 1.386(10) . ? N27 C77 1.358(10) . ? N27 C81 1.390(10) . ? N28 C81 1.347(11) . ? N28 C84 1.348(12) . ? C1 C2 1.391(14) . ? C2 C3 1.360(15) . ? C3 C4 1.407(13) . ? C4 C5 1.397(12) . ? C4 C6 1.420(12) . ? C6 C7 1.352(12) . ? C7 C8 1.435(11) . ? C9 C10 1.380(12) . ? C10 C11 1.382(12) . ? C11 C12 1.378(12) . ? C12 C13 1.375(12) . ? C14 C15 1.425(13) . ? C15 C16 1.346(12) . ? C16 C17 1.454(13) . ? C17 C18 1.387(13) . ? C17 C19 1.419(13) . ? C19 C20 1.366(15) . ? C20 C21 1.392(16) . ? C22 C23 1.393(14) . ? C23 C24 1.353(14) . ? C24 C25 1.370(13) . ? C25 C26 1.416(12) . ? C25 C27 1.424(12) . ? C27 C28 1.341(12) . ? C28 C29 1.429(11) . ? C30 C31 1.392(12) . ? C31 C32 1.379(13) . ? C32 C33 1.381(13) . ? C33 C34 1.387(12) . ? C35 C36 1.435(14) . ? C36 C37 1.350(14) . ? C37 C38 1.417(13) . ? C38 C40 1.401(14) . ? C38 C39 1.413(14) . ? C40 C41 1.363(14) . ? C41 C42 1.379(15) . ? C43 C44 1.368(18) . ? C44 C45 1.379(17) . ? C45 C46 1.394(14) . ? C46 C47 1.393(15) . ? C46 C48 1.404(14) . ? C48 C49 1.373(13) . ? C49 C50 1.416(13) . ? C51 C52 1.390(12) . ? C52 C53 1.387(12) . ? C53 C54 1.388(13) . ? C54 C55 1.370(13) . ? C56 C57 1.424(13) . ? C57 C58 1.364(13) . ? C58 C59 1.420(15) . ? C59 C60 1.378(14) . ? C59 C61 1.434(14) . ? C61 C62 1.362(17) . ? C62 C63 1.396(16) . ? C64 C65 1.403(16) . ? C65 C66 1.389(16) . ? C66 C67 1.404(13) . ? C67 C68 1.404(15) . ? C67 C69 1.421(15) . ? C69 C70 1.333(13) . ? C70 C71 1.417(14) . ? C72 C73 1.368(13) . ? C73 C74 1.384(13) . ? C74 C75 1.398(12) . ? C75 C76 1.349(13) . ? C77 C78 1.433(12) . ? C78 C79 1.344(12) . ? C79 C80 1.417(13) . ? C80 C81 1.401(12) . ? C80 C82 1.416(12) . ? C82 C83 1.367(15) . ? C83 C84 1.382(15) . ? P1 F2 1.571(6) . ? P1 F3 1.579(6) . ? P1 F4 1.587(6) . ? P1 F1 1.587(6) . ? P1 F5 1.588(6) . ? P1 F6 1.593(6) . ? P2 F11 1.566(9) . ? P2 F12 1.568(8) . ? P2 F9 1.576(7) . ? P2 F7 1.581(7) . ? P2 F10 1.598(7) . ? P2 F8 1.615(6) . ? P3 F17 1.478(12) . ? P3 F14 1.521(9) . ? P3 F16 1.563(11) . ? P3 F13 1.567(10) . ? P3 F18 1.594(11) . ? P3 F15 1.611(9) . ? P4 F19 1.519(14) . ? P4 F21 1.544(15) . ? P4 F22 1.552(14) . ? P4 F24 1.555(14) . ? P4 F23 1.563(14) . ? P4 F20 1.576(9) . ? P5 F26 1.511(13) . ? P5 F25 1.526(9) . ? P5 F27 1.527(13) . ? P5 F30 1.528(14) . ? P5 F29 1.572(12) . ? P5 F28 1.599(14) . ? N29 C85 1.142(17) . ? C85 C86 1.44(2) . ? N30 C87 1.10(2) . ? C87 C88 1.54(3) . ? N31 C89 1.14(3) . ? C89 C90 1.45(4) . ? N32 C91 1.25(2) . ? C91 C92 1.41(3) . ? N33 C93 1.128(10) . ? C93 C94 1.535(10) . ? N34 C95 1.122(10) . ? C95 C96 1.515(10) . ? N35 C97 1.125(10) . ? C97 C98 1.514(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 N22 Ni1 N1 90.2(3) . . ? N22 Ni1 N15 166.0(3) . . ? N1 Ni1 N15 89.6(3) . . ? N22 Ni1 N8 88.9(3) . . ? N1 Ni1 N8 165.2(3) . . ? N15 Ni1 N8 87.7(3) . . ? N22 Ni1 Cl1 97.5(2) . . ? N1 Ni1 Cl1 96.6(2) . . ? N15 Ni1 Cl1 96.4(2) . . ? N8 Ni1 Cl1 98.2(2) . . ? N22 Ni1 Ni2 82.05(19) . . ? N1 Ni1 Ni2 82.53(19) . . ? N15 Ni1 Ni2 84.0(2) . . ? N8 Ni1 Ni2 82.7(2) . . ? Cl1 Ni1 Ni2 179.01(10) . . ? N2 Ni2 N16 89.8(3) . . ? N2 Ni2 N9 174.8(3) . . ? N16 Ni2 N9 89.7(3) . . ? N2 Ni2 N23 90.4(3) . . ? N16 Ni2 N23 174.9(3) . . ? N9 Ni2 N23 89.6(3) . . ? N2 Ni2 Ni3 87.23(19) . . ? N16 Ni2 Ni3 88.4(2) . . ? N9 Ni2 Ni3 87.54(19) . . ? N23 Ni2 Ni3 86.6(2) . . ? N2 Ni2 Ni1 93.01(19) . . ? N16 Ni2 Ni1 91.7(2) . . ? N9 Ni2 Ni1 92.22(19) . . ? N23 Ni2 Ni1 93.4(2) . . ? Ni3 Ni2 Ni1 179.76(6) . . ? N10 Ni3 N17 90.5(3) . . ? N10 Ni3 N3 179.5(3) . . ? N17 Ni3 N3 89.4(3) . . ? N10 Ni3 N24 89.4(3) . . ? N17 Ni3 N24 179.3(3) . . ? N3 Ni3 N24 90.7(3) . . ? N10 Ni3 Ni4 88.61(19) . . ? N17 Ni3 Ni4 89.9(2) . . ? N3 Ni3 Ni4 90.9(2) . . ? N24 Ni3 Ni4 89.3(2) . . ? N10 Ni3 Ni2 90.2(2) . . ? N17 Ni3 Ni2 89.5(2) . . ? N3 Ni3 Ni2 90.3(2) . . ? N24 Ni3 Ni2 91.3(2) . . ? Ni4 Ni3 Ni2 178.63(6) . . ? N25 Ni4 N18 179.7(3) . . ? N25 Ni4 N11 89.1(3) . . ? N18 Ni4 N11 90.5(3) . . ? N25 Ni4 N4 90.3(3) . . ? N18 Ni4 N4 90.0(3) . . ? N11 Ni4 N4 179.2(3) . . ? N25 Ni4 Ni3 90.55(19) . . ? N18 Ni4 Ni3 89.45(19) . . ? N11 Ni4 Ni3 90.63(19) . . ? N4 Ni4 Ni3 88.85(19) . . ? N25 Ni4 Ni5 89.75(19) . . ? N18 Ni4 Ni5 90.25(19) . . ? N11 Ni4 Ni5 89.41(19) . . ? N4 Ni4 Ni5 91.11(19) . . ? Ni3 Ni4 Ni5 179.70(7) . . ? N26 Ni5 N19 179.0(3) . . ? N26 Ni5 N5 90.1(3) . . ? N19 Ni5 N5 90.5(3) . . ? N26 Ni5 N12 89.3(3) . . ? N19 Ni5 N12 90.1(3) . . ? N5 Ni5 N12 179.3(3) . . ? N26 Ni5 Ni4 89.8(2) . . ? N19 Ni5 Ni4 89.4(2) . . ? N5 Ni5 Ni4 88.7(2) . . ? N12 Ni5 Ni4 90.9(2) . . ? N26 Ni5 Ni6 90.3(2) . . ? N19 Ni5 Ni6 90.5(2) . . ? N5 Ni5 Ni6 90.5(2) . . ? N12 Ni5 Ni6 89.9(2) . . ? Ni4 Ni5 Ni6 179.20(7) . . ? N27 Ni6 N20 174.9(3) . . ? N27 Ni6 N6 90.9(3) . . ? N20 Ni6 N6 89.5(3) . . ? N27 Ni6 N13 89.7(3) . . ? N20 Ni6 N13 89.4(3) . . ? N6 Ni6 N13 174.4(3) . . ? N27 Ni6 Ni5 87.66(19) . . ? N20 Ni6 Ni5 87.3(2) . . ? N6 Ni6 Ni5 86.8(2) . . ? N13 Ni6 Ni5 87.6(2) . . ? N27 Ni6 Ni7 92.62(19) . . ? N20 Ni6 Ni7 92.5(2) . . ? N6 Ni6 Ni7 92.8(2) . . ? N13 Ni6 Ni7 92.7(2) . . ? Ni5 Ni6 Ni7 179.58(7) . . ? N7 Ni7 N21 87.2(3) . . ? N7 Ni7 N28 92.4(3) . . ? N21 Ni7 N28 166.3(3) . . ? N7 Ni7 N14 164.5(3) . . ? N21 Ni7 N14 88.1(3) . . ? N28 Ni7 N14 88.7(3) . . ? N7 Ni7 Cl2 96.4(2) . . ? N21 Ni7 Cl2 96.6(2) . . ? N28 Ni7 Cl2 97.0(2) . . ? N14 Ni7 Cl2 98.8(2) . . ? N7 Ni7 Ni6 82.2(2) . . ? N21 Ni7 Ni6 83.4(2) . . ? N28 Ni7 Ni6 83.06(19) . . ? N14 Ni7 Ni6 82.60(19) . . ? Cl2 Ni7 Ni6 178.57(9) . . ? C1 N1 C5 117.1(8) . . ? C1 N1 Ni1 119.5(6) . . ? C5 N1 Ni1 123.0(6) . . ? C8 N2 C5 119.3(7) . . ? C8 N2 Ni2 120.5(5) . . ? C5 N2 Ni2 120.0(5) . . ? C8 N3 C9 124.0(7) . . ? C8 N3 Ni3 116.9(5) . . ? C9 N3 Ni3 118.9(5) . . ? C13 N4 C9 120.7(7) . . ? C13 N4 Ni4 118.6(5) . . ? C9 N4 Ni4 120.7(5) . . ? C14 N5 C13 123.3(7) . . ? C14 N5 Ni5 116.3(6) . . ? C13 N5 Ni5 119.9(5) . . ? C14 N6 C18 118.6(8) . . ? C14 N6 Ni6 121.6(6) . . ? C18 N6 Ni6 119.2(6) . . ? C21 N7 C18 116.3(9) . . ? C21 N7 Ni7 120.1(7) . . ? C18 N7 Ni7 123.4(6) . . ? C22 N8 C26 118.0(8) . . ? C22 N8 Ni1 119.5(6) . . ? C26 N8 Ni1 121.8(6) . . ? C26 N9 C29 119.6(7) . . ? C26 N9 Ni2 120.2(5) . . ? C29 N9 Ni2 119.8(5) . . ? C29 N10 C30 122.9(7) . . ? C29 N10 Ni3 116.9(5) . . ? C30 N10 Ni3 120.0(5) . . ? C30 N11 C34 120.9(7) . . ? C30 N11 Ni4 119.0(5) . . ? C34 N11 Ni4 120.1(5) . . ? C35 N12 C34 124.0(8) . . ? C35 N12 Ni5 117.3(6) . . ? C34 N12 Ni5 118.2(6) . . ? C35 N13 C39 120.4(8) . . ? C35 N13 Ni6 120.0(6) . . ? C39 N13 Ni6 119.3(6) . . ? C39 N14 C42 118.1(8) . . ? C39 N14 Ni7 123.0(6) . . ? C42 N14 Ni7 118.3(6) . . ? C43 N15 C47 116.9(10) . . ? C43 N15 Ni1 120.2(8) . . ? C47 N15 Ni1 122.3(6) . . ? C50 N16 C47 117.0(8) . . ? C50 N16 Ni2 120.3(6) . . ? C47 N16 Ni2 122.3(6) . . ? C50 N17 C51 122.0(8) . . ? C50 N17 Ni3 118.4(5) . . ? C51 N17 Ni3 119.4(6) . . ? C51 N18 C55 120.6(7) . . ? C51 N18 Ni4 120.1(5) . . ? C55 N18 Ni4 119.3(6) . . ? C56 N19 C55 123.4(7) . . ? C56 N19 Ni5 116.1(6) . . ? C55 N19 Ni5 120.1(5) . . ? C56 N20 C60 118.3(7) . . ? C56 N20 Ni6 120.5(5) . . ? C60 N20 Ni6 120.7(6) . . ? C63 N21 C60 117.1(9) . . ? C63 N21 Ni7 119.4(7) . . ? C60 N21 Ni7 122.8(6) . . ? C64 N22 C68 117.9(9) . . ? C64 N22 Ni1 118.3(7) . . ? C68 N22 Ni1 123.6(6) . . ? C71 N23 C68 120.2(8) . . ? C71 N23 Ni2 120.7(6) . . ? C68 N23 Ni2 118.5(7) . . ? C71 N24 C72 123.7(8) . . ? C71 N24 Ni3 115.4(6) . . ? C72 N24 Ni3 120.2(5) . . ? C76 N25 C72 120.5(7) . . ? C76 N25 Ni4 120.2(5) . . ? C72 N25 Ni4 119.3(6) . . ? C77 N26 C76 124.0(7) . . ? C77 N26 Ni5 116.8(5) . . ? C76 N26 Ni5 119.1(5) . . ? C77 N27 C81 119.2(7) . . ? C77 N27 Ni6 120.3(5) . . ? C81 N27 Ni6 120.2(5) . . ? C81 N28 C84 117.5(8) . . ? C81 N28 Ni7 122.6(6) . . ? C84 N28 Ni7 119.0(6) . . ? N1 C1 C2 123.8(9) . . ? C3 C2 C1 119.7(9) . . ? C2 C3 C4 118.2(9) . . ? C5 C4 C3 118.9(8) . . ? C5 C4 C6 117.9(8) . . ? C3 C4 C6 123.3(8) . . ? N1 C5 N2 115.7(7) . . ? N1 C5 C4 122.1(7) . . ? N2 C5 C4 122.2(8) . . ? C7 C6 C4 120.2(8) . . ? C6 C7 C8 120.1(8) . . ? N3 C8 N2 116.3(7) . . ? N3 C8 C7 123.2(7) . . ? N2 C8 C7 120.1(7) . . ? N4 C9 C10 120.5(7) . . ? N4 C9 N3 115.1(7) . . ? C10 C9 N3 124.0(7) . . ? C9 C10 C11 117.9(8) . . ? C12 C11 C10 121.4(8) . . ? C13 C12 C11 118.7(8) . . ? N4 C13 C12 120.2(7) . . ? N4 C13 N5 115.7(7) . . ? C12 C13 N5 124.0(7) . . ? N6 C14 N5 115.3(8) . . ? N6 C14 C15 121.8(8) . . ? N5 C14 C15 122.6(8) . . ? C16 C15 C14 120.2(9) . . ? C15 C16 C17 118.8(9) . . ? C18 C17 C19 119.5(9) . . ? C18 C17 C16 118.9(8) . . ? C19 C17 C16 121.6(9) . . ? N7 C18 N6 115.7(8) . . ? N7 C18 C17 122.7(8) . . ? N6 C18 C17 121.6(8) . . ? C20 C19 C17 117.8(10) . . ? C19 C20 C21 119.2(9) . . ? N7 C21 C20 124.4(10) . . ? N8 C22 C23 123.1(9) . . ? C24 C23 C22 118.9(10) . . ? C23 C24 C25 120.1(9) . . ? C24 C25 C26 118.6(8) . . ? C24 C25 C27 124.7(8) . . ? C26 C25 C27 116.7(8) . . ? N9 C26 N8 116.7(7) . . ? N9 C26 C25 122.2(7) . . ? N8 C26 C25 121.1(8) . . ? C28 C27 C25 121.3(8) . . ? C27 C28 C29 119.4(7) . . ? N9 C29 N10 116.1(7) . . ? N9 C29 C28 120.7(7) . . ? N10 C29 C28 122.9(7) . . ? N11 C30 C31 120.9(8) . . ? N11 C30 N10 114.9(7) . . ? C31 C30 N10 124.1(7) . . ? C32 C31 C30 118.0(8) . . ? C31 C32 C33 121.0(9) . . ? C32 C33 C34 119.0(8) . . ? N11 C34 C33 119.8(7) . . ? N11 C34 N12 116.0(7) . . ? C33 C34 N12 124.1(8) . . ? N12 C35 N13 116.6(8) . . ? N12 C35 C36 123.8(8) . . ? N13 C35 C36 119.4(8) . . ? C37 C36 C35 121.2(9) . . ? C36 C37 C38 119.3(10) . . ? C40 C38 C39 118.3(9) . . ? C40 C38 C37 123.0(10) . . ? C39 C38 C37 118.8(9) . . ? N14 C39 N13 117.2(8) . . ? N14 C39 C38 122.0(8) . . ? N13 C39 C38 120.8(8) . . ? C41 C40 C38 118.7(11) . . ? C40 C41 C42 119.7(10) . . ? N14 C42 C41 123.0(9) . . ? N15 C43 C44 123.0(11) . . ? C43 C44 C45 120.8(11) . . ? C44 C45 C46 118.1(12) . . ? C47 C46 C45 118.8(10) . . ? C47 C46 C48 118.0(9) . . ? C45 C46 C48 123.1(11) . . ? N15 C47 N16 114.2(9) . . ? N15 C47 C46 122.4(8) . . ? N16 C47 C46 123.4(8) . . ? C49 C48 C46 119.8(10) . . ? C48 C49 C50 119.9(9) . . ? N16 C50 N17 114.6(8) . . ? N16 C50 C49 121.5(8) . . ? N17 C50 C49 123.4(8) . . ? N18 C51 N17 114.9(7) . . ? N18 C51 C52 120.9(7) . . ? N17 C51 C52 124.1(8) . . ? C53 C52 C51 118.4(8) . . ? C52 C53 C54 120.0(9) . . ? C55 C54 C53 120.3(9) . . ? C54 C55 N18 119.7(8) . . ? C54 C55 N19 124.9(8) . . ? N18 C55 N19 115.2(7) . . ? N19 C56 N20 116.4(7) . . ? N19 C56 C57 123.1(8) . . ? N20 C56 C57 120.3(8) . . ? C58 C57 C56 121.2(9) . . ? C57 C58 C59 118.8(9) . . ? C60 C59 C58 118.8(9) . . ? C60 C59 C61 119.3(10) . . ? C58 C59 C61 121.8(10) . . ? N21 C60 C59 122.4(8) . . ? N21 C60 N20 115.1(8) . . ? C59 C60 N20 122.6(9) . . ? C62 C61 C59 117.8(11) . . ? C61 C62 C63 119.7(10) . . ? N21 C63 C62 123.8(11) . . ? N22 C64 C65 122.8(10) . . ? C66 C65 C64 120.1(9) . . ? C65 C66 C67 117.3(11) . . ? C66 C67 C68 119.6(10) . . ? C66 C67 C69 123.4(11) . . ? C68 C67 C69 117.0(8) . . ? N22 C68 N23 116.2(9) . . ? N22 C68 C67 122.2(8) . . ? N23 C68 C67 121.5(9) . . ? C70 C69 C67 121.0(11) . . ? C69 C70 C71 120.9(10) . . ? N24 C71 N23 116.7(9) . . ? N24 C71 C70 123.5(9) . . ? N23 C71 C70 119.3(8) . . ? C73 C72 N25 119.8(8) . . ? C73 C72 N24 125.0(8) . . ? N25 C72 N24 115.0(8) . . ? C72 C73 C74 119.8(8) . . ? C73 C74 C75 118.9(9) . . ? C76 C75 C74 120.5(9) . . ? C75 C76 N25 119.9(8) . . ? C75 C76 N26 125.1(8) . . ? N25 C76 N26 114.8(7) . . ? N26 C77 N27 116.7(7) . . ? N26 C77 C78 122.7(7) . . ? N27 C77 C78 120.5(7) . . ? C79 C78 C77 120.6(8) . . ? C78 C79 C80 119.3(8) . . ? C81 C80 C82 118.0(9) . . ? C81 C80 C79 119.3(8) . . ? C82 C80 C79 122.6(9) . . ? N28 C81 N27 116.4(8) . . ? N28 C81 C80 122.7(8) . . ? N27 C81 C80 120.8(7) . . ? C83 C82 C80 118.8(10) . . ? C82 C83 C84 119.4(9) . . ? N28 C84 C83 123.4(9) . . ? F2 P1 F3 90.0(3) . . ? F2 P1 F4 91.3(4) . . ? F3 P1 F4 90.9(3) . . ? F2 P1 F1 179.8(4) . . ? F3 P1 F1 90.1(4) . . ? F4 P1 F1 88.9(4) . . ? F2 P1 F5 90.6(3) . . ? F3 P1 F5 179.1(4) . . ? F4 P1 F5 89.7(3) . . ? F1 P1 F5 89.3(4) . . ? F2 P1 F6 90.1(3) . . ? F3 P1 F6 88.9(3) . . ? F4 P1 F6 178.6(4) . . ? F1 P1 F6 89.7(4) . . ? F5 P1 F6 90.5(3) . . ? F11 P2 F12 178.2(5) . . ? F11 P2 F9 90.0(5) . . ? F12 P2 F9 91.8(5) . . ? F11 P2 F7 90.0(5) . . ? F12 P2 F7 89.9(4) . . ? F9 P2 F7 90.9(4) . . ? F11 P2 F10 89.7(5) . . ? F12 P2 F10 88.6(4) . . ? F9 P2 F10 177.8(4) . . ? F7 P2 F10 91.2(4) . . ? F11 P2 F8 90.8(4) . . ? F12 P2 F8 89.3(4) . . ? F9 P2 F8 89.3(3) . . ? F7 P2 F8 179.2(5) . . ? F10 P2 F8 88.5(4) . . ? F17 P3 F14 89.4(7) . . ? F17 P3 F16 86.1(7) . . ? F14 P3 F16 95.1(6) . . ? F17 P3 F13 94.0(7) . . ? F14 P3 F13 175.2(6) . . ? F16 P3 F13 88.6(6) . . ? F17 P3 F18 178.4(8) . . ? F14 P3 F18 90.4(6) . . ? F16 P3 F18 92.4(7) . . ? F13 P3 F18 86.4(6) . . ? F17 P3 F15 92.1(7) . . ? F14 P3 F15 88.3(5) . . ? F16 P3 F15 176.2(7) . . ? F13 P3 F15 88.1(5) . . ? F18 P3 F15 89.4(5) . . ? F19 P4 F21 156.8(11) . . ? F19 P4 F22 80.6(10) . . ? F21 P4 F22 81.0(10) . . ? F19 P4 F24 89.8(10) . . ? F21 P4 F24 79.1(9) . . ? F22 P4 F24 98.4(10) . . ? F19 P4 F23 87.8(10) . . ? F21 P4 F23 104.4(10) . . ? F22 P4 F23 84.9(10) . . ? F24 P4 F23 175.5(11) . . ? F19 P4 F20 110.4(11) . . ? F21 P4 F20 89.1(10) . . ? F22 P4 F20 168.6(10) . . ? F24 P4 F20 85.1(10) . . ? F23 P4 F20 92.1(10) . . ? F26 P5 F25 104.2(10) . . ? F26 P5 F27 92.3(10) . . ? F25 P5 F27 162.4(10) . . ? F26 P5 F30 88.5(10) . . ? F25 P5 F30 89.3(9) . . ? F27 P5 F30 85.0(9) . . ? F26 P5 F29 92.7(9) . . ? F25 P5 F29 88.3(8) . . ? F27 P5 F29 97.1(9) . . ? F30 P5 F29 177.6(10) . . ? F26 P5 F28 177.8(11) . . ? F25 P5 F28 76.0(9) . . ? F27 P5 F28 87.8(9) . . ? F30 P5 F28 93.7(9) . . ? F29 P5 F28 85.1(9) . . ? N29 C85 C86 177.4(18) . . ? N30 C87 C88 162(2) . . ? N31 C89 C90 165(3) . . ? N32 C91 C92 167(2) . . ? N33 C93 C94 151(2) . . ? N34 C95 C96 170(6) . . ? N35 C97 C98 170(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.408 _refine_diff_density_min -1.146 _refine_diff_density_rms 0.167 # Attachment 'compound 5.cif' data_ic13083 _database_code_depnum_ccdc_archive 'CCDC 753225' #TrackingRef 'compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H114 Cl2 F24 N46 Ni9 O2 P4' _chemical_formula_weight 3555.86 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' 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.5457(4) _cell_length_b 13.4606(1) _cell_length_c 26.7809(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.0311(5) _cell_angle_gamma 90.00 _cell_volume 14079.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour deep-brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7224 _exptl_absorpt_coefficient_mu 1.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.917 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82821 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16112 _reflns_number_gt 10209 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(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^)+(0.0820P)^2^+2.9442P] 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_number_reflns 16112 _refine_ls_number_parameters 996 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1480 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 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 0.654250(9) 0.65750(3) 0.542029(13) 0.02265(11) Uani 1 1 d . . . Ni2 Ni 0.614134(8) 0.65136(3) 0.465367(13) 0.01964(10) Uani 1 1 d . . . Ni3 Ni 0.575885(8) 0.64787(3) 0.392354(12) 0.01917(10) Uani 1 1 d . . . Ni4 Ni 0.537783(8) 0.64849(3) 0.320556(12) 0.01890(10) Uani 1 1 d . . . Ni5 Ni 0.5000 0.64914(4) 0.2500 0.02304(13) Uani 1 2 d S . . Cl1 Cl 0.693612(19) 0.66318(6) 0.61617(3) 0.03430(19) Uani 1 1 d . . . N1 N 0.64332(6) 0.50457(18) 0.54340(8) 0.0255(5) Uani 1 1 d . . . N2 N 0.59489(5) 0.52660(17) 0.48270(8) 0.0217(5) Uani 1 1 d . . . N3 N 0.54794(5) 0.55689(17) 0.42151(8) 0.0209(5) Uani 1 1 d . . . N4 N 0.50349(5) 0.59746(17) 0.35707(8) 0.0198(5) Uani 1 1 d . . . N5 N 0.68902(6) 0.62705(18) 0.49236(8) 0.0250(5) Uani 1 1 d . . . N6 N 0.64486(5) 0.57967(18) 0.42910(8) 0.0221(5) Uani 1 1 d . . . N7 N 0.59899(5) 0.54036(17) 0.36758(8) 0.0219(5) Uani 1 1 d . . . N8 N 0.55061(5) 0.51475(17) 0.30693(8) 0.0224(5) Uani 1 1 d . . . N9 N 0.5000 0.5074(2) 0.2500 0.0227(7) Uani 1 2 d S . . N10 N 0.65516(6) 0.80851(18) 0.52516(8) 0.0243(5) Uani 1 1 d . . . N11 N 0.63047(6) 0.77596(17) 0.44211(8) 0.0230(5) Uani 1 1 d . . . N12 N 0.60364(6) 0.73687(18) 0.36209(8) 0.0238(5) Uani 1 1 d . . . N13 N 0.57234(5) 0.69706(18) 0.28371(8) 0.0215(5) Uani 1 1 d . . . N14 N 0.53617(5) 0.64903(17) 0.21121(8) 0.0214(5) Uani 1 1 d . . . N15 N 0.61081(6) 0.68254(18) 0.57495(8) 0.0254(5) Uani 1 1 d . . . N16 N 0.58000(5) 0.72025(18) 0.49600(8) 0.0216(5) Uani 1 1 d . . . N17 N 0.55213(5) 0.75559(18) 0.41615(8) 0.0226(5) Uani 1 1 d . . . N18 N 0.52501(5) 0.78176(17) 0.33408(8) 0.0213(5) Uani 1 1 d . . . N19 N 0.5000 0.7902(2) 0.2500 0.0215(7) Uani 1 2 d S . . C1 C 0.66256(7) 0.4462(2) 0.57678(11) 0.0319(7) Uani 1 1 d . . . H1 H 0.6834 0.4727 0.5943 0.038 Uiso 1 1 calc R . . C2 C 0.65406(8) 0.3491(2) 0.58749(12) 0.0363(8) Uani 1 1 d . . . H2 H 0.6689 0.3104 0.6112 0.044 Uiso 1 1 calc R . . C3 C 0.62371(8) 0.3102(2) 0.56309(11) 0.0339(7) Uani 1 1 d . . . H3 H 0.6169 0.2449 0.5705 0.041 Uiso 1 1 calc R . . C4 C 0.61369(7) 0.4653(2) 0.51785(10) 0.0238(6) Uani 1 1 d . . . C5 C 0.60311(7) 0.3687(2) 0.52713(11) 0.0275(7) Uani 1 1 d . . . C6 C 0.57184(7) 0.3346(2) 0.49826(11) 0.0299(7) Uani 1 1 d . . . H6 H 0.5641 0.2690 0.5029 0.036 Uiso 1 1 calc R . . C7 C 0.55327(7) 0.3956(2) 0.46437(10) 0.0265(7) Uani 1 1 d . . . H7 H 0.5324 0.3724 0.4455 0.032 Uiso 1 1 calc R . . C8 C 0.56453(7) 0.4945(2) 0.45655(10) 0.0220(6) Uani 1 1 d . . . C9 C 0.51288(6) 0.5520(2) 0.40261(10) 0.0211(6) Uani 1 1 d . . . C10 C 0.48831(7) 0.5111(2) 0.42780(10) 0.0243(6) Uani 1 1 d . . . H10 H 0.4946 0.4817 0.4602 0.029 Uiso 1 1 calc R . . C11 C 0.45425(7) 0.5136(2) 0.40520(11) 0.0259(6) Uani 1 1 d . . . H11 H 0.4373 0.4837 0.4218 0.031 Uiso 1 1 calc R . . C12 C 0.46968(7) 0.6031(2) 0.33534(10) 0.0226(6) Uani 1 1 d . . . C13 C 0.44462(7) 0.5587(2) 0.35912(10) 0.0256(6) Uani 1 1 d . . . H13 H 0.4213 0.5595 0.3437 0.031 Uiso 1 1 calc R . . C14 C 0.72240(7) 0.6362(2) 0.50876(11) 0.0295(7) Uani 1 1 d . . . H14 H 0.7293 0.6693 0.5400 0.035 Uiso 1 1 calc R . . C15 C 0.74766(7) 0.6005(3) 0.48318(11) 0.0345(8) Uani 1 1 d . . . H15 H 0.7711 0.6102 0.4965 0.041 Uiso 1 1 calc R . . C16 C 0.73841(7) 0.5510(3) 0.43848(11) 0.0331(7) Uani 1 1 d . . . H16 H 0.7553 0.5233 0.4210 0.040 Uiso 1 1 calc R . . C17 C 0.67937(7) 0.5828(2) 0.44681(10) 0.0235(6) Uani 1 1 d . . . C18 C 0.70346(7) 0.5420(2) 0.41891(11) 0.0270(7) Uani 1 1 d . . . C19 C 0.69097(7) 0.4964(2) 0.37179(11) 0.0305(7) Uani 1 1 d . . . H19 H 0.7066 0.4684 0.3521 0.037 Uiso 1 1 calc R . . C20 C 0.65682(7) 0.4928(2) 0.35485(11) 0.0274(7) Uani 1 1 d . . . H20 H 0.6486 0.4620 0.3234 0.033 Uiso 1 1 calc R . . C21 C 0.63317(7) 0.5348(2) 0.38392(10) 0.0221(6) Uani 1 1 d . . . C22 C 0.58091(7) 0.4766(2) 0.33134(10) 0.0222(6) Uani 1 1 d . . . C23 C 0.59016(7) 0.3807(2) 0.32185(10) 0.0262(7) Uani 1 1 d . . . H23 H 0.6103 0.3521 0.3404 0.031 Uiso 1 1 calc R . . C24 C 0.56963(7) 0.3263(2) 0.28474(11) 0.0277(7) Uani 1 1 d . . . H24 H 0.5765 0.2613 0.2767 0.033 Uiso 1 1 calc R . . C25 C 0.52947(7) 0.4592(2) 0.27226(10) 0.0221(6) Uani 1 1 d . . . C26 C 0.53962(7) 0.3648(2) 0.25945(10) 0.0247(6) Uani 1 1 d . . . H26 H 0.5260 0.3276 0.2336 0.030 Uiso 1 1 calc R . . C27 C 0.66744(7) 0.8757(2) 0.56065(11) 0.0278(7) Uani 1 1 d . . . H27 H 0.6725 0.8537 0.5947 0.033 Uiso 1 1 calc R . . C28 C 0.67312(7) 0.9740(2) 0.55078(11) 0.0299(7) Uani 1 1 d . . . H28 H 0.6809 1.0188 0.5775 0.036 Uiso 1 1 calc R . . C29 C 0.66739(7) 1.0061(2) 0.50174(12) 0.0307(7) Uani 1 1 d . . . H29 H 0.6726 1.0727 0.4938 0.037 Uiso 1 1 calc R . . C30 C 0.64662(7) 0.8420(2) 0.47704(11) 0.0251(7) Uani 1 1 d . . . C31 C 0.65376(7) 0.9397(2) 0.46322(11) 0.0264(7) Uani 1 1 d . . . C32 C 0.64539(7) 0.9671(2) 0.41149(11) 0.0295(7) Uani 1 1 d . . . H32 H 0.6504 1.0321 0.4010 0.035 Uiso 1 1 calc R . . C33 C 0.63025(7) 0.9006(2) 0.37730(11) 0.0274(7) Uani 1 1 d . . . H33 H 0.6250 0.9187 0.3427 0.033 Uiso 1 1 calc R . . C34 C 0.62212(7) 0.8031(2) 0.39298(10) 0.0242(6) Uani 1 1 d . . . C35 C 0.60158(7) 0.7371(2) 0.30956(10) 0.0232(6) Uani 1 1 d . . . C36 C 0.62754(7) 0.7675(2) 0.28379(11) 0.0277(7) Uani 1 1 d . . . H36 H 0.6488 0.7899 0.3017 0.033 Uiso 1 1 calc R . . C37 C 0.62202(7) 0.7645(2) 0.23154(11) 0.0307(7) Uani 1 1 d . . . H37 H 0.6392 0.7883 0.2134 0.037 Uiso 1 1 calc R . . C38 C 0.59170(7) 0.7272(2) 0.20544(11) 0.0278(11) Uani 1.000(11) 1 d . . . H38 H 0.5877 0.7276 0.1695 0.033 Uiso 1 1 calc R . . C39 C 0.56713(6) 0.6893(2) 0.23206(10) 0.0220(6) Uani 1 1 d . . . C40 C 0.61219(7) 0.6747(2) 0.62513(11) 0.0300(7) Uani 1 1 d . . . H40 H 0.6324 0.6482 0.6444 0.036 Uiso 1 1 calc R . . C41 C 0.58593(8) 0.7027(3) 0.65035(11) 0.0340(8) Uani 1 1 d . . . H41 H 0.5881 0.6950 0.6860 0.041 Uiso 1 1 calc R . . C42 C 0.55683(7) 0.7418(2) 0.62352(11) 0.0319(7) Uani 1 1 d . . . H42 H 0.5387 0.7631 0.6404 0.038 Uiso 1 1 calc R . . C43 C 0.58121(7) 0.7179(2) 0.54775(10) 0.0231(6) Uani 1 1 d . . . C44 C 0.55381(7) 0.7503(2) 0.57095(10) 0.0257(7) Uani 1 1 d . . . C45 C 0.52432(7) 0.7879(2) 0.53901(11) 0.0275(7) Uani 1 1 d . . . H45 H 0.5050 0.8090 0.5533 0.033 Uiso 1 1 calc R . . C46 C 0.52369(7) 0.7937(2) 0.48887(11) 0.0263(7) Uani 1 1 d . . . H46 H 0.5042 0.8207 0.4680 0.032 Uiso 1 1 calc R . . C47 C 0.55215(7) 0.7596(2) 0.46666(10) 0.0226(6) Uani 1 1 d . . . C48 C 0.53284(6) 0.8191(2) 0.38204(10) 0.0222(6) Uani 1 1 d . . . C49 C 0.52372(7) 0.9142(2) 0.39280(11) 0.0276(7) Uani 1 1 d . . . H49 H 0.5305 0.9417 0.4255 0.033 Uiso 1 1 calc R . . C50 C 0.50425(7) 0.9695(2) 0.35455(11) 0.0298(7) Uani 1 1 d . . . H50 H 0.4966 1.0340 0.3619 0.036 Uiso 1 1 calc R . . C51 C 0.49601(7) 0.9323(2) 0.30653(11) 0.0278(7) Uani 1 1 d . . . H51 H 0.4828 0.9709 0.2808 0.033 Uiso 1 1 calc R . . C52 C 0.50707(7) 0.8374(2) 0.29561(10) 0.0228(6) Uani 1 1 d . . . P1 P 0.78307(2) 0.38509(8) 0.31531(4) 0.0438(2) Uani 1 1 d . . . F1 F 0.74399(6) 0.3704(2) 0.29477(12) 0.1066(11) Uani 1 1 d . . . F2 F 0.77662(8) 0.49776(18) 0.32770(10) 0.0902(9) Uani 1 1 d . . . F3 F 0.77594(7) 0.3592(2) 0.37021(9) 0.0795(8) Uani 1 1 d . . . F4 F 0.78884(7) 0.27177(18) 0.30406(10) 0.0854(8) Uani 1 1 d . . . F5 F 0.79024(10) 0.4112(2) 0.26123(9) 0.1128(12) Uani 1 1 d . . . F6 F 0.82179(6) 0.3953(3) 0.33767(11) 0.1081(12) Uani 1 1 d . . . P2 P 0.57278(2) 0.04569(7) 0.54215(4) 0.0387(2) Uani 1 1 d . . . F7 F 0.58326(6) -0.05127(17) 0.51504(12) 0.0854(9) Uani 1 1 d . . . F8 F 0.55108(8) -0.01532(18) 0.57525(14) 0.1112(13) Uani 1 1 d . . . F9 F 0.59526(6) 0.10834(16) 0.50969(8) 0.0659(7) Uani 1 1 d . . . F10 F 0.60515(6) 0.0370(3) 0.58383(9) 0.1075(12) Uani 1 1 d . . . F11 F 0.54119(6) 0.0601(3) 0.49989(11) 0.1231(14) Uani 1 1 d . . . F12 F 0.56203(6) 0.14457(15) 0.56905(8) 0.0546(6) Uani 1 1 d . . . C53 C 0.66832(16) 0.2004(5) 0.2800(3) 0.103(2) Uani 1 1 d . . . C54 C 0.69314(17) 0.1882(5) 0.2458(3) 0.126(2) Uani 1 1 d . . . H54A H 0.6926 0.1195 0.2336 0.190 Uiso 1 1 calc R . . H54B H 0.7161 0.2036 0.2637 0.190 Uiso 1 1 calc R . . H54C H 0.6875 0.2334 0.2170 0.190 Uiso 1 1 calc R . . N20 N 0.64912(15) 0.2085(6) 0.3059(3) 0.165(3) Uani 1 1 d . . . C55 C 0.71682(9) 0.7635(3) 0.36840(15) 0.0438(9) Uani 1 1 d . . . C56 C 0.72973(11) 0.7268(3) 0.32416(14) 0.0603(11) Uani 1 1 d . . . H56A H 0.7432 0.7789 0.3110 0.090 Uiso 1 1 calc R . . H56B H 0.7105 0.7082 0.2982 0.090 Uiso 1 1 calc R . . H56C H 0.7442 0.6685 0.3334 0.090 Uiso 1 1 calc R . . N21 N 0.70669(8) 0.7916(3) 0.40325(13) 0.0548(8) Uani 1 1 d . . . C57 C 0.54991(10) 0.1895(3) 0.37527(13) 0.0461(9) Uani 1 1 d . . . C58 C 0.58138(10) 0.1342(3) 0.38550(16) 0.0618(11) Uani 1 1 d . . . H58A H 0.5921 0.1454 0.4206 0.093 Uiso 1 1 calc R . . H58B H 0.5969 0.1562 0.3626 0.093 Uiso 1 1 calc R . . H58C H 0.5765 0.0632 0.3803 0.093 Uiso 1 1 calc R . . N22 N 0.52494(9) 0.2326(3) 0.36723(13) 0.0592(9) Uani 1 1 d . . . C59 C 0.73088(13) 0.0381(4) 0.3863(2) 0.1022(19) Uani 1 1 d . . . H59A H 0.7248 -0.0104 0.4107 0.153 Uiso 1 1 calc R . . H59B H 0.7523 0.0178 0.3751 0.153 Uiso 1 1 calc R . . H59C H 0.7126 0.0415 0.3571 0.153 Uiso 1 1 calc R . . C60 C 0.73530(15) 0.1329(5) 0.4096(3) 0.134(3) Uani 1 1 d . . . H60A H 0.7542 0.1294 0.4385 0.161 Uiso 1 1 calc R . . H60B H 0.7419 0.1814 0.3850 0.161 Uiso 1 1 calc R . . C61 C 0.70495(18) 0.2662(4) 0.4409(3) 0.132(3) Uani 1 1 d . . . H61A H 0.7092 0.3084 0.4123 0.159 Uiso 1 1 calc R . . H61B H 0.7235 0.2787 0.4696 0.159 Uiso 1 1 calc R . . C62 C 0.67168(17) 0.2936(4) 0.4557(2) 0.109(2) Uani 1 1 d . . . H62A H 0.6530 0.2693 0.4302 0.163 Uiso 1 1 calc R . . H62B H 0.6702 0.3660 0.4583 0.163 Uiso 1 1 calc R . . H62C H 0.6698 0.2636 0.4885 0.163 Uiso 1 1 calc R . . O1 O 0.70552(9) 0.1664(2) 0.42688(14) 0.0910(11) Uani 1 1 d . . . C63 C 0.66495(18) 0.5069(4) 0.21953(17) 0.0769(15) Uani 1 1 d . . . C64 C 0.70066(14) 0.5305(4) 0.21617(16) 0.0822(15) Uani 1 1 d . . . H64A H 0.7081 0.4910 0.1892 0.123 Uiso 1 1 calc R . . H64B H 0.7151 0.5150 0.2484 0.123 Uiso 1 1 calc R . . H64C H 0.7027 0.6014 0.2087 0.123 Uiso 1 1 calc R . . N23 N 0.63713(16) 0.4894(4) 0.22047(17) 0.1100(18) Uani 1 1 d . . . C65 C 0.59244(15) 0.0297(5) 0.2351(2) 0.0942(18) Uani 1 1 d . . . C66 C 0.6085(2) 0.0229(5) 0.1926(2) 0.137(3) Uani 1 1 d . . . H66A H 0.6290 -0.0188 0.2003 0.205 Uiso 1 1 calc R . . H66B H 0.6151 0.0894 0.1828 0.205 Uiso 1 1 calc R . . H66C H 0.5928 -0.0069 0.1647 0.205 Uiso 1 1 calc R . . N24 N 0.58040(17) 0.0332(6) 0.2699(3) 0.178(3) 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 0.01762(19) 0.0305(2) 0.0187(2) -0.00108(15) -0.00053(15) 0.00018(15) Ni2 0.01562(19) 0.0248(2) 0.0179(2) -0.00121(14) 0.00092(15) 0.00026(14) Ni3 0.01552(19) 0.0243(2) 0.0172(2) -0.00097(14) 0.00117(15) -0.00004(14) Ni4 0.01578(19) 0.0231(2) 0.0176(2) -0.00045(14) 0.00216(15) -0.00001(14) Ni5 0.0200(3) 0.0281(3) 0.0207(3) 0.000 0.0022(2) 0.000 Cl1 0.0276(4) 0.0450(5) 0.0284(4) 0.0003(3) -0.0016(3) 0.0013(3) N1 0.0234(12) 0.0299(14) 0.0216(13) -0.0015(11) -0.0012(10) 0.0022(11) N2 0.0183(11) 0.0275(14) 0.0181(12) 0.0003(10) -0.0004(9) 0.0002(10) N3 0.0173(11) 0.0264(13) 0.0184(12) -0.0004(10) 0.0007(9) -0.0018(10) N4 0.0144(11) 0.0250(13) 0.0203(12) -0.0004(10) 0.0035(9) -0.0007(10) N5 0.0175(12) 0.0356(15) 0.0209(13) 0.0008(11) -0.0003(10) 0.0002(10) N6 0.0168(11) 0.0308(14) 0.0180(12) -0.0004(10) 0.0005(9) 0.0025(10) N7 0.0170(11) 0.0286(14) 0.0193(12) -0.0035(10) 0.0005(9) 0.0025(10) N8 0.0221(12) 0.0263(13) 0.0190(12) -0.0013(10) 0.0034(10) 0.0000(10) N9 0.0180(16) 0.031(2) 0.0187(17) 0.000 0.0014(13) 0.000 N10 0.0194(12) 0.0320(14) 0.0209(12) -0.0030(11) 0.0019(9) 0.0016(10) N11 0.0199(12) 0.0268(14) 0.0220(13) -0.0001(10) 0.0028(10) -0.0010(10) N12 0.0189(12) 0.0323(14) 0.0202(12) -0.0009(11) 0.0027(9) -0.0031(10) N13 0.0165(11) 0.0293(14) 0.0186(12) 0.0006(10) 0.0024(9) -0.0017(10) N14 0.0169(11) 0.0279(14) 0.0192(12) -0.0010(10) 0.0023(9) 0.0000(10) N15 0.0215(12) 0.0327(15) 0.0201(13) -0.0008(11) -0.0022(10) 0.0011(11) N16 0.0164(11) 0.0296(14) 0.0180(12) -0.0006(10) 0.0006(9) 0.0003(10) N17 0.0185(11) 0.0297(14) 0.0193(12) -0.0012(10) 0.0017(9) 0.0012(10) N18 0.0206(12) 0.0239(13) 0.0187(12) -0.0019(10) 0.0014(10) 0.0004(10) N19 0.0182(16) 0.0270(19) 0.0188(17) 0.000 0.0012(13) 0.000 C1 0.0246(15) 0.040(2) 0.0285(17) 0.0027(14) -0.0051(13) 0.0026(14) C2 0.0351(18) 0.038(2) 0.0311(18) 0.0093(14) -0.0093(14) 0.0059(15) C3 0.0364(18) 0.0312(18) 0.0325(18) 0.0051(14) 0.0001(14) 0.0009(14) C4 0.0227(14) 0.0302(17) 0.0183(14) 0.0003(12) 0.0027(11) 0.0046(12) C5 0.0249(15) 0.0307(17) 0.0267(16) 0.0023(13) 0.0037(12) 0.0012(13) C6 0.0268(16) 0.0312(18) 0.0315(17) 0.0036(14) 0.0037(13) -0.0012(13) C7 0.0224(14) 0.0313(18) 0.0251(16) -0.0014(13) 0.0014(12) 0.0003(13) C8 0.0210(14) 0.0263(16) 0.0186(14) -0.0011(12) 0.0032(11) -0.0013(12) C9 0.0176(13) 0.0274(16) 0.0178(14) -0.0027(12) 0.0013(11) 0.0004(12) C10 0.0238(14) 0.0319(17) 0.0167(14) 0.0031(12) 0.0015(11) -0.0010(13) C11 0.0207(14) 0.0338(17) 0.0235(15) 0.0024(13) 0.0041(12) -0.0025(12) C12 0.0194(14) 0.0270(16) 0.0209(15) -0.0031(12) 0.0021(11) 0.0012(12) C13 0.0175(14) 0.0333(17) 0.0252(16) 0.0025(13) 0.0012(12) -0.0008(12) C14 0.0201(15) 0.043(2) 0.0240(16) -0.0009(14) 0.0005(12) 0.0015(13) C15 0.0189(15) 0.051(2) 0.0322(18) -0.0019(15) -0.0002(13) 0.0011(14) C16 0.0186(14) 0.051(2) 0.0298(17) -0.0046(15) 0.0046(12) 0.0026(14) C17 0.0175(14) 0.0292(17) 0.0235(15) 0.0004(12) 0.0021(11) 0.0014(12) C18 0.0228(15) 0.0315(18) 0.0261(16) 0.0002(13) 0.0025(12) 0.0040(13) C19 0.0242(15) 0.0413(19) 0.0271(16) -0.0060(14) 0.0067(12) 0.0049(14) C20 0.0224(15) 0.0355(18) 0.0242(15) -0.0074(13) 0.0033(12) 0.0009(13) C21 0.0184(13) 0.0255(16) 0.0220(15) 0.0004(12) 0.0014(11) 0.0011(12) C22 0.0182(13) 0.0306(17) 0.0177(14) 0.0013(12) 0.0029(11) 0.0003(12) C23 0.0203(14) 0.0328(18) 0.0244(15) -0.0002(13) -0.0001(12) 0.0023(13) C24 0.0276(15) 0.0287(17) 0.0276(16) -0.0014(13) 0.0063(13) 0.0047(13) C25 0.0201(13) 0.0282(16) 0.0176(14) 0.0023(12) 0.0023(11) 0.0000(12) C26 0.0238(15) 0.0286(17) 0.0204(15) -0.0023(12) -0.0002(12) -0.0021(12) C27 0.0178(14) 0.0407(19) 0.0245(16) -0.0067(14) 0.0019(12) 0.0008(13) C28 0.0228(15) 0.0351(19) 0.0303(17) -0.0109(14) -0.0003(13) -0.0016(13) C29 0.0219(14) 0.0291(18) 0.0399(19) -0.0052(14) 0.0010(13) -0.0006(13) C30 0.0157(13) 0.0333(18) 0.0256(16) -0.0044(13) 0.0007(12) -0.0012(12) C31 0.0199(14) 0.0307(17) 0.0280(16) -0.0045(13) 0.0019(12) -0.0012(12) C32 0.0259(15) 0.0311(18) 0.0305(17) 0.0006(14) 0.0011(13) -0.0038(13) C33 0.0253(15) 0.0335(18) 0.0226(15) 0.0027(13) 0.0014(12) -0.0002(13) C34 0.0183(14) 0.0313(17) 0.0230(15) -0.0038(13) 0.0031(11) 0.0011(12) C35 0.0179(13) 0.0299(17) 0.0217(15) 0.0005(12) 0.0023(11) 0.0010(12) C36 0.0182(14) 0.0381(19) 0.0265(16) -0.0021(13) 0.0025(12) -0.0060(13) C37 0.0247(15) 0.042(2) 0.0276(16) -0.0023(14) 0.0093(13) -0.0058(14) C38 0.0255(17) 0.037(2) 0.0214(17) -0.0002(13) 0.0056(12) -0.0041(13) C39 0.0171(13) 0.0266(16) 0.0217(15) 0.0008(12) 0.0019(11) 0.0035(12) C40 0.0250(15) 0.0412(19) 0.0224(16) 0.0004(14) -0.0006(12) -0.0015(14) C41 0.0301(16) 0.052(2) 0.0201(15) 0.0006(14) 0.0037(13) 0.0023(15) C42 0.0278(16) 0.046(2) 0.0242(16) -0.0033(14) 0.0105(13) 0.0019(14) C43 0.0223(14) 0.0276(16) 0.0196(14) -0.0035(12) 0.0044(11) -0.0042(12) C44 0.0222(15) 0.0324(18) 0.0225(15) 0.0006(13) 0.0035(12) -0.0006(13) C45 0.0239(15) 0.0342(18) 0.0253(16) -0.0028(13) 0.0067(12) 0.0005(13) C46 0.0210(14) 0.0324(18) 0.0251(16) 0.0017(13) 0.0022(12) 0.0029(12) C47 0.0201(14) 0.0264(16) 0.0202(15) -0.0028(12) 0.0000(11) -0.0025(12) C48 0.0161(13) 0.0299(17) 0.0203(15) -0.0006(12) 0.0021(11) -0.0029(12) C49 0.0312(16) 0.0320(18) 0.0185(15) -0.0042(13) 0.0008(12) 0.0005(13) C50 0.0330(16) 0.0265(17) 0.0298(17) -0.0013(13) 0.0046(13) 0.0029(13) C51 0.0264(15) 0.0326(18) 0.0237(16) 0.0019(13) 0.0018(12) 0.0037(13) C52 0.0165(13) 0.0287(17) 0.0228(15) 0.0012(12) 0.0016(11) -0.0009(12) P1 0.0396(5) 0.0505(6) 0.0406(5) -0.0126(4) 0.0039(4) 0.0049(4) F1 0.0519(16) 0.134(3) 0.121(2) -0.037(2) -0.0266(16) 0.0122(16) F2 0.143(3) 0.0511(16) 0.0781(18) -0.0102(13) 0.0234(17) 0.0159(16) F3 0.111(2) 0.0787(19) 0.0535(15) -0.0087(13) 0.0271(14) -0.0214(15) F4 0.114(2) 0.0588(16) 0.0778(17) -0.0265(14) -0.0026(15) 0.0237(15) F5 0.197(4) 0.104(2) 0.0441(15) -0.0112(15) 0.0378(18) -0.024(2) F6 0.0398(14) 0.180(3) 0.104(2) -0.075(2) 0.0102(14) -0.0019(17) P2 0.0300(4) 0.0322(5) 0.0535(6) -0.0029(4) 0.0055(4) 0.0008(4) F7 0.0661(16) 0.0413(14) 0.165(3) -0.0268(15) 0.0671(17) -0.0073(11) F8 0.120(2) 0.0411(15) 0.204(4) -0.0039(17) 0.123(3) -0.0096(15) F9 0.1043(19) 0.0392(13) 0.0650(15) -0.0015(11) 0.0468(13) -0.0028(12) F10 0.0567(16) 0.208(4) 0.0570(16) 0.0313(19) 0.0072(13) 0.0499(19) F11 0.0552(16) 0.206(4) 0.095(2) -0.085(2) -0.0293(14) 0.0637(19) F12 0.0725(15) 0.0414(12) 0.0543(13) -0.0117(10) 0.0235(11) -0.0051(10) C53 0.071(4) 0.116(5) 0.125(5) -0.020(4) 0.023(4) 0.027(3) C54 0.125(5) 0.135(6) 0.130(5) -0.009(5) 0.053(4) -0.028(5) N20 0.096(4) 0.191(7) 0.214(7) -0.044(6) 0.047(5) 0.055(4) C55 0.0330(19) 0.050(2) 0.046(2) 0.0066(18) 0.0001(17) -0.0017(17) C56 0.063(3) 0.073(3) 0.043(2) -0.004(2) 0.0057(19) -0.007(2) N21 0.0474(19) 0.060(2) 0.057(2) 0.0042(18) 0.0071(16) 0.0044(16) C57 0.046(2) 0.053(2) 0.044(2) 0.0025(18) 0.0203(18) -0.0074(19) C58 0.058(3) 0.067(3) 0.062(3) 0.011(2) 0.014(2) 0.009(2) N22 0.0449(19) 0.068(2) 0.070(2) 0.0024(18) 0.0264(17) -0.0016(18) C59 0.082(4) 0.079(4) 0.157(6) 0.003(4) 0.054(4) 0.019(3) C60 0.087(4) 0.084(5) 0.248(9) -0.019(5) 0.082(5) -0.001(3) C61 0.157(7) 0.061(4) 0.192(7) -0.021(4) 0.068(6) 0.002(4) C62 0.176(6) 0.054(3) 0.120(5) 0.001(3) 0.095(5) 0.009(4) O1 0.101(3) 0.062(2) 0.121(3) 0.008(2) 0.054(2) 0.0092(19) C63 0.113(5) 0.074(4) 0.037(2) -0.013(2) -0.011(3) -0.010(3) C64 0.121(5) 0.068(3) 0.050(3) -0.005(2) -0.011(3) -0.001(3) N23 0.123(4) 0.136(5) 0.066(3) -0.023(3) -0.001(3) -0.022(4) C65 0.095(4) 0.118(5) 0.067(4) -0.032(3) 0.004(3) 0.016(3) C66 0.227(8) 0.116(5) 0.078(4) 0.025(4) 0.057(5) 0.082(5) N24 0.122(5) 0.277(9) 0.136(6) -0.101(6) 0.029(4) -0.027(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 N15 2.078(2) . ? Ni1 N10 2.084(2) . ? Ni1 N5 2.098(2) . ? Ni1 N1 2.105(2) . ? Ni1 Cl1 2.3240(8) . ? Ni1 Ni2 2.3909(4) . ? Ni2 N16 1.924(2) . ? Ni2 N6 1.929(2) . ? Ni2 N2 1.930(2) . ? Ni2 N11 1.935(2) . ? Ni2 Ni3 2.2771(4) . ? Ni3 N7 1.887(2) . ? Ni3 N12 1.891(2) . ? Ni3 N17 1.892(2) . ? Ni3 N3 1.898(2) . ? Ni3 Ni4 2.2490(4) . ? Ni4 N18 1.914(2) . ? Ni4 N4 1.919(2) . ? Ni4 N8 1.921(2) . ? Ni4 N13 1.921(2) . ? Ni4 Ni5 2.2174(3) . ? Ni5 N14 1.895(2) 2_655 ? Ni5 N14 1.895(2) . ? Ni5 N19 1.899(3) . ? Ni5 N9 1.907(3) . ? Ni5 Ni4 2.2174(3) 2_655 ? N1 C1 1.335(4) . ? N1 C4 1.367(3) . ? N2 C8 1.362(3) . ? N2 C4 1.379(3) . ? N3 C8 1.350(3) . ? N3 C9 1.401(3) . ? N4 C9 1.363(3) . ? N4 C12 1.374(3) . ? N5 C14 1.330(3) . ? N5 C17 1.358(3) . ? N6 C21 1.366(3) . ? N6 C17 1.373(3) . ? N7 C21 1.356(3) . ? N7 C22 1.405(3) . ? N8 C25 1.370(3) . ? N8 C22 1.371(3) . ? N9 C25 1.385(3) 2_655 ? N9 C25 1.385(3) . ? N10 C27 1.346(4) . ? N10 C30 1.357(4) . ? N11 C34 1.355(3) . ? N11 C30 1.373(3) . ? N12 C34 1.350(4) . ? N12 C35 1.396(3) . ? N13 C35 1.362(3) . ? N13 C39 1.370(3) . ? N14 C39 1.375(3) . ? N14 C12 1.378(3) 2_655 ? N15 C40 1.341(4) . ? N15 C43 1.364(3) . ? N16 C47 1.356(3) . ? N16 C43 1.380(3) . ? N17 C47 1.354(3) . ? N17 C48 1.388(3) . ? N18 C48 1.368(3) . ? N18 C52 1.377(3) . ? N19 C52 1.366(3) . ? N19 C52 1.366(3) 2_655 ? C1 C2 1.391(4) . ? C2 C3 1.377(4) . ? C3 C5 1.402(4) . ? C4 C5 1.399(4) . ? C5 C6 1.427(4) . ? C6 C7 1.352(4) . ? C7 C8 1.429(4) . ? C9 C10 1.381(4) . ? C10 C11 1.388(4) . ? C11 C13 1.374(4) . ? C12 N14 1.378(3) 2_655 ? C12 C13 1.394(4) . ? C14 C15 1.383(4) . ? C15 C16 1.368(4) . ? C16 C18 1.404(4) . ? C17 C18 1.411(4) . ? C18 C19 1.420(4) . ? C19 C20 1.356(4) . ? C20 C21 1.424(4) . ? C22 C23 1.376(4) . ? C23 C24 1.389(4) . ? C24 C26 1.373(4) . ? C25 C26 1.392(4) . ? C27 C28 1.375(4) . ? C28 C29 1.367(4) . ? C29 C31 1.407(4) . ? C30 C31 1.407(4) . ? C31 C32 1.422(4) . ? C32 C33 1.352(4) . ? C33 C34 1.430(4) . ? C35 C36 1.385(4) . ? C36 C37 1.382(4) . ? C37 C38 1.384(4) . ? C38 C39 1.389(4) . ? C40 C41 1.377(4) . ? C41 C42 1.363(4) . ? C42 C44 1.399(4) . ? C43 C44 1.400(4) . ? C44 C45 1.427(4) . ? C45 C46 1.341(4) . ? C46 C47 1.429(4) . ? C48 C49 1.374(4) . ? C49 C50 1.396(4) . ? C50 C51 1.371(4) . ? C51 C52 1.396(4) . ? P1 F5 1.559(3) . ? P1 F6 1.560(2) . ? P1 F1 1.569(3) . ? P1 F4 1.578(3) . ? P1 F3 1.579(3) . ? P1 F2 1.582(3) . ? P2 F11 1.560(2) . ? P2 F8 1.561(3) . ? P2 F10 1.565(2) . ? P2 F7 1.580(2) . ? P2 F9 1.581(2) . ? P2 F12 1.602(2) . ? C53 N20 1.112(8) . ? C53 C54 1.452(8) . ? C55 N21 1.137(4) . ? C55 C56 1.449(5) . ? C57 N22 1.136(5) . ? C57 C58 1.440(6) . ? C59 C60 1.419(7) . ? C60 O1 1.406(6) . ? C61 O1 1.395(6) . ? C61 C62 1.479(8) . ? C63 N23 1.129(7) . ? C63 C64 1.464(8) . ? C65 N24 1.112(7) . ? C65 C66 1.391(8) . ? 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 Ni1 N10 88.70(9) . . ? N15 Ni1 N5 165.56(9) . . ? N10 Ni1 N5 91.02(9) . . ? N15 Ni1 N1 88.02(9) . . ? N10 Ni1 N1 165.54(9) . . ? N5 Ni1 N1 88.67(9) . . ? N15 Ni1 Cl1 96.87(6) . . ? N10 Ni1 Cl1 96.96(6) . . ? N5 Ni1 Cl1 97.49(6) . . ? N1 Ni1 Cl1 97.42(6) . . ? N15 Ni1 Ni2 83.61(6) . . ? N10 Ni1 Ni2 83.07(6) . . ? N5 Ni1 Ni2 82.03(6) . . ? N1 Ni1 Ni2 82.57(6) . . ? Cl1 Ni1 Ni2 179.52(3) . . ? N16 Ni2 N6 174.36(9) . . ? N16 Ni2 N2 89.27(10) . . ? N6 Ni2 N2 89.38(10) . . ? N16 Ni2 N11 90.67(10) . . ? N6 Ni2 N11 90.17(10) . . ? N2 Ni2 N11 174.64(9) . . ? N16 Ni2 Ni3 87.71(6) . . ? N6 Ni2 Ni3 86.75(6) . . ? N2 Ni2 Ni3 87.40(6) . . ? N11 Ni2 Ni3 87.24(7) . . ? N16 Ni2 Ni1 91.87(6) . . ? N6 Ni2 Ni1 93.68(6) . . ? N2 Ni2 Ni1 93.27(6) . . ? N11 Ni2 Ni1 92.08(7) . . ? Ni3 Ni2 Ni1 179.20(2) . . ? N7 Ni3 N12 89.40(10) . . ? N7 Ni3 N17 178.99(10) . . ? N12 Ni3 N17 90.64(10) . . ? N7 Ni3 N3 89.73(10) . . ? N12 Ni3 N3 178.82(10) . . ? N17 Ni3 N3 90.22(10) . . ? N7 Ni3 Ni4 89.93(6) . . ? N12 Ni3 Ni4 89.27(7) . . ? N17 Ni3 Ni4 89.06(7) . . ? N3 Ni3 Ni4 89.94(6) . . ? N7 Ni3 Ni2 91.41(6) . . ? N12 Ni3 Ni2 90.17(7) . . ? N17 Ni3 Ni2 89.60(7) . . ? N3 Ni3 Ni2 90.64(6) . . ? Ni4 Ni3 Ni2 178.54(2) . . ? N18 Ni4 N4 90.60(10) . . ? N18 Ni4 N8 179.96(11) . . ? N4 Ni4 N8 89.43(10) . . ? N18 Ni4 N13 90.49(10) . . ? N4 Ni4 N13 178.92(10) . . ? N8 Ni4 N13 89.48(10) . . ? N18 Ni4 Ni5 89.72(7) . . ? N4 Ni4 Ni5 90.00(6) . . ? N8 Ni4 Ni5 90.25(7) . . ? N13 Ni4 Ni5 89.96(6) . . ? N18 Ni4 Ni3 90.17(6) . . ? N4 Ni4 Ni3 89.73(6) . . ? N8 Ni4 Ni3 89.85(6) . . ? N13 Ni4 Ni3 90.31(6) . . ? Ni5 Ni4 Ni3 179.706(19) . . ? N14 Ni5 N14 179.91(16) 2_655 . ? N14 Ni5 N19 90.05(7) 2_655 . ? N14 Ni5 N19 90.05(7) . . ? N14 Ni5 N9 89.95(7) 2_655 . ? N14 Ni5 N9 89.95(7) . . ? N19 Ni5 N9 180.000(2) . . ? N14 Ni5 Ni4 90.08(7) 2_655 2_655 ? N14 Ni5 Ni4 89.92(7) . 2_655 ? N19 Ni5 Ni4 90.223(16) . 2_655 ? N9 Ni5 Ni4 89.777(16) . 2_655 ? N14 Ni5 Ni4 89.92(6) 2_655 . ? N14 Ni5 Ni4 90.08(7) . . ? N19 Ni5 Ni4 90.223(16) . . ? N9 Ni5 Ni4 89.777(16) . . ? Ni4 Ni5 Ni4 179.55(3) 2_655 . ? C1 N1 C4 117.5(3) . . ? C1 N1 Ni1 119.35(19) . . ? C4 N1 Ni1 122.13(18) . . ? C8 N2 C4 119.9(2) . . ? C8 N2 Ni2 120.10(18) . . ? C4 N2 Ni2 119.63(18) . . ? C8 N3 C9 124.6(2) . . ? C8 N3 Ni3 115.90(17) . . ? C9 N3 Ni3 119.26(18) . . ? C9 N4 C12 121.0(2) . . ? C9 N4 Ni4 120.09(17) . . ? C12 N4 Ni4 118.87(18) . . ? C14 N5 C17 117.5(2) . . ? C14 N5 Ni1 119.21(19) . . ? C17 N5 Ni1 122.40(17) . . ? C21 N6 C17 119.9(2) . . ? C21 N6 Ni2 120.97(17) . . ? C17 N6 Ni2 118.77(18) . . ? C21 N7 C22 124.3(2) . . ? C21 N7 Ni3 116.23(18) . . ? C22 N7 Ni3 119.32(17) . . ? C25 N8 C22 120.9(2) . . ? C25 N8 Ni4 119.29(18) . . ? C22 N8 Ni4 119.84(18) . . ? C25 N9 C25 124.1(3) 2_655 . ? C25 N9 Ni5 117.97(17) 2_655 . ? C25 N9 Ni5 117.97(17) . . ? C27 N10 C30 117.1(3) . . ? C27 N10 Ni1 121.24(19) . . ? C30 N10 Ni1 121.32(19) . . ? C34 N11 C30 120.2(2) . . ? C34 N11 Ni2 120.20(19) . . ? C30 N11 Ni2 119.01(18) . . ? C34 N12 C35 123.8(2) . . ? C34 N12 Ni3 116.77(18) . . ? C35 N12 Ni3 119.16(18) . . ? C35 N13 C39 121.6(2) . . ? C35 N13 Ni4 119.27(17) . . ? C39 N13 Ni4 119.10(17) . . ? C39 N14 C12 123.8(2) . 2_655 ? C39 N14 Ni5 118.55(17) . . ? C12 N14 Ni5 117.54(17) 2_655 . ? C40 N15 C43 117.4(2) . . ? C40 N15 Ni1 120.42(18) . . ? C43 N15 Ni1 121.84(18) . . ? C47 N16 C43 119.2(2) . . ? C47 N16 Ni2 120.10(18) . . ? C43 N16 Ni2 120.06(18) . . ? C47 N17 C48 123.2(2) . . ? C47 N17 Ni3 116.39(18) . . ? C48 N17 Ni3 120.03(18) . . ? C48 N18 C52 121.1(2) . . ? C48 N18 Ni4 119.60(18) . . ? C52 N18 Ni4 119.26(18) . . ? C52 N19 C52 124.6(3) . 2_655 ? C52 N19 Ni5 117.72(17) . . ? C52 N19 Ni5 117.72(17) 2_655 . ? N1 C1 C2 124.1(3) . . ? C3 C2 C1 118.7(3) . . ? C2 C3 C5 118.8(3) . . ? N1 C4 N2 116.0(3) . . ? N1 C4 C5 121.8(2) . . ? N2 C4 C5 122.2(2) . . ? C4 C5 C3 119.1(3) . . ? C4 C5 C6 117.4(3) . . ? C3 C5 C6 123.5(3) . . ? C7 C6 C5 120.1(3) . . ? C6 C7 C8 121.0(3) . . ? N3 C8 N2 116.9(2) . . ? N3 C8 C7 123.6(2) . . ? N2 C8 C7 119.3(2) . . ? N4 C9 C10 120.1(2) . . ? N4 C9 N3 114.7(2) . . ? C10 C9 N3 125.1(2) . . ? C9 C10 C11 119.1(3) . . ? C13 C11 C10 121.0(3) . . ? N4 C12 N14 115.0(2) . 2_655 ? N4 C12 C13 119.8(2) . . ? N14 C12 C13 125.1(2) 2_655 . ? C11 C13 C12 118.9(2) . . ? N5 C14 C15 124.1(3) . . ? C16 C15 C14 119.2(3) . . ? C15 C16 C18 118.7(3) . . ? N5 C17 N6 116.6(2) . . ? N5 C17 C18 121.9(2) . . ? N6 C17 C18 121.5(2) . . ? C16 C18 C17 118.4(3) . . ? C16 C18 C19 123.6(3) . . ? C17 C18 C19 118.0(2) . . ? C20 C19 C18 120.1(3) . . ? C19 C20 C21 120.5(3) . . ? N7 C21 N6 116.3(2) . . ? N7 C21 C20 123.5(2) . . ? N6 C21 C20 120.0(2) . . ? N8 C22 C23 120.1(2) . . ? N8 C22 N7 114.4(2) . . ? C23 C22 N7 125.4(2) . . ? C22 C23 C24 119.0(3) . . ? C26 C24 C23 121.1(3) . . ? N8 C25 N9 114.7(3) . . ? N8 C25 C26 119.8(2) . . ? N9 C25 C26 125.3(3) . . ? C24 C26 C25 118.9(3) . . ? N10 C27 C28 124.2(3) . . ? C29 C28 C27 118.8(3) . . ? C28 C29 C31 119.3(3) . . ? N10 C30 N11 116.8(3) . . ? N10 C30 C31 122.0(3) . . ? N11 C30 C31 121.2(3) . . ? C30 C31 C29 118.1(3) . . ? C30 C31 C32 118.2(3) . . ? C29 C31 C32 123.6(3) . . ? C33 C32 C31 119.9(3) . . ? C32 C33 C34 120.4(3) . . ? N12 C34 N11 116.3(3) . . ? N12 C34 C33 123.4(3) . . ? N11 C34 C33 120.0(2) . . ? N13 C35 C36 120.0(2) . . ? N13 C35 N12 114.9(2) . . ? C36 C35 N12 124.9(2) . . ? C37 C36 C35 119.0(3) . . ? C36 C37 C38 120.5(3) . . ? C37 C38 C39 119.6(3) . . ? N13 C39 N14 115.0(2) . . ? N13 C39 C38 118.9(2) . . ? N14 C39 C38 125.9(2) . . ? N15 C40 C41 123.7(3) . . ? C42 C41 C40 119.1(3) . . ? C41 C42 C44 119.6(3) . . ? N15 C43 N16 115.9(2) . . ? N15 C43 C44 122.1(2) . . ? N16 C43 C44 122.1(2) . . ? C42 C44 C43 118.1(3) . . ? C42 C44 C45 124.4(3) . . ? C43 C44 C45 117.5(2) . . ? C46 C45 C44 120.4(3) . . ? C45 C46 C47 120.4(3) . . ? N17 C47 N16 115.9(2) . . ? N17 C47 C46 123.5(2) . . ? N16 C47 C46 120.4(2) . . ? N18 C48 C49 120.7(2) . . ? N18 C48 N17 114.3(2) . . ? C49 C48 N17 124.8(2) . . ? C48 C49 C50 118.4(3) . . ? C51 C50 C49 121.1(3) . . ? C50 C51 C52 119.6(3) . . ? N19 C52 N18 115.1(2) . . ? N19 C52 C51 125.9(3) . . ? N18 C52 C51 118.9(2) . . ? F5 P1 F6 91.48(19) . . ? F5 P1 F1 90.88(19) . . ? F6 P1 F1 177.1(2) . . ? F5 P1 F4 89.31(16) . . ? F6 P1 F4 89.77(16) . . ? F1 P1 F4 88.60(16) . . ? F5 P1 F3 179.7(2) . . ? F6 P1 F3 88.29(16) . . ? F1 P1 F3 89.36(17) . . ? F4 P1 F3 90.95(15) . . ? F5 P1 F2 92.13(17) . . ? F6 P1 F2 90.89(17) . . ? F1 P1 F2 90.68(17) . . ? F4 P1 F2 178.40(18) . . ? F3 P1 F2 87.61(15) . . ? F11 P2 F8 91.6(2) . . ? F11 P2 F10 176.9(2) . . ? F8 P2 F10 90.96(19) . . ? F11 P2 F7 90.41(16) . . ? F8 P2 F7 91.93(14) . . ? F10 P2 F7 91.27(17) . . ? F11 P2 F9 89.45(18) . . ? F8 P2 F9 178.76(19) . . ? F10 P2 F9 87.95(15) . . ? F7 P2 F9 88.70(12) . . ? F11 P2 F12 89.11(13) . . ? F8 P2 F12 88.47(13) . . ? F10 P2 F12 89.20(16) . . ? F7 P2 F12 179.38(17) . . ? F9 P2 F12 90.91(12) . . ? N20 C53 C54 179.1(9) . . ? N21 C55 C56 179.5(5) . . ? N22 C57 C58 179.5(4) . . ? O1 C60 C59 112.4(5) . . ? O1 C61 C62 111.4(5) . . ? C61 O1 C60 116.6(5) . . ? N23 C63 C64 177.7(6) . . ? N24 C65 C66 177.7(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.775 _refine_diff_density_min -1.216 _refine_diff_density_rms 0.159