# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_4 _database_code_depnum_ccdc_archive 'CCDC 896901' #TrackingRef 'CIF(1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H62 N3 Ni' _chemical_formula_weight 775.75 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2859(11) _cell_length_b 20.3988(17) _cell_length_c 17.3454(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.232(2) _cell_angle_gamma 90.00 _cell_volume 4290.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description red _exptl_crystal_colour block _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 0.490 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27399 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0991 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.30 _reflns_number_total 10072 _reflns_number_gt 6535 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10072 _refine_ls_number_parameters 503 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _refine_ls_shift/su_max 0.042 _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 -0.06018(2) 0.287195(14) 0.816795(17) 0.01811(9) Uani 1 1 d . . . N1 N -0.06263(15) 0.20459(9) 0.96267(10) 0.0182(4) Uani 1 1 d . . . C3 C 0.10199(19) 0.21750(11) 1.03148(13) 0.0193(5) Uani 1 1 d . . . H3A H 0.1652 0.2150 1.0708 0.023 Uiso 1 1 calc R . . C21 C 0.18376(18) 0.28917(12) 0.94225(13) 0.0198(5) Uani 1 1 d . . . C51 C -0.15000(19) 0.31804(12) 0.70698(13) 0.0201(5) Uani 1 1 d . . . N3 N 0.04556(18) 0.35018(10) 0.78995(12) 0.0213(5) Uani 1 1 d . . . C316 C 0.08853(19) 0.43149(11) 0.69221(13) 0.0184(5) Uani 1 1 d . . . N2 N 0.09095(15) 0.25348(9) 0.96255(10) 0.0165(4) Uani 1 1 d . . . C52 C -0.1460(2) 0.25181(12) 0.68263(14) 0.0265(6) Uani 1 1 d . . . C312 C -0.08113(19) 0.36837(11) 0.67521(13) 0.0176(5) Uani 1 1 d . . . C1 C -0.01087(19) 0.24618(10) 0.91783(12) 0.0160(5) Uani 1 1 d . . . C315 C 0.0521(2) 0.45950(11) 0.61971(13) 0.0225(6) Uani 1 1 d . . . H31A H 0.0976 0.4911 0.6002 0.027 Uiso 1 1 calc R . . C313 C -0.1151(2) 0.39798(11) 0.60362(13) 0.0209(5) Uani 1 1 d . . . H31B H -0.1848 0.3872 0.5741 0.025 Uiso 1 1 calc R . . C2 C 0.0057(2) 0.18732(11) 1.03100(13) 0.0210(5) Uani 1 1 d . . . H2A H -0.0127 0.1590 1.0705 0.025 Uiso 1 1 calc R . . C311 C 0.02137(19) 0.38336(11) 0.72142(13) 0.0175(5) Uani 1 1 d . . . C25 C 0.3439(2) 0.29236(15) 0.88185(15) 0.0361(7) Uani 1 1 d . . . H25A H 0.3918 0.2731 0.8503 0.043 Uiso 1 1 calc R . . C16 C -0.2596(2) 0.21986(12) 0.96426(13) 0.0262(6) Uani 1 1 d . . . C62 C 0.2959(2) 0.42785(12) 0.72567(14) 0.0234(6) Uani 1 1 d . . . C66 C 0.1943(2) 0.50311(11) 0.79473(14) 0.0235(6) Uani 1 1 d . . . C61 C 0.1950(2) 0.45352(11) 0.73890(13) 0.0194(5) Uani 1 1 d . . . C53 C -0.2278(2) 0.20884(13) 0.69783(15) 0.0348(7) Uani 1 1 d . . . H53A H -0.2247 0.1645 0.6814 0.042 Uiso 1 1 calc R . . C26 C 0.2498(2) 0.25779(13) 0.89565(14) 0.0283(6) Uani 1 1 d . . . C161 C -0.2383(2) 0.29003(12) 0.99162(14) 0.0284(6) Uani 1 1 d . . . H16A H -0.1810 0.3086 0.9629 0.034 Uiso 1 1 calc R . . C12 C -0.1886(2) 0.11415(12) 0.92347(14) 0.0278(6) Uani 1 1 d . . . C314 C -0.0475(2) 0.44341(11) 0.57485(13) 0.0239(6) Uani 1 1 d . . . H31C H -0.0695 0.4631 0.5251 0.029 Uiso 1 1 calc R . . C221 C 0.1303(2) 0.38454(12) 1.02404(14) 0.0277(6) Uani 1 1 d . . . H22A H 0.1084 0.3503 1.0598 0.033 Uiso 1 1 calc R . . C11 C -0.1740(2) 0.17993(12) 0.94664(13) 0.0214(5) Uani 1 1 d . . . C163 C -0.1926(3) 0.29289(13) 1.07857(16) 0.0454(8) Uani 1 1 d . . . H16B H -0.1276 0.2645 1.0898 0.068 Uiso 1 1 calc R . . H16C H -0.2490 0.2779 1.1086 0.068 Uiso 1 1 calc R . . H16D H -0.1717 0.3381 1.0933 0.068 Uiso 1 1 calc R . . C63 C 0.3935(2) 0.45250(12) 0.76740(14) 0.0285(6) Uani 1 1 d . . . H63A H 0.4617 0.4356 0.7570 0.034 Uiso 1 1 calc R . . C23 C 0.3001(2) 0.38327(13) 0.95810(15) 0.0328(7) Uani 1 1 d . . . H23A H 0.3179 0.4259 0.9784 0.039 Uiso 1 1 calc R . . C22 C 0.2061(2) 0.35215(12) 0.97429(14) 0.0244(6) Uani 1 1 d . . . C162 C -0.3396(2) 0.33432(14) 0.97526(16) 0.0422(8) Uani 1 1 d . . . H16E H -0.3698 0.3328 0.9195 0.063 Uiso 1 1 calc R . . H16F H -0.3184 0.3794 0.9902 0.063 Uiso 1 1 calc R . . H16G H -0.3955 0.3191 1.0056 0.063 Uiso 1 1 calc R . . C64 C 0.3945(2) 0.50077(12) 0.82349(15) 0.0279(6) Uani 1 1 d . . . C65 C 0.2939(2) 0.52530(12) 0.83596(14) 0.0272(6) Uani 1 1 d . . . H65A H 0.2928 0.5586 0.8741 0.033 Uiso 1 1 calc R . . C222 C 0.0246(2) 0.41038(12) 0.97464(15) 0.0317(6) Uani 1 1 d . . . H22B H -0.0114 0.3749 0.9420 0.048 Uiso 1 1 calc R . . H22C H 0.0429 0.4462 0.9413 0.048 Uiso 1 1 calc R . . H22D H -0.0253 0.4266 1.0091 0.048 Uiso 1 1 calc R . . C55 C -0.3112(2) 0.29053(15) 0.76527(15) 0.0419(8) Uani 1 1 d . . . H55A H -0.3673 0.3036 0.7939 0.050 Uiso 1 1 calc R . . C13 C -0.2940(2) 0.08885(14) 0.91831(16) 0.0386(7) Uani 1 1 d . . . H13A H -0.3077 0.0449 0.9015 0.046 Uiso 1 1 calc R . . C56 C -0.2290(2) 0.33595(13) 0.75456(14) 0.0290(6) Uani 1 1 d . . . C15 C -0.3636(2) 0.19063(14) 0.95882(15) 0.0346(7) Uani 1 1 d . . . H15A H -0.4242 0.2156 0.9703 0.042 Uiso 1 1 calc R . . C24 C 0.3676(2) 0.35336(15) 0.91313(16) 0.0385(7) Uani 1 1 d . . . H24A H 0.4322 0.3754 0.9034 0.046 Uiso 1 1 calc R . . C261 C 0.2218(2) 0.19099(13) 0.85992(16) 0.0344(7) Uani 1 1 d . . . H26A H 0.1550 0.1743 0.8799 0.041 Uiso 1 1 calc R . . C54 C -0.3134(2) 0.22774(15) 0.73581(15) 0.0373(8) Uani 1 1 d . . . C121 C -0.0940(2) 0.07299(12) 0.90293(15) 0.0318(7) Uani 1 1 d . . . H12A H -0.0250 0.0881 0.9368 0.038 Uiso 1 1 calc R . . C661 C 0.0867(2) 0.53315(12) 0.80769(15) 0.0323(7) Uani 1 1 d . . . H66A H 0.1010 0.5672 0.8479 0.048 Uiso 1 1 calc R . . H66B H 0.0395 0.4991 0.8248 0.048 Uiso 1 1 calc R . . H66C H 0.0496 0.5527 0.7588 0.048 Uiso 1 1 calc R . . C521 C -0.0642(2) 0.23088(12) 0.63143(17) 0.0380(7) Uani 1 1 d . . . H52A H -0.0968 0.2365 0.5765 0.057 Uiso 1 1 calc R . . H52B H -0.0451 0.1847 0.6414 0.057 Uiso 1 1 calc R . . H52C H 0.0024 0.2578 0.6432 0.057 Uiso 1 1 calc R . . C621 C 0.2980(2) 0.37289(13) 0.66737(15) 0.0364(7) Uani 1 1 d . . . H62A H 0.2404 0.3409 0.6733 0.055 Uiso 1 1 calc R . . H62B H 0.3702 0.3513 0.6768 0.055 Uiso 1 1 calc R . . H62C H 0.2848 0.3908 0.6143 0.055 Uiso 1 1 calc R . . C14 C -0.3788(2) 0.12560(15) 0.93687(16) 0.0410(8) Uani 1 1 d . . . H14A H -0.4495 0.1063 0.9347 0.049 Uiso 1 1 calc R . . C122 C -0.0794(3) 0.08438(13) 0.81799(16) 0.0435(8) Uani 1 1 d . . . H12B H -0.0706 0.1314 0.8091 0.065 Uiso 1 1 calc R . . H12C H -0.1446 0.0682 0.7831 0.065 Uiso 1 1 calc R . . H12D H -0.0139 0.0609 0.8074 0.065 Uiso 1 1 calc R . . C223 C 0.1849(2) 0.44084(13) 1.07527(16) 0.0426(8) Uani 1 1 d . . . H22E H 0.2529 0.4250 1.1072 0.064 Uiso 1 1 calc R . . H22F H 0.1342 0.4566 1.1094 0.064 Uiso 1 1 calc R . . H22G H 0.2023 0.4768 1.0418 0.064 Uiso 1 1 calc R . . C561 C -0.2347(2) 0.40571(13) 0.78310(15) 0.0365(7) Uani 1 1 d . . . H56A H -0.3039 0.4259 0.7582 0.055 Uiso 1 1 calc R . . H56B H -0.1723 0.4307 0.7697 0.055 Uiso 1 1 calc R . . H56C H -0.2316 0.4057 0.8399 0.055 Uiso 1 1 calc R . . C641 C 0.5006(2) 0.52424(14) 0.87107(17) 0.0427(8) Uani 1 1 d . . . H64A H 0.4984 0.5720 0.8764 0.064 Uiso 1 1 calc R . . H64B H 0.5626 0.5120 0.8449 0.064 Uiso 1 1 calc R . . H64C H 0.5099 0.5040 0.9230 0.064 Uiso 1 1 calc R . . C123 C -0.1069(3) -0.00032(13) 0.91806(18) 0.0495(9) Uani 1 1 d . . . H12E H -0.1158 -0.0071 0.9726 0.074 Uiso 1 1 calc R . . H12F H -0.0411 -0.0237 0.9076 0.074 Uiso 1 1 calc R . . H12G H -0.1720 -0.0171 0.8836 0.074 Uiso 1 1 calc R . . C541 C -0.4078(3) 0.18152(16) 0.74255(17) 0.0593(10) Uani 1 1 d . . . H54A H -0.3940 0.1391 0.7194 0.089 Uiso 1 1 calc R . . H54B H -0.4767 0.2001 0.7149 0.089 Uiso 1 1 calc R . . H54C H -0.4138 0.1754 0.7977 0.089 Uiso 1 1 calc R . . C262 C 0.3150(3) 0.14114(15) 0.88197(18) 0.0625(10) Uani 1 1 d . . . H26B H 0.2934 0.0990 0.8570 0.094 Uiso 1 1 calc R . . H26C H 0.3292 0.1355 0.9388 0.094 Uiso 1 1 calc R . . H26D H 0.3820 0.1570 0.8641 0.094 Uiso 1 1 calc R . . C263 C 0.1947(3) 0.19503(15) 0.77213(18) 0.0689(12) Uani 1 1 d . . . H26E H 0.1327 0.2251 0.7574 0.103 Uiso 1 1 calc R . . H26F H 0.1748 0.1514 0.7508 0.103 Uiso 1 1 calc R . . H26G H 0.2592 0.2112 0.7512 0.103 Uiso 1 1 calc R . . H H 0.104(2) 0.3614(11) 0.8152(14) 0.026(8) Uiso 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 0.01713(17) 0.02094(17) 0.01580(15) 0.00436(13) 0.00127(12) -0.00139(14) N1 0.0186(11) 0.0196(11) 0.0160(10) 0.0025(8) 0.0013(8) -0.0028(8) C3 0.0208(13) 0.0206(13) 0.0150(11) 0.0009(10) -0.0018(10) 0.0003(11) C21 0.0135(12) 0.0281(14) 0.0166(12) 0.0098(11) -0.0009(10) 0.0002(11) C51 0.0185(13) 0.0258(14) 0.0140(12) 0.0053(10) -0.0036(10) -0.0028(10) N3 0.0177(12) 0.0260(12) 0.0186(11) 0.0052(9) -0.0017(10) -0.0039(9) C316 0.0222(14) 0.0158(12) 0.0182(12) 0.0004(10) 0.0067(11) 0.0022(10) N2 0.0170(11) 0.0170(11) 0.0156(10) 0.0024(8) 0.0032(8) 0.0003(8) C52 0.0230(15) 0.0274(15) 0.0257(14) 0.0053(11) -0.0066(11) -0.0029(11) C312 0.0202(13) 0.0166(13) 0.0160(12) -0.0014(10) 0.0028(10) 0.0022(10) C1 0.0168(13) 0.0151(12) 0.0168(11) -0.0024(10) 0.0044(10) -0.0007(10) C315 0.0283(15) 0.0192(13) 0.0212(13) 0.0030(10) 0.0077(11) -0.0030(11) C313 0.0214(14) 0.0229(14) 0.0172(12) 0.0016(10) -0.0005(11) 0.0016(10) C2 0.0254(15) 0.0219(13) 0.0149(12) 0.0046(10) 0.0009(11) -0.0016(11) C311 0.0207(13) 0.0155(12) 0.0167(12) -0.0002(10) 0.0044(10) 0.0023(10) C25 0.0195(15) 0.062(2) 0.0291(15) 0.0189(15) 0.0099(12) 0.0147(14) C16 0.0245(14) 0.0360(16) 0.0179(12) 0.0066(11) 0.0025(11) -0.0042(12) C62 0.0238(15) 0.0270(15) 0.0208(13) 0.0024(11) 0.0075(11) -0.0009(11) C66 0.0279(15) 0.0211(14) 0.0226(13) 0.0034(11) 0.0073(12) -0.0022(11) C61 0.0237(14) 0.0184(13) 0.0167(12) 0.0052(10) 0.0054(11) -0.0027(10) C53 0.0357(17) 0.0279(15) 0.0340(15) 0.0082(13) -0.0147(13) -0.0099(13) C26 0.0207(14) 0.0392(17) 0.0245(14) 0.0120(12) 0.0023(12) 0.0088(12) C161 0.0239(14) 0.0363(16) 0.0265(14) 0.0042(12) 0.0082(12) 0.0056(12) C12 0.0323(16) 0.0292(15) 0.0197(13) 0.0053(11) -0.0029(12) -0.0112(12) C314 0.0327(16) 0.0246(14) 0.0141(12) 0.0043(10) 0.0023(11) 0.0002(11) C221 0.0333(16) 0.0222(14) 0.0254(14) -0.0011(11) -0.0021(12) -0.0068(12) C11 0.0192(14) 0.0290(15) 0.0151(12) 0.0073(10) -0.0003(10) -0.0074(11) C163 0.050(2) 0.0370(18) 0.0430(18) -0.0095(14) -0.0110(15) 0.0107(15) C63 0.0217(15) 0.0340(16) 0.0311(15) 0.0068(12) 0.0083(12) -0.0011(12) C23 0.0239(16) 0.0353(17) 0.0355(16) 0.0127(13) -0.0062(13) -0.0080(12) C22 0.0198(14) 0.0276(15) 0.0224(13) 0.0094(11) -0.0075(11) -0.0049(11) C162 0.0394(19) 0.060(2) 0.0280(15) 0.0023(14) 0.0082(14) 0.0174(15) C64 0.0272(15) 0.0282(15) 0.0270(14) 0.0069(12) 0.0002(12) -0.0086(12) C65 0.0361(17) 0.0204(14) 0.0247(14) -0.0020(11) 0.0039(12) -0.0067(12) C222 0.0353(17) 0.0265(15) 0.0321(15) -0.0029(12) 0.0014(13) 0.0017(12) C55 0.0325(17) 0.074(2) 0.0203(14) 0.0005(15) 0.0064(13) -0.0172(16) C13 0.0371(18) 0.0393(18) 0.0364(17) 0.0069(14) -0.0032(14) -0.0157(14) C56 0.0280(16) 0.0412(17) 0.0183(13) 0.0024(12) 0.0049(12) -0.0067(12) C15 0.0216(15) 0.056(2) 0.0265(15) 0.0087(13) 0.0055(12) -0.0010(13) C24 0.0231(16) 0.048(2) 0.0411(18) 0.0232(15) -0.0034(14) -0.0087(14) C261 0.0318(17) 0.0412(18) 0.0335(16) 0.0012(13) 0.0153(13) 0.0130(13) C54 0.0368(18) 0.054(2) 0.0169(13) 0.0106(13) -0.0086(13) -0.0251(14) C121 0.0385(17) 0.0215(15) 0.0324(15) -0.0008(12) -0.0040(13) -0.0027(12) C661 0.0359(17) 0.0305(16) 0.0315(15) -0.0093(12) 0.0085(13) 0.0017(12) C521 0.0357(18) 0.0255(16) 0.0508(19) -0.0093(13) 0.0004(15) 0.0014(12) C621 0.0302(17) 0.0439(18) 0.0373(17) -0.0074(14) 0.0119(14) 0.0072(13) C14 0.0293(17) 0.057(2) 0.0347(17) 0.0105(15) -0.0006(14) -0.0246(15) C122 0.057(2) 0.0359(17) 0.0372(17) -0.0024(14) 0.0059(16) 0.0098(15) C223 0.048(2) 0.0329(17) 0.0419(18) -0.0070(14) -0.0082(15) -0.0067(14) C561 0.0332(17) 0.0486(19) 0.0313(16) -0.0044(13) 0.0160(14) 0.0047(14) C641 0.0363(18) 0.0438(19) 0.0446(18) 0.0049(15) -0.0043(15) -0.0158(14) C123 0.061(2) 0.0285(17) 0.053(2) 0.0030(14) -0.0118(17) -0.0067(15) C541 0.055(2) 0.089(3) 0.0304(17) 0.0137(17) -0.0039(16) -0.0480(19) C262 0.086(3) 0.061(2) 0.0387(19) 0.0092(16) 0.0039(19) 0.035(2) C263 0.104(3) 0.056(2) 0.0375(19) -0.0077(16) -0.017(2) 0.035(2) _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 N3 1.936(2) . ? Ni1 C1 1.949(2) . ? Ni1 C51 2.137(2) . ? Ni1 C56 2.396(3) . ? Ni1 C52 2.502(2) . ? N1 C1 1.374(3) . ? N1 C2 1.384(3) . ? N1 C11 1.443(3) . ? C3 C2 1.332(3) . ? C3 N2 1.391(3) . ? C21 C26 1.390(3) . ? C21 C22 1.409(3) . ? C21 N2 1.443(3) . ? C51 C52 1.419(3) . ? C51 C56 1.420(3) . ? C51 C312 1.491(3) . ? N3 C311 1.359(3) . ? C316 C315 1.389(3) . ? C316 C311 1.427(3) . ? C316 C61 1.493(3) . ? N2 C1 1.370(3) . ? C52 C53 1.390(3) . ? C52 C521 1.506(4) . ? C312 C313 1.384(3) . ? C312 C311 1.414(3) . ? C315 C314 1.380(3) . ? C313 C314 1.390(3) . ? C25 C24 1.370(4) . ? C25 C26 1.407(4) . ? C16 C15 1.399(3) . ? C16 C11 1.401(3) . ? C16 C161 1.517(3) . ? C62 C63 1.391(3) . ? C62 C61 1.398(3) . ? C62 C621 1.513(3) . ? C66 C65 1.391(3) . ? C66 C61 1.401(3) . ? C66 C661 1.506(3) . ? C53 C54 1.383(4) . ? C26 C261 1.514(4) . ? C161 C163 1.524(3) . ? C161 C162 1.527(3) . ? C12 C13 1.384(4) . ? C12 C11 1.404(3) . ? C12 C121 1.521(4) . ? C221 C22 1.519(3) . ? C221 C222 1.530(3) . ? C221 C223 1.539(3) . ? C63 C64 1.383(3) . ? C23 C24 1.370(4) . ? C23 C22 1.385(3) . ? C64 C65 1.382(3) . ? C64 C641 1.505(3) . ? C55 C54 1.378(4) . ? C55 C56 1.404(3) . ? C13 C14 1.363(4) . ? C56 C561 1.512(3) . ? C15 C14 1.384(4) . ? C261 C263 1.508(4) . ? C261 C262 1.534(4) . ? C54 C541 1.513(4) . ? C121 C122 1.530(3) . ? C121 C123 1.531(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni1 C1 112.17(9) . . ? N3 Ni1 C51 81.99(9) . . ? C1 Ni1 C51 165.81(9) . . ? N3 Ni1 C56 100.49(9) . . ? C1 Ni1 C56 134.85(9) . . ? C51 Ni1 C56 35.93(8) . . ? N3 Ni1 C52 99.59(9) . . ? C1 Ni1 C52 137.42(9) . . ? C51 Ni1 C52 34.48(8) . . ? C56 Ni1 C52 59.69(8) . . ? C1 N1 C2 111.69(19) . . ? C1 N1 C11 128.10(18) . . ? C2 N1 C11 120.20(18) . . ? C2 C3 N2 105.9(2) . . ? C26 C21 C22 123.7(2) . . ? C26 C21 N2 117.9(2) . . ? C22 C21 N2 118.4(2) . . ? C52 C51 C56 118.5(2) . . ? C52 C51 C312 119.8(2) . . ? C56 C51 C312 121.3(2) . . ? C52 C51 Ni1 86.99(14) . . ? C56 C51 Ni1 82.02(14) . . ? C312 C51 Ni1 106.84(15) . . ? C311 N3 Ni1 118.68(17) . . ? C315 C316 C311 118.9(2) . . ? C315 C316 C61 119.6(2) . . ? C311 C316 C61 121.4(2) . . ? C1 N2 C3 112.56(19) . . ? C1 N2 C21 127.01(18) . . ? C3 N2 C21 120.27(19) . . ? C53 C52 C51 118.9(2) . . ? C53 C52 C521 120.3(2) . . ? C51 C52 C521 120.2(2) . . ? C53 C52 Ni1 102.42(17) . . ? C51 C52 Ni1 58.53(12) . . ? C521 C52 Ni1 114.12(17) . . ? C313 C312 C311 121.9(2) . . ? C313 C312 C51 121.6(2) . . ? C311 C312 C51 116.5(2) . . ? N2 C1 N1 102.12(18) . . ? N2 C1 Ni1 125.90(16) . . ? N1 C1 Ni1 131.98(17) . . ? C314 C315 C316 122.7(2) . . ? C312 C313 C314 120.1(2) . . ? C3 C2 N1 107.7(2) . . ? N3 C311 C312 116.0(2) . . ? N3 C311 C316 126.6(2) . . ? C312 C311 C316 117.4(2) . . ? C24 C25 C26 121.1(2) . . ? C15 C16 C11 116.5(2) . . ? C15 C16 C161 122.2(2) . . ? C11 C16 C161 121.3(2) . . ? C63 C62 C61 119.5(2) . . ? C63 C62 C621 120.7(2) . . ? C61 C62 C621 119.9(2) . . ? C65 C66 C61 119.2(2) . . ? C65 C66 C661 120.8(2) . . ? C61 C66 C661 120.0(2) . . ? C62 C61 C66 119.2(2) . . ? C62 C61 C316 121.4(2) . . ? C66 C61 C316 119.3(2) . . ? C54 C53 C52 122.9(3) . . ? C21 C26 C25 116.1(2) . . ? C21 C26 C261 122.5(2) . . ? C25 C26 C261 121.4(2) . . ? C16 C161 C163 111.3(2) . . ? C16 C161 C162 114.0(2) . . ? C163 C161 C162 108.8(2) . . ? C13 C12 C11 116.7(3) . . ? C13 C12 C121 121.4(2) . . ? C11 C12 C121 121.9(2) . . ? C315 C314 C313 118.9(2) . . ? C22 C221 C222 112.0(2) . . ? C22 C221 C223 113.7(2) . . ? C222 C221 C223 108.6(2) . . ? C16 C11 C12 123.5(2) . . ? C16 C11 N1 118.5(2) . . ? C12 C11 N1 117.5(2) . . ? C64 C63 C62 122.2(2) . . ? C24 C23 C22 120.8(3) . . ? C23 C22 C21 117.0(2) . . ? C23 C22 C221 121.5(2) . . ? C21 C22 C221 121.5(2) . . ? C65 C64 C63 117.4(2) . . ? C65 C64 C641 121.1(2) . . ? C63 C64 C641 121.5(3) . . ? C64 C65 C66 122.5(2) . . ? C54 C55 C56 122.4(3) . . ? C14 C13 C12 121.5(3) . . ? C55 C56 C51 118.7(2) . . ? C55 C56 C561 120.4(2) . . ? C51 C56 C561 120.3(2) . . ? C55 C56 Ni1 104.79(19) . . ? C51 C56 Ni1 62.05(13) . . ? C561 C56 Ni1 108.98(17) . . ? C14 C15 C16 120.6(3) . . ? C25 C24 C23 121.3(3) . . ? C263 C261 C26 111.3(2) . . ? C263 C261 C262 108.8(2) . . ? C26 C261 C262 112.5(2) . . ? C55 C54 C53 117.7(2) . . ? C55 C54 C541 121.4(3) . . ? C53 C54 C541 120.9(3) . . ? C12 C121 C122 110.7(2) . . ? C12 C121 C123 113.3(2) . . ? C122 C121 C123 110.2(2) . . ? C13 C14 C15 121.2(3) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.568 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.064 data_5 _database_code_depnum_ccdc_archive 'CCDC 896902' #TrackingRef 'CIF(1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H78 Cl4 N3 Ni' _chemical_formula_weight 1029.75 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P(2)1/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.2763(15) _cell_length_b 10.7269(7) _cell_length_c 24.4104(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.0530(10) _cell_angle_gamma 90.00 _cell_volume 5529.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2196 _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.1901 _exptl_absorpt_correction_T_max 0.3151 _exptl_absorpt_process_details 'Norton et. al.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker P4' _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 34798 _diffrn_reflns_av_R_equivalents 0.1440 _diffrn_reflns_av_sigmaI/netI 0.1132 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.29 _reflns_number_total 12904 _reflns_number_gt 9466 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0891P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12904 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1733 _refine_ls_wR_factor_gt 0.1623 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.182001(14) 0.86394(3) 0.209215(12) 0.01335(10) Uani 1 1 d . . . N3 N 0.26339(10) 0.8530(2) 0.25566(8) 0.0152(4) Uani 1 1 d . . . N1 N 0.23847(9) 0.9395(2) 0.10914(8) 0.0152(4) Uani 1 1 d . . . C26 C 0.04593(11) 0.7968(2) 0.06989(9) 0.0156(5) Uani 1 1 d . . . C1 C 0.18463(11) 0.9140(2) 0.13233(10) 0.0133(5) Uani 1 1 d . . . N2 N 0.13856(9) 0.93191(19) 0.08901(8) 0.0141(4) Uani 1 1 d . . . C421 C 0.13457(11) 1.0439(2) 0.30685(10) 0.0172(5) Uani 1 1 d . . . H42A H 0.1802 1.0325 0.3216 0.021 Uiso 1 1 calc R . . C31 C 0.26377(11) 0.8279(2) 0.31000(9) 0.0129(5) Uani 1 1 d . . . C36 C 0.31773(11) 0.8162(2) 0.35065(10) 0.0158(5) Uani 1 1 d . . . C33 C 0.19645(11) 0.7860(2) 0.38285(10) 0.0158(5) Uani 1 1 d . . . H33A H 0.1553 0.7751 0.3934 0.019 Uiso 1 1 calc R . . C11 C 0.30253(11) 0.9323(2) 0.13707(10) 0.0154(5) Uani 1 1 d . . . C56 C 0.42537(11) 0.9193(2) 0.35087(10) 0.0182(5) Uani 1 1 d . . . C22 C 0.03278(11) 1.0139(2) 0.10058(10) 0.0162(5) Uani 1 1 d . . . C43 C 0.05504(11) 0.9242(2) 0.23978(10) 0.0170(5) Uani 1 1 d . . . H43A H 0.0303 0.9980 0.2346 0.020 Uiso 1 1 calc R . . C44 C 0.03359(11) 0.8149(2) 0.21335(10) 0.0153(5) Uani 1 1 d . . . H44A H -0.0064 0.8136 0.1913 0.018 Uiso 1 1 calc R . . C21 C 0.07063(11) 0.9127(2) 0.08787(9) 0.0142(5) Uani 1 1 d . . . C41 C 0.14822(10) 0.8141(2) 0.28411(9) 0.0132(5) Uani 1 1 d . . . C161 C 0.28346(12) 1.1424(2) 0.18145(11) 0.0205(5) Uani 1 1 d . . . H16A H 0.2384 1.1138 0.1757 0.025 Uiso 1 1 calc R . . C261 C 0.08837(12) 0.6907(2) 0.05536(10) 0.0184(5) Uani 1 1 d . . . H26A H 0.1314 0.7042 0.0759 0.022 Uiso 1 1 calc R . . C32 C 0.20345(11) 0.8092(2) 0.32807(10) 0.0134(5) Uani 1 1 d . . . C3 C 0.16319(12) 0.9673(2) 0.04128(10) 0.0174(5) Uani 1 1 d . . . H3A H 0.1399 0.9842 0.0063 0.021 Uiso 1 1 calc R . . C45 C 0.07019(11) 0.7078(2) 0.21886(10) 0.0169(5) Uani 1 1 d . . . H45A H 0.0557 0.6349 0.1991 0.020 Uiso 1 1 calc R . . C222 C 0.01416(13) 1.2166(3) 0.15097(11) 0.0236(6) Uani 1 1 d . . . H22A H -0.0058 1.1672 0.1779 0.035 Uiso 1 1 calc R . . H22B H -0.0184 1.2471 0.1222 0.035 Uiso 1 1 calc R . . H22C H 0.0365 1.2876 0.1697 0.035 Uiso 1 1 calc R . . C24 C -0.05830(12) 0.8809(3) 0.07554(10) 0.0201(6) Uani 1 1 d . . . H24A H -0.1029 0.8702 0.0713 0.024 Uiso 1 1 calc R . . C16 C 0.32451(11) 1.0311(2) 0.17177(10) 0.0173(5) Uani 1 1 d . . . C461 C 0.16645(11) 0.5845(2) 0.26201(10) 0.0180(5) Uani 1 1 d . . . H46A H 0.2120 0.6085 0.2705 0.022 Uiso 1 1 calc R . . C42 C 0.11287(11) 0.9265(2) 0.27405(9) 0.0148(5) Uani 1 1 d . . . C25 C -0.01968(12) 0.7825(3) 0.06405(10) 0.0187(5) Uani 1 1 d . . . H25A H -0.0381 0.7049 0.0521 0.022 Uiso 1 1 calc R . . C13 C 0.40113(12) 0.8258(3) 0.15224(11) 0.0225(6) Uani 1 1 d . . . H13A H 0.4276 0.7574 0.1458 0.027 Uiso 1 1 calc R . . C221 C 0.06132(12) 1.1353(2) 0.12468(10) 0.0183(5) Uani 1 1 d . . . H22D H 0.0957 1.1123 0.1546 0.022 Uiso 1 1 calc R . . C15 C 0.38696(12) 1.0219(3) 0.19688(11) 0.0211(6) Uani 1 1 d . . . H15A H 0.4039 1.0863 0.2210 0.025 Uiso 1 1 calc R . . C262 C 0.06511(14) 0.5620(2) 0.07138(11) 0.0251(6) Uani 1 1 d . . . H26B H 0.0602 0.5614 0.1108 0.038 Uiso 1 1 calc R . . H26C H 0.0960 0.4985 0.0639 0.038 Uiso 1 1 calc R . . H26D H 0.0242 0.5439 0.0497 0.038 Uiso 1 1 calc R . . C51 C 0.38410(11) 0.8185(2) 0.33587(10) 0.0158(5) Uani 1 1 d . . . C23 C -0.03258(11) 0.9944(3) 0.09311(10) 0.0192(5) Uani 1 1 d . . . H23A H -0.0600 1.0608 0.1003 0.023 Uiso 1 1 calc R . . C34 C 0.24932(12) 0.7787(3) 0.42255(10) 0.0192(5) Uani 1 1 d . . . H34A H 0.2448 0.7650 0.4603 0.023 Uiso 1 1 calc R . . C52 C 0.40686(12) 0.7125(2) 0.30976(11) 0.0193(5) Uani 1 1 d . . . C2 C 0.22605(12) 0.9732(3) 0.05402(10) 0.0189(5) Uani 1 1 d . . . H2A H 0.2562 0.9959 0.0301 0.023 Uiso 1 1 calc R . . C35 C 0.30857(11) 0.7920(2) 0.40538(10) 0.0167(5) Uani 1 1 d . . . H35A H 0.3448 0.7842 0.4321 0.020 Uiso 1 1 calc R . . C55 C 0.48821(12) 0.9117(3) 0.33976(11) 0.0234(6) Uani 1 1 d . . . H55A H 0.5163 0.9791 0.3497 0.028 Uiso 1 1 calc R . . C14 C 0.42478(12) 0.9206(3) 0.18740(11) 0.0227(6) Uani 1 1 d . . . H14A H 0.4671 0.9164 0.2051 0.027 Uiso 1 1 calc R . . C561 C 0.40428(12) 1.0335(3) 0.38068(11) 0.0235(6) Uani 1 1 d . . . H56A H 0.3569 1.0344 0.3764 0.028 Uiso 1 1 calc R . . C462 C 0.14838(13) 0.5124(3) 0.31174(11) 0.0248(6) Uani 1 1 d . . . H46B H 0.1523 0.5671 0.3441 0.037 Uiso 1 1 calc R . . H46C H 0.1767 0.4407 0.3191 0.037 Uiso 1 1 calc R . . H46D H 0.1046 0.4831 0.3039 0.037 Uiso 1 1 calc R . . C521 C 0.36410(13) 0.6007(3) 0.29553(12) 0.0235(6) Uani 1 1 d . . . H52A H 0.3199 0.6325 0.2859 0.028 Uiso 1 1 calc R . . C54 C 0.51012(12) 0.8079(3) 0.31460(11) 0.0240(6) Uani 1 1 d . . . H54A H 0.5530 0.8040 0.3076 0.029 Uiso 1 1 calc R . . C223 C 0.09175(14) 1.2158(3) 0.08288(12) 0.0279(6) Uani 1 1 d . . . H22E H 0.1218 1.1652 0.0651 0.042 Uiso 1 1 calc R . . H22F H 0.1141 1.2861 0.1021 0.042 Uiso 1 1 calc R . . H22G H 0.0587 1.2473 0.0548 0.042 Uiso 1 1 calc R . . C53 C 0.46964(12) 0.7099(3) 0.29956(11) 0.0233(6) Uani 1 1 d . . . H53A H 0.4850 0.6392 0.2819 0.028 Uiso 1 1 calc R . . C162 C 0.29050(15) 1.2450(3) 0.13901(13) 0.0324(7) Uani 1 1 d . . . H16B H 0.2821 1.2102 0.1017 0.049 Uiso 1 1 calc R . . H16C H 0.3337 1.2784 0.1448 0.049 Uiso 1 1 calc R . . H16D H 0.2602 1.3120 0.1434 0.049 Uiso 1 1 calc R . . C463 C 0.16077(13) 0.4999(3) 0.21115(11) 0.0257(6) Uani 1 1 d . . . H46E H 0.1863 0.4248 0.2195 0.039 Uiso 1 1 calc R . . H46F H 0.1760 0.5445 0.1803 0.039 Uiso 1 1 calc R . . H46G H 0.1163 0.4764 0.2011 0.039 Uiso 1 1 calc R . . C12 C 0.33901(12) 0.8292(3) 0.12607(10) 0.0184(5) Uani 1 1 d . . . C121 C 0.31185(13) 0.7233(3) 0.08849(11) 0.0245(6) Uani 1 1 d . . . H12A H 0.2833 0.7622 0.0576 0.029 Uiso 1 1 calc R . . C422 C 0.12929(13) 1.1621(2) 0.27205(11) 0.0229(6) Uani 1 1 d . . . H42B H 0.1431 1.2338 0.2954 0.034 Uiso 1 1 calc R . . H42C H 0.0852 1.1740 0.2560 0.034 Uiso 1 1 calc R . . H42D H 0.1562 1.1546 0.2424 0.034 Uiso 1 1 calc R . . C163 C 0.29616(13) 1.1932(3) 0.24012(12) 0.0280(6) Uani 1 1 d . . . H16E H 0.2684 1.2646 0.2441 0.042 Uiso 1 1 calc R . . H16F H 0.3405 1.2197 0.2476 0.042 Uiso 1 1 calc R . . H16G H 0.2878 1.1279 0.2664 0.042 Uiso 1 1 calc R . . C46 C 0.12820(11) 0.7049(2) 0.25303(10) 0.0150(5) Uani 1 1 d . . . C423 C 0.09721(12) 1.0579(3) 0.35610(11) 0.0230(6) Uani 1 1 d . . . H42E H 0.1109 1.1336 0.3767 0.034 Uiso 1 1 calc R . . H42F H 0.1048 0.9852 0.3803 0.034 Uiso 1 1 calc R . . H42G H 0.0519 1.0639 0.3429 0.034 Uiso 1 1 calc R . . C522 C 0.38174(15) 0.5271(3) 0.24593(13) 0.0345(7) Uani 1 1 d . . . H52B H 0.3531 0.4557 0.2390 0.052 Uiso 1 1 calc R . . H52C H 0.4255 0.4973 0.2538 0.052 Uiso 1 1 calc R . . H52D H 0.3779 0.5812 0.2133 0.052 Uiso 1 1 calc R . . C122 C 0.27094(14) 0.6351(3) 0.11882(14) 0.0335(7) Uani 1 1 d . . . H12B H 0.2540 0.5686 0.0937 0.050 Uiso 1 1 calc R . . H12C H 0.2359 0.6819 0.1314 0.050 Uiso 1 1 calc R . . H12D H 0.2969 0.5984 0.1507 0.050 Uiso 1 1 calc R . . C263 C 0.09486(15) 0.6897(3) -0.00667(11) 0.0295(7) Uani 1 1 d . . . H26E H 0.1083 0.7723 -0.0179 0.044 Uiso 1 1 calc R . . H26F H 0.0539 0.6687 -0.0276 0.044 Uiso 1 1 calc R . . H26G H 0.1265 0.6275 -0.0141 0.044 Uiso 1 1 calc R . . C562 C 0.42809(16) 1.0271(3) 0.44261(12) 0.0349(7) Uani 1 1 d . . . H56B H 0.4144 1.1018 0.4610 0.052 Uiso 1 1 calc R . . H56C H 0.4744 1.0226 0.4478 0.052 Uiso 1 1 calc R . . H56D H 0.4106 0.9529 0.4586 0.052 Uiso 1 1 calc R . . C563 C 0.42678(14) 1.1563(3) 0.35784(12) 0.0290(6) Uani 1 1 d . . . H56E H 0.4117 1.2262 0.3786 0.044 Uiso 1 1 calc R . . H56F H 0.4099 1.1640 0.3188 0.044 Uiso 1 1 calc R . . H56G H 0.4732 1.1574 0.3615 0.044 Uiso 1 1 calc R . . C523 C 0.3641(2) 0.5136(3) 0.34474(15) 0.0485(9) Uani 1 1 d . . . H52E H 0.3526 0.5605 0.3765 0.073 Uiso 1 1 calc R . . H52F H 0.4063 0.4773 0.3539 0.073 Uiso 1 1 calc R . . H52G H 0.3331 0.4467 0.3355 0.073 Uiso 1 1 calc R . . C123 C 0.36184(16) 0.6501(3) 0.06267(14) 0.0417(9) Uani 1 1 d . . . H12E H 0.3414 0.5837 0.0393 0.063 Uiso 1 1 calc R . . H12F H 0.3919 0.6132 0.0919 0.063 Uiso 1 1 calc R . . H12G H 0.3845 0.7061 0.0402 0.063 Uiso 1 1 calc R . . H H 0.3008(12) 0.860(2) 0.2456(10) 0.004(6) Uiso 1 1 d . . . Cl1 Cl 0.20076(4) 0.13616(9) 0.49575(3) 0.0454(2) Uani 1 1 d . . . Cl2 Cl 0.25376(4) 0.24702(9) 0.40252(4) 0.0477(2) Uani 1 1 d . . . Cl3 Cl 0.62095(5) 0.87585(13) 0.99107(6) 0.0788(4) Uani 1 1 d . . . Cl4 Cl 0.48693(6) 0.82796(13) 0.97188(7) 0.0952(5) Uani 1 1 d . . . C999 C 0.25199(16) 0.1148(3) 0.44494(14) 0.0364(7) Uani 1 1 d . . . H99A H 0.2953 0.0974 0.4631 0.044 Uiso 1 1 calc R . . H99B H 0.2378 0.0418 0.4219 0.044 Uiso 1 1 calc R . . C998 C 0.5523(3) 0.8873(5) 0.94415(17) 0.0846(17) Uani 1 1 d . . . H99C H 0.5446 0.9758 0.9340 0.101 Uiso 1 1 calc R . . H99D H 0.5583 0.8407 0.9102 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01331(16) 0.01984(19) 0.00757(16) 0.00132(12) 0.00397(11) -0.00003(12) N3 0.0107(10) 0.0237(12) 0.0118(10) 0.0030(8) 0.0040(8) -0.0001(8) N1 0.0123(9) 0.0260(12) 0.0080(9) 0.0029(8) 0.0033(7) 0.0012(8) C26 0.0197(12) 0.0209(13) 0.0066(11) 0.0034(9) 0.0036(9) 0.0004(10) C1 0.0128(11) 0.0147(12) 0.0127(11) -0.0014(9) 0.0030(9) 0.0000(9) N2 0.0139(10) 0.0199(11) 0.0096(10) 0.0009(8) 0.0060(8) -0.0019(8) C421 0.0169(12) 0.0212(14) 0.0137(12) -0.0012(10) 0.0031(9) 0.0033(10) C31 0.0146(11) 0.0143(12) 0.0107(11) 0.0005(9) 0.0047(9) 0.0019(9) C36 0.0165(12) 0.0163(13) 0.0158(12) 0.0015(10) 0.0064(9) -0.0002(9) C33 0.0157(11) 0.0203(13) 0.0124(12) 0.0014(10) 0.0061(9) -0.0008(9) C11 0.0122(11) 0.0244(14) 0.0103(11) 0.0064(10) 0.0041(9) -0.0010(9) C56 0.0164(12) 0.0240(14) 0.0142(12) 0.0022(11) 0.0024(9) -0.0028(10) C22 0.0209(12) 0.0215(14) 0.0072(11) 0.0037(10) 0.0056(9) 0.0025(10) C43 0.0160(12) 0.0224(14) 0.0136(12) 0.0046(10) 0.0060(9) 0.0034(10) C44 0.0110(11) 0.0254(14) 0.0097(11) 0.0021(10) 0.0018(9) -0.0017(9) C21 0.0130(11) 0.0228(13) 0.0074(11) 0.0030(10) 0.0033(9) -0.0004(9) C41 0.0132(11) 0.0174(12) 0.0103(11) 0.0023(9) 0.0070(9) -0.0018(9) C161 0.0165(12) 0.0214(14) 0.0236(14) -0.0006(11) 0.0021(10) 0.0021(10) C261 0.0198(12) 0.0224(14) 0.0135(12) -0.0001(10) 0.0040(10) -0.0002(10) C32 0.0145(11) 0.0150(12) 0.0109(11) -0.0005(9) 0.0031(9) 0.0000(9) C3 0.0216(12) 0.0225(14) 0.0085(11) 0.0032(10) 0.0042(9) -0.0001(10) C45 0.0178(12) 0.0222(14) 0.0114(12) -0.0002(10) 0.0048(9) -0.0034(10) C222 0.0310(15) 0.0229(15) 0.0176(13) 0.0001(11) 0.0058(11) 0.0072(11) C24 0.0139(12) 0.0333(16) 0.0133(12) 0.0065(11) 0.0026(9) -0.0006(10) C16 0.0173(12) 0.0212(13) 0.0147(12) 0.0046(10) 0.0080(9) -0.0007(10) C461 0.0165(12) 0.0190(13) 0.0192(13) 0.0009(10) 0.0044(10) 0.0012(9) C42 0.0140(11) 0.0220(13) 0.0096(11) 0.0013(10) 0.0057(9) 0.0011(9) C25 0.0209(12) 0.0256(14) 0.0099(11) 0.0013(10) 0.0035(9) -0.0053(10) C13 0.0156(12) 0.0305(15) 0.0222(14) 0.0024(12) 0.0064(10) 0.0042(10) C221 0.0206(12) 0.0210(14) 0.0140(12) 0.0000(10) 0.0043(10) 0.0017(10) C15 0.0188(12) 0.0255(14) 0.0193(13) 0.0008(11) 0.0036(10) -0.0054(10) C262 0.0365(16) 0.0198(14) 0.0199(14) 0.0000(11) 0.0067(12) -0.0007(11) C51 0.0139(11) 0.0210(13) 0.0127(12) 0.0040(10) 0.0022(9) -0.0002(9) C23 0.0184(12) 0.0266(15) 0.0133(12) 0.0043(10) 0.0049(10) 0.0049(10) C34 0.0230(13) 0.0270(14) 0.0085(11) 0.0009(10) 0.0055(10) -0.0001(10) C52 0.0186(12) 0.0211(14) 0.0187(13) 0.0039(11) 0.0045(10) 0.0008(10) C2 0.0213(12) 0.0276(15) 0.0089(12) 0.0046(10) 0.0066(10) -0.0009(10) C35 0.0174(12) 0.0213(13) 0.0108(12) 0.0012(10) -0.0004(9) 0.0001(9) C55 0.0179(13) 0.0296(15) 0.0227(14) 0.0026(12) 0.0025(10) -0.0032(11) C14 0.0133(12) 0.0320(16) 0.0227(14) 0.0052(12) 0.0014(10) -0.0006(10) C561 0.0209(13) 0.0261(15) 0.0239(14) -0.0057(12) 0.0042(11) -0.0031(11) C462 0.0344(15) 0.0193(14) 0.0209(14) 0.0035(11) 0.0043(11) -0.0018(11) C521 0.0196(13) 0.0215(14) 0.0305(15) -0.0028(12) 0.0081(11) 0.0006(10) C54 0.0132(12) 0.0323(16) 0.0274(15) 0.0041(12) 0.0060(10) 0.0014(10) C223 0.0389(16) 0.0223(15) 0.0249(15) 0.0006(12) 0.0131(12) -0.0025(12) C53 0.0186(13) 0.0258(15) 0.0261(15) 0.0008(12) 0.0055(11) 0.0042(10) C162 0.0368(17) 0.0290(17) 0.0301(16) 0.0011(13) 0.0000(13) 0.0019(13) C463 0.0306(14) 0.0239(15) 0.0239(15) -0.0035(12) 0.0090(12) 0.0012(11) C12 0.0199(12) 0.0254(14) 0.0110(12) 0.0023(10) 0.0062(9) 0.0025(10) C121 0.0243(13) 0.0313(16) 0.0175(13) -0.0064(12) 0.0015(11) 0.0057(11) C422 0.0275(14) 0.0192(14) 0.0223(14) -0.0011(11) 0.0036(11) 0.0007(10) C163 0.0297(15) 0.0270(16) 0.0285(16) -0.0037(12) 0.0079(12) 0.0010(12) C46 0.0163(11) 0.0193(13) 0.0108(11) 0.0015(10) 0.0066(9) -0.0007(9) C423 0.0249(14) 0.0285(16) 0.0164(13) -0.0037(11) 0.0054(10) 0.0069(11) C522 0.0327(16) 0.0352(18) 0.0357(18) -0.0095(14) 0.0041(13) -0.0030(13) C122 0.0310(16) 0.0300(17) 0.0395(18) -0.0097(14) 0.0040(13) -0.0010(12) C263 0.0442(17) 0.0264(16) 0.0213(15) 0.0014(12) 0.0173(13) 0.0041(13) C562 0.0487(19) 0.0332(18) 0.0241(16) -0.0074(13) 0.0096(14) -0.0117(14) C563 0.0294(15) 0.0291(16) 0.0282(16) -0.0023(13) 0.0019(12) -0.0037(12) C523 0.079(3) 0.0269(18) 0.045(2) -0.0001(16) 0.0283(19) -0.0139(17) C123 0.0360(17) 0.056(2) 0.0339(18) -0.0180(16) 0.0083(14) 0.0096(15) Cl1 0.0492(5) 0.0616(6) 0.0274(4) -0.0037(4) 0.0127(4) -0.0052(4) Cl2 0.0480(5) 0.0506(6) 0.0442(5) 0.0163(4) 0.0049(4) -0.0069(4) Cl3 0.0514(6) 0.1065(11) 0.0822(9) 0.0159(7) 0.0235(6) -0.0097(6) Cl4 0.0544(7) 0.0746(9) 0.1485(14) -0.0063(9) -0.0201(8) -0.0157(6) C999 0.0386(17) 0.0353(18) 0.0370(18) 0.0092(15) 0.0120(14) 0.0078(14) C998 0.134(5) 0.089(4) 0.028(2) 0.002(2) -0.001(3) -0.017(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 N3 1.953(2) . ? Ni1 C1 1.959(2) . ? Ni1 C41 2.114(2) . ? Ni1 C46 2.380(2) . ? Ni1 C42 2.385(2) . ? N3 C31 1.352(3) . ? N1 C1 1.366(3) . ? N1 C2 1.387(3) . ? N1 C11 1.449(3) . ? C26 C25 1.394(3) . ? C26 C21 1.399(4) . ? C26 C261 1.522(3) . ? C1 N2 1.364(3) . ? N2 C3 1.388(3) . ? N2 C21 1.457(3) . ? C421 C422 1.522(4) . ? C421 C423 1.528(3) . ? C421 C42 1.533(3) . ? C31 C32 1.422(3) . ? C31 C36 1.428(3) . ? C36 C35 1.398(3) . ? C36 C51 1.500(3) . ? C33 C32 1.386(3) . ? C33 C34 1.394(3) . ? C11 C12 1.396(4) . ? C11 C16 1.400(4) . ? C56 C55 1.399(4) . ? C56 C51 1.413(3) . ? C56 C561 1.520(4) . ? C22 C23 1.396(3) . ? C22 C21 1.409(3) . ? C22 C221 1.524(4) . ? C43 C44 1.388(4) . ? C43 C42 1.401(3) . ? C44 C45 1.385(3) . ? C41 C42 1.427(3) . ? C41 C46 1.431(3) . ? C41 C32 1.492(3) . ? C161 C16 1.515(3) . ? C161 C163 1.525(4) . ? C161 C162 1.531(4) . ? C261 C262 1.533(4) . ? C261 C263 1.537(4) . ? C3 C2 1.337(3) . ? C45 C46 1.403(3) . ? C222 C221 1.529(3) . ? C24 C23 1.381(4) . ? C24 C25 1.387(4) . ? C16 C15 1.397(3) . ? C461 C46 1.528(3) . ? C461 C462 1.528(4) . ? C461 C463 1.530(4) . ? C13 C14 1.385(4) . ? C13 C12 1.396(4) . ? C221 C223 1.539(4) . ? C15 C14 1.388(4) . ? C51 C52 1.417(4) . ? C34 C35 1.384(3) . ? C52 C53 1.389(4) . ? C52 C521 1.519(4) . ? C55 C54 1.380(4) . ? C561 C563 1.530(4) . ? C561 C562 1.536(4) . ? C521 C523 1.522(4) . ? C521 C522 1.530(4) . ? C54 C53 1.380(4) . ? C12 C121 1.528(4) . ? C121 C123 1.520(4) . ? C121 C122 1.536(4) . ? Cl1 C999 1.764(3) . ? Cl2 C999 1.759(3) . ? Cl3 C998 1.746(5) . ? Cl4 C998 1.741(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni1 C1 116.41(9) . . ? N3 Ni1 C41 81.62(9) . . ? C1 Ni1 C41 161.90(9) . . ? N3 Ni1 C46 97.89(8) . . ? C1 Ni1 C46 134.32(9) . . ? C41 Ni1 C46 36.54(9) . . ? N3 Ni1 C42 101.93(8) . . ? C1 Ni1 C42 130.61(9) . . ? C41 Ni1 C42 36.34(9) . . ? C46 Ni1 C42 62.21(8) . . ? C31 N3 Ni1 118.64(16) . . ? C1 N1 C2 112.62(19) . . ? C1 N1 C11 125.60(19) . . ? C2 N1 C11 121.8(2) . . ? C25 C26 C21 117.6(2) . . ? C25 C26 C261 120.6(2) . . ? C21 C26 C261 121.8(2) . . ? N2 C1 N1 102.10(19) . . ? N2 C1 Ni1 132.75(17) . . ? N1 C1 Ni1 125.15(16) . . ? C1 N2 C3 112.3(2) . . ? C1 N2 C21 127.69(19) . . ? C3 N2 C21 119.9(2) . . ? C422 C421 C423 110.3(2) . . ? C422 C421 C42 113.3(2) . . ? C423 C421 C42 109.8(2) . . ? N3 C31 C32 115.8(2) . . ? N3 C31 C36 127.3(2) . . ? C32 C31 C36 116.8(2) . . ? C35 C36 C31 119.1(2) . . ? C35 C36 C51 118.6(2) . . ? C31 C36 C51 122.1(2) . . ? C32 C33 C34 120.5(2) . . ? C12 C11 C16 124.3(2) . . ? C12 C11 N1 117.7(2) . . ? C16 C11 N1 118.0(2) . . ? C55 C56 C51 118.9(2) . . ? C55 C56 C561 119.0(2) . . ? C51 C56 C561 122.0(2) . . ? C23 C22 C21 116.3(2) . . ? C23 C22 C221 121.4(2) . . ? C21 C22 C221 122.1(2) . . ? C44 C43 C42 120.5(2) . . ? C45 C44 C43 120.4(2) . . ? C26 C21 C22 123.4(2) . . ? C26 C21 N2 117.7(2) . . ? C22 C21 N2 118.6(2) . . ? C42 C41 C46 119.0(2) . . ? C42 C41 C32 120.4(2) . . ? C46 C41 C32 120.6(2) . . ? C42 C41 Ni1 82.25(14) . . ? C46 C41 Ni1 81.91(14) . . ? C32 C41 Ni1 108.02(15) . . ? C16 C161 C163 112.9(2) . . ? C16 C161 C162 110.8(2) . . ? C163 C161 C162 111.0(2) . . ? C26 C261 C262 113.2(2) . . ? C26 C261 C263 111.2(2) . . ? C262 C261 C263 108.4(2) . . ? C33 C32 C31 122.2(2) . . ? C33 C32 C41 122.1(2) . . ? C31 C32 C41 115.7(2) . . ? C2 C3 N2 106.7(2) . . ? C44 C45 C46 121.3(2) . . ? C23 C24 C25 120.8(2) . . ? C15 C16 C11 116.1(2) . . ? C15 C16 C161 121.5(2) . . ? C11 C16 C161 122.3(2) . . ? C46 C461 C462 111.1(2) . . ? C46 C461 C463 113.4(2) . . ? C462 C461 C463 110.0(2) . . ? C43 C42 C41 119.6(2) . . ? C43 C42 C421 120.8(2) . . ? C41 C42 C421 119.1(2) . . ? C43 C42 Ni1 99.60(16) . . ? C41 C42 Ni1 61.41(12) . . ? C421 C42 Ni1 114.02(15) . . ? C24 C25 C26 120.4(2) . . ? C14 C13 C12 121.1(3) . . ? C22 C221 C222 113.5(2) . . ? C22 C221 C223 113.8(2) . . ? C222 C221 C223 108.0(2) . . ? C14 C15 C16 121.5(2) . . ? C56 C51 C52 119.7(2) . . ? C56 C51 C36 121.6(2) . . ? C52 C51 C36 118.6(2) . . ? C24 C23 C22 121.5(2) . . ? C35 C34 C33 118.1(2) . . ? C53 C52 C51 119.1(2) . . ? C53 C52 C521 120.3(2) . . ? C51 C52 C521 120.5(2) . . ? C3 C2 N1 106.2(2) . . ? C34 C35 C36 123.2(2) . . ? C54 C55 C56 121.1(3) . . ? C13 C14 C15 120.3(2) . . ? C56 C561 C563 113.3(2) . . ? C56 C561 C562 110.8(2) . . ? C563 C561 C562 108.5(2) . . ? C52 C521 C523 111.3(2) . . ? C52 C521 C522 113.0(2) . . ? C523 C521 C522 109.4(3) . . ? C53 C54 C55 119.9(2) . . ? C54 C53 C52 121.3(3) . . ? C13 C12 C11 116.8(2) . . ? C13 C12 C121 121.5(2) . . ? C11 C12 C121 121.8(2) . . ? C123 C121 C12 113.6(2) . . ? C123 C121 C122 110.4(3) . . ? C12 C121 C122 111.3(2) . . ? C45 C46 C41 118.7(2) . . ? C45 C46 C461 121.2(2) . . ? C41 C46 C461 119.8(2) . . ? C45 C46 Ni1 98.83(16) . . ? C41 C46 Ni1 61.55(12) . . ? C461 C46 Ni1 113.15(15) . . ? Cl2 C999 Cl1 111.64(18) . . ? Cl4 C998 Cl3 111.3(2) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.397 _refine_diff_density_min -1.166 _refine_diff_density_rms 0.098 data_7 _database_code_depnum_ccdc_archive 'CCDC 896903' #TrackingRef 'CIF(1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H84 B F24 N3 Ni O' _chemical_formula_weight 1713.09 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' B B 0.0013 0.0007 '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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9077(17) _cell_length_b 34.624(4) _cell_length_c 19.650(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.756(2) _cell_angle_gamma 90.00 _cell_volume 8363.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8253 _exptl_absorpt_correction_T_max 0.9364 _exptl_absorpt_process_details 'Norton et. al.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 80470 _diffrn_reflns_av_R_equivalents 0.1469 _diffrn_reflns_av_sigmaI/netI 0.1100 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14742 _reflns_number_gt 8683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14742 _refine_ls_number_parameters 1097 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1426 _refine_ls_R_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.2497 _refine_ls_wR_factor_gt 0.2231 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.011 _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 0.72359(5) 0.344953(19) 0.86195(3) 0.0331(2) Uani 1 1 d . . . C3 C 0.4602(4) 0.33304(15) 0.6995(3) 0.0404(13) Uani 1 1 d . . . H3A H 0.4005 0.3164 0.6789 0.049 Uiso 1 1 calc R . . F652 F 0.0797(3) 0.49462(9) 0.42092(17) 0.0521(9) Uani 1 1 d . . . C31 C 0.9259(4) 0.32544(15) 0.9815(3) 0.0358(12) Uani 1 1 d . . . N1 N 0.5779(3) 0.38143(11) 0.7208(2) 0.0294(9) Uani 1 1 d . . . F651 F 0.2232(3) 0.45996(9) 0.4593(2) 0.0644(11) Uani 1 1 d . . . N2 N 0.5411(3) 0.32827(11) 0.7639(2) 0.0341(10) Uani 1 1 d . . . C62 C 0.3317(4) 0.58678(12) 0.5730(2) 0.0233(10) Uani 1 1 d . . . H62A H 0.3704 0.6094 0.5937 0.028 Uiso 1 1 calc R . . C36 C 1.0120(4) 0.30209(15) 0.9801(3) 0.0424(14) Uani 1 1 d . . . C41 C 0.8471(4) 0.38646(15) 1.0150(3) 0.0392(13) Uani 1 1 d . . . C61 C 0.2303(3) 0.57961(12) 0.5828(2) 0.0221(10) Uani 1 1 d . . . C66 C 0.1785(4) 0.54623(12) 0.5503(2) 0.0219(10) Uani 1 1 d . . . H66A H 0.1087 0.5403 0.5542 0.026 Uiso 1 1 calc R . . C63 C 0.3781(4) 0.56228(12) 0.5345(2) 0.0228(10) Uani 1 1 d . . . N3 N 0.8145(3) 0.31399(13) 0.9423(2) 0.0332(10) Uani 1 1 d . . . C33 C 1.0463(5) 0.37132(18) 1.0548(3) 0.0510(16) Uani 1 1 d . . . H33A H 1.0589 0.3951 1.0801 0.061 Uiso 1 1 calc R . . C651 C 0.1617(4) 0.48616(15) 0.4795(3) 0.0359(12) Uani 1 1 d . . . C64 C 0.3253(4) 0.52887(12) 0.5046(2) 0.0247(10) Uani 1 1 d . . . H64A H 0.3574 0.5115 0.4795 0.030 Uiso 1 1 calc R . . C51 C 0.9942(4) 0.26579(15) 0.9370(3) 0.0406(13) Uani 1 1 d . . . C65 C 0.2241(4) 0.52133(12) 0.5124(2) 0.0239(10) Uani 1 1 d . . . C21 C 0.5595(4) 0.29650(14) 0.8154(3) 0.0387(13) Uani 1 1 d . . . C32 C 0.9395(4) 0.36044(15) 1.0182(3) 0.0405(13) Uani 1 1 d . . . C2 C 0.4842(4) 0.36643(15) 0.6723(3) 0.0379(13) Uani 1 1 d . . . H2A H 0.4443 0.3777 0.6280 0.046 Uiso 1 1 calc R . . C11 C 0.6253(4) 0.41760(13) 0.7099(2) 0.0296(11) Uani 1 1 d . . . C34 C 1.1340(5) 0.34826(18) 1.0552(4) 0.0603(18) Uani 1 1 d . . . H34A H 1.2060 0.3559 1.0810 0.072 Uiso 1 1 calc R . . C1 C 0.6152(4) 0.35727(14) 0.7780(3) 0.0308(11) Uani 1 1 d . . . F633 F 0.5038(3) 0.60806(9) 0.5197(2) 0.0731(12) Uani 1 1 d . . . C93 C -0.0441(4) 0.65576(14) 0.4526(3) 0.0337(12) Uani 1 1 d . . . F653 F 0.1157(3) 0.46772(8) 0.52245(17) 0.0489(8) Uani 1 1 d . . . C91 C 0.1083(4) 0.64063(13) 0.5589(2) 0.0251(10) Uani 1 1 d . . . F632 F 0.5674(2) 0.55835(12) 0.5798(2) 0.0749(12) Uani 1 1 d . . . C75 C 0.4143(4) 0.62747(17) 0.7989(3) 0.0434(14) Uani 1 1 d . . . F631 F 0.5031(3) 0.55512(12) 0.4691(2) 0.0726(12) Uani 1 1 d . . . C92 C 0.0070(4) 0.63153(13) 0.5103(3) 0.0302(11) Uani 1 1 d . . . H92A H -0.0282 0.6083 0.5166 0.036 Uiso 1 1 calc R . . C71 C 0.2568(4) 0.63162(14) 0.6914(3) 0.0307(11) Uani 1 1 d . . . C82 C 0.1158(4) 0.55373(15) 0.6937(2) 0.0334(12) Uani 1 1 d . . . H82A H 0.1817 0.5416 0.6934 0.040 Uiso 1 1 calc R . . F753 F 0.4871(4) 0.57544(18) 0.8752(3) 0.138(2) Uani 1 1 d . . . C96 C 0.1552(4) 0.67425(14) 0.5444(3) 0.0323(12) Uani 1 1 d . . . H96A H 0.2253 0.6811 0.5749 0.039 Uiso 1 1 calc R . . C81 C 0.0871(4) 0.58871(14) 0.6579(2) 0.0283(11) Uani 1 1 d . . . C631 C 0.4874(4) 0.57103(13) 0.5267(3) 0.0281(11) Uani 1 1 d . . . C22 C 0.5343(4) 0.30358(16) 0.8797(3) 0.0466(15) Uani 1 1 d . . . C73 C 0.3022(5) 0.68398(17) 0.7797(3) 0.0472(15) Uani 1 1 d . . . B1 B 0.1719(4) 0.61039(15) 0.6227(3) 0.0260(12) Uani 1 1 d . . . F752 F 0.5669(4) 0.58994(14) 0.8022(2) 0.0934(15) Uani 1 1 d . . . C16 C 0.5677(4) 0.45156(14) 0.7138(3) 0.0350(12) Uani 1 1 d . . . C15 C 0.6126(5) 0.48579(16) 0.6992(3) 0.0484(15) Uani 1 1 d . . . H15A H 0.5766 0.5095 0.7015 0.058 Uiso 1 1 calc R . . C14 C 0.7066(5) 0.48639(17) 0.6818(3) 0.0513(16) Uani 1 1 d . . . H14A H 0.7337 0.5103 0.6706 0.062 Uiso 1 1 calc R . . C42 C 0.7889(4) 0.40285(15) 0.9500(3) 0.0432(14) Uani 1 1 d . . . C13 C 0.7625(5) 0.45343(17) 0.6802(3) 0.0471(15) Uani 1 1 d . . . H13A H 0.8299 0.4547 0.6701 0.056 Uiso 1 1 calc R . . C24 C 0.6098(6) 0.2408(2) 0.9187(4) 0.068(2) Uani 1 1 d . . . H24A H 0.6284 0.2214 0.9545 0.082 Uiso 1 1 calc R . . C74 C 0.3924(5) 0.66337(18) 0.8214(3) 0.0522(16) Uani 1 1 d . . . H74A H 0.4381 0.6740 0.8647 0.063 Uiso 1 1 calc R . . C121 C 0.7823(5) 0.38053(17) 0.6874(3) 0.0474(15) Uani 1 1 d . . . H12A H 0.7705 0.3620 0.7233 0.057 Uiso 1 1 calc R . . C43 C 0.7089(5) 0.42956(17) 0.9474(4) 0.0589(18) Uani 1 1 d . . . H43A H 0.6703 0.4413 0.9032 0.071 Uiso 1 1 calc R . . C441 C 0.5987(8) 0.4705(3) 1.0069(5) 0.118(4) Uani 1 1 d . . . H44A H 0.6108 0.4925 0.9791 0.177 Uiso 1 1 calc R . . H44B H 0.6045 0.4789 1.0555 0.177 Uiso 1 1 calc R . . H44C H 0.5260 0.4598 0.9843 0.177 Uiso 1 1 calc R . . C76 C 0.3467(4) 0.61210(15) 0.7358(3) 0.0372(13) Uani 1 1 d . . . H76A H 0.3623 0.5870 0.7221 0.045 Uiso 1 1 calc R . . F751 F 0.5808(3) 0.62603(15) 0.8907(3) 0.1125(18) Uani 1 1 d . . . C161 C 0.4597(5) 0.45201(16) 0.7307(3) 0.0453(14) Uani 1 1 d . . . H16A H 0.4464 0.4255 0.7464 0.054 Uiso 1 1 calc R . . C12 C 0.7226(4) 0.41764(15) 0.6933(3) 0.0342(12) Uani 1 1 d . . . C52 C 0.9531(4) 0.23254(16) 0.9608(3) 0.0448(14) Uani 1 1 d . . . C23 C 0.5617(5) 0.2746(2) 0.9312(4) 0.0613(18) Uani 1 1 d . . . H23A H 0.5472 0.2781 0.9754 0.074 Uiso 1 1 calc R . . C44 C 0.6842(6) 0.4395(2) 1.0100(4) 0.069(2) Uani 1 1 d . . . C123 C 0.9067(5) 0.3859(2) 0.7041(4) 0.080(2) Uani 1 1 d . . . H12B H 0.9363 0.3982 0.7509 0.120 Uiso 1 1 calc R . . H12C H 0.9213 0.4022 0.6673 0.120 Uiso 1 1 calc R . . H12D H 0.9411 0.3606 0.7046 0.120 Uiso 1 1 calc R . . C222 C 0.3512(6) 0.3338(2) 0.8553(4) 0.080(2) Uani 1 1 d . . . H22A H 0.3368 0.3256 0.8056 0.120 Uiso 1 1 calc R . . H22B H 0.3134 0.3582 0.8567 0.120 Uiso 1 1 calc R . . H22C H 0.3249 0.3140 0.8817 0.120 Uiso 1 1 calc R . . C25 C 0.6310(5) 0.23497(16) 0.8550(4) 0.063(2) Uani 1 1 d . . . H25A H 0.6632 0.2113 0.8475 0.076 Uiso 1 1 calc R . . C751 C 0.5128(5) 0.6047(2) 0.8418(3) 0.0572(17) Uani 1 1 d . . . C221 C 0.4742(5) 0.33950(19) 0.8899(3) 0.0545(16) Uani 1 1 d . . . H22D H 0.4977 0.3612 0.8644 0.065 Uiso 1 1 calc R . . C53 C 0.9374(5) 0.19931(16) 0.9196(4) 0.0513(16) Uani 1 1 d . . . H53A H 0.9096 0.1769 0.9360 0.062 Uiso 1 1 calc R . . C54 C 0.9604(5) 0.19768(17) 0.8563(4) 0.0529(16) Uani 1 1 d . . . F852 F -0.2554(3) 0.58269(10) 0.7013(3) 0.0778(13) Uani 1 1 d . . . F931 F -0.1780(4) 0.66094(15) 0.3407(2) 0.1142(19) Uani 1 1 d . . . F831 F 0.0890(4) 0.46995(12) 0.7172(3) 0.1049(16) Uani 1 1 d . . . F832 F 0.1864(3) 0.49769(12) 0.8075(2) 0.0879(14) Uani 1 1 d . . . F951 F 0.2514(4) 0.72786(11) 0.4597(3) 0.0948(16) Uani 1 1 d . . . F952 F 0.2011(4) 0.75537(11) 0.5368(3) 0.0907(14) Uani 1 1 d . . . F833 F 0.0183(7) 0.4800(3) 0.7919(7) 0.065(4) Uani 0.67(4) 1 d P . . C94 C 0.0046(4) 0.68925(14) 0.4409(3) 0.0368(13) Uani 1 1 d . . . H94A H -0.0300 0.7056 0.4017 0.044 Uiso 1 1 calc R . . C86 C -0.0099(4) 0.60516(14) 0.6605(2) 0.0300(11) Uani 1 1 d . . . H86A H -0.0326 0.6291 0.6372 0.036 Uiso 1 1 calc R . . C72 C 0.2365(4) 0.66789(15) 0.7159(3) 0.0387(13) Uani 1 1 d . . . H72A H 0.1755 0.6822 0.6880 0.046 Uiso 1 1 calc R . . F851 F -0.2212(3) 0.62928(14) 0.6444(3) 0.1023(17) Uani 1 1 d . . . C85 C -0.0748(4) 0.58730(15) 0.6966(3) 0.0361(12) Uani 1 1 d . . . C35 C 1.1160(4) 0.31433(17) 1.0178(3) 0.0516(16) Uani 1 1 d . . . H35A H 1.1764 0.2987 1.0177 0.062 Uiso 1 1 calc R . . F953 F 0.0971(10) 0.7609(3) 0.4371(11) 0.081(5) Uani 0.73(5) 1 d P . . C26 C 0.6067(5) 0.26273(15) 0.8016(3) 0.0467(15) Uani 1 1 d . . . C831 C 0.0853(5) 0.4976(2) 0.7651(3) 0.0563(18) Uani 1 1 d . . . F732 F 0.1816(4) 0.73569(14) 0.7715(3) 0.141(3) Uani 1 1 d . . . C851 C -0.1779(5) 0.60647(17) 0.6992(3) 0.0469(15) Uani 1 1 d . . . F853 F -0.1625(3) 0.62847(17) 0.7553(3) 0.130(2) Uani 1 1 d . . . C84 C -0.0444(4) 0.55270(16) 0.7319(3) 0.0397(13) Uani 1 1 d . . . H84A H -0.0885 0.5408 0.7568 0.048 Uiso 1 1 calc R . . C46 C 0.8205(5) 0.39516(18) 1.0777(3) 0.0511(16) Uani 1 1 d . . . F731 F 0.2847(5) 0.72393(14) 0.8720(3) 0.123(2) Uani 1 1 d . . . C83 C 0.0516(4) 0.53577(16) 0.7300(3) 0.0378(13) Uani 1 1 d . . . C45 C 0.7405(6) 0.4220(2) 1.0728(4) 0.0660(19) Uani 1 1 d . . . H45A H 0.7233 0.4287 1.1150 0.079 Uiso 1 1 calc R . . C95 C 0.1054(4) 0.69860(14) 0.4876(3) 0.0349(12) Uani 1 1 d . . . C951 C 0.1611(5) 0.73472(18) 0.4759(4) 0.0536(16) Uani 1 1 d . . . C731 C 0.2778(6) 0.7223(2) 0.8045(4) 0.067(2) Uani 1 1 d . . . C931 C -0.1535(5) 0.64519(17) 0.4041(4) 0.0534(17) Uani 1 1 d . . . C162 C 0.3650(5) 0.46265(17) 0.6662(3) 0.0519(15) Uani 1 1 d . . . H16B H 0.3647 0.4458 0.6260 0.078 Uiso 1 1 calc R . . H16C H 0.3724 0.4896 0.6531 0.078 Uiso 1 1 calc R . . H16D H 0.2967 0.4594 0.6775 0.078 Uiso 1 1 calc R . . C561 C 1.0563(6) 0.30146(19) 0.8427(4) 0.071(2) Uani 1 1 d . . . H56A H 1.1246 0.3105 0.8765 0.106 Uiso 1 1 calc R . . H56B H 1.0010 0.3217 0.8356 0.106 Uiso 1 1 calc R . . H56C H 1.0680 0.2954 0.7969 0.106 Uiso 1 1 calc R . . F932 F -0.1689(5) 0.60948(14) 0.3920(4) 0.171(4) Uani 1 1 d . . . F733 F 0.3466(5) 0.74928(13) 0.7983(3) 0.129(2) Uani 1 1 d . . . F933 F -0.2309(4) 0.6562(3) 0.4277(3) 0.180(4) Uani 1 1 d . . . C56 C 1.0177(5) 0.26520(16) 0.8724(3) 0.0485(15) Uani 1 1 d . . . C541 C 0.9396(6) 0.16184(18) 0.8106(5) 0.077(2) Uani 1 1 d . . . H54A H 0.9178 0.1407 0.8364 0.115 Uiso 1 1 calc R . . H54B H 1.0061 0.1546 0.7995 0.115 Uiso 1 1 calc R . . H54C H 0.8813 0.1669 0.7660 0.115 Uiso 1 1 calc R . . C461 C 0.8752(5) 0.3759(2) 1.1475(3) 0.0624(18) Uani 1 1 d . . . H46A H 0.8369 0.3825 1.1820 0.094 Uiso 1 1 calc R . . H46B H 0.9509 0.3847 1.1656 0.094 Uiso 1 1 calc R . . H46C H 0.8738 0.3478 1.1406 0.094 Uiso 1 1 calc R . . C55 C 1.0030(5) 0.23104(18) 0.8336(4) 0.0592(18) Uani 1 1 d . . . H55A H 1.0223 0.2301 0.7906 0.071 Uiso 1 1 calc R . . C261 C 0.6291(7) 0.25712(19) 0.7317(4) 0.076(2) Uani 1 1 d . . . H26A H 0.5849 0.2767 0.6975 0.091 Uiso 1 1 calc R . . C223 C 0.4993(7) 0.3508(2) 0.9672(4) 0.091(3) Uani 1 1 d . . . H22E H 0.5774 0.3477 0.9914 0.137 Uiso 1 1 calc R . . H22F H 0.4583 0.3342 0.9902 0.137 Uiso 1 1 calc R . . H22G H 0.4785 0.3778 0.9704 0.137 Uiso 1 1 calc R . . C521 C 0.9297(6) 0.23159(19) 1.0314(4) 0.069(2) Uani 1 1 d . . . H52A H 0.8882 0.2547 1.0359 0.104 Uiso 1 1 calc R . . H52B H 0.9984 0.2311 1.0704 0.104 Uiso 1 1 calc R . . H52C H 0.8872 0.2084 1.0337 0.104 Uiso 1 1 calc R . . O999 O 0.1923(6) 0.4521(2) 0.0249(4) 0.136(2) Uani 1 1 d . . . C163 C 0.4634(6) 0.4806(2) 0.7927(4) 0.079(2) Uani 1 1 d . . . H16E H 0.5282 0.4753 0.8332 0.119 Uiso 1 1 calc R . . H16F H 0.3981 0.4772 0.8075 0.119 Uiso 1 1 calc R . . H16G H 0.4664 0.5071 0.7762 0.119 Uiso 1 1 calc R . . C122 C 0.7335(8) 0.3627(2) 0.6142(4) 0.095(3) Uani 1 1 d . . . H12E H 0.6559 0.3578 0.6060 0.143 Uiso 1 1 calc R . . H12F H 0.7705 0.3383 0.6115 0.143 Uiso 1 1 calc R . . H12G H 0.7426 0.3805 0.5776 0.143 Uiso 1 1 calc R . . C998 C 0.143(2) 0.4786(4) 0.0633(8) 0.282(15) Uani 1 1 d . . . H99C H 0.1375 0.5041 0.0399 0.338 Uiso 1 1 calc R . . H99J H 0.0674 0.4696 0.0564 0.338 Uiso 1 1 calc R . . C997 C 0.135(2) 0.4444(5) -0.0473(7) 0.277(13) Uani 1 1 d . . . H99K H 0.1177 0.4691 -0.0737 0.332 Uiso 1 1 calc R . . H99L H 0.0662 0.4312 -0.0503 0.332 Uiso 1 1 calc R . . C996 C 0.2024(17) 0.4190(4) -0.0826(10) 0.287(14) Uani 1 1 d . . . H99D H 0.1703 0.4201 -0.1346 0.430 Uiso 1 1 calc R . . H99E H 0.2021 0.3923 -0.0663 0.430 Uiso 1 1 calc R . . H99F H 0.2774 0.4286 -0.0693 0.430 Uiso 1 1 calc R . . C999 C 0.1850(14) 0.4834(5) 0.1265(8) 0.228(10) Uani 1 1 d . . . H99G H 0.1372 0.4991 0.1457 0.342 Uiso 1 1 calc R . . H99H H 0.2547 0.4967 0.1344 0.342 Uiso 1 1 calc R . . H99I H 0.1973 0.4583 0.1507 0.342 Uiso 1 1 calc R . . C262 C 0.7459(9) 0.2644(3) 0.7382(5) 0.132(4) Uani 1 1 d . . . H26B H 0.7714 0.2873 0.7678 0.198 Uiso 1 1 calc R . . H26C H 0.7533 0.2686 0.6906 0.198 Uiso 1 1 calc R . . H26D H 0.7896 0.2420 0.7604 0.198 Uiso 1 1 calc R . . C263 C 0.5935(13) 0.2175(3) 0.7000(6) 0.182(6) Uani 1 1 d . . . H26E H 0.6314 0.2112 0.6652 0.273 Uiso 1 1 calc R . . H26F H 0.5148 0.2175 0.6763 0.273 Uiso 1 1 calc R . . H26G H 0.6115 0.1981 0.7382 0.273 Uiso 1 1 calc R . . H1 H 0.816(4) 0.2852(16) 0.925(3) 0.046(15) Uiso 1 1 d . . . H2 H 0.772(5) 0.3126(17) 0.969(3) 0.07(2) Uiso 1 1 d . . . F954 F 0.131(3) 0.7432(19) 0.407(2) 0.092(19) Uani 0.27(5) 1 d P . . F834 F 0.053(5) 0.497(2) 0.822(3) 0.18(2) Uani 0.33(4) 1 d P . . C421 C 0.8041(5) 0.39059(16) 0.8819(3) 0.0476(15) Uani 1 1 d . . . H42A H 0.8818 0.3859 0.8872 0.057 Uiso 1 1 calc R . . H42B H 0.7752 0.4101 0.8440 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0285(4) 0.0386(4) 0.0289(4) 0.0031(3) 0.0041(3) 0.0028(3) C3 0.035(3) 0.036(3) 0.038(3) 0.001(2) -0.008(2) -0.006(2) F652 0.046(2) 0.0485(19) 0.051(2) -0.0152(15) -0.0009(17) -0.0155(15) C31 0.029(3) 0.038(3) 0.034(3) 0.002(2) -0.001(2) -0.004(2) N1 0.029(2) 0.026(2) 0.032(2) 0.0038(18) 0.0063(19) 0.0030(18) F651 0.0428(19) 0.0385(19) 0.120(3) -0.0436(19) 0.037(2) -0.0131(15) N2 0.034(2) 0.027(2) 0.034(2) 0.0057(18) -0.0018(19) -0.0026(19) C62 0.025(3) 0.020(2) 0.022(2) -0.0012(19) 0.003(2) -0.0043(19) C36 0.033(3) 0.039(3) 0.052(4) 0.002(3) 0.009(3) 0.004(3) C41 0.033(3) 0.044(3) 0.036(3) -0.008(3) 0.005(2) -0.005(2) C61 0.021(2) 0.021(2) 0.021(2) 0.0026(19) 0.0021(19) 0.0024(19) C66 0.019(2) 0.023(2) 0.021(2) 0.0011(19) 0.0025(19) -0.0007(19) C63 0.021(2) 0.021(2) 0.025(2) 0.0040(19) 0.005(2) 0.0035(19) N3 0.024(2) 0.040(3) 0.034(3) 0.001(2) 0.006(2) 0.0029(19) C33 0.042(4) 0.054(4) 0.047(4) -0.011(3) -0.001(3) -0.007(3) C651 0.028(3) 0.034(3) 0.045(3) -0.013(3) 0.012(3) 0.001(2) C64 0.025(3) 0.023(2) 0.028(3) 0.001(2) 0.011(2) 0.007(2) C51 0.027(3) 0.038(3) 0.056(4) 0.002(3) 0.011(3) 0.007(2) C65 0.022(2) 0.021(2) 0.027(3) 0.0005(19) 0.004(2) -0.0008(19) C21 0.034(3) 0.029(3) 0.040(3) 0.009(2) -0.008(2) -0.009(2) C32 0.038(3) 0.044(3) 0.037(3) -0.004(3) 0.007(3) -0.004(3) C2 0.035(3) 0.040(3) 0.031(3) 0.006(2) 0.000(2) 0.001(2) C11 0.028(3) 0.030(3) 0.027(3) 0.006(2) 0.003(2) 0.001(2) C34 0.031(3) 0.062(4) 0.075(5) -0.001(4) -0.004(3) 0.002(3) C1 0.028(3) 0.027(3) 0.035(3) 0.000(2) 0.008(2) 0.004(2) F633 0.053(2) 0.0308(19) 0.158(4) 0.003(2) 0.067(2) -0.0060(15) C93 0.034(3) 0.025(3) 0.038(3) 0.000(2) 0.004(2) 0.001(2) F653 0.059(2) 0.0317(17) 0.062(2) -0.0083(15) 0.0269(18) -0.0171(15) C91 0.024(3) 0.023(2) 0.029(3) -0.010(2) 0.009(2) 0.001(2) F632 0.0212(17) 0.123(3) 0.075(3) 0.047(2) 0.0057(17) 0.0023(19) C75 0.030(3) 0.061(4) 0.036(3) -0.010(3) 0.006(2) -0.003(3) F631 0.045(2) 0.112(3) 0.075(3) -0.041(2) 0.0407(19) -0.032(2) C92 0.032(3) 0.020(3) 0.037(3) -0.003(2) 0.007(2) -0.003(2) C71 0.023(3) 0.041(3) 0.028(3) -0.012(2) 0.009(2) -0.005(2) C82 0.028(3) 0.049(3) 0.023(3) -0.004(2) 0.007(2) 0.004(2) F753 0.054(3) 0.184(6) 0.158(5) 0.102(5) 0.004(3) 0.015(3) C96 0.020(3) 0.034(3) 0.041(3) -0.011(2) 0.007(2) 0.001(2) C81 0.025(3) 0.035(3) 0.021(2) -0.009(2) 0.002(2) -0.003(2) C631 0.023(3) 0.026(3) 0.035(3) -0.006(2) 0.009(2) -0.001(2) C22 0.036(3) 0.045(3) 0.054(4) 0.015(3) 0.006(3) -0.006(3) C73 0.041(3) 0.055(4) 0.044(3) -0.023(3) 0.011(3) -0.012(3) B1 0.022(3) 0.029(3) 0.026(3) -0.012(2) 0.004(2) -0.001(2) F752 0.082(3) 0.133(4) 0.059(3) 0.009(2) 0.012(2) 0.062(3) C16 0.037(3) 0.030(3) 0.035(3) 0.006(2) 0.006(2) 0.003(2) C15 0.058(4) 0.030(3) 0.050(4) 0.002(3) 0.005(3) 0.005(3) C14 0.048(4) 0.040(4) 0.057(4) 0.014(3) 0.003(3) -0.011(3) C42 0.040(3) 0.034(3) 0.050(4) -0.005(3) 0.006(3) -0.002(3) C13 0.035(3) 0.062(4) 0.040(3) 0.017(3) 0.006(3) 0.000(3) C24 0.064(5) 0.056(4) 0.074(5) 0.037(4) 0.004(4) -0.013(4) C74 0.040(3) 0.077(5) 0.033(3) -0.025(3) 0.003(3) -0.017(3) C121 0.051(4) 0.057(4) 0.037(3) 0.016(3) 0.018(3) 0.022(3) C43 0.070(4) 0.038(3) 0.059(4) -0.006(3) 0.005(3) 0.013(3) C441 0.125(8) 0.129(8) 0.097(7) -0.012(6) 0.027(6) 0.087(7) C76 0.028(3) 0.043(3) 0.038(3) -0.010(2) 0.005(2) -0.002(2) F751 0.053(3) 0.151(4) 0.097(3) -0.060(3) -0.031(2) 0.019(3) C161 0.046(3) 0.046(3) 0.047(3) 0.009(3) 0.019(3) 0.015(3) C12 0.029(3) 0.042(3) 0.029(3) 0.010(2) 0.006(2) 0.006(2) C52 0.035(3) 0.040(3) 0.054(4) 0.010(3) 0.007(3) 0.008(3) C23 0.051(4) 0.075(5) 0.056(4) 0.029(4) 0.013(3) 0.001(4) C44 0.073(5) 0.071(5) 0.059(5) -0.015(4) 0.014(4) 0.029(4) C123 0.057(5) 0.101(6) 0.096(6) 0.024(5) 0.042(4) 0.028(4) C222 0.056(5) 0.110(6) 0.077(5) 0.002(4) 0.023(4) 0.006(4) C25 0.062(4) 0.023(3) 0.086(5) 0.012(3) -0.004(4) 0.000(3) C751 0.032(3) 0.093(5) 0.036(3) -0.004(4) -0.005(3) -0.009(3) C221 0.045(4) 0.064(4) 0.055(4) 0.007(3) 0.016(3) -0.002(3) C53 0.040(3) 0.031(3) 0.080(5) 0.010(3) 0.013(3) 0.007(3) C54 0.036(3) 0.038(3) 0.085(5) -0.004(3) 0.020(3) 0.010(3) F852 0.040(2) 0.056(2) 0.150(4) 0.005(2) 0.047(2) 0.0015(18) F931 0.091(3) 0.145(4) 0.066(3) 0.046(3) -0.036(2) -0.051(3) F831 0.151(5) 0.051(3) 0.109(4) 0.029(3) 0.034(3) 0.012(3) F832 0.058(3) 0.087(3) 0.100(3) 0.038(2) -0.003(2) 0.016(2) F951 0.104(4) 0.056(2) 0.161(5) -0.027(3) 0.096(4) -0.035(2) F952 0.122(4) 0.057(2) 0.109(3) -0.027(2) 0.059(3) -0.049(2) F833 0.045(5) 0.062(5) 0.090(7) 0.036(4) 0.024(4) -0.008(4) C94 0.046(3) 0.026(3) 0.040(3) 0.001(2) 0.015(3) 0.006(2) C86 0.031(3) 0.029(3) 0.028(3) -0.009(2) 0.006(2) -0.001(2) C72 0.030(3) 0.045(3) 0.038(3) -0.010(3) 0.005(2) -0.005(2) F851 0.061(3) 0.121(4) 0.147(4) 0.070(3) 0.065(3) 0.050(3) C85 0.028(3) 0.045(3) 0.035(3) -0.013(3) 0.010(2) -0.003(2) C35 0.026(3) 0.045(4) 0.075(4) 0.000(3) 0.003(3) 0.003(3) F953 0.080(5) 0.028(4) 0.116(9) 0.029(5) 0.003(5) -0.014(4) C26 0.048(4) 0.028(3) 0.051(4) -0.001(3) -0.003(3) -0.002(3) C831 0.046(4) 0.083(5) 0.047(4) 0.024(4) 0.024(3) 0.028(4) F732 0.110(4) 0.100(4) 0.160(5) -0.099(4) -0.038(4) 0.044(3) C851 0.037(3) 0.044(3) 0.063(4) -0.013(3) 0.019(3) 0.000(3) F853 0.050(3) 0.179(5) 0.146(5) -0.121(4) 0.006(3) 0.025(3) C84 0.036(3) 0.055(4) 0.031(3) -0.001(3) 0.013(2) -0.001(3) C46 0.050(4) 0.057(4) 0.045(4) -0.017(3) 0.013(3) 0.004(3) F731 0.193(6) 0.106(4) 0.073(3) -0.043(3) 0.044(3) 0.034(4) C83 0.034(3) 0.051(3) 0.028(3) 0.004(2) 0.009(2) 0.001(3) C45 0.068(5) 0.075(5) 0.050(4) -0.014(3) 0.012(4) 0.021(4) C95 0.036(3) 0.026(3) 0.045(3) -0.007(2) 0.017(3) -0.005(2) C951 0.060(4) 0.046(4) 0.064(5) -0.003(3) 0.031(4) -0.010(3) C731 0.059(5) 0.061(5) 0.069(5) -0.039(4) 0.001(4) -0.008(4) C931 0.039(4) 0.041(4) 0.063(4) 0.017(3) -0.011(3) -0.008(3) C162 0.041(3) 0.058(4) 0.053(4) 0.011(3) 0.008(3) 0.006(3) C561 0.070(5) 0.068(5) 0.089(5) -0.002(4) 0.048(4) -0.010(4) F932 0.122(4) 0.071(3) 0.203(6) 0.031(3) -0.124(4) -0.047(3) F733 0.170(5) 0.063(3) 0.179(6) -0.061(3) 0.092(5) -0.031(3) F933 0.030(3) 0.385(11) 0.106(4) -0.109(5) -0.006(3) -0.014(4) C56 0.038(3) 0.038(3) 0.073(4) 0.000(3) 0.021(3) 0.002(3) C541 0.056(4) 0.049(4) 0.134(7) -0.025(4) 0.044(5) 0.000(3) C461 0.056(4) 0.085(5) 0.041(4) -0.011(3) 0.008(3) 0.008(4) C55 0.047(4) 0.057(4) 0.082(5) -0.015(4) 0.033(4) -0.002(3) C261 0.101(6) 0.056(4) 0.054(4) -0.010(3) -0.002(4) 0.042(4) C223 0.100(7) 0.113(7) 0.061(5) -0.003(5) 0.024(5) 0.013(5) C521 0.075(5) 0.060(4) 0.065(5) 0.017(3) 0.009(4) -0.005(4) O999 0.144(6) 0.165(7) 0.105(6) 0.002(5) 0.047(5) -0.020(5) C163 0.059(5) 0.117(6) 0.057(4) -0.014(4) 0.011(4) 0.039(4) C122 0.137(8) 0.081(5) 0.057(5) -0.005(4) 0.014(5) 0.068(5) C998 0.63(4) 0.136(12) 0.163(14) -0.088(11) 0.25(2) -0.170(18) C997 0.47(4) 0.212(18) 0.080(10) 0.053(11) -0.020(15) -0.06(2) C996 0.49(3) 0.162(13) 0.33(2) 0.163(15) 0.30(2) 0.248(19) C999 0.33(2) 0.237(17) 0.189(15) -0.108(14) 0.183(17) -0.186(17) C262 0.142(10) 0.197(11) 0.072(6) 0.004(7) 0.053(7) 0.063(9) C263 0.318(19) 0.078(7) 0.126(9) -0.059(7) 0.034(11) -0.038(9) F954 0.096(19) 0.08(3) 0.093(19) 0.044(18) 0.019(14) -0.048(19) F834 0.25(4) 0.21(4) 0.13(3) 0.15(3) 0.16(3) 0.18(3) C421 0.060(4) 0.047(3) 0.031(3) 0.009(3) 0.007(3) 0.032(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 C1 1.858(5) . ? Ni1 C421 1.866(6) . ? Ni1 N3 1.972(4) . ? C3 C2 1.349(7) . ? C3 N2 1.383(6) . ? F652 C651 1.338(6) . ? C31 C36 1.381(7) . ? C31 C32 1.394(7) . ? C31 N3 1.463(6) . ? N1 C1 1.366(6) . ? N1 C2 1.391(6) . ? N1 C11 1.439(6) . ? F651 C651 1.343(6) . ? N2 C1 1.355(6) . ? N2 C21 1.465(6) . ? C62 C63 1.389(6) . ? C62 C61 1.401(6) . ? C36 C35 1.387(8) . ? C36 C51 1.494(8) . ? C41 C42 1.390(7) . ? C41 C46 1.408(8) . ? C41 C32 1.481(8) . ? C61 C66 1.389(6) . ? C61 B1 1.638(7) . ? C66 C65 1.382(6) . ? C63 C64 1.379(6) . ? C63 C631 1.495(6) . ? C33 C34 1.384(8) . ? C33 C32 1.398(8) . ? C651 F653 1.334(6) . ? C651 C65 1.494(7) . ? C64 C65 1.386(6) . ? C51 C56 1.391(8) . ? C51 C52 1.407(8) . ? C21 C26 1.383(8) . ? C21 C22 1.418(8) . ? C11 C12 1.390(7) . ? C11 C16 1.406(7) . ? C34 C35 1.367(8) . ? F633 C631 1.313(5) . ? C93 C94 1.371(7) . ? C93 C92 1.403(7) . ? C93 C931 1.488(7) . ? C91 C96 1.381(7) . ? C91 C92 1.400(7) . ? C91 B1 1.648(7) . ? F632 C631 1.301(6) . ? C75 C74 1.378(8) . ? C75 C76 1.386(7) . ? C75 C751 1.516(8) . ? F631 C631 1.327(5) . ? C71 C76 1.395(7) . ? C71 C72 1.398(7) . ? C71 B1 1.631(7) . ? C82 C81 1.393(7) . ? C82 C83 1.394(7) . ? F753 C751 1.304(8) . ? C96 C95 1.391(7) . ? C81 C86 1.391(7) . ? C81 B1 1.643(7) . ? C22 C23 1.392(8) . ? C22 C221 1.511(8) . ? C73 C74 1.398(8) . ? C73 C72 1.398(7) . ? C73 C731 1.479(8) . ? F752 C751 1.299(7) . ? C16 C15 1.387(7) . ? C16 C161 1.529(7) . ? C15 C14 1.358(8) . ? C14 C13 1.356(8) . ? C42 C43 1.376(8) . ? C42 C421 1.473(8) . ? C13 C12 1.395(7) . ? C24 C25 1.375(10) . ? C24 C23 1.381(10) . ? C121 C122 1.516(9) . ? C121 C12 1.521(7) . ? C121 C123 1.548(9) . ? C43 C44 1.405(9) . ? C441 C44 1.526(9) . ? F751 C751 1.314(7) . ? C161 C162 1.514(8) . ? C161 C163 1.557(8) . ? C52 C53 1.385(8) . ? C52 C521 1.507(9) . ? C44 C45 1.369(9) . ? C222 C221 1.537(9) . ? C25 C26 1.388(8) . ? C221 C223 1.506(9) . ? C53 C54 1.366(9) . ? C54 C55 1.409(9) . ? C54 C541 1.508(9) . ? F852 C851 1.306(6) . ? F931 C931 1.308(7) . ? F831 C831 1.353(8) . ? F832 C831 1.318(7) . ? F951 C951 1.320(7) . ? F951 F954 1.67(4) . ? F952 C951 1.353(7) . ? F833 F834 0.86(9) . ? F833 C831 1.295(12) . ? C94 C95 1.383(7) . ? C86 C85 1.395(7) . ? F851 C851 1.315(7) . ? C85 C84 1.379(7) . ? C85 C851 1.502(7) . ? F953 F954 1.04(6) . ? F953 C951 1.304(10) . ? C26 C261 1.499(9) . ? C831 F834 1.31(2) . ? C831 C83 1.492(8) . ? F732 C731 1.299(8) . ? C851 F853 1.303(7) . ? C84 C83 1.382(7) . ? C46 C45 1.370(8) . ? C46 C461 1.494(8) . ? F731 C731 1.303(8) . ? C95 C951 1.495(8) . ? C951 F954 1.33(3) . ? C731 F733 1.320(8) . ? C931 F932 1.263(7) . ? C931 F933 1.281(8) . ? C561 C56 1.531(8) . ? C56 C55 1.389(8) . ? C261 C262 1.496(13) . ? C261 C263 1.520(11) . ? O999 C997 1.409(15) . ? O999 C998 1.455(17) . ? C998 C999 1.206(19) . ? C997 C996 1.54(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 C421 102.3(2) . . ? C1 Ni1 N3 159.8(2) . . ? C421 Ni1 N3 97.8(2) . . ? C2 C3 N2 105.3(4) . . ? C36 C31 C32 123.0(5) . . ? C36 C31 N3 119.9(5) . . ? C32 C31 N3 117.1(5) . . ? C1 N1 C2 110.5(4) . . ? C1 N1 C11 126.6(4) . . ? C2 N1 C11 122.9(4) . . ? C1 N2 C3 112.8(4) . . ? C1 N2 C21 117.3(4) . . ? C3 N2 C21 129.8(4) . . ? C63 C62 C61 122.8(4) . . ? C31 C36 C35 117.6(5) . . ? C31 C36 C51 121.2(5) . . ? C35 C36 C51 121.1(5) . . ? C42 C41 C46 120.6(5) . . ? C42 C41 C32 119.3(5) . . ? C46 C41 C32 120.1(5) . . ? C66 C61 C62 115.0(4) . . ? C66 C61 B1 122.3(4) . . ? C62 C61 B1 122.4(4) . . ? C65 C66 C61 122.8(4) . . ? C64 C63 C62 120.3(4) . . ? C64 C63 C631 119.1(4) . . ? C62 C63 C631 120.6(4) . . ? C31 N3 Ni1 121.5(3) . . ? C34 C33 C32 121.6(6) . . ? F653 C651 F652 105.1(4) . . ? F653 C651 F651 106.4(4) . . ? F652 C651 F651 106.1(4) . . ? F653 C651 C65 113.7(4) . . ? F652 C651 C65 112.0(4) . . ? F651 C651 C65 112.9(4) . . ? C63 C64 C65 118.2(4) . . ? C56 C51 C52 120.1(5) . . ? C56 C51 C36 119.4(5) . . ? C52 C51 C36 120.5(5) . . ? C66 C65 C64 120.8(4) . . ? C66 C65 C651 118.7(4) . . ? C64 C65 C651 120.5(4) . . ? C26 C21 C22 123.7(5) . . ? C26 C21 N2 119.1(5) . . ? C22 C21 N2 116.9(5) . . ? C31 C32 C33 116.7(5) . . ? C31 C32 C41 122.3(5) . . ? C33 C32 C41 120.8(5) . . ? C3 C2 N1 107.8(4) . . ? C12 C11 C16 122.9(4) . . ? C12 C11 N1 119.5(4) . . ? C16 C11 N1 117.6(4) . . ? C35 C34 C33 119.2(6) . . ? N2 C1 N1 103.6(4) . . ? N2 C1 Ni1 107.7(3) . . ? N1 C1 Ni1 148.5(4) . . ? C94 C93 C92 121.0(5) . . ? C94 C93 C931 119.6(5) . . ? C92 C93 C931 119.3(4) . . ? C96 C91 C92 115.2(4) . . ? C96 C91 B1 123.0(4) . . ? C92 C91 B1 121.4(4) . . ? C74 C75 C76 119.9(5) . . ? C74 C75 C751 120.7(5) . . ? C76 C75 C751 119.4(5) . . ? C91 C92 C93 121.8(4) . . ? C76 C71 C72 115.3(4) . . ? C76 C71 B1 121.3(4) . . ? C72 C71 B1 122.7(4) . . ? C81 C82 C83 122.6(5) . . ? C91 C96 C95 123.5(4) . . ? C86 C81 C82 116.2(5) . . ? C86 C81 B1 123.5(4) . . ? C82 C81 B1 120.1(4) . . ? F632 C631 F633 107.4(4) . . ? F632 C631 F631 104.7(4) . . ? F633 C631 F631 104.2(4) . . ? F632 C631 C63 113.1(4) . . ? F633 C631 C63 113.3(4) . . ? F631 C631 C63 113.4(4) . . ? C23 C22 C21 116.5(6) . . ? C23 C22 C221 121.6(6) . . ? C21 C22 C221 121.8(5) . . ? C74 C73 C72 119.4(5) . . ? C74 C73 C731 119.2(5) . . ? C72 C73 C731 121.4(6) . . ? C71 B1 C61 113.5(4) . . ? C71 B1 C81 102.9(4) . . ? C61 B1 C81 111.6(4) . . ? C71 B1 C91 113.4(4) . . ? C61 B1 C91 104.1(4) . . ? C81 B1 C91 111.7(4) . . ? C15 C16 C11 116.2(5) . . ? C15 C16 C161 120.2(5) . . ? C11 C16 C161 123.6(4) . . ? C14 C15 C16 121.8(5) . . ? C13 C14 C15 121.0(5) . . ? C43 C42 C41 119.9(6) . . ? C43 C42 C421 117.7(5) . . ? C41 C42 C421 122.2(5) . . ? C14 C13 C12 121.0(5) . . ? C25 C24 C23 120.7(6) . . ? C75 C74 C73 119.2(5) . . ? C122 C121 C12 110.0(5) . . ? C122 C121 C123 110.7(6) . . ? C12 C121 C123 113.6(5) . . ? C42 C43 C44 120.0(6) . . ? C75 C76 C71 123.3(5) . . ? C162 C161 C16 112.1(5) . . ? C162 C161 C163 109.0(5) . . ? C16 C161 C163 111.3(5) . . ? C11 C12 C13 117.0(5) . . ? C11 C12 C121 122.1(5) . . ? C13 C12 C121 120.8(5) . . ? C53 C52 C51 119.2(6) . . ? C53 C52 C521 119.0(5) . . ? C51 C52 C521 121.8(5) . . ? C24 C23 C22 120.7(7) . . ? C45 C44 C43 118.8(6) . . ? C45 C44 C441 121.7(6) . . ? C43 C44 C441 119.5(7) . . ? C24 C25 C26 121.7(6) . . ? F752 C751 F753 105.3(7) . . ? F752 C751 F751 107.4(5) . . ? F753 C751 F751 106.5(6) . . ? F752 C751 C75 112.6(5) . . ? F753 C751 C75 112.6(5) . . ? F751 C751 C75 112.0(6) . . ? C223 C221 C22 112.7(6) . . ? C223 C221 C222 110.7(6) . . ? C22 C221 C222 109.8(5) . . ? C54 C53 C52 122.2(6) . . ? C53 C54 C55 118.0(6) . . ? C53 C54 C541 121.9(6) . . ? C55 C54 C541 120.1(6) . . ? C951 F951 F954 51(2) . . ? F834 F833 C831 71(2) . . ? C93 C94 C95 118.2(5) . . ? C81 C86 C85 121.6(5) . . ? C73 C72 C71 122.7(5) . . ? C84 C85 C86 121.2(5) . . ? C84 C85 C851 119.0(5) . . ? C86 C85 C851 119.8(5) . . ? C34 C35 C36 121.9(5) . . ? F954 F953 C951 68.1(13) . . ? C21 C26 C25 116.6(6) . . ? C21 C26 C261 120.6(5) . . ? C25 C26 C261 122.8(6) . . ? F833 C831 F834 39(4) . . ? F833 C831 F832 113.5(7) . . ? F834 C831 F832 88(3) . . ? F833 C831 F831 96.8(8) . . ? F834 C831 F831 132(4) . . ? F832 C831 F831 101.7(5) . . ? F833 C831 C83 118.0(7) . . ? F834 C831 C83 106.4(17) . . ? F832 C831 C83 112.6(6) . . ? F831 C831 C83 111.9(5) . . ? F853 C851 F852 105.3(5) . . ? F853 C851 F851 105.0(6) . . ? F852 C851 F851 105.4(5) . . ? F853 C851 C85 112.2(5) . . ? F852 C851 C85 114.7(5) . . ? F851 C851 C85 113.4(5) . . ? C85 C84 C83 118.3(5) . . ? C45 C46 C41 117.6(6) . . ? C45 C46 C461 120.2(6) . . ? C41 C46 C461 122.3(5) . . ? C84 C83 C82 120.2(5) . . ? C84 C83 C831 120.0(5) . . ? C82 C83 C831 119.8(5) . . ? C44 C45 C46 123.1(6) . . ? C94 C95 C96 120.2(5) . . ? C94 C95 C951 119.6(5) . . ? C96 C95 C951 120.2(5) . . ? F953 C951 F951 115.6(12) . . ? F953 C951 F954 47(3) . . ? F951 C951 F954 78(3) . . ? F953 C951 F952 98.8(10) . . ? F951 C951 F952 100.5(5) . . ? F954 C951 F952 135(3) . . ? F953 C951 C95 114.9(6) . . ? F951 C951 C95 112.8(5) . . ? F954 C951 C95 109.8(16) . . ? F952 C951 C95 112.3(5) . . ? F732 C731 F731 104.5(7) . . ? F732 C731 F733 105.6(7) . . ? F731 C731 F733 103.0(6) . . ? F732 C731 C73 115.0(5) . . ? F731 C731 C73 114.7(7) . . ? F733 C731 C73 112.8(6) . . ? F932 C931 F933 105.3(7) . . ? F932 C931 F931 104.5(6) . . ? F933 C931 F931 103.5(6) . . ? F932 C931 C93 115.2(5) . . ? F933 C931 C93 112.8(6) . . ? F931 C931 C93 114.4(5) . . ? C55 C56 C51 118.9(5) . . ? C55 C56 C561 119.6(6) . . ? C51 C56 C561 121.5(5) . . ? C56 C55 C54 121.6(6) . . ? C262 C261 C26 111.8(6) . . ? C262 C261 C263 110.9(8) . . ? C26 C261 C263 111.9(8) . . ? C997 O999 C998 117.7(15) . . ? C999 C998 O999 119(2) . . ? O999 C997 C996 111.7(19) . . ? F953 F954 C951 65(3) . . ? F953 F954 F951 107(3) . . ? C951 F954 F951 50.6(12) . . ? F833 F834 C831 70(3) . . ? C42 C421 Ni1 102.4(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.193 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.088 data_8 _database_code_depnum_ccdc_archive 'CCDC 896904' #TrackingRef 'CIF(1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C197 H204 B2 F48 N6 Ni2 O4' _chemical_formula_weight 3770.70 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' B B 0.0013 0.0007 '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' 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 14.7621(15) _cell_length_b 16.7885(17) _cell_length_c 21.465(2) _cell_angle_alpha 102.291(2) _cell_angle_beta 106.901(2) _cell_angle_gamma 105.812(2) _cell_volume 4644.3(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1958 _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8372 _exptl_absorpt_correction_T_max 0.9411 _exptl_absorpt_process_details 'Norton et. al.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45508 _diffrn_reflns_av_R_equivalents 0.1008 _diffrn_reflns_av_sigmaI/netI 0.0927 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16317 _reflns_number_gt 11500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0860P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16317 _refine_ls_number_parameters 1229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1626 _refine_ls_wR_factor_gt 0.1540 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.007 _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 0.84154(3) 0.70967(2) 0.707688(17) 0.02004(12) Uani 1 1 d . . . C13 C 0.9943(2) 0.9835(2) 0.89331(16) 0.0297(7) Uani 1 1 d . . . H13A H 1.0095 1.0365 0.8826 0.036 Uiso 1 1 calc R . . C11 C 0.8861(2) 0.83713(18) 0.86836(14) 0.0237(6) Uani 1 1 d . . . C12 C 0.9038(2) 0.91449(18) 0.85122(15) 0.0251(7) Uani 1 1 d . . . C121 C 0.8302(2) 0.9267(2) 0.79159(16) 0.0312(7) Uani 1 1 d . . . H12A H 0.7767 0.8684 0.7629 0.037 Uiso 1 1 calc R . . C122 C 0.8826(3) 0.9624(2) 0.74688(17) 0.0412(8) Uani 1 1 d . . . H12B H 0.9117 0.9214 0.7284 0.062 Uiso 1 1 calc R . . H12C H 0.9367 1.0189 0.7744 0.062 Uiso 1 1 calc R . . H12D H 0.8332 0.9700 0.7089 0.062 Uiso 1 1 calc R . . C16 C 0.9529(2) 0.82799(19) 0.92552(15) 0.0266(7) Uani 1 1 d . . . C15 C 1.0413(2) 0.8999(2) 0.96569(15) 0.0289(7) Uani 1 1 d . . . H15A H 1.0884 0.8959 1.0048 0.035 Uiso 1 1 calc R . . N3 N 0.92086(19) 0.72188(18) 0.64668(12) 0.0242(6) Uani 1 1 d . . . N2 N 0.67542(17) 0.64402(15) 0.75718(12) 0.0234(5) Uani 1 1 d . . . N1 N 0.79096(17) 0.76457(15) 0.82827(12) 0.0231(5) Uani 1 1 d . . . C21 C 0.6215(2) 0.55953(18) 0.70470(15) 0.0239(6) Uani 1 1 d . . . C3 C 0.6437(2) 0.6693(2) 0.81000(15) 0.0317(7) Uani 1 1 d . . . H3A H 0.5826 0.6388 0.8144 0.038 Uiso 1 1 calc R . . C1 C 0.7673(2) 0.70352(18) 0.76681(14) 0.0207(6) Uani 1 1 d . . . C31 C 0.8820(2) 0.67985(18) 0.57278(14) 0.0236(7) Uani 1 1 d . . . C32 C 0.8171(2) 0.70868(18) 0.52924(14) 0.0250(7) Uani 1 1 d . . . C41 C 0.7737(2) 0.77342(19) 0.55567(15) 0.0268(7) Uani 1 1 d . . . C42 C 0.7237(2) 0.75755(19) 0.60074(14) 0.0255(7) Uani 1 1 d . . . C421 C 0.7206(2) 0.6838(2) 0.62927(15) 0.0232(6) Uani 1 1 d . . . C46 C 0.7724(2) 0.8441(2) 0.53045(16) 0.0342(8) Uani 1 1 d . . . C45 C 0.7193(3) 0.8954(2) 0.54963(16) 0.0391(8) Uani 1 1 d . . . H45A H 0.7194 0.9436 0.5331 0.047 Uiso 1 1 calc R . . C61 C 0.4672(2) 0.21295(19) 0.83968(14) 0.0264(7) Uani 1 1 d . . . O1 O 0.97905(14) 0.73612(12) 0.78309(10) 0.0263(5) Uani 1 1 d . . . C71 C 0.6302(2) 0.20791(18) 0.80739(15) 0.0261(7) Uani 1 1 d . . . C81 C 0.6386(2) 0.27389(18) 0.94044(15) 0.0247(7) Uani 1 1 d . . . C91 C 0.5627(2) 0.10052(18) 0.86812(15) 0.0253(7) Uani 1 1 d . . . B1 B 0.5773(3) 0.2002(2) 0.86445(17) 0.0265(8) Uani 1 1 d . . . C2 C 0.7147(2) 0.7447(2) 0.85385(16) 0.0327(7) Uani 1 1 d . . . H2A H 0.7131 0.7783 0.8949 0.039 Uiso 1 1 calc R . . C96 C 0.6086(2) 0.08115(19) 0.92649(16) 0.0267(7) Uani 1 1 d . . . H96A H 0.6496 0.1276 0.9680 0.032 Uiso 1 1 calc R . . C94 C 0.5390(2) -0.0736(2) 0.86622(16) 0.0309(7) Uani 1 1 d . . . H94A H 0.5308 -0.1319 0.8656 0.037 Uiso 1 1 calc R . . C92 C 0.5045(2) 0.02895(19) 0.80867(16) 0.0282(7) Uani 1 1 d . . . H92A H 0.4712 0.0391 0.7677 0.034 Uiso 1 1 calc R . . C95 C 0.5963(2) -0.00479(19) 0.92580(16) 0.0268(7) Uani 1 1 d . . . C93 C 0.4936(2) -0.05584(19) 0.80723(16) 0.0302(7) Uani 1 1 d . . . C66 C 0.3823(2) 0.16420(19) 0.84877(15) 0.0278(7) Uani 1 1 d . . . H66A H 0.3843 0.1157 0.8645 0.033 Uiso 1 1 calc R . . C63 C 0.3708(2) 0.3008(2) 0.79902(15) 0.0330(8) Uani 1 1 d . . . C62 C 0.4585(2) 0.2821(2) 0.81421(15) 0.0313(7) Uani 1 1 d . . . H62A H 0.5148 0.3172 0.8073 0.038 Uiso 1 1 calc R . . C64 C 0.2877(2) 0.2524(2) 0.80990(15) 0.0344(8) Uani 1 1 d . . . H64A H 0.2276 0.2657 0.8000 0.041 Uiso 1 1 calc R . . C65 C 0.2944(2) 0.1841(2) 0.83556(15) 0.0321(7) Uani 1 1 d . . . C72 C 0.7336(2) 0.22283(19) 0.82215(16) 0.0286(7) Uani 1 1 d . . . H72A H 0.7767 0.2354 0.8683 0.034 Uiso 1 1 calc R . . C76 C 0.5715(2) 0.18816(19) 0.73835(16) 0.0336(8) Uani 1 1 d . . . H76A H 0.5012 0.1782 0.7259 0.040 Uiso 1 1 calc R . . C75 C 0.6112(3) 0.1823(2) 0.68690(16) 0.0374(8) Uani 1 1 d . . . C73 C 0.7751(2) 0.2199(2) 0.77163(17) 0.0338(8) Uani 1 1 d . . . C74 C 0.7135(3) 0.1991(2) 0.70308(17) 0.0391(8) Uani 1 1 d . . . H74A H 0.7413 0.1964 0.6683 0.047 Uiso 1 1 calc R . . C84 C 0.7216(2) 0.40253(19) 1.07220(16) 0.0311(7) Uani 1 1 d . . . H84A H 0.7491 0.4456 1.1161 0.037 Uiso 1 1 calc R . . C85 C 0.7656(2) 0.41114(19) 1.02425(15) 0.0297(7) Uani 1 1 d . . . C86 C 0.7246(2) 0.34842(19) 0.95921(15) 0.0268(7) Uani 1 1 d . . . H86A H 0.7559 0.3566 0.9270 0.032 Uiso 1 1 calc R . . C82 C 0.5969(2) 0.26695(18) 0.99097(15) 0.0264(7) Uani 1 1 d . . . H82A H 0.5391 0.2170 0.9808 0.032 Uiso 1 1 calc R . . C83 C 0.6360(2) 0.32917(19) 1.05472(15) 0.0287(7) Uani 1 1 d . . . C651 C 0.2092(3) 0.1330(2) 0.85217(18) 0.0421(9) Uani 1 1 d . . . C831 C 0.5888(3) 0.3163(2) 1.10641(17) 0.0404(8) Uani 1 1 d . . . C851 C 0.8599(3) 0.4886(2) 1.04399(17) 0.0392(8) Uani 1 1 d . . . C731 C 0.8861(3) 0.2393(3) 0.7905(2) 0.0458(9) Uani 1 1 d . . . C751 C 0.5419(3) 0.1567(3) 0.6146(2) 0.0564(11) Uani 1 1 d . . . F652 F 0.18525(18) 0.04701(14) 0.82766(14) 0.0717(7) Uani 1 1 d . . . F651 F 0.23182(16) 0.15050(17) 0.91919(11) 0.0658(7) Uani 1 1 d . . . F653 F 0.12427(15) 0.14913(17) 0.82844(12) 0.0685(7) Uani 1 1 d . . . F851 F 0.93943(15) 0.48313(14) 1.08905(12) 0.0637(6) Uani 1 1 d . . . F852 F 0.8862(2) 0.50114(18) 0.99281(12) 0.1063(12) Uani 1 1 d . . . F831 F 0.62781(17) 0.27291(19) 1.14478(12) 0.0787(8) Uani 1 1 d . . . F732 F 0.92933(18) 0.30181(17) 0.76863(16) 0.0859(9) Uani 1 1 d . . . F731 F 0.9349(5) 0.2437(14) 0.8512(5) 0.117(5) Uani 0.73(3) 1 d P . . F951 F 0.68365(15) -0.08604(12) 0.97723(11) 0.0520(6) Uani 1 1 d . . . C951 C 0.6435(2) -0.0242(2) 0.98951(18) 0.0366(8) Uani 1 1 d . . . C44 C 0.6663(3) 0.8789(2) 0.59178(16) 0.0376(8) Uani 1 1 d . . . C43 C 0.6703(2) 0.8105(2) 0.61718(15) 0.0299(7) Uani 1 1 d . . . H43A H 0.6353 0.7991 0.6470 0.036 Uiso 1 1 calc R . . C34 C 0.8220(2) 0.6079(2) 0.43230(16) 0.0325(7) Uani 1 1 d . . . H34A H 0.8039 0.5853 0.3841 0.039 Uiso 1 1 calc R . . C35 C 0.8821(2) 0.5777(2) 0.47608(15) 0.0320(7) Uani 1 1 d . . . H35A H 0.9037 0.5328 0.4577 0.038 Uiso 1 1 calc R . . C33 C 0.7880(2) 0.67114(19) 0.45898(15) 0.0293(7) Uani 1 1 d . . . H33A H 0.7435 0.6895 0.4284 0.035 Uiso 1 1 calc R . . C36 C 0.9118(2) 0.61180(19) 0.54677(15) 0.0283(7) Uani 1 1 d . . . C51 C 0.9703(2) 0.5737(2) 0.59345(15) 0.0299(7) Uani 1 1 d . . . C54 C 1.0769(3) 0.5022(2) 0.68269(16) 0.0397(9) Uani 1 1 d . . . C52 C 0.9181(2) 0.4985(2) 0.60523(15) 0.0318(8) Uani 1 1 d . . . C53 C 0.9722(2) 0.4637(2) 0.64927(16) 0.0367(8) Uani 1 1 d . . . H53A H 0.9369 0.4125 0.6568 0.044 Uiso 1 1 calc R . . C55 C 1.1276(3) 0.5751(2) 0.66933(16) 0.0407(9) Uani 1 1 d . . . H55A H 1.1991 0.6017 0.6918 0.049 Uiso 1 1 calc R . . C56 C 1.0765(2) 0.6104(2) 0.62393(15) 0.0340(8) Uani 1 1 d . . . C521 C 0.8041(2) 0.4560(2) 0.57136(18) 0.0421(9) Uani 1 1 d . . . H52A H 0.7815 0.4026 0.5831 0.063 Uiso 1 1 calc R . . H52B H 0.7841 0.4415 0.5214 0.063 Uiso 1 1 calc R . . H52C H 0.7727 0.4964 0.5876 0.063 Uiso 1 1 calc R . . C541 C 1.1321(3) 0.4652(3) 0.73359(17) 0.0528(11) Uani 1 1 d . . . H54A H 1.2047 0.5001 0.7530 0.079 Uiso 1 1 calc R . . H54B H 1.1217 0.4047 0.7102 0.079 Uiso 1 1 calc R . . H54C H 1.1055 0.4668 0.7705 0.079 Uiso 1 1 calc R . . C161 C 0.9318(2) 0.7458(2) 0.94683(16) 0.0325(7) Uani 1 1 d . . . H16A H 0.8768 0.6970 0.9069 0.039 Uiso 1 1 calc R . . C162 C 1.0239(3) 0.7188(2) 0.96802(17) 0.0409(9) Uani 1 1 d . . . H16B H 1.0521 0.7151 0.9319 0.061 Uiso 1 1 calc R . . H16C H 1.0034 0.6617 0.9749 0.061 Uiso 1 1 calc R . . H16D H 1.0753 0.7622 1.0109 0.061 Uiso 1 1 calc R . . C123 C 0.7785(3) 0.9872(3) 0.8183(2) 0.0569(11) Uani 1 1 d . . . H12E H 0.7424 0.9615 0.8452 0.085 Uiso 1 1 calc R . . H12F H 0.7303 0.9941 0.7794 0.085 Uiso 1 1 calc R . . H12G H 0.8299 1.0443 0.8475 0.085 Uiso 1 1 calc R . . C23 C 0.4795(2) 0.4637(2) 0.60461(16) 0.0329(7) Uani 1 1 d . . . H23A H 0.4175 0.4526 0.5687 0.039 Uiso 1 1 calc R . . C25 C 0.6063(2) 0.4120(2) 0.66067(17) 0.0380(8) Uani 1 1 d . . . H25A H 0.6310 0.3656 0.6629 0.046 Uiso 1 1 calc R . . C26 C 0.6603(2) 0.49352(19) 0.71116(16) 0.0292(7) Uani 1 1 d . . . C24 C 0.5179(2) 0.3977(2) 0.60768(17) 0.0375(8) Uani 1 1 d . . . H24A H 0.4833 0.3422 0.5732 0.045 Uiso 1 1 calc R . . C22 C 0.5299(2) 0.54569(19) 0.65301(15) 0.0271(7) Uani 1 1 d . . . C261 C 0.7521(2) 0.5056(2) 0.77215(16) 0.0344(8) Uani 1 1 d . . . H26A H 0.7942 0.5692 0.7917 0.041 Uiso 1 1 calc R . . C221 C 0.4839(2) 0.6166(2) 0.64970(17) 0.0331(8) Uani 1 1 d . . . H22A H 0.5374 0.6739 0.6806 0.040 Uiso 1 1 calc R . . C222 C 0.3964(2) 0.5991(2) 0.6761(2) 0.0497(10) Uani 1 1 d . . . H22B H 0.4215 0.5971 0.7230 0.075 Uiso 1 1 calc R . . H22C H 0.3429 0.5432 0.6463 0.075 Uiso 1 1 calc R . . H22D H 0.3688 0.6460 0.6756 0.075 Uiso 1 1 calc R . . C314 C 1.1530(2) 0.7871(2) 0.79968(16) 0.0366(8) Uani 1 1 d . . . H31A H 1.2194 0.8323 0.8308 0.044 Uiso 1 1 calc R . . H31B H 1.1522 0.7720 0.7523 0.044 Uiso 1 1 calc R . . C313 C 1.1311(2) 0.7069(2) 0.82299(16) 0.0378(8) Uani 1 1 d . . . H31C H 1.1544 0.7234 0.8737 0.045 Uiso 1 1 calc R . . H31D H 1.1639 0.6672 0.8064 0.045 Uiso 1 1 calc R . . C312 C 1.0161(2) 0.6650(2) 0.78987(16) 0.0320(7) Uani 1 1 d . . . H31E H 0.9955 0.6218 0.7443 0.038 Uiso 1 1 calc R . . H31F H 0.9887 0.6350 0.8190 0.038 Uiso 1 1 calc R . . C315 C 1.0663(2) 0.8173(2) 0.80341(16) 0.0318(7) Uani 1 1 d . . . H31G H 1.0819 0.8540 0.8506 0.038 Uiso 1 1 calc R . . H31H H 1.0525 0.8511 0.7716 0.038 Uiso 1 1 calc R . . C14 C 1.0620(2) 0.9771(2) 0.94988(15) 0.0289(7) Uani 1 1 d . . . H14A H 1.1226 1.0253 0.9779 0.035 Uiso 1 1 calc R . . C631 C 0.3634(3) 0.3737(3) 0.7699(2) 0.0488(10) Uani 1 1 d . . . C931 C 0.4346(3) -0.1304(2) 0.74229(18) 0.0399(8) Uani 1 1 d . . . F932 F 0.3950(2) -0.10701(13) 0.68849(10) 0.0693(7) Uani 1 1 d . . . F933 F 0.35750(16) -0.19035(13) 0.74687(10) 0.0573(6) Uani 1 1 d . . . F931 F 0.49092(18) -0.17434(15) 0.72439(13) 0.0749(7) Uani 1 1 d . . . F953 F 0.71870(15) 0.04527(12) 1.03859(9) 0.0468(5) Uani 1 1 d . . . F952 F 0.57626(16) -0.05546(15) 1.01655(11) 0.0611(6) Uani 1 1 d . . . F631 F 0.3239(2) 0.42439(15) 0.80208(13) 0.0733(7) Uani 1 1 d . . . F632 F 0.45216(19) 0.42797(17) 0.77617(15) 0.0846(9) Uani 1 1 d . . . F633 F 0.3026(2) 0.34504(17) 0.70583(12) 0.0897(9) Uani 1 1 d . . . F833 F 0.49003(15) 0.27059(14) 1.07936(10) 0.0523(5) Uani 1 1 d . . . F832 F 0.5993(2) 0.39074(15) 1.14958(13) 0.0908(10) Uani 1 1 d . . . F853 F 0.85325(18) 0.56242(14) 1.07567(16) 0.0900(9) Uani 1 1 d . . . F733 F 0.9068(2) 0.17439(18) 0.7587(2) 0.1150(12) Uani 1 1 d . . . F752 F 0.4716(2) 0.19186(16) 0.60618(11) 0.0824(9) Uani 1 1 d . . . F753 F 0.4869(3) 0.07406(18) 0.58898(15) 0.1457(19) Uani 1 1 d . . . F751 F 0.5812(5) 0.1306(16) 0.5699(3) 0.094(7) Uani 0.395(18) 1 d P . . C561 C 1.1341(3) 0.6854(2) 0.60529(18) 0.0474(10) Uani 1 1 d . . . H56A H 1.2051 0.7102 0.6370 0.071 Uiso 1 1 calc R . . H56B H 1.1037 0.7304 0.6086 0.071 Uiso 1 1 calc R . . H56C H 1.1309 0.6639 0.5582 0.071 Uiso 1 1 calc R . . C461 C 0.8262(3) 0.8669(2) 0.48290(18) 0.0494(10) Uani 1 1 d . . . H46A H 0.8527 0.9304 0.4934 0.074 Uiso 1 1 calc R . . H46B H 0.7784 0.8399 0.4352 0.074 Uiso 1 1 calc R . . H46C H 0.8824 0.8451 0.4893 0.074 Uiso 1 1 calc R . . C223 C 0.4467(3) 0.6227(2) 0.57685(18) 0.0480(10) Uani 1 1 d . . . H22E H 0.5021 0.6303 0.5596 0.072 Uiso 1 1 calc R . . H22F H 0.4245 0.6727 0.5778 0.072 Uiso 1 1 calc R . . H22G H 0.3898 0.5690 0.5466 0.072 Uiso 1 1 calc R . . C441 C 0.6090(3) 0.9355(3) 0.6108(2) 0.0543(11) Uani 1 1 d . . . H44A H 0.5629 0.9064 0.6306 0.081 Uiso 1 1 calc R . . H44B H 0.5699 0.9455 0.5696 0.081 Uiso 1 1 calc R . . H44C H 0.6570 0.9917 0.6445 0.081 Uiso 1 1 calc R . . C163 C 0.8946(3) 0.7592(2) 1.00663(18) 0.0446(9) Uani 1 1 d . . . H16E H 0.8764 0.7047 1.0176 0.067 Uiso 1 1 calc R . . H16F H 0.8350 0.7762 0.9935 0.067 Uiso 1 1 calc R . . H16G H 0.9486 0.8053 1.0469 0.067 Uiso 1 1 calc R . . C263 C 0.8186(3) 0.4571(2) 0.7548(2) 0.0617(12) Uani 1 1 d . . . H26B H 0.8383 0.4731 0.7180 0.093 Uiso 1 1 calc R . . H26C H 0.7812 0.3941 0.7395 0.093 Uiso 1 1 calc R . . H26D H 0.8796 0.4726 0.7955 0.093 Uiso 1 1 calc R . . C262 C 0.7171(3) 0.4783(4) 0.8274(2) 0.0870(17) Uani 1 1 d . . . H26E H 0.7760 0.4961 0.8700 0.130 Uiso 1 1 calc R . . H26F H 0.6830 0.4148 0.8119 0.130 Uiso 1 1 calc R . . H26G H 0.6700 0.5067 0.8358 0.130 Uiso 1 1 calc R . . O999 O 0.0712(2) 0.89968(18) 0.66973(16) 0.0735(9) Uani 1 1 d . . . C998 C 0.2099(4) 1.0034(3) 0.6624(2) 0.0748(14) Uani 1 1 d . . . H99A H 0.2480 1.0578 0.7018 0.090 Uiso 1 1 calc R . . H99B H 0.2518 0.9960 0.6346 0.090 Uiso 1 1 calc R . . C999 C 0.1789(4) 0.9257(3) 0.6859(3) 0.0794(14) Uani 1 1 d . . . H99C H 0.1953 0.8774 0.6620 0.095 Uiso 1 1 calc R . . H99D H 0.2153 0.9412 0.7360 0.095 Uiso 1 1 calc R . . C996 C 0.0392(4) 0.9634(4) 0.6479(3) 0.0843(15) Uani 1 1 d . . . H99E H 0.0388 1.0070 0.6869 0.101 Uiso 1 1 calc R . . H99F H -0.0301 0.9366 0.6122 0.101 Uiso 1 1 calc R . . C886 C 0.9392(6) 0.1445(5) 0.5988(4) 0.136(3) Uani 1 1 d . . . H88A H 0.9466 0.1001 0.5639 0.164 Uiso 1 1 calc R . . H88B H 0.9034 0.1145 0.6246 0.164 Uiso 1 1 calc R . . C887 C 0.8839(7) 0.1930(5) 0.5665(4) 0.141(3) Uani 1 1 d . . . H88C H 0.8818 0.2395 0.6026 0.169 Uiso 1 1 calc R . . H88D H 0.9207 0.2216 0.5407 0.169 Uiso 1 1 calc R . . C997 C 0.1107(5) 1.0041(5) 0.6202(4) 0.133(3) Uani 1 1 d . . . H99G H 0.1140 1.0647 0.6237 0.160 Uiso 1 1 calc R . . H99H H 0.0910 0.9709 0.5714 0.160 Uiso 1 1 calc R . . C888 C 0.7841(6) 0.1408(6) 0.5215(4) 0.141(3) Uani 1 1 d . . . H88E H 0.7489 0.1118 0.5479 0.169 Uiso 1 1 calc R . . H88F H 0.7876 0.0944 0.4861 0.169 Uiso 1 1 calc R . . C885 C 1.0392(7) 0.2090(5) 0.6458(5) 0.200(5) Uani 1 1 d . . . H88G H 1.0796 0.1797 0.6701 0.300 Uiso 1 1 calc R . . H88H H 1.0305 0.2533 0.6791 0.300 Uiso 1 1 calc R . . H88I H 1.0742 0.2371 0.6194 0.300 Uiso 1 1 calc R . . C889 C 0.7202(8) 0.1844(6) 0.4858(4) 0.176(4) Uani 1 1 d . . . H88J H 0.6495 0.1442 0.4641 0.263 Uiso 1 1 calc R . . H88K H 0.7439 0.2008 0.4506 0.263 Uiso 1 1 calc R . . H88L H 0.7249 0.2368 0.5191 0.263 Uiso 1 1 calc R . . C777 C 0.5000 0.5000 1.0000 0.111(3) Uani 1 2 d S . . C779 C 0.6433(5) 0.5965(6) 0.9782(4) 0.139(3) Uani 1 1 d . . . C778 C 0.5789(7) 0.5705(6) 1.0174(5) 0.069(4) Uani 0.542(14) 1 d P . . C776 C 0.5623(7) 0.5230(7) 0.9617(5) 0.059(4) Uani 0.458(14) 1 d P . . H1 H 0.945(3) 0.778(2) 0.6554(17) 0.041(10) Uiso 1 1 d . . . H3 H 0.664(2) 0.6699(18) 0.6431(14) 0.026(8) Uiso 1 1 d . . . H4 H 0.725(2) 0.6310(18) 0.5994(14) 0.019(7) Uiso 1 1 d . . . H2 H 0.970(2) 0.7041(18) 0.6666(14) 0.023(8) Uiso 1 1 d . . . F734 F 0.9368(11) 0.3024(15) 0.8521(12) 0.074(8) Uani 0.27(3) 1 d P . . F754 F 0.5856(4) 0.2034(7) 0.5779(3) 0.079(3) Uani 0.605(18) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0178(2) 0.0223(2) 0.0194(2) 0.00503(16) 0.00676(16) 0.00766(16) C13 0.0350(18) 0.0241(17) 0.0354(18) 0.0078(14) 0.0231(16) 0.0092(14) C11 0.0228(16) 0.0233(16) 0.0230(15) 0.0015(13) 0.0116(13) 0.0063(13) C12 0.0271(17) 0.0229(16) 0.0265(16) 0.0047(13) 0.0147(14) 0.0081(13) C121 0.0301(18) 0.0271(17) 0.0324(18) 0.0092(14) 0.0091(15) 0.0070(14) C122 0.044(2) 0.042(2) 0.038(2) 0.0197(17) 0.0148(17) 0.0116(17) C16 0.0297(17) 0.0247(16) 0.0266(16) 0.0032(13) 0.0161(14) 0.0090(14) C15 0.0267(17) 0.0352(18) 0.0219(16) 0.0026(14) 0.0095(13) 0.0112(15) N3 0.0209(14) 0.0264(16) 0.0210(13) 0.0022(12) 0.0068(11) 0.0069(13) N2 0.0203(13) 0.0249(13) 0.0245(13) 0.0081(11) 0.0100(11) 0.0055(11) N1 0.0223(13) 0.0224(13) 0.0241(13) 0.0054(11) 0.0124(11) 0.0046(11) C21 0.0205(16) 0.0222(16) 0.0259(16) 0.0058(13) 0.0096(13) 0.0033(13) C3 0.0255(17) 0.0369(19) 0.0297(17) 0.0061(15) 0.0164(14) 0.0032(15) C1 0.0191(15) 0.0204(15) 0.0218(15) 0.0083(13) 0.0048(12) 0.0077(13) C31 0.0188(15) 0.0250(16) 0.0201(15) -0.0006(13) 0.0076(13) 0.0030(13) C32 0.0264(16) 0.0220(16) 0.0222(15) 0.0041(13) 0.0109(13) 0.0027(13) C41 0.0268(17) 0.0273(17) 0.0236(16) 0.0069(13) 0.0065(13) 0.0095(14) C42 0.0221(16) 0.0289(17) 0.0217(15) 0.0077(13) 0.0043(13) 0.0080(14) C421 0.0207(16) 0.0276(17) 0.0231(16) 0.0101(14) 0.0088(13) 0.0089(14) C46 0.041(2) 0.0312(18) 0.0267(17) 0.0109(15) 0.0100(15) 0.0085(16) C45 0.054(2) 0.0302(19) 0.0322(19) 0.0119(15) 0.0079(17) 0.0205(17) C61 0.0269(17) 0.0235(16) 0.0241(16) 0.0053(13) 0.0040(13) 0.0094(14) O1 0.0207(11) 0.0274(11) 0.0267(11) 0.0031(9) 0.0060(9) 0.0097(9) C71 0.0276(17) 0.0162(15) 0.0308(17) 0.0078(13) 0.0060(14) 0.0072(13) C81 0.0212(16) 0.0223(16) 0.0305(17) 0.0123(13) 0.0043(13) 0.0102(13) C91 0.0207(16) 0.0226(16) 0.0311(17) 0.0080(14) 0.0097(13) 0.0059(13) B1 0.0268(19) 0.0238(18) 0.0263(18) 0.0091(15) 0.0050(15) 0.0091(16) C2 0.0317(18) 0.0366(19) 0.0303(17) 0.0077(15) 0.0190(15) 0.0074(15) C96 0.0209(16) 0.0234(16) 0.0342(17) 0.0079(14) 0.0083(14) 0.0087(13) C94 0.0285(17) 0.0213(16) 0.047(2) 0.0120(15) 0.0190(16) 0.0095(14) C92 0.0268(17) 0.0265(17) 0.0310(17) 0.0097(14) 0.0102(14) 0.0091(14) C95 0.0202(16) 0.0279(17) 0.0374(18) 0.0142(15) 0.0123(14) 0.0114(14) C93 0.0282(17) 0.0254(17) 0.0365(18) 0.0080(14) 0.0134(15) 0.0087(14) C66 0.0287(17) 0.0254(17) 0.0248(16) 0.0046(13) 0.0055(14) 0.0103(14) C63 0.0336(19) 0.0337(18) 0.0283(17) 0.0096(15) 0.0036(15) 0.0157(16) C62 0.0295(18) 0.0297(18) 0.0323(18) 0.0097(15) 0.0077(15) 0.0114(15) C64 0.0271(18) 0.044(2) 0.0286(17) 0.0073(15) 0.0029(14) 0.0190(16) C65 0.0280(18) 0.0370(19) 0.0279(17) 0.0080(15) 0.0073(14) 0.0119(15) C72 0.0318(18) 0.0252(17) 0.0290(17) 0.0116(14) 0.0105(14) 0.0089(14) C76 0.0333(19) 0.0267(17) 0.0345(19) 0.0089(15) 0.0045(15) 0.0108(15) C75 0.041(2) 0.038(2) 0.0294(18) 0.0117(15) 0.0083(16) 0.0134(17) C73 0.0353(19) 0.0312(18) 0.0377(19) 0.0153(15) 0.0134(16) 0.0128(15) C74 0.047(2) 0.043(2) 0.0336(19) 0.0151(16) 0.0205(17) 0.0166(18) C84 0.0360(19) 0.0224(17) 0.0254(17) 0.0076(14) 0.0015(14) 0.0068(15) C85 0.0295(17) 0.0236(17) 0.0305(17) 0.0139(14) 0.0031(14) 0.0058(14) C86 0.0264(17) 0.0278(17) 0.0265(16) 0.0135(14) 0.0054(13) 0.0111(14) C82 0.0238(16) 0.0194(16) 0.0303(17) 0.0073(14) 0.0042(14) 0.0058(13) C83 0.0310(18) 0.0253(17) 0.0310(17) 0.0129(14) 0.0090(14) 0.0117(14) C651 0.031(2) 0.054(2) 0.043(2) 0.0155(19) 0.0128(17) 0.0174(18) C831 0.043(2) 0.035(2) 0.0336(19) 0.0062(17) 0.0125(17) 0.0061(17) C851 0.040(2) 0.031(2) 0.0318(19) 0.0096(16) 0.0048(16) -0.0004(16) C731 0.046(2) 0.053(3) 0.057(3) 0.028(2) 0.032(2) 0.023(2) C751 0.062(3) 0.056(3) 0.036(2) 0.004(2) 0.005(2) 0.021(2) F652 0.0648(16) 0.0459(14) 0.112(2) 0.0199(14) 0.0579(15) 0.0088(12) F651 0.0513(14) 0.107(2) 0.0519(14) 0.0341(14) 0.0312(12) 0.0279(14) F653 0.0306(12) 0.1015(19) 0.0908(17) 0.0569(16) 0.0229(12) 0.0289(13) F851 0.0320(12) 0.0573(14) 0.0752(16) 0.0262(12) -0.0047(11) -0.0014(10) F852 0.094(2) 0.103(2) 0.0426(14) 0.0190(14) 0.0104(14) -0.0647(17) F831 0.0561(15) 0.140(2) 0.0810(17) 0.0850(18) 0.0382(14) 0.0439(16) F732 0.0526(15) 0.0810(19) 0.149(3) 0.0689(19) 0.0481(17) 0.0243(14) F731 0.042(3) 0.292(15) 0.064(4) 0.103(7) 0.033(3) 0.081(5) F951 0.0468(12) 0.0357(11) 0.0663(14) 0.0174(10) 0.0023(11) 0.0232(10) C951 0.0320(19) 0.0320(19) 0.049(2) 0.0195(17) 0.0122(17) 0.0140(16) C44 0.043(2) 0.041(2) 0.0271(18) 0.0074(16) 0.0049(16) 0.0231(17) C43 0.0310(18) 0.0374(19) 0.0232(16) 0.0083(14) 0.0084(14) 0.0179(15) C34 0.0320(18) 0.0339(18) 0.0217(16) 0.0009(14) 0.0088(14) 0.0044(15) C35 0.0294(18) 0.0330(18) 0.0267(17) -0.0025(14) 0.0097(14) 0.0110(15) C33 0.0282(17) 0.0304(18) 0.0257(16) 0.0079(14) 0.0087(14) 0.0072(14) C36 0.0215(16) 0.0296(17) 0.0247(16) -0.0013(14) 0.0066(13) 0.0050(14) C51 0.0245(17) 0.0369(19) 0.0217(16) -0.0053(14) 0.0048(13) 0.0161(15) C54 0.038(2) 0.053(2) 0.0262(18) -0.0029(16) 0.0056(16) 0.0315(19) C52 0.0285(18) 0.0315(18) 0.0261(17) -0.0018(14) 0.0012(14) 0.0148(15) C53 0.037(2) 0.0354(19) 0.0316(18) -0.0009(15) 0.0053(16) 0.0207(16) C55 0.0262(18) 0.063(3) 0.0252(18) -0.0070(17) 0.0056(15) 0.0245(18) C56 0.0254(17) 0.046(2) 0.0219(16) -0.0078(15) 0.0069(14) 0.0164(16) C521 0.0310(19) 0.037(2) 0.045(2) 0.0083(17) 0.0012(16) 0.0087(16) C541 0.053(2) 0.078(3) 0.033(2) 0.009(2) 0.0095(18) 0.047(2) C161 0.042(2) 0.0282(17) 0.0265(17) 0.0089(14) 0.0118(15) 0.0114(15) C162 0.056(2) 0.043(2) 0.0308(18) 0.0158(16) 0.0170(17) 0.0244(18) C123 0.047(2) 0.084(3) 0.056(2) 0.029(2) 0.021(2) 0.040(2) C23 0.0237(17) 0.0321(18) 0.0349(18) 0.0059(15) 0.0073(14) 0.0055(14) C25 0.036(2) 0.0227(17) 0.051(2) 0.0118(16) 0.0118(17) 0.0079(15) C26 0.0273(17) 0.0252(17) 0.0333(17) 0.0118(14) 0.0106(14) 0.0054(14) C24 0.0315(19) 0.0255(18) 0.042(2) 0.0023(15) 0.0080(16) 0.0024(15) C22 0.0228(16) 0.0281(17) 0.0310(17) 0.0076(14) 0.0136(14) 0.0076(14) C261 0.0312(18) 0.0289(18) 0.0394(19) 0.0157(15) 0.0084(15) 0.0067(15) C221 0.0203(16) 0.0288(18) 0.045(2) 0.0058(15) 0.0087(15) 0.0087(14) C222 0.0266(19) 0.035(2) 0.079(3) 0.0033(19) 0.0220(19) 0.0076(16) C314 0.0230(17) 0.051(2) 0.0279(18) -0.0005(16) 0.0094(14) 0.0109(16) C313 0.0280(18) 0.053(2) 0.0267(17) 0.0023(16) 0.0051(14) 0.0202(17) C312 0.0293(18) 0.0376(19) 0.0282(17) 0.0056(15) 0.0056(14) 0.0195(15) C315 0.0249(17) 0.0315(18) 0.0287(17) -0.0031(14) 0.0091(14) 0.0052(14) C14 0.0251(17) 0.0281(17) 0.0280(17) 0.0009(14) 0.0126(14) 0.0041(14) C631 0.042(2) 0.053(2) 0.061(3) 0.030(2) 0.014(2) 0.027(2) C931 0.049(2) 0.0246(18) 0.041(2) 0.0062(16) 0.0150(18) 0.0103(17) F932 0.106(2) 0.0409(13) 0.0345(12) 0.0053(10) 0.0047(12) 0.0155(13) F933 0.0538(14) 0.0421(12) 0.0456(12) 0.0028(10) 0.0092(11) -0.0100(10) F931 0.0707(16) 0.0526(14) 0.0820(17) -0.0158(13) 0.0295(14) 0.0203(13) F953 0.0512(13) 0.0362(11) 0.0405(11) 0.0141(9) -0.0008(10) 0.0147(10) F952 0.0479(13) 0.0904(17) 0.0688(15) 0.0593(14) 0.0279(12) 0.0275(13) F631 0.0908(19) 0.0607(15) 0.0872(18) 0.0320(14) 0.0269(15) 0.0550(15) F632 0.0604(16) 0.0823(18) 0.148(3) 0.0853(19) 0.0408(17) 0.0404(15) F633 0.142(3) 0.0751(18) 0.0427(14) 0.0303(13) 0.0024(15) 0.0505(18) F833 0.0368(12) 0.0672(15) 0.0483(12) 0.0115(11) 0.0201(10) 0.0123(11) F832 0.134(2) 0.0430(14) 0.0764(17) -0.0116(13) 0.0740(18) -0.0112(14) F853 0.0576(16) 0.0256(13) 0.162(3) 0.0124(15) 0.0313(17) 0.0011(11) F733 0.0626(18) 0.0699(19) 0.225(4) 0.037(2) 0.067(2) 0.0349(16) F752 0.107(2) 0.0681(16) 0.0454(14) 0.0110(12) -0.0162(14) 0.0450(16) F753 0.196(4) 0.0541(19) 0.082(2) -0.0221(16) -0.075(2) 0.058(2) F751 0.053(4) 0.180(19) 0.021(3) 0.010(5) 0.010(3) 0.022(6) C561 0.0292(19) 0.063(3) 0.037(2) -0.0032(18) 0.0126(16) 0.0097(18) C461 0.074(3) 0.034(2) 0.044(2) 0.0189(18) 0.029(2) 0.0131(19) C223 0.031(2) 0.044(2) 0.055(2) 0.0106(18) -0.0025(17) 0.0177(17) C441 0.065(3) 0.057(2) 0.052(2) 0.018(2) 0.015(2) 0.045(2) C163 0.061(2) 0.044(2) 0.045(2) 0.0229(18) 0.0307(19) 0.0230(19) C263 0.045(2) 0.040(2) 0.074(3) 0.004(2) -0.008(2) 0.020(2) C262 0.053(3) 0.147(5) 0.075(3) 0.083(3) 0.018(2) 0.026(3) O999 0.076(2) 0.0440(17) 0.078(2) 0.0117(16) 0.0288(18) -0.0061(16) C998 0.063(3) 0.079(3) 0.066(3) 0.015(3) 0.037(3) -0.008(3) C999 0.075(3) 0.064(3) 0.100(4) 0.016(3) 0.050(3) 0.016(3) C996 0.063(3) 0.100(4) 0.085(4) 0.044(3) 0.030(3) 0.008(3) C886 0.128(6) 0.140(7) 0.119(6) 0.008(5) 0.037(5) 0.050(6) C887 0.146(7) 0.158(8) 0.102(5) 0.018(5) 0.024(5) 0.070(7) C997 0.095(5) 0.175(7) 0.153(6) 0.115(6) 0.060(5) 0.019(5) C888 0.139(7) 0.174(8) 0.114(6) 0.033(6) 0.052(6) 0.066(7) C885 0.220(10) 0.113(6) 0.207(9) -0.035(6) 0.155(9) -0.047(6) C889 0.228(11) 0.196(9) 0.143(7) 0.092(7) 0.107(7) 0.064(8) C777 0.080(6) 0.156(9) 0.147(8) 0.115(8) 0.053(6) 0.054(7) C779 0.117(6) 0.204(8) 0.184(7) 0.148(7) 0.086(6) 0.089(6) C778 0.075(7) 0.074(7) 0.054(7) 0.013(5) 0.027(5) 0.023(5) C776 0.056(6) 0.070(7) 0.044(7) 0.024(6) 0.015(5) 0.013(5) F734 0.009(5) 0.086(13) 0.071(10) -0.028(7) -0.002(6) -0.007(5) F754 0.097(4) 0.106(7) 0.026(2) 0.024(3) 0.014(2) 0.030(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 C1 1.904(3) . ? Ni1 C421 1.931(3) . ? Ni1 N3 2.001(2) . ? Ni1 O1 2.0567(19) . ? C13 C14 1.376(4) . ? C13 C12 1.397(4) . ? C11 C16 1.401(4) . ? C11 C12 1.402(4) . ? C11 N1 1.454(4) . ? C12 C121 1.512(4) . ? C121 C122 1.517(4) . ? C121 C123 1.540(5) . ? C16 C15 1.396(4) . ? C16 C161 1.525(4) . ? C15 C14 1.384(4) . ? N3 C31 1.455(4) . ? N2 C1 1.375(4) . ? N2 C3 1.377(4) . ? N2 C21 1.448(4) . ? N1 C1 1.369(3) . ? N1 C2 1.384(4) . ? C21 C26 1.393(4) . ? C21 C22 1.400(4) . ? C3 C2 1.335(4) . ? C31 C32 1.397(4) . ? C31 C36 1.398(4) . ? C32 C33 1.388(4) . ? C32 C41 1.497(4) . ? C41 C42 1.403(4) . ? C41 C46 1.407(4) . ? C42 C43 1.396(4) . ? C42 C421 1.490(4) . ? C46 C45 1.390(4) . ? C46 C461 1.514(4) . ? C45 C44 1.380(5) . ? C61 C66 1.389(4) . ? C61 C62 1.406(4) . ? C61 B1 1.644(4) . ? O1 C312 1.460(3) . ? O1 C315 1.473(3) . ? C71 C76 1.394(4) . ? C71 C72 1.403(4) . ? C71 B1 1.641(5) . ? C81 C86 1.401(4) . ? C81 C82 1.403(4) . ? C81 B1 1.638(4) . ? C91 C96 1.391(4) . ? C91 C92 1.399(4) . ? C91 B1 1.651(4) . ? C96 C95 1.401(4) . ? C94 C95 1.376(4) . ? C94 C93 1.384(4) . ? C92 C93 1.381(4) . ? C95 C951 1.490(4) . ? C93 C931 1.492(4) . ? C66 C65 1.393(4) . ? C63 C62 1.378(4) . ? C63 C64 1.387(4) . ? C63 C631 1.503(5) . ? C64 C65 1.388(4) . ? C65 C651 1.499(5) . ? C72 C73 1.391(4) . ? C76 C75 1.391(4) . ? C75 C74 1.378(5) . ? C75 C751 1.482(5) . ? C73 C74 1.394(5) . ? C73 C731 1.491(5) . ? C84 C85 1.380(4) . ? C84 C83 1.391(4) . ? C85 C86 1.400(4) . ? C85 C851 1.498(4) . ? C82 C83 1.379(4) . ? C83 C831 1.494(4) . ? C651 F651 1.324(4) . ? C651 F652 1.333(4) . ? C651 F653 1.333(4) . ? C831 F831 1.322(4) . ? C831 F833 1.327(4) . ? C831 F832 1.328(4) . ? C851 F852 1.305(4) . ? C851 F853 1.324(4) . ? C851 F851 1.326(4) . ? C731 F731 1.268(6) . ? C731 F733 1.316(4) . ? C731 F732 1.321(4) . ? C731 F734 1.352(13) . ? C751 F753 1.300(5) . ? C751 F752 1.314(5) . ? C751 F751 1.316(10) . ? C751 F754 1.391(7) . ? F732 F734 1.76(3) . ? F731 F734 0.975(15) . ? F951 C951 1.345(4) . ? C951 F952 1.334(4) . ? C951 F953 1.339(4) . ? C44 C43 1.380(4) . ? C44 C441 1.503(4) . ? C34 C35 1.375(4) . ? C34 C33 1.381(4) . ? C35 C36 1.389(4) . ? C36 C51 1.494(4) . ? C51 C56 1.403(4) . ? C51 C52 1.403(5) . ? C54 C55 1.384(5) . ? C54 C53 1.391(5) . ? C54 C541 1.514(5) . ? C52 C53 1.386(4) . ? C52 C521 1.511(4) . ? C55 C56 1.390(5) . ? C56 C561 1.516(5) . ? C161 C162 1.524(4) . ? C161 C163 1.534(4) . ? C23 C24 1.380(4) . ? C23 C22 1.383(4) . ? C25 C24 1.380(4) . ? C25 C26 1.398(4) . ? C26 C261 1.516(4) . ? C22 C221 1.527(4) . ? C261 C263 1.511(5) . ? C261 C262 1.530(5) . ? C221 C223 1.535(5) . ? C221 C222 1.538(4) . ? C314 C315 1.516(4) . ? C314 C313 1.521(5) . ? C313 C312 1.521(4) . ? C631 F633 1.301(4) . ? C631 F632 1.327(4) . ? C631 F631 1.340(4) . ? C931 F932 1.324(4) . ? C931 F931 1.336(4) . ? C931 F933 1.342(4) . ? F753 F751 1.669(13) . ? F751 F754 1.178(15) . ? O999 C996 1.397(6) . ? O999 C999 1.440(5) . ? C998 C997 1.485(7) . ? C998 C999 1.501(6) . ? C996 C997 1.441(6) . ? C886 C887 1.444(9) . ? C886 C885 1.473(9) . ? C887 C888 1.408(9) . ? C888 C889 1.485(10) . ? C777 C778 1.306(10) 2_667 ? C777 C778 1.306(10) . ? C777 C776 1.434(10) 2_667 ? C777 C776 1.434(10) . ? C779 C776 1.357(11) . ? C779 C778 1.483(11) . ? C778 C776 1.202(11) . ? 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 C1 Ni1 C421 91.74(12) . . ? C1 Ni1 N3 177.44(12) . . ? C421 Ni1 N3 88.40(12) . . ? C1 Ni1 O1 95.05(10) . . ? C421 Ni1 O1 173.17(11) . . ? N3 Ni1 O1 84.86(9) . . ? C14 C13 C12 122.0(3) . . ? C16 C11 C12 123.0(3) . . ? C16 C11 N1 117.7(3) . . ? C12 C11 N1 119.1(3) . . ? C13 C12 C11 116.8(3) . . ? C13 C12 C121 119.6(3) . . ? C11 C12 C121 123.6(3) . . ? C12 C121 C122 111.4(3) . . ? C12 C121 C123 110.0(3) . . ? C122 C121 C123 110.8(3) . . ? C15 C16 C11 117.1(3) . . ? C15 C16 C161 119.4(3) . . ? C11 C16 C161 123.5(3) . . ? C14 C15 C16 121.5(3) . . ? C31 N3 Ni1 126.04(19) . . ? C1 N2 C3 111.2(2) . . ? C1 N2 C21 126.8(2) . . ? C3 N2 C21 121.5(2) . . ? C1 N1 C2 111.2(2) . . ? C1 N1 C11 127.5(2) . . ? C2 N1 C11 121.1(2) . . ? C26 C21 C22 122.9(3) . . ? C26 C21 N2 117.7(3) . . ? C22 C21 N2 119.3(2) . . ? C2 C3 N2 107.3(3) . . ? N1 C1 N2 103.2(2) . . ? N1 C1 Ni1 126.3(2) . . ? N2 C1 Ni1 130.2(2) . . ? C32 C31 C36 121.3(3) . . ? C32 C31 N3 119.7(3) . . ? C36 C31 N3 119.0(3) . . ? C33 C32 C31 117.7(3) . . ? C33 C32 C41 119.8(3) . . ? C31 C32 C41 122.4(2) . . ? C42 C41 C46 119.5(3) . . ? C42 C41 C32 118.9(3) . . ? C46 C41 C32 121.2(3) . . ? C43 C42 C41 118.8(3) . . ? C43 C42 C421 118.2(3) . . ? C41 C42 C421 123.0(3) . . ? C42 C421 Ni1 112.7(2) . . ? C45 C46 C41 119.0(3) . . ? C45 C46 C461 118.1(3) . . ? C41 C46 C461 122.9(3) . . ? C44 C45 C46 122.4(3) . . ? C66 C61 C62 116.2(3) . . ? C66 C61 B1 123.6(3) . . ? C62 C61 B1 119.8(3) . . ? C312 O1 C315 108.9(2) . . ? C312 O1 Ni1 119.21(17) . . ? C315 O1 Ni1 122.82(17) . . ? C76 C71 C72 115.4(3) . . ? C76 C71 B1 121.0(3) . . ? C72 C71 B1 123.1(3) . . ? C86 C81 C82 115.5(3) . . ? C86 C81 B1 126.6(3) . . ? C82 C81 B1 117.7(3) . . ? C96 C91 C92 115.8(3) . . ? C96 C91 B1 124.5(3) . . ? C92 C91 B1 119.6(3) . . ? C81 B1 C71 116.5(3) . . ? C81 B1 C61 102.9(2) . . ? C71 B1 C61 111.0(2) . . ? C81 B1 C91 111.9(2) . . ? C71 B1 C91 103.9(2) . . ? C61 B1 C91 110.8(2) . . ? C3 C2 N1 107.1(3) . . ? C91 C96 C95 121.9(3) . . ? C95 C94 C93 118.5(3) . . ? C93 C92 C91 122.6(3) . . ? C94 C95 C96 120.6(3) . . ? C94 C95 C951 118.4(3) . . ? C96 C95 C951 121.0(3) . . ? C92 C93 C94 120.5(3) . . ? C92 C93 C931 121.2(3) . . ? C94 C93 C931 118.3(3) . . ? C61 C66 C65 122.2(3) . . ? C62 C63 C64 120.7(3) . . ? C62 C63 C631 120.5(3) . . ? C64 C63 C631 118.8(3) . . ? C63 C62 C61 122.1(3) . . ? C63 C64 C65 118.6(3) . . ? C64 C65 C66 120.2(3) . . ? C64 C65 C651 120.8(3) . . ? C66 C65 C651 118.9(3) . . ? C73 C72 C71 122.3(3) . . ? C75 C76 C71 123.0(3) . . ? C74 C75 C76 120.3(3) . . ? C74 C75 C751 120.6(3) . . ? C76 C75 C751 119.0(3) . . ? C72 C73 C74 120.4(3) . . ? C72 C73 C731 120.1(3) . . ? C74 C73 C731 119.5(3) . . ? C75 C74 C73 118.5(3) . . ? C85 C84 C83 118.3(3) . . ? C84 C85 C86 121.0(3) . . ? C84 C85 C851 118.3(3) . . ? C86 C85 C851 120.7(3) . . ? C85 C86 C81 121.7(3) . . ? C83 C82 C81 123.1(3) . . ? C82 C83 C84 120.3(3) . . ? C82 C83 C831 120.0(3) . . ? C84 C83 C831 119.6(3) . . ? F651 C651 F652 105.3(3) . . ? F651 C651 F653 105.6(3) . . ? F652 C651 F653 106.9(3) . . ? F651 C651 C65 112.2(3) . . ? F652 C651 C65 112.8(3) . . ? F653 C651 C65 113.3(3) . . ? F831 C831 F833 104.5(3) . . ? F831 C831 F832 106.2(3) . . ? F833 C831 F832 105.4(3) . . ? F831 C831 C83 112.6(3) . . ? F833 C831 C83 114.2(3) . . ? F832 C831 C83 113.2(3) . . ? F852 C851 F853 106.8(3) . . ? F852 C851 F851 106.2(3) . . ? F853 C851 F851 103.7(3) . . ? F852 C851 C85 114.6(3) . . ? F853 C851 C85 112.7(3) . . ? F851 C851 C85 112.1(3) . . ? F731 C731 F733 96.9(9) . . ? F731 C731 F732 115.5(8) . . ? F733 C731 F732 100.4(3) . . ? F731 C731 F734 43.5(8) . . ? F733 C731 F734 132.5(12) . . ? F732 C731 F734 82.4(13) . . ? F731 C731 C73 116.2(4) . . ? F733 C731 C73 112.8(3) . . ? F732 C731 C73 112.8(3) . . ? F734 C731 C73 109.3(7) . . ? F753 C751 F752 101.2(4) . . ? F753 C751 F751 79.3(9) . . ? F752 C751 F751 127.8(8) . . ? F753 C751 F754 123.1(5) . . ? F752 C751 F754 90.7(5) . . ? F751 C751 F754 51.5(7) . . ? F753 C751 C75 113.2(4) . . ? F752 C751 C75 113.9(3) . . ? F751 C751 C75 113.4(5) . . ? F754 C751 C75 111.7(4) . . ? C731 F732 F734 49.6(6) . . ? F734 F731 C731 72.8(11) . . ? F952 C951 F953 107.5(3) . . ? F952 C951 F951 105.1(3) . . ? F953 C951 F951 106.2(3) . . ? F952 C951 C95 112.3(3) . . ? F953 C951 C95 113.4(3) . . ? F951 C951 C95 111.7(3) . . ? C43 C44 C45 117.8(3) . . ? C43 C44 C441 121.4(3) . . ? C45 C44 C441 120.8(3) . . ? C44 C43 C42 122.5(3) . . ? C35 C34 C33 119.4(3) . . ? C34 C35 C36 121.1(3) . . ? C34 C33 C32 121.8(3) . . ? C35 C36 C31 118.5(3) . . ? C35 C36 C51 120.4(3) . . ? C31 C36 C51 121.0(3) . . ? C56 C51 C52 119.8(3) . . ? C56 C51 C36 121.0(3) . . ? C52 C51 C36 119.2(3) . . ? C55 C54 C53 118.6(3) . . ? C55 C54 C541 121.8(3) . . ? C53 C54 C541 119.7(4) . . ? C53 C52 C51 119.3(3) . . ? C53 C52 C521 119.8(3) . . ? C51 C52 C521 120.9(3) . . ? C52 C53 C54 121.5(3) . . ? C54 C55 C56 121.7(3) . . ? C55 C56 C51 119.1(3) . . ? C55 C56 C561 120.8(3) . . ? C51 C56 C561 120.0(3) . . ? C162 C161 C16 113.3(3) . . ? C162 C161 C163 108.6(3) . . ? C16 C161 C163 110.1(2) . . ? C24 C23 C22 121.0(3) . . ? C24 C25 C26 121.3(3) . . ? C21 C26 C25 116.9(3) . . ? C21 C26 C261 122.7(3) . . ? C25 C26 C261 120.3(3) . . ? C23 C24 C25 120.2(3) . . ? C23 C22 C21 117.7(3) . . ? C23 C22 C221 119.8(3) . . ? C21 C22 C221 122.5(3) . . ? C263 C261 C26 114.2(3) . . ? C263 C261 C262 110.1(3) . . ? C26 C261 C262 109.2(3) . . ? C22 C221 C223 112.1(3) . . ? C22 C221 C222 109.7(3) . . ? C223 C221 C222 110.3(3) . . ? C315 C314 C313 102.2(3) . . ? C314 C313 C312 102.7(3) . . ? O1 C312 C313 106.0(3) . . ? O1 C315 C314 104.7(2) . . ? C13 C14 C15 119.6(3) . . ? F633 C631 F632 109.1(3) . . ? F633 C631 F631 104.5(3) . . ? F632 C631 F631 104.7(3) . . ? F633 C631 C63 112.3(3) . . ? F632 C631 C63 113.9(3) . . ? F631 C631 C63 111.6(3) . . ? F932 C931 F931 105.5(3) . . ? F932 C931 F933 106.5(3) . . ? F931 C931 F933 104.8(3) . . ? F932 C931 C93 114.0(3) . . ? F931 C931 C93 112.4(3) . . ? F933 C931 C93 112.9(3) . . ? C751 F753 F751 50.8(7) . . ? F754 F751 C751 67.5(10) . . ? F754 F751 F753 111.2(9) . . ? C751 F751 F753 49.9(4) . . ? C996 O999 C999 108.1(3) . . ? C997 C998 C999 102.4(4) . . ? O999 C999 C998 107.2(4) . . ? O999 C996 C997 106.0(5) . . ? C887 C886 C885 106.0(8) . . ? C888 C887 C886 113.3(8) . . ? C996 C997 C998 105.6(4) . . ? C887 C888 C889 117.7(9) . . ? C778 C777 C778 180.0(13) 2_667 . ? C778 C777 C776 51.8(5) 2_667 2_667 ? C778 C777 C776 128.2(5) . 2_667 ? C778 C777 C776 128.2(5) 2_667 . ? C778 C777 C776 51.8(5) . . ? C776 C777 C776 180.000(6) 2_667 . ? C776 C779 C778 49.8(5) . . ? C776 C778 C777 69.6(7) . . ? C776 C778 C779 59.6(7) . . ? C777 C778 C779 129.2(8) . . ? C778 C776 C779 70.5(8) . . ? C778 C776 C777 58.6(7) . . ? C779 C776 C777 129.1(9) . . ? F731 F734 C731 63.6(7) . . ? F731 F734 F732 102.6(13) . . ? C731 F734 F732 48.1(8) . . ? F751 F754 C751 61.0(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 0.716 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.072 data_9 _database_code_depnum_ccdc_archive 'CCDC 896905' #TrackingRef 'CIF(1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H96 B F24 N3 Ni O' _chemical_formula_weight 1797.25 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' B B 0.0013 0.0007 '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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7476(12) _cell_length_b 20.1891(19) _cell_length_c 33.921(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.696(2) _cell_angle_gamma 90.00 _cell_volume 8729.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 0.322 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.2075 _exptl_absorpt_correction_T_max 0.2793 _exptl_absorpt_process_details 'Norton et. al.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker P4' _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 55707 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.28 _reflns_number_total 20189 _reflns_number_gt 12414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0478P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20189 _refine_ls_number_parameters 1112 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.885 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.16969(2) 0.744000(14) 0.404749(8) 0.01975(8) Uani 1 1 d . . . F853 F 0.38056(12) 0.67483(7) 0.23726(4) 0.0361(4) Uani 1 1 d . . . F633 F 1.07053(12) 1.00245(7) 0.17949(4) 0.0416(4) Uani 1 1 d . . . F632 F 1.08743(11) 0.89707(7) 0.17177(4) 0.0348(4) Uani 1 1 d . . . F852 F 0.23917(12) 0.72893(7) 0.22465(5) 0.0397(4) Uani 1 1 d . . . F851 F 0.30801(12) 0.66686(7) 0.18039(4) 0.0361(4) Uani 1 1 d . . . F631 F 1.01777(12) 0.95580(7) 0.12583(4) 0.0397(4) Uani 1 1 d . . . N1 N 0.12036(15) 0.88318(9) 0.37323(5) 0.0196(4) Uani 1 1 d . . . N3 N 0.19787(16) 0.72527(9) 0.45732(6) 0.0208(5) Uani 1 1 d . . . C81 C 0.56907(18) 0.80897(10) 0.17811(6) 0.0176(5) Uani 1 1 d . . . N2 N 0.28122(15) 0.87388(9) 0.39048(5) 0.0189(4) Uani 1 1 d . . . F733 F 0.69000(18) 0.61978(8) 0.02301(5) 0.0674(6) Uani 1 1 d . . . F933 F 0.74540(15) 0.61236(8) 0.31929(4) 0.0513(5) Uani 1 1 d . . . C46 C 0.03046(19) 0.66140(10) 0.38962(6) 0.0200(5) Uani 1 1 d . . . C1 C 0.19049(18) 0.83801(11) 0.38763(6) 0.0179(5) Uani 1 1 d . . . C21 C 0.38367(18) 0.84923(10) 0.40211(7) 0.0198(5) Uani 1 1 d . . . F953 F 0.95107(14) 0.59359(8) 0.15929(5) 0.0569(5) Uani 1 1 d . . . F653 F 0.77959(13) 1.07356(7) 0.25546(5) 0.0512(5) Uani 1 1 d . . . C91 C 0.74621(18) 0.74089(10) 0.20035(6) 0.0182(5) Uani 1 1 d . . . C35 C 0.10865(18) 0.55363(11) 0.46040(7) 0.0205(5) Uani 1 1 d . . . H35A H 0.0820 0.5215 0.4424 0.025 Uiso 1 1 calc R . . C36 C 0.13534(18) 0.61606(11) 0.44720(6) 0.0179(5) Uani 1 1 d . . . F952 F 1.05391(13) 0.65147(8) 0.19404(6) 0.0650(6) Uani 1 1 d . . . C41 C 0.12680(19) 0.63642(10) 0.40477(6) 0.0184(5) Uani 1 1 d . . . C34 C 0.12094(18) 0.53794(11) 0.50003(7) 0.0214(5) Uani 1 1 d . . . H34A H 0.0997 0.4957 0.5094 0.026 Uiso 1 1 calc R . . F951 F 0.99023(15) 0.56167(9) 0.21661(6) 0.0682(6) Uani 1 1 d . . . F652 F 0.63198(14) 1.03815(9) 0.23687(6) 0.0649(6) Uani 1 1 d . . . C631 C 1.0222(2) 0.94852(12) 0.16529(7) 0.0267(6) Uani 1 1 d . . . C53 C 0.2708(2) 0.77072(12) 0.59235(7) 0.0277(6) Uani 1 1 d . . . H53A H 0.2390 0.8026 0.6090 0.033 Uiso 1 1 calc R . . C66 C 0.72074(19) 0.91336(11) 0.21260(6) 0.0210(5) Uani 1 1 d . . . H66A H 0.6541 0.9055 0.2239 0.025 Uiso 1 1 calc R . . C11 C 0.00957(18) 0.87518(11) 0.36492(7) 0.0197(5) Uani 1 1 d . . . C51 C 0.25746(19) 0.68858(11) 0.54131(6) 0.0208(5) Uani 1 1 d . . . C62 C 0.86084(18) 0.88092(10) 0.17170(6) 0.0185(5) Uani 1 1 d . . . H62A H 0.8926 0.8501 0.1543 0.022 Uiso 1 1 calc R . . C71 C 0.71246(17) 0.78214(11) 0.12584(6) 0.0173(5) Uani 1 1 d . . . C93 C 0.7510(2) 0.67614(11) 0.26120(6) 0.0224(5) Uani 1 1 d . . . C92 C 0.70889(19) 0.72678(11) 0.23788(6) 0.0209(5) Uani 1 1 d . . . H92A H 0.6529 0.7525 0.2479 0.025 Uiso 1 1 calc R . . C86 C 0.50284(18) 0.75891(11) 0.19155(6) 0.0190(5) Uani 1 1 d . . . H86A H 0.5326 0.7173 0.1985 0.023 Uiso 1 1 calc R . . C22 C 0.41089(19) 0.84988(11) 0.44225(7) 0.0224(5) Uani 1 1 d . . . C42 C 0.21569(19) 0.62948(11) 0.38026(7) 0.0210(5) Uani 1 1 d . . . C72 C 0.69764(18) 0.71728(11) 0.11224(6) 0.0191(5) Uani 1 1 d . . . H72A H 0.6767 0.6842 0.1304 0.023 Uiso 1 1 calc R . . F932 F 0.70240(17) 0.71359(8) 0.32373(4) 0.0622(6) Uani 1 1 d . . . C32 C 0.19502(18) 0.64650(11) 0.51340(6) 0.0186(5) Uani 1 1 d . . . C31 C 0.17667(18) 0.66398(10) 0.47355(6) 0.0178(5) Uani 1 1 d . . . C33 C 0.16398(19) 0.58356(11) 0.52595(6) 0.0209(5) Uani 1 1 d . . . H33A H 0.1727 0.5719 0.5529 0.025 Uiso 1 1 calc R . . C52 C 0.2088(2) 0.73641(11) 0.56513(6) 0.0238(6) Uani 1 1 d . . . C3 C 0.2670(2) 0.93908(11) 0.37883(7) 0.0235(6) Uani 1 1 d . . . H3A H 0.3187 0.9729 0.3784 0.028 Uiso 1 1 calc R . . C65 C 0.7761(2) 0.96986(11) 0.22340(6) 0.0217(5) Uani 1 1 d . . . C85 C 0.39555(19) 0.76747(11) 0.19515(6) 0.0214(5) Uani 1 1 d . . . C12 C -0.02233(19) 0.85565(11) 0.32684(7) 0.0222(5) Uani 1 1 d . . . C82 C 0.51803(19) 0.86819(11) 0.16707(6) 0.0212(5) Uani 1 1 d . . . H82A H 0.5588 0.9034 0.1568 0.025 Uiso 1 1 calc R . . F732 F 0.78167(18) 0.59287(8) 0.07122(7) 0.0929(8) Uani 1 1 d . . . C26 C 0.45256(19) 0.83093(11) 0.37244(7) 0.0234(5) Uani 1 1 d . . . C61 C 0.76011(18) 0.86748(10) 0.18547(6) 0.0178(5) Uani 1 1 d . . . C221 C 0.3377(2) 0.87936(11) 0.47301(7) 0.0265(6) Uani 1 1 d . . . H22A H 0.2640 0.8677 0.4654 0.032 Uiso 1 1 calc R . . C261 C 0.4234(2) 0.83948(12) 0.32891(7) 0.0282(6) Uani 1 1 d . . . H26A H 0.3694 0.8753 0.3272 0.034 Uiso 1 1 calc R . . C95 C 0.87625(19) 0.65344(11) 0.21162(7) 0.0222(5) Uani 1 1 d . . . C73 C 0.71246(19) 0.69961(11) 0.07320(6) 0.0200(5) Uani 1 1 d . . . C2 C 0.1662(2) 0.94475(11) 0.36841(7) 0.0242(6) Uani 1 1 d . . . H2A H 0.1322 0.9838 0.3593 0.029 Uiso 1 1 calc R . . B1 B 0.6959(2) 0.80031(12) 0.17277(7) 0.0185(6) Uani 1 1 d . . . F931 F 0.60026(15) 0.64520(11) 0.29541(5) 0.0690(6) Uani 1 1 d . . . C931 C 0.7005(2) 0.66156(12) 0.29965(7) 0.0306(6) Uani 1 1 d . . . C63 C 0.91646(19) 0.93752(11) 0.18241(6) 0.0198(5) Uani 1 1 d . . . C731 C 0.7007(2) 0.62861(12) 0.06134(7) 0.0273(6) Uani 1 1 d . . . C43 C 0.2041(2) 0.64621(11) 0.34034(7) 0.0237(6) Uani 1 1 d . . . H43A H 0.2622 0.6412 0.3233 0.028 Uiso 1 1 calc R . . C74 C 0.74202(19) 0.74647(11) 0.04561(7) 0.0236(5) Uani 1 1 d . . . H74A H 0.7537 0.7344 0.0189 0.028 Uiso 1 1 calc R . . C96 C 0.83248(18) 0.70337(11) 0.18848(7) 0.0211(5) Uani 1 1 d . . . H96A H 0.8624 0.7124 0.1635 0.025 Uiso 1 1 calc R . . C64 C 0.8744(2) 0.98309(11) 0.20828(6) 0.0228(5) Uani 1 1 d . . . H64A H 0.9117 1.0221 0.2154 0.027 Uiso 1 1 calc R . . C94 C 0.8351(2) 0.63855(11) 0.24823(7) 0.0250(6) Uani 1 1 d . . . H94A H 0.8636 0.6038 0.2639 0.030 Uiso 1 1 calc R . . C84 C 0.34799(19) 0.82653(11) 0.18488(7) 0.0231(5) Uani 1 1 d . . . H84A H 0.2745 0.8325 0.1875 0.028 Uiso 1 1 calc R . . C851 C 0.3304(2) 0.71021(12) 0.20917(7) 0.0260(6) Uani 1 1 d . . . C951 C 0.9678(2) 0.61590(12) 0.19644(8) 0.0310(6) Uani 1 1 d . . . C45 C 0.0251(2) 0.67824(11) 0.34952(7) 0.0250(6) Uani 1 1 d . . . H45A H -0.0383 0.6958 0.3389 0.030 Uiso 1 1 calc R . . C44 C 0.1103(2) 0.66974(11) 0.32519(7) 0.0251(6) Uani 1 1 d . . . H44A H 0.1042 0.6801 0.2979 0.030 Uiso 1 1 calc R . . F731 F 0.62002(19) 0.60005(9) 0.07691(7) 0.1003(9) Uani 1 1 d . . . C13 C -0.1296(2) 0.85630(12) 0.31907(7) 0.0286(6) Uani 1 1 d . . . H13A H -0.1546 0.8428 0.2938 0.034 Uiso 1 1 calc R . . C262 C 0.5149(2) 0.86094(14) 0.30380(8) 0.0410(7) Uani 1 1 d . . . H26B H 0.5457 0.9015 0.3148 0.062 Uiso 1 1 calc R . . H26C H 0.4901 0.8693 0.2768 0.062 Uiso 1 1 calc R . . H26D H 0.5680 0.8258 0.3036 0.062 Uiso 1 1 calc R . . C651 C 0.7256(2) 1.01807(13) 0.25077(8) 0.0343(7) Uani 1 1 d . . . F651 F 0.7077(2) 0.99312(9) 0.28546(5) 0.0904(8) Uani 1 1 d . . . C521 C 0.0917(2) 0.74896(11) 0.56263(7) 0.0262(6) Uani 1 1 d . . . H52A H 0.0635 0.7251 0.5390 0.031 Uiso 1 1 calc R . . C75 C 0.75408(19) 0.81153(11) 0.05811(7) 0.0214(5) Uani 1 1 d . . . C16 C -0.0607(2) 0.89530(11) 0.39394(7) 0.0239(6) Uani 1 1 d . . . C54 C 0.3770(2) 0.75948(12) 0.59566(7) 0.0309(6) Uani 1 1 d . . . H54A H 0.4178 0.7840 0.6142 0.037 Uiso 1 1 calc R . . C76 C 0.73892(18) 0.82853(11) 0.09706(6) 0.0201(5) Uani 1 1 d . . . H76A H 0.7468 0.8736 0.1046 0.024 Uiso 1 1 calc R . . C421 C 0.31623(19) 0.59840(11) 0.39572(7) 0.0239(6) Uani 1 1 d . . . H42A H 0.3165 0.6023 0.4251 0.029 Uiso 1 1 calc R . . C83 C 0.41119(19) 0.87709(11) 0.17062(7) 0.0238(5) Uani 1 1 d . . . C56 C 0.3657(2) 0.67606(11) 0.54489(7) 0.0242(6) Uani 1 1 d . . . C25 C 0.5498(2) 0.80656(12) 0.38443(8) 0.0300(6) Uani 1 1 d . . . H25A H 0.5982 0.7920 0.3652 0.036 Uiso 1 1 calc R . . C24 C 0.5770(2) 0.80324(12) 0.42404(8) 0.0330(6) Uani 1 1 d . . . H24A H 0.6431 0.7853 0.4317 0.040 Uiso 1 1 calc R . . F831 F 0.30553(13) 0.96655(7) 0.18977(5) 0.0509(5) Uani 1 1 d . . . F751 F 0.73687(13) 0.91957(7) 0.03276(4) 0.0446(4) Uani 1 1 d . . . F832 F 0.29046(13) 0.93511(8) 0.12984(5) 0.0515(5) Uani 1 1 d . . . F833 F 0.42821(13) 0.98802(7) 0.14869(6) 0.0553(5) Uani 1 1 d . . . F752 F 0.88905(14) 0.87933(9) 0.03496(6) 0.0725(6) Uani 1 1 d . . . F753 F 0.77724(19) 0.84516(8) -0.00774(5) 0.0757(7) Uani 1 1 d . . . C461 C -0.06663(19) 0.66299(11) 0.41514(7) 0.0224(5) Uani 1 1 d . . . H46A H -0.0426 0.6647 0.4433 0.027 Uiso 1 1 calc R . . O999 O 0.52171(19) 0.51955(10) 0.14786(8) 0.0683(8) Uani 1 1 d . . . C122 C 0.0074(2) 0.79326(12) 0.26243(7) 0.0315(6) Uani 1 1 d . . . H12A H -0.0223 0.7534 0.2744 0.047 Uiso 1 1 calc R . . H12B H 0.0618 0.7806 0.2437 0.047 Uiso 1 1 calc R . . H12C H -0.0481 0.8178 0.2486 0.047 Uiso 1 1 calc R . . C121 C 0.0560(2) 0.83739(12) 0.29496(7) 0.0259(6) Uani 1 1 d . . . H12D H 0.1150 0.8123 0.3077 0.031 Uiso 1 1 calc R . . C751 C 0.7896(2) 0.86303(12) 0.02950(7) 0.0310(6) Uani 1 1 d . . . C123 C 0.1020(2) 0.89929(13) 0.27548(7) 0.0377(7) Uani 1 1 d . . . H12E H 0.1339 0.9278 0.2957 0.057 Uiso 1 1 calc R . . H12F H 0.0460 0.9236 0.2617 0.057 Uiso 1 1 calc R . . H12G H 0.1555 0.8861 0.2565 0.057 Uiso 1 1 calc R . . C561 C 0.4207(2) 0.62396(12) 0.52007(7) 0.0278(6) Uani 1 1 d . . . H56A H 0.3657 0.6004 0.5042 0.033 Uiso 1 1 calc R . . C422 C 0.4158(2) 0.63147(14) 0.38074(8) 0.0377(7) Uani 1 1 d . . . H42B H 0.4150 0.6786 0.3877 0.056 Uiso 1 1 calc R . . H42C H 0.4191 0.6268 0.3520 0.056 Uiso 1 1 calc R . . H42D H 0.4773 0.6103 0.3929 0.056 Uiso 1 1 calc R . . C23 C 0.5098(2) 0.82550(12) 0.45239(7) 0.0302(6) Uani 1 1 d . . . H23A H 0.5310 0.8243 0.4793 0.036 Uiso 1 1 calc R . . C14 C -0.2006(2) 0.87596(12) 0.34701(8) 0.0318(6) Uani 1 1 d . . . H14A H -0.2734 0.8765 0.3407 0.038 Uiso 1 1 calc R . . C462 C -0.1295(2) 0.59892(12) 0.40949(7) 0.0305(6) Uani 1 1 d . . . H46B H -0.0841 0.5608 0.4151 0.046 Uiso 1 1 calc R . . H46C H -0.1556 0.5964 0.3822 0.046 Uiso 1 1 calc R . . H46D H -0.1889 0.5986 0.4276 0.046 Uiso 1 1 calc R . . C15 C -0.1669(2) 0.89484(12) 0.38408(8) 0.0296(6) Uani 1 1 d . . . H15A H -0.2169 0.9077 0.4032 0.035 Uiso 1 1 calc R . . C161 C -0.0254(2) 0.91999(12) 0.43422(7) 0.0322(6) Uani 1 1 d . . . H16A H 0.0518 0.9122 0.4370 0.039 Uiso 1 1 calc R . . C423 C 0.3152(2) 0.52414(12) 0.38536(8) 0.0349(7) Uani 1 1 d . . . H42E H 0.2506 0.5039 0.3951 0.052 Uiso 1 1 calc R . . H42F H 0.3760 0.5024 0.3977 0.052 Uiso 1 1 calc R . . H42G H 0.3182 0.5188 0.3567 0.052 Uiso 1 1 calc R . . C463 C -0.1353(2) 0.72318(13) 0.40767(8) 0.0373(7) Uani 1 1 d . . . H46E H -0.0939 0.7635 0.4117 0.056 Uiso 1 1 calc R . . H46F H -0.1943 0.7228 0.4260 0.056 Uiso 1 1 calc R . . H46G H -0.1623 0.7221 0.3805 0.056 Uiso 1 1 calc R . . C562 C 0.4761(2) 0.57229(13) 0.54601(8) 0.0402(7) Uani 1 1 d . . . H56B H 0.4254 0.5526 0.5641 0.060 Uiso 1 1 calc R . . H56C H 0.5324 0.5936 0.5613 0.060 Uiso 1 1 calc R . . H56D H 0.5058 0.5376 0.5293 0.060 Uiso 1 1 calc R . . C831 C 0.3599(2) 0.94152(13) 0.15981(9) 0.0357(7) Uani 1 1 d . . . C55 C 0.4245(2) 0.71274(12) 0.57210(7) 0.0291(6) Uani 1 1 d . . . H55A H 0.4980 0.7055 0.5744 0.035 Uiso 1 1 calc R . . C222 C 0.3582(2) 0.85344(13) 0.51428(7) 0.0342(7) Uani 1 1 d . . . H22B H 0.3518 0.8051 0.5144 0.051 Uiso 1 1 calc R . . H22C H 0.3070 0.8725 0.5323 0.051 Uiso 1 1 calc R . . H22D H 0.4292 0.8659 0.5228 0.051 Uiso 1 1 calc R . . C223 C 0.3466(2) 0.95559(12) 0.47412(8) 0.0400(7) Uani 1 1 d . . . H22E H 0.3320 0.9735 0.4478 0.060 Uiso 1 1 calc R . . H22F H 0.4176 0.9682 0.4825 0.060 Uiso 1 1 calc R . . H22G H 0.2957 0.9734 0.4928 0.060 Uiso 1 1 calc R . . C263 C 0.3731(3) 0.77652(14) 0.31237(8) 0.0459(8) Uani 1 1 d . . . H26E H 0.3137 0.7638 0.3288 0.069 Uiso 1 1 calc R . . H26F H 0.4251 0.7407 0.3124 0.069 Uiso 1 1 calc R . . H26G H 0.3484 0.7846 0.2853 0.069 Uiso 1 1 calc R . . C522 C 0.0364(2) 0.72222(15) 0.59862(8) 0.0470(8) Uani 1 1 d . . . H52B H 0.0524 0.6750 0.6017 0.070 Uiso 1 1 calc R . . H52C H -0.0395 0.7281 0.5953 0.070 Uiso 1 1 calc R . . H52D H 0.0607 0.7463 0.6221 0.070 Uiso 1 1 calc R . . C563 C 0.4964(2) 0.65568(13) 0.49129(8) 0.0390(7) Uani 1 1 d . . . H56E H 0.4587 0.6882 0.4750 0.058 Uiso 1 1 calc R . . H56F H 0.5263 0.6214 0.4743 0.058 Uiso 1 1 calc R . . H56G H 0.5529 0.6779 0.5060 0.058 Uiso 1 1 calc R . . C998 C 0.4278(3) 0.53872(18) 0.12682(13) 0.0865(16) Uani 1 1 d . . . H99A H 0.4327 0.5858 0.1189 0.104 Uiso 1 1 calc R . . H99B H 0.3664 0.5338 0.1442 0.104 Uiso 1 1 calc R . . C999 C 0.4136(3) 0.49708(18) 0.09154(13) 0.0771(13) Uani 1 1 d . . . H99C H 0.3487 0.5098 0.0777 0.116 Uiso 1 1 calc R . . H99D H 0.4094 0.4505 0.0994 0.116 Uiso 1 1 calc R . . H99E H 0.4733 0.5033 0.0740 0.116 Uiso 1 1 calc R . . C523 C 0.0657(3) 0.82261(14) 0.55786(10) 0.0561(9) Uani 1 1 d . . . H52E H 0.1008 0.8400 0.5345 0.084 Uiso 1 1 calc R . . H52F H 0.0900 0.8468 0.5813 0.084 Uiso 1 1 calc R . . H52G H -0.0103 0.8281 0.5547 0.084 Uiso 1 1 calc R . . C162 C -0.0799(3) 0.88332(17) 0.46733(8) 0.0671(11) Uani 1 1 d . . . H16B H -0.0652 0.8358 0.4652 0.101 Uiso 1 1 calc R . . H16C H -0.1558 0.8907 0.4653 0.101 Uiso 1 1 calc R . . H16D H -0.0540 0.8998 0.4928 0.101 Uiso 1 1 calc R . . C163 C -0.0454(3) 0.99473(14) 0.43750(9) 0.0589(10) Uani 1 1 d . . . H16E H -0.0084 1.0178 0.4164 0.088 Uiso 1 1 calc R . . H16F H -0.0196 1.0107 0.4631 0.088 Uiso 1 1 calc R . . H16G H -0.1208 1.0034 0.4351 0.088 Uiso 1 1 calc R . . C997 C 0.5432(4) 0.55960(17) 0.18077(14) 0.102(2) Uani 1 1 d . . . H99K H 0.4811 0.5608 0.1980 0.122 Uiso 1 1 calc R . . H99L H 0.5580 0.6054 0.1720 0.122 Uiso 1 1 calc R . . C996 C 0.6338(4) 0.5337(3) 0.20302(18) 0.166(3) Uani 1 1 d . . . H99G H 0.6476 0.5621 0.2260 0.250 Uiso 1 1 calc R . . H99H H 0.6955 0.5333 0.1861 0.250 Uiso 1 1 calc R . . H99I H 0.6188 0.4886 0.2119 0.250 Uiso 1 1 calc R . . H H 0.2246(19) 0.7493(11) 0.4749(7) 0.022(7) Uiso 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 0.02649(18) 0.01611(15) 0.01657(15) 0.00223(12) -0.00225(13) -0.00155(13) F853 0.0399(10) 0.0343(8) 0.0341(9) 0.0120(7) -0.0038(7) -0.0102(7) F633 0.0346(10) 0.0358(9) 0.0547(10) -0.0155(7) 0.0079(8) -0.0175(7) F632 0.0236(8) 0.0370(9) 0.0439(9) -0.0010(7) 0.0032(7) 0.0021(7) F852 0.0292(9) 0.0341(9) 0.0563(10) 0.0007(7) 0.0172(8) -0.0055(7) F851 0.0522(11) 0.0300(8) 0.0261(8) -0.0051(6) 0.0030(7) -0.0188(7) F631 0.0418(10) 0.0501(10) 0.0275(8) 0.0065(7) 0.0072(7) -0.0140(8) N1 0.0229(12) 0.0165(10) 0.0193(10) 0.0017(8) -0.0021(9) -0.0010(8) N3 0.0267(12) 0.0171(10) 0.0186(11) -0.0019(8) -0.0028(9) -0.0029(9) C81 0.0226(13) 0.0172(11) 0.0131(11) -0.0028(9) -0.0011(10) -0.0002(10) N2 0.0227(11) 0.0181(10) 0.0157(10) 0.0010(8) -0.0019(8) -0.0004(9) F733 0.138(2) 0.0310(9) 0.0325(10) -0.0121(7) -0.0079(11) -0.0083(11) F933 0.0826(14) 0.0404(9) 0.0311(9) 0.0163(7) 0.0051(9) 0.0160(9) C46 0.0275(14) 0.0147(11) 0.0178(12) -0.0027(9) -0.0034(10) 0.0011(10) C1 0.0229(13) 0.0206(12) 0.0102(11) 0.0002(9) -0.0017(10) -0.0014(10) C21 0.0210(14) 0.0154(11) 0.0230(12) 0.0022(9) -0.0037(11) -0.0032(10) F953 0.0530(12) 0.0635(12) 0.0540(11) -0.0236(9) -0.0056(9) 0.0244(9) F653 0.0458(11) 0.0363(9) 0.0718(12) -0.0327(8) 0.0053(9) -0.0022(8) C91 0.0215(13) 0.0143(11) 0.0189(11) -0.0017(9) -0.0009(10) -0.0040(10) C35 0.0231(14) 0.0163(11) 0.0220(12) -0.0013(10) -0.0016(11) 0.0003(10) C36 0.0187(13) 0.0187(12) 0.0161(11) 0.0002(9) -0.0011(10) 0.0034(10) F952 0.0284(10) 0.0424(10) 0.1245(17) -0.0215(10) 0.0102(11) -0.0022(8) C41 0.0278(14) 0.0121(11) 0.0152(11) -0.0033(9) -0.0014(10) -0.0027(10) C34 0.0224(14) 0.0170(12) 0.0248(13) 0.0050(10) 0.0025(11) -0.0010(10) F951 0.0735(14) 0.0511(11) 0.0805(13) 0.0286(10) 0.0230(11) 0.0371(10) F652 0.0383(11) 0.0647(12) 0.0915(14) -0.0483(11) -0.0084(10) 0.0152(9) C631 0.0284(15) 0.0256(13) 0.0261(14) -0.0012(11) 0.0001(12) -0.0075(12) C53 0.0392(17) 0.0252(13) 0.0187(12) -0.0015(10) -0.0014(12) -0.0001(12) C66 0.0216(14) 0.0227(12) 0.0188(12) 0.0010(10) 0.0022(10) -0.0005(10) C11 0.0201(13) 0.0167(12) 0.0223(12) 0.0036(10) -0.0054(10) 0.0011(10) C51 0.0277(14) 0.0207(12) 0.0138(11) 0.0043(9) -0.0034(10) -0.0025(11) C62 0.0243(14) 0.0144(11) 0.0169(12) -0.0011(9) -0.0001(10) 0.0026(10) C71 0.0144(12) 0.0177(11) 0.0199(12) 0.0027(9) -0.0013(10) 0.0015(9) C93 0.0295(15) 0.0203(12) 0.0173(12) 0.0007(10) -0.0057(11) -0.0052(11) C92 0.0227(14) 0.0185(12) 0.0215(12) -0.0036(10) -0.0023(11) -0.0013(10) C86 0.0241(13) 0.0175(12) 0.0153(11) -0.0005(9) 0.0011(10) 0.0006(10) C22 0.0255(14) 0.0178(12) 0.0238(13) 0.0025(10) -0.0027(11) -0.0030(10) C42 0.0266(14) 0.0163(12) 0.0202(12) -0.0026(9) -0.0006(11) -0.0012(10) C72 0.0191(13) 0.0186(12) 0.0197(12) 0.0034(10) -0.0002(10) -0.0011(10) F932 0.1226(18) 0.0385(10) 0.0260(9) -0.0049(7) 0.0179(10) 0.0042(10) C32 0.0208(13) 0.0177(12) 0.0171(12) 0.0012(9) -0.0002(10) 0.0029(10) C31 0.0169(13) 0.0172(11) 0.0192(12) 0.0003(9) 0.0010(10) 0.0027(9) C33 0.0252(14) 0.0226(12) 0.0148(12) 0.0036(10) -0.0019(10) 0.0016(10) C52 0.0315(15) 0.0231(13) 0.0168(12) 0.0041(10) -0.0011(11) -0.0010(11) C3 0.0299(15) 0.0147(12) 0.0259(13) 0.0032(10) -0.0019(11) -0.0031(10) C65 0.0284(15) 0.0189(12) 0.0179(12) -0.0041(10) -0.0014(11) 0.0033(11) C85 0.0256(14) 0.0206(12) 0.0181(12) -0.0014(10) 0.0036(10) -0.0032(10) C12 0.0257(14) 0.0170(12) 0.0237(13) 0.0044(10) -0.0044(11) -0.0003(10) C82 0.0249(14) 0.0191(12) 0.0198(12) 0.0020(10) 0.0037(11) -0.0035(10) F732 0.1058(19) 0.0249(10) 0.146(2) -0.0288(11) -0.0808(16) 0.0240(11) C26 0.0254(15) 0.0177(12) 0.0269(13) -0.0029(10) -0.0016(11) -0.0015(10) C61 0.0221(13) 0.0140(11) 0.0173(12) 0.0039(9) -0.0023(10) 0.0018(10) C221 0.0313(15) 0.0250(13) 0.0230(13) 0.0014(10) -0.0029(11) -0.0043(11) C261 0.0301(16) 0.0296(14) 0.0250(14) -0.0023(11) 0.0022(12) 0.0015(12) C95 0.0210(14) 0.0183(12) 0.0271(13) -0.0017(10) -0.0038(11) -0.0008(10) C73 0.0222(14) 0.0158(11) 0.0219(12) -0.0022(10) 0.0004(10) 0.0009(10) C2 0.0297(15) 0.0149(12) 0.0277(13) 0.0059(10) -0.0027(11) -0.0016(10) B1 0.0212(15) 0.0164(13) 0.0178(13) 0.0007(11) 0.0001(11) 0.0004(11) F931 0.0467(12) 0.1279(18) 0.0326(10) 0.0277(10) 0.0024(9) -0.0215(12) C931 0.0396(18) 0.0297(14) 0.0222(13) 0.0015(11) -0.0070(12) 0.0018(13) C63 0.0213(13) 0.0200(12) 0.0179(12) 0.0037(9) -0.0018(10) -0.0012(10) C731 0.0387(17) 0.0208(13) 0.0225(13) -0.0020(11) 0.0038(12) -0.0015(12) C43 0.0282(15) 0.0223(12) 0.0206(13) -0.0004(10) 0.0031(11) -0.0010(11) C74 0.0256(14) 0.0256(13) 0.0195(12) -0.0023(10) 0.0028(10) -0.0006(11) C96 0.0210(13) 0.0199(12) 0.0224(12) -0.0007(10) -0.0010(11) -0.0039(10) C64 0.0301(15) 0.0154(12) 0.0229(13) -0.0002(10) -0.0053(11) -0.0010(10) C94 0.0292(15) 0.0195(12) 0.0260(13) 0.0030(10) -0.0107(12) -0.0010(11) C84 0.0186(13) 0.0258(13) 0.0250(13) -0.0013(10) 0.0025(11) -0.0008(11) C851 0.0264(15) 0.0274(13) 0.0243(13) -0.0013(11) 0.0025(12) -0.0026(11) C951 0.0291(16) 0.0225(13) 0.0411(17) 0.0010(12) -0.0099(13) 0.0035(12) C45 0.0288(15) 0.0243(13) 0.0218(13) 0.0003(10) -0.0031(11) 0.0062(11) C44 0.0383(17) 0.0221(13) 0.0149(12) 0.0019(10) -0.0029(11) 0.0030(11) F731 0.127(2) 0.0470(11) 0.1290(19) -0.0524(12) 0.0927(17) -0.0555(13) C13 0.0282(15) 0.0299(14) 0.0275(14) 0.0018(11) -0.0085(12) -0.0003(12) C262 0.0429(19) 0.0488(18) 0.0315(16) 0.0083(13) 0.0049(14) -0.0045(15) C651 0.0355(17) 0.0312(15) 0.0362(16) -0.0129(13) -0.0002(14) 0.0002(13) F651 0.181(3) 0.0511(12) 0.0403(11) -0.0002(9) 0.0537(14) 0.0361(13) C521 0.0298(15) 0.0269(13) 0.0219(12) -0.0049(11) -0.0005(11) 0.0002(12) C75 0.0224(14) 0.0208(12) 0.0211(12) 0.0041(10) 0.0024(10) -0.0010(10) C16 0.0271(15) 0.0198(12) 0.0247(13) 0.0025(10) 0.0001(11) -0.0004(11) C54 0.0410(17) 0.0308(14) 0.0207(13) -0.0046(11) -0.0102(12) -0.0056(13) C76 0.0208(13) 0.0155(11) 0.0240(13) -0.0010(10) -0.0004(10) 0.0005(10) C421 0.0248(14) 0.0273(13) 0.0198(12) 0.0010(10) -0.0010(11) 0.0040(11) C83 0.0239(14) 0.0211(12) 0.0265(13) 0.0027(10) 0.0012(11) 0.0013(11) C56 0.0293(15) 0.0222(13) 0.0210(13) 0.0035(10) -0.0060(11) 0.0017(11) C25 0.0263(15) 0.0292(14) 0.0345(15) -0.0032(12) 0.0054(12) 0.0029(12) C24 0.0244(15) 0.0332(15) 0.0412(16) 0.0045(12) -0.0068(13) 0.0039(12) F831 0.0493(11) 0.0326(9) 0.0712(12) 0.0018(8) 0.0139(10) 0.0164(8) F751 0.0571(12) 0.0302(9) 0.0469(10) 0.0177(7) 0.0099(9) 0.0046(8) F832 0.0401(11) 0.0506(10) 0.0636(12) 0.0223(9) -0.0101(9) 0.0091(8) F833 0.0317(10) 0.0265(9) 0.1080(15) 0.0268(9) 0.0101(10) 0.0027(7) F752 0.0314(11) 0.0743(13) 0.1118(17) 0.0635(12) 0.0028(11) -0.0089(10) F753 0.159(2) 0.0447(11) 0.0235(9) 0.0010(8) 0.0252(11) -0.0285(12) C461 0.0265(14) 0.0228(12) 0.0181(12) -0.0014(10) -0.0007(11) 0.0040(11) O999 0.0532(16) 0.0258(11) 0.127(2) -0.0143(13) 0.0436(15) -0.0025(11) C122 0.0409(17) 0.0315(14) 0.0220(13) -0.0019(11) -0.0056(12) 0.0036(13) C121 0.0281(15) 0.0283(13) 0.0212(13) 0.0011(10) -0.0028(11) 0.0014(11) C751 0.0421(18) 0.0254(14) 0.0256(14) 0.0003(11) 0.0080(13) -0.0027(13) C123 0.052(2) 0.0400(16) 0.0214(14) 0.0002(12) 0.0052(13) -0.0061(14) C561 0.0270(15) 0.0271(14) 0.0292(14) -0.0026(11) -0.0055(12) 0.0011(11) C422 0.0261(16) 0.0471(17) 0.0397(16) 0.0065(13) -0.0007(13) 0.0032(13) C23 0.0332(16) 0.0306(14) 0.0265(14) 0.0040(11) -0.0077(12) -0.0013(12) C14 0.0206(14) 0.0341(15) 0.0407(16) 0.0059(12) -0.0058(13) 0.0003(12) C462 0.0321(16) 0.0338(15) 0.0256(14) -0.0034(11) 0.0032(12) -0.0020(12) C15 0.0284(16) 0.0271(14) 0.0333(15) 0.0011(11) 0.0066(12) 0.0044(12) C161 0.0370(17) 0.0341(15) 0.0255(14) -0.0053(12) 0.0016(12) 0.0007(13) C423 0.0379(17) 0.0306(15) 0.0361(16) 0.0034(12) -0.0013(13) 0.0088(13) C463 0.0379(18) 0.0357(15) 0.0384(16) 0.0066(13) 0.0069(14) 0.0117(13) C562 0.0442(19) 0.0369(16) 0.0396(17) 0.0018(13) -0.0041(14) 0.0112(14) C831 0.0231(16) 0.0305(15) 0.0535(19) 0.0095(13) 0.0056(14) 0.0024(12) C55 0.0288(15) 0.0304(14) 0.0280(14) 0.0025(11) -0.0085(12) -0.0010(12) C222 0.0456(19) 0.0303(14) 0.0266(14) 0.0027(11) -0.0019(13) -0.0059(13) C223 0.063(2) 0.0264(14) 0.0304(15) -0.0012(12) 0.0058(15) 0.0003(14) C263 0.063(2) 0.0491(18) 0.0257(15) -0.0041(13) 0.0004(15) -0.0153(16) C522 0.0401(19) 0.060(2) 0.0408(17) 0.0107(15) 0.0056(15) -0.0058(16) C563 0.0412(18) 0.0411(16) 0.0346(16) -0.0022(13) 0.0005(14) 0.0045(14) C998 0.085(3) 0.061(2) 0.115(4) 0.050(2) 0.076(3) 0.045(2) C999 0.048(2) 0.058(2) 0.126(4) 0.032(2) 0.028(2) 0.0110(19) C523 0.041(2) 0.0398(18) 0.088(3) 0.0182(17) 0.0047(18) 0.0063(15) C162 0.102(3) 0.076(2) 0.0228(16) -0.0016(16) 0.0062(18) -0.029(2) C163 0.087(3) 0.0382(18) 0.051(2) -0.0162(15) -0.0083(19) 0.0015(18) C997 0.127(4) 0.035(2) 0.146(4) -0.035(2) 0.107(4) -0.029(2) C996 0.060(3) 0.204(6) 0.235(7) -0.191(6) 0.004(4) -0.026(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 N3 1.854(2) . ? Ni1 C1 2.003(2) . ? Ni1 C41 2.240(2) . ? Ni1 C46 2.484(2) . ? F853 C851 1.346(3) . ? F633 C631 1.338(3) . ? F632 C631 1.347(3) . ? F852 C851 1.336(3) . ? F851 C851 1.339(3) . ? F631 C631 1.347(3) . ? N1 C1 1.363(3) . ? N1 C2 1.384(3) . ? N1 C11 1.446(3) . ? N3 C31 1.382(3) . ? C81 C86 1.397(3) . ? C81 C82 1.410(3) . ? C81 B1 1.638(3) . ? N2 C1 1.367(3) . ? N2 C3 1.386(3) . ? N2 C21 1.448(3) . ? F733 C731 1.318(3) . ? F933 C931 1.322(3) . ? C46 C45 1.403(3) . ? C46 C41 1.418(3) . ? C46 C461 1.519(3) . ? C21 C26 1.393(3) . ? C21 C22 1.401(3) . ? F953 C951 1.353(3) . ? F653 C651 1.324(3) . ? C91 C92 1.394(3) . ? C91 C96 1.399(3) . ? C91 B1 1.647(3) . ? C35 C36 1.381(3) . ? C35 C34 1.388(3) . ? C36 C31 1.415(3) . ? C36 C41 1.500(3) . ? F952 C951 1.315(3) . ? C41 C42 1.420(3) . ? C34 C33 1.382(3) . ? F951 C951 1.321(3) . ? F652 C651 1.340(3) . ? C631 C63 1.491(3) . ? C53 C54 1.377(4) . ? C53 C52 1.392(3) . ? C66 C65 1.388(3) . ? C66 C61 1.403(3) . ? C11 C16 1.399(3) . ? C11 C12 1.406(3) . ? C51 C56 1.407(3) . ? C51 C52 1.408(3) . ? C51 C32 1.494(3) . ? C62 C63 1.391(3) . ? C62 C61 1.398(3) . ? C71 C76 1.397(3) . ? C71 C72 1.400(3) . ? C71 B1 1.650(3) . ? C93 C94 1.390(3) . ? C93 C92 1.396(3) . ? C93 C931 1.491(3) . ? C86 C85 1.385(3) . ? C22 C23 1.393(3) . ? C22 C221 1.529(3) . ? C42 C43 1.402(3) . ? C42 C421 1.515(3) . ? C72 C73 1.387(3) . ? F932 C931 1.331(3) . ? C32 C33 1.399(3) . ? C32 C31 1.414(3) . ? C52 C521 1.515(3) . ? C3 C2 1.333(3) . ? C65 C64 1.385(3) . ? C65 C651 1.496(3) . ? C85 C84 1.380(3) . ? C85 C851 1.504(3) . ? C12 C13 1.389(3) . ? C12 C121 1.526(3) . ? C82 C83 1.381(3) . ? F732 C731 1.300(3) . ? C26 C25 1.389(3) . ? C26 C261 1.528(3) . ? C61 B1 1.639(3) . ? C221 C222 1.514(3) . ? C221 C223 1.544(3) . ? C261 C262 1.516(3) . ? C261 C263 1.527(3) . ? C95 C94 1.387(3) . ? C95 C96 1.390(3) . ? C95 C951 1.489(3) . ? C73 C74 1.386(3) . ? C73 C731 1.496(3) . ? F931 C931 1.326(3) . ? C63 C64 1.384(3) . ? C731 F731 1.297(3) . ? C43 C44 1.381(3) . ? C74 C75 1.388(3) . ? C84 C83 1.391(3) . ? C45 C44 1.383(3) . ? C13 C14 1.377(3) . ? C651 F651 1.303(3) . ? C521 C522 1.517(3) . ? C521 C523 1.532(3) . ? C75 C76 1.381(3) . ? C75 C751 1.496(3) . ? C16 C15 1.391(3) . ? C16 C161 1.517(3) . ? C54 C55 1.381(3) . ? C421 C422 1.527(3) . ? C421 C423 1.540(3) . ? C83 C831 1.499(3) . ? C56 C55 1.395(3) . ? C56 C561 1.524(3) . ? C25 C24 1.385(3) . ? C24 C23 1.372(4) . ? F831 C831 1.337(3) . ? F751 C751 1.330(3) . ? F832 C831 1.346(3) . ? F833 C831 1.338(3) . ? F752 C751 1.320(3) . ? F753 C751 1.321(3) . ? C461 C463 1.517(3) . ? C461 C462 1.532(3) . ? O999 C997 1.403(5) . ? O999 C998 1.440(5) . ? C122 C121 1.542(3) . ? C121 C123 1.534(3) . ? C561 C563 1.522(3) . ? C561 C562 1.531(3) . ? C14 C15 1.378(3) . ? C161 C162 1.520(4) . ? C161 C163 1.534(4) . ? C998 C999 1.472(5) . ? C997 C996 1.468(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni1 C1 116.57(9) . . ? N3 Ni1 C41 81.16(8) . . ? C1 Ni1 C41 162.17(8) . . ? N3 Ni1 C46 101.03(8) . . ? C1 Ni1 C46 132.28(9) . . ? C41 Ni1 C46 34.45(8) . . ? C1 N1 C2 111.5(2) . . ? C1 N1 C11 129.04(19) . . ? C2 N1 C11 119.36(19) . . ? C31 N3 Ni1 121.95(16) . . ? C86 C81 C82 114.9(2) . . ? C86 C81 B1 124.05(19) . . ? C82 C81 B1 120.9(2) . . ? C1 N2 C3 112.0(2) . . ? C1 N2 C21 126.64(18) . . ? C3 N2 C21 121.24(19) . . ? C45 C46 C41 118.0(2) . . ? C45 C46 C461 121.1(2) . . ? C41 C46 C461 120.60(19) . . ? C45 C46 Ni1 93.67(15) . . ? C41 C46 Ni1 63.29(12) . . ? C461 C46 Ni1 116.94(14) . . ? N1 C1 N2 102.80(18) . . ? N1 C1 Ni1 130.47(17) . . ? N2 C1 Ni1 126.59(17) . . ? C26 C21 C22 123.6(2) . . ? C26 C21 N2 118.0(2) . . ? C22 C21 N2 118.2(2) . . ? C92 C91 C96 115.5(2) . . ? C92 C91 B1 122.2(2) . . ? C96 C91 B1 122.23(19) . . ? C36 C35 C34 119.8(2) . . ? C35 C36 C31 120.7(2) . . ? C35 C36 C41 123.08(19) . . ? C31 C36 C41 116.18(19) . . ? C46 C41 C42 121.1(2) . . ? C46 C41 C36 119.8(2) . . ? C42 C41 C36 119.1(2) . . ? C46 C41 Ni1 82.26(13) . . ? C42 C41 Ni1 84.20(13) . . ? C36 C41 Ni1 104.55(13) . . ? C33 C34 C35 120.2(2) . . ? F633 C631 F632 106.8(2) . . ? F633 C631 F631 106.43(19) . . ? F632 C631 F631 105.36(19) . . ? F633 C631 C63 113.3(2) . . ? F632 C631 C63 112.38(19) . . ? F631 C631 C63 112.1(2) . . ? C54 C53 C52 121.4(2) . . ? C65 C66 C61 122.1(2) . . ? C16 C11 C12 123.2(2) . . ? C16 C11 N1 117.5(2) . . ? C12 C11 N1 118.8(2) . . ? C56 C51 C52 120.8(2) . . ? C56 C51 C32 117.8(2) . . ? C52 C51 C32 121.2(2) . . ? C63 C62 C61 122.7(2) . . ? C76 C71 C72 115.4(2) . . ? C76 C71 B1 124.07(19) . . ? C72 C71 B1 120.49(19) . . ? C94 C93 C92 120.9(2) . . ? C94 C93 C931 120.8(2) . . ? C92 C93 C931 118.2(2) . . ? C91 C92 C93 122.3(2) . . ? C85 C86 C81 122.7(2) . . ? C23 C22 C21 116.7(2) . . ? C23 C22 C221 121.8(2) . . ? C21 C22 C221 121.4(2) . . ? C43 C42 C41 117.8(2) . . ? C43 C42 C421 120.8(2) . . ? C41 C42 C421 121.1(2) . . ? C73 C72 C71 122.4(2) . . ? C33 C32 C31 118.3(2) . . ? C33 C32 C51 118.31(19) . . ? C31 C32 C51 123.0(2) . . ? N3 C31 C32 125.0(2) . . ? N3 C31 C36 115.70(19) . . ? C32 C31 C36 119.3(2) . . ? C34 C33 C32 121.6(2) . . ? C53 C52 C51 118.1(2) . . ? C53 C52 C521 120.3(2) . . ? C51 C52 C521 121.5(2) . . ? C2 C3 N2 106.2(2) . . ? C64 C65 C66 121.3(2) . . ? C64 C65 C651 120.2(2) . . ? C66 C65 C651 118.5(2) . . ? C84 C85 C86 121.1(2) . . ? C84 C85 C851 120.1(2) . . ? C86 C85 C851 118.8(2) . . ? C13 C12 C11 116.4(2) . . ? C13 C12 C121 121.3(2) . . ? C11 C12 C121 122.3(2) . . ? C83 C82 C81 122.7(2) . . ? C25 C26 C21 116.8(2) . . ? C25 C26 C261 121.9(2) . . ? C21 C26 C261 121.3(2) . . ? C62 C61 C66 115.4(2) . . ? C62 C61 B1 122.05(19) . . ? C66 C61 B1 122.5(2) . . ? C222 C221 C22 113.4(2) . . ? C222 C221 C223 108.1(2) . . ? C22 C221 C223 111.1(2) . . ? C262 C261 C263 110.7(2) . . ? C262 C261 C26 113.3(2) . . ? C263 C261 C26 110.9(2) . . ? C94 C95 C96 120.6(2) . . ? C94 C95 C951 120.4(2) . . ? C96 C95 C951 119.0(2) . . ? C74 C73 C72 120.7(2) . . ? C74 C73 C731 120.0(2) . . ? C72 C73 C731 119.3(2) . . ? C3 C2 N1 107.4(2) . . ? C81 B1 C61 111.91(18) . . ? C81 B1 C91 113.15(18) . . ? C61 B1 C91 105.26(18) . . ? C81 B1 C71 105.60(18) . . ? C61 B1 C71 111.60(18) . . ? C91 B1 C71 109.43(18) . . ? F933 C931 F931 106.1(2) . . ? F933 C931 F932 106.2(2) . . ? F931 C931 F932 105.9(2) . . ? F933 C931 C93 113.6(2) . . ? F931 C931 C93 112.3(2) . . ? F932 C931 C93 112.1(2) . . ? C64 C63 C62 120.8(2) . . ? C64 C63 C631 120.5(2) . . ? C62 C63 C631 118.8(2) . . ? F731 C731 F732 106.2(2) . . ? F731 C731 F733 105.6(2) . . ? F732 C731 F733 104.6(2) . . ? F731 C731 C73 113.2(2) . . ? F732 C731 C73 112.7(2) . . ? F733 C731 C73 113.8(2) . . ? C44 C43 C42 121.5(2) . . ? C73 C74 C75 118.0(2) . . ? C95 C96 C91 122.8(2) . . ? C63 C64 C65 117.7(2) . . ? C95 C94 C93 117.8(2) . . ? C85 C84 C83 117.9(2) . . ? F852 C851 F851 107.0(2) . . ? F852 C851 F853 106.26(19) . . ? F851 C851 F853 105.33(19) . . ? F852 C851 C85 113.2(2) . . ? F851 C851 C85 112.66(19) . . ? F853 C851 C85 111.8(2) . . ? F952 C951 F951 108.0(2) . . ? F952 C951 F953 104.3(2) . . ? F951 C951 F953 103.7(2) . . ? F952 C951 C95 113.7(2) . . ? F951 C951 C95 114.1(2) . . ? F953 C951 C95 112.1(2) . . ? C44 C45 C46 121.3(2) . . ? C43 C44 C45 120.2(2) . . ? C14 C13 C12 121.7(2) . . ? F651 C651 F653 108.4(2) . . ? F651 C651 F652 105.7(2) . . ? F653 C651 F652 104.2(2) . . ? F651 C651 C65 113.0(2) . . ? F653 C651 C65 113.5(2) . . ? F652 C651 C65 111.5(2) . . ? C52 C521 C522 111.3(2) . . ? C52 C521 C523 112.4(2) . . ? C522 C521 C523 109.2(2) . . ? C76 C75 C74 120.7(2) . . ? C76 C75 C751 119.7(2) . . ? C74 C75 C751 119.5(2) . . ? C15 C16 C11 117.3(2) . . ? C15 C16 C161 119.7(2) . . ? C11 C16 C161 123.0(2) . . ? C53 C54 C55 120.2(2) . . ? C75 C76 C71 122.7(2) . . ? C42 C421 C422 114.0(2) . . ? C42 C421 C423 108.6(2) . . ? C422 C421 C423 110.8(2) . . ? C82 C83 C84 120.7(2) . . ? C82 C83 C831 121.3(2) . . ? C84 C83 C831 118.0(2) . . ? C55 C56 C51 118.7(2) . . ? C55 C56 C561 119.0(2) . . ? C51 C56 C561 122.3(2) . . ? C24 C25 C26 120.9(2) . . ? C23 C24 C25 120.8(2) . . ? C463 C461 C46 113.23(19) . . ? C463 C461 C462 110.8(2) . . ? C46 C461 C462 109.83(18) . . ? C997 O999 C998 113.1(3) . . ? C12 C121 C123 111.4(2) . . ? C12 C121 C122 112.7(2) . . ? C123 C121 C122 108.34(19) . . ? F752 C751 F753 107.8(2) . . ? F752 C751 F751 105.1(2) . . ? F753 C751 F751 105.0(2) . . ? F752 C751 C75 112.3(2) . . ? F753 C751 C75 113.4(2) . . ? F751 C751 C75 112.6(2) . . ? C563 C561 C56 111.3(2) . . ? C563 C561 C562 111.4(2) . . ? C56 C561 C562 111.4(2) . . ? C24 C23 C22 120.9(2) . . ? C13 C14 C15 120.5(2) . . ? C14 C15 C16 120.9(2) . . ? C16 C161 C162 111.9(2) . . ? C16 C161 C163 109.9(2) . . ? C162 C161 C163 110.3(2) . . ? F831 C831 F833 107.1(2) . . ? F831 C831 F832 105.5(2) . . ? F833 C831 F832 106.2(2) . . ? F831 C831 C83 111.8(2) . . ? F833 C831 C83 113.3(2) . . ? F832 C831 C83 112.5(2) . . ? C54 C55 C56 120.7(2) . . ? O999 C998 C999 110.0(3) . . ? O999 C997 C996 110.4(3) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.735 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.066