Supplementary Material (ESI) for Chemical Science This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1475 loop_ _publ_author_name 'Hillhouse, Gregory' 'Laskowski, Carl' _publ_contact_author_name 'Hillhouse, Gregory' _publ_contact_author_email g-hillhouse@uchicago.edu _publ_section_title ; Synthesis and carbene-transfer reactivity of dimeric nickel carbene cations supported by N-heterocyclic carbene ligands ; # Attachment 'Carbene.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 791319' #TrackingRef 'Carbene.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H96 B Cl3 F24 N4 Ni2' _chemical_formula_weight 2044.39 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.022(3) _cell_length_b 18.047(4) _cell_length_c 20.367(4) _cell_angle_alpha 105.350(4) _cell_angle_beta 111.153(4) _cell_angle_gamma 100.049(4) _cell_volume 4736.7(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour green _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 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4364 _exptl_absorpt_correction_T_max 0.6757 _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 24831 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.1288 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16471 _reflns_number_gt 9484 _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^)+(0.0944P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16471 _refine_ls_number_parameters 1223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1157 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1866 _refine_ls_wR_factor_gt 0.1728 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _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 Ni2 Ni 0.21506(5) 0.41135(4) 0.27708(4) 0.02120(18) Uani 1 1 d . . . Ni1 Ni 0.15705(5) 0.52816(4) 0.27164(4) 0.02057(18) Uani 1 1 d . . . Cl1 Cl 0.22846(10) 0.50286(8) 0.37643(7) 0.0285(3) Uani 1 1 d . . . N1 N 0.0349(3) 0.6399(2) 0.2849(2) 0.0203(10) Uani 1 1 d . . . N3 N 0.2261(3) 0.2502(2) 0.2716(2) 0.0198(10) Uani 1 1 d . . . C12 C -0.0909(4) 0.5246(3) 0.2714(3) 0.0239(12) Uani 1 1 d . . . C5 C 0.2897(4) 0.2027(3) 0.2717(3) 0.0270(13) Uani 1 1 d . . . H5A H 0.2828 0.1524 0.2788 0.032 Uiso 1 1 calc R . . C2 C 0.2595(3) 0.3191(3) 0.2615(3) 0.0206(12) Uani 1 1 d . . . C3 C 0.0411(4) 0.7199(3) 0.3199(3) 0.0242(12) Uani 1 1 d . . . H3A H -0.0128 0.7423 0.3124 0.029 Uiso 1 1 calc R . . C1 C 0.1271(4) 0.6290(3) 0.3093(3) 0.0216(12) Uani 1 1 d . . . N2 N 0.1897(3) 0.7020(3) 0.3591(2) 0.0213(10) Uani 1 1 d . . . C4 C 0.1371(4) 0.7583(3) 0.3658(3) 0.0256(12) Uani 1 1 d . . . H4A H 0.1648 0.8136 0.3971 0.031 Uiso 1 1 calc R . . C11 C -0.0588(3) 0.5770(3) 0.2390(3) 0.0190(11) Uani 1 1 d . . . C35 C 0.0238(4) 0.2190(3) 0.3333(3) 0.0266(13) Uani 1 1 d . . . H35A H 0.0121 0.2378 0.3767 0.032 Uiso 1 1 calc R . . C51 C 0.1670(4) 0.4852(3) 0.1671(3) 0.0215(12) Uani 1 1 d . . . C56 C 0.1126(4) 0.5390(3) 0.1513(3) 0.0246(12) Uani 1 1 d . . . H55A H 0.0402 0.5110 0.1167 0.029 Uiso 1 1 calc R . . C31 C 0.1296(3) 0.2215(3) 0.2710(3) 0.0195(11) Uani 1 1 d . . . C32 C 0.0528(4) 0.1674(3) 0.2032(3) 0.0233(12) Uani 1 1 d . . . C16 C -0.1156(4) 0.5719(3) 0.1658(3) 0.0263(13) Uani 1 1 d . . . C15 C -0.2054(4) 0.5117(4) 0.1235(3) 0.0351(14) Uani 1 1 d . . . H15A H -0.2448 0.5067 0.0733 0.042 Uiso 1 1 calc R . . C34 C -0.0524(4) 0.1652(3) 0.2691(3) 0.0290(13) Uani 1 1 d . . . H34A H -0.1156 0.1453 0.2687 0.035 Uiso 1 1 calc R . . C52 C 0.2641(4) 0.5006(3) 0.1678(3) 0.0281(13) Uani 1 1 d . . . H53A H 0.3040 0.4670 0.1815 0.034 Uiso 1 1 calc R . . C13 C -0.1821(4) 0.4650(3) 0.2271(3) 0.0301(14) Uani 1 1 d . . . H13A H -0.2060 0.4284 0.2473 0.036 Uiso 1 1 calc R . . C55 C 0.1529(4) 0.6040(3) 0.1347(3) 0.0311(14) Uani 1 1 d . . . H56A H 0.1164 0.6409 0.1249 0.037 Uiso 1 1 calc R . . C36 C 0.1197(4) 0.2482(3) 0.3381(3) 0.0207(12) Uani 1 1 d . . . C6 C 0.3631(4) 0.2425(3) 0.2596(3) 0.0288(13) Uani 1 1 d . . . H6A H 0.4182 0.2255 0.2564 0.035 Uiso 1 1 calc R . . C26 C 0.3729(4) 0.7344(3) 0.3968(3) 0.0282(13) Uani 1 1 d . . . C321 C 0.0666(4) 0.1387(3) 0.1318(3) 0.0284(13) Uani 1 1 d . . . H32A H 0.1317 0.1745 0.1403 0.034 Uiso 1 1 calc R . . C161 C -0.0845(4) 0.6327(4) 0.1324(3) 0.0326(14) Uani 1 1 d . . . H16A H -0.0113 0.6613 0.1633 0.039 Uiso 1 1 calc R . . C21 C 0.2911(4) 0.7178(3) 0.4150(3) 0.0234(12) Uani 1 1 d . . . C53 C 0.2994(4) 0.5614(3) 0.1495(3) 0.0301(14) Uani 1 1 d . . . H52A H 0.3627 0.5687 0.1479 0.036 Uiso 1 1 calc R . . F653 F 1.0025(2) 0.9233(2) 0.19487(19) 0.0445(9) Uani 1 1 d . . . F652 F 1.1377(2) 1.0044(2) 0.2883(2) 0.0518(10) Uani 1 1 d . . . F651 F 1.0743(3) 0.8896(2) 0.2886(2) 0.0524(10) Uani 1 1 d . . . C651 C 1.0515(4) 0.9509(4) 0.2694(3) 0.0319(14) Uani 1 1 d . . . C84 C 0.6497(4) 1.1052(4) 0.0990(3) 0.0334(14) Uani 1 1 d . . . H84A H 0.6370 1.1353 0.0666 0.040 Uiso 1 1 calc R . . C64 C 1.0400(4) 1.0375(3) 0.3813(3) 0.0252(13) Uani 1 1 d . . . H64A H 1.1106 1.0514 0.4079 0.030 Uiso 1 1 calc R . . C71 C 0.6466(3) 0.9832(3) 0.3076(3) 0.0225(12) Uani 1 1 d . . . C65 C 0.9920(4) 0.9872(3) 0.3085(3) 0.0236(12) Uani 1 1 d . . . C61 C 0.8289(4) 0.9951(3) 0.3039(3) 0.0221(12) Uani 1 1 d . . . N4 N 0.3437(3) 0.3125(3) 0.2526(2) 0.0241(10) Uani 1 1 d . . . B1 B 0.7063(4) 0.9651(4) 0.2540(4) 0.0260(15) Uani 1 1 d . . . C72 C 0.6789(4) 0.9763(3) 0.3777(3) 0.0276(13) Uani 1 1 d . . . H72A H 0.7369 0.9594 0.3947 0.033 Uiso 1 1 calc R . . C513 C -0.1358(4) 0.3200(4) 0.0451(3) 0.0368(15) Uani 1 1 d . . . H51A H -0.1754 0.3144 -0.0053 0.044 Uiso 1 1 calc R . . C362 C 0.1804(4) 0.3569(4) 0.4660(3) 0.0365(15) Uani 1 1 d . . . H36A H 0.1452 0.3893 0.4407 0.055 Uiso 1 1 calc R . . H36B H 0.2414 0.3924 0.5105 0.055 Uiso 1 1 calc R . . H36C H 0.1369 0.3256 0.4815 0.055 Uiso 1 1 calc R . . C81 C 0.6835(4) 1.0131(3) 0.1954(3) 0.0259(13) Uani 1 1 d . . . C512 C -0.0358(4) 0.3636(3) 0.0800(3) 0.0286(13) Uani 1 1 d . . . H51B H -0.0069 0.3864 0.0526 0.034 Uiso 1 1 calc R . . C63 C 0.9836(4) 1.0682(3) 0.4160(3) 0.0229(12) Uani 1 1 d . . . C514 C -0.1787(4) 0.2842(3) 0.0838(3) 0.0340(14) Uani 1 1 d . . . H51C H -0.2475 0.2539 0.0597 0.041 Uiso 1 1 calc R . . C22 C 0.3026(4) 0.7191(3) 0.4853(3) 0.0267(13) Uani 1 1 d . . . C62 C 0.8801(4) 1.0477(3) 0.3763(3) 0.0240(12) Uani 1 1 d . . . H62A H 0.8436 1.0714 0.4009 0.029 Uiso 1 1 calc R . . C33 C -0.0394(4) 0.1390(3) 0.2047(3) 0.0297(13) Uani 1 1 d . . . H33A H -0.0939 0.1010 0.1601 0.036 Uiso 1 1 calc R . . C361 C 0.2078(4) 0.3001(3) 0.4123(3) 0.0248(12) Uani 1 1 d . . . H36D H 0.2576 0.3332 0.4014 0.030 Uiso 1 1 calc R . . C515 C -0.1219(4) 0.2929(3) 0.1557(3) 0.0289(13) Uani 1 1 d . . . H51D H -0.1510 0.2683 0.1820 0.035 Uiso 1 1 calc R . . C363 C 0.2575(4) 0.2453(3) 0.4497(3) 0.0316(14) Uani 1 1 d . . . H36E H 0.2763 0.2096 0.4150 0.047 Uiso 1 1 calc R . . H36F H 0.2104 0.2129 0.4618 0.047 Uiso 1 1 calc R . . H36G H 0.3174 0.2784 0.4961 0.047 Uiso 1 1 calc R . . C92 C 0.5841(4) 0.8220(4) 0.1454(3) 0.0301(14) Uani 1 1 d . . . H92A H 0.5508 0.8499 0.1156 0.036 Uiso 1 1 calc R . . C162 C -0.1014(4) 0.5946(4) 0.0516(3) 0.0403(16) Uani 1 1 d . . . H16B H -0.0708 0.5509 0.0473 0.060 Uiso 1 1 calc R . . H16C H -0.0710 0.6353 0.0360 0.060 Uiso 1 1 calc R . . H16D H -0.1735 0.5730 0.0190 0.060 Uiso 1 1 calc R . . C54 C 0.2441(4) 0.6151(3) 0.1324(3) 0.0322(14) Uani 1 1 d . . . H51E H 0.2699 0.6583 0.1196 0.039 Uiso 1 1 calc R . . C83 C 0.6611(4) 1.0293(4) 0.0749(3) 0.0341(14) Uani 1 1 d . . . C85 C 0.6575(4) 1.1356(3) 0.1712(3) 0.0270(13) Uani 1 1 d . . . C511 C 0.0235(4) 0.3750(3) 0.1542(3) 0.0240(12) Uani 1 1 d . . . C24 C 0.4804(4) 0.7522(4) 0.5245(4) 0.0419(16) Uani 1 1 d . . . H24A H 0.5459 0.7631 0.5621 0.050 Uiso 1 1 calc R . . C86 C 0.6738(3) 1.0913(3) 0.2177(3) 0.0276(13) Uani 1 1 d . . . H86A H 0.6788 1.1143 0.2670 0.033 Uiso 1 1 calc R . . C122 C -0.0434(4) 0.4568(3) 0.3686(3) 0.0368(15) Uani 1 1 d . . . H12A H -0.0204 0.4206 0.3377 0.055 Uiso 1 1 calc R . . H12B H -0.1133 0.4309 0.3563 0.055 Uiso 1 1 calc R . . H12C H -0.0019 0.4685 0.4221 0.055 Uiso 1 1 calc R . . C82 C 0.6774(4) 0.9852(4) 0.1221(3) 0.0296(13) Uani 1 1 d . . . H82A H 0.6847 0.9334 0.1040 0.036 Uiso 1 1 calc R . . C50 C 0.1290(3) 0.4250(3) 0.1939(3) 0.0201(12) Uani 1 1 d . . . C25 C 0.4665(4) 0.7506(3) 0.4534(3) 0.0353(15) Uani 1 1 d . . . H25A H 0.5233 0.7610 0.4431 0.042 Uiso 1 1 calc R . . C91 C 0.6675(4) 0.8662(3) 0.2150(3) 0.0262(13) Uani 1 1 d . . . C14 C -0.2388(4) 0.4583(4) 0.1534(4) 0.0387(15) Uani 1 1 d . . . H14A H -0.3008 0.4169 0.1236 0.046 Uiso 1 1 calc R . . C121 C -0.0350(4) 0.5347(3) 0.3529(3) 0.0259(13) Uani 1 1 d . . . H12D H 0.0375 0.5612 0.3688 0.031 Uiso 1 1 calc R . . C76 C 0.5567(4) 1.0025(3) 0.2839(3) 0.0263(13) Uani 1 1 d . . . H76A H 0.5285 1.0049 0.2348 0.032 Uiso 1 1 calc R . . F851 F 0.5716(3) 1.2127(2) 0.2223(3) 0.0676(12) Uani 1 1 d . . . F852 F 0.7276(3) 1.2677(2) 0.2596(2) 0.0532(10) Uani 1 1 d . . . F853 F 0.6262(3) 1.2526(2) 0.1497(2) 0.0574(11) Uani 1 1 d . . . C74 C 0.5451(4) 1.0167(3) 0.4006(3) 0.0295(14) Uani 1 1 d . . . H74A H 0.5138 1.0314 0.4329 0.035 Uiso 1 1 calc R . . C41 C 0.4027(4) 0.3677(3) 0.2326(3) 0.0289(14) Uani 1 1 d . . . C66 C 0.8884(4) 0.9644(3) 0.2699(3) 0.0265(13) Uani 1 1 d . . . H66A H 0.8567 0.9272 0.2195 0.032 Uiso 1 1 calc R . . C516 C -0.0216(4) 0.3373(3) 0.1914(3) 0.0244(12) Uani 1 1 d . . . H51F H 0.0174 0.3423 0.2418 0.029 Uiso 1 1 calc R . . C95 C 0.6743(4) 0.7384(3) 0.2309(3) 0.0280(13) Uani 1 1 d . . . C75 C 0.5074(4) 1.0183(3) 0.3296(3) 0.0273(13) Uani 1 1 d . . . C43 C 0.5271(4) 0.4879(4) 0.2650(4) 0.0436(17) Uani 1 1 d . . . H43A H 0.5743 0.5379 0.3007 0.052 Uiso 1 1 calc R . . C42 C 0.4702(4) 0.4394(3) 0.2874(3) 0.0303(14) Uani 1 1 d . . . C221 C 0.2147(4) 0.7046(3) 0.5072(3) 0.0283(13) Uani 1 1 d . . . H22A H 0.1513 0.6855 0.4600 0.034 Uiso 1 1 calc R . . C46 C 0.3882(4) 0.3423(3) 0.1573(4) 0.0352(15) Uani 1 1 d . . . C93 C 0.5492(4) 0.7377(4) 0.1193(3) 0.0362(16) Uani 1 1 d . . . C94 C 0.5944(4) 0.6949(4) 0.1624(3) 0.0364(15) Uani 1 1 d . . . H94A H 0.5708 0.6377 0.1451 0.044 Uiso 1 1 calc R . . C851 C 0.6454(4) 1.2162(4) 0.1996(4) 0.0371(15) Uani 1 1 d . . . C222 C 0.2162(5) 0.7837(4) 0.5591(3) 0.0447(17) Uani 1 1 d . . . H22B H 0.1592 0.7743 0.5717 0.067 Uiso 1 1 calc R . . H22C H 0.2117 0.8228 0.5335 0.067 Uiso 1 1 calc R . . H22D H 0.2786 0.8049 0.6054 0.067 Uiso 1 1 calc R . . C23 C 0.3985(4) 0.7380(3) 0.5412(3) 0.0350(14) Uani 1 1 d . . . H23A H 0.4082 0.7412 0.5907 0.042 Uiso 1 1 calc R . . C163 C -0.1416(4) 0.6965(4) 0.1367(3) 0.0394(15) Uani 1 1 d . . . H16E H -0.1283 0.7236 0.1893 0.059 Uiso 1 1 calc R . . H16F H -0.2135 0.6698 0.1067 0.059 Uiso 1 1 calc R . . H16G H -0.1189 0.7363 0.1169 0.059 Uiso 1 1 calc R . . C421 C 0.4860(4) 0.4643(3) 0.3670(3) 0.0369(15) Uani 1 1 d . . . H42A H 0.4269 0.4313 0.3690 0.044 Uiso 1 1 calc R . . C44 C 0.5159(5) 0.4646(4) 0.1922(5) 0.057(2) Uani 1 1 d . . . H44A H 0.5563 0.4984 0.1785 0.068 Uiso 1 1 calc R . . C322 C 0.0736(5) 0.0517(3) 0.1142(3) 0.0397(15) Uani 1 1 d . . . H32B H 0.1264 0.0485 0.1580 0.059 Uiso 1 1 calc R . . H32C H 0.0895 0.0368 0.0707 0.059 Uiso 1 1 calc R . . H32D H 0.0095 0.0146 0.1026 0.059 Uiso 1 1 calc R . . F951 F 0.8220(2) 0.72931(19) 0.32035(19) 0.0404(8) Uani 1 1 d . . . F731 F 0.7721(2) 1.0351(2) 0.54128(18) 0.0438(9) Uani 1 1 d . . . F931 F 0.4421(3) 0.7322(3) 0.0008(2) 0.0832(17) Uani 1 1 d . . . F932 F 0.3802(2) 0.6618(2) 0.05055(18) 0.0533(11) Uani 1 1 d . . . F733 F 0.6799(3) 0.9149(2) 0.4990(2) 0.0647(12) Uani 1 1 d . . . F831 F 0.5890(3) 0.9233(3) -0.04196(19) 0.0548(10) Uani 1 1 d . . . F952 F 0.6860(3) 0.6913(2) 0.3302(2) 0.0577(11) Uani 1 1 d . . . F832 F 0.7436(3) 0.9827(3) 0.0013(2) 0.0773(14) Uani 1 1 d . . . F953 F 0.7111(3) 0.6181(2) 0.2416(2) 0.0606(11) Uani 1 1 d . . . F751 F 0.3912(3) 1.0808(3) 0.3536(2) 0.0691(13) Uani 1 1 d . . . F933 F 0.4809(3) 0.6247(3) 0.0061(2) 0.0971(18) Uani 1 1 d . . . F732 F 0.6302(3) 1.0138(3) 0.5432(2) 0.0865(17) Uani 1 1 d . . . F752 F 0.4086(3) 1.0778(3) 0.2545(3) 0.105(2) Uani 1 1 d . . . F753 F 0.3333(3) 0.9747(3) 0.2633(3) 0.0919(17) Uani 1 1 d . . . C731 C 0.6766(4) 0.9892(4) 0.5008(3) 0.0347(15) Uani 1 1 d . . . F833 F 0.6354(5) 1.0407(3) -0.0421(3) 0.1061(19) Uani 1 1 d . . . C951 C 0.7231(4) 0.6940(4) 0.2796(4) 0.0367(15) Uani 1 1 d . . . C73 C 0.6316(4) 0.9926(3) 0.4247(3) 0.0246(12) Uani 1 1 d . . . C261 C 0.3581(4) 0.7382(4) 0.3212(3) 0.0333(14) Uani 1 1 d . . . H26A H 0.2992 0.6917 0.2820 0.040 Uiso 1 1 calc R . . C96 C 0.7117(4) 0.8214(3) 0.2564(3) 0.0261(13) Uani 1 1 d . . . H96A H 0.7689 0.8486 0.3032 0.031 Uiso 1 1 calc R . . C461 C 0.3092(4) 0.2658(4) 0.0972(3) 0.0362(15) Uani 1 1 d . . . H46A H 0.3036 0.2241 0.1206 0.043 Uiso 1 1 calc R . . C45 C 0.4486(5) 0.3944(4) 0.1390(4) 0.0498(18) Uani 1 1 d . . . H45A H 0.4422 0.3802 0.0888 0.060 Uiso 1 1 calc R . . C323 C -0.0148(4) 0.1440(3) 0.0640(3) 0.0345(14) Uani 1 1 d . . . H32E H -0.0167 0.1998 0.0744 0.052 Uiso 1 1 calc R . . H32F H -0.0796 0.1090 0.0539 0.052 Uiso 1 1 calc R . . H32G H -0.0006 0.1266 0.0200 0.052 Uiso 1 1 calc R . . C751 C 0.4109(4) 1.0374(4) 0.2994(4) 0.0384(16) Uani 1 1 d . . . C262 C 0.4502(4) 0.7318(4) 0.3049(4) 0.0503(18) Uani 1 1 d . . . H26B H 0.4681 0.6843 0.3131 0.076 Uiso 1 1 calc R . . H26C H 0.5067 0.7802 0.3388 0.076 Uiso 1 1 calc R . . H26D H 0.4339 0.7269 0.2525 0.076 Uiso 1 1 calc R . . C263 C 0.3358(5) 0.8154(4) 0.3140(4) 0.0500(18) Uani 1 1 d . . . H26E H 0.2720 0.8160 0.3166 0.075 Uiso 1 1 calc R . . H26F H 0.3315 0.8182 0.2655 0.075 Uiso 1 1 calc R . . H26G H 0.3894 0.8619 0.3551 0.075 Uiso 1 1 calc R . . C123 C -0.0706(5) 0.5906(4) 0.4014(3) 0.0409(16) Uani 1 1 d . . . H12E H -0.0614 0.6423 0.3938 0.061 Uiso 1 1 calc R . . H12F H -0.0316 0.5994 0.4546 0.061 Uiso 1 1 calc R . . H12G H -0.1416 0.5661 0.3870 0.061 Uiso 1 1 calc R . . C462 C 0.2062(4) 0.2820(4) 0.0673(3) 0.0408(16) Uani 1 1 d . . . H46B H 0.1882 0.3007 0.1092 0.061 Uiso 1 1 calc R . . H46C H 0.1550 0.2321 0.0293 0.061 Uiso 1 1 calc R . . H46D H 0.2105 0.3233 0.0447 0.061 Uiso 1 1 calc R . . C223 C 0.2134(4) 0.6399(4) 0.5429(3) 0.0404(16) Uani 1 1 d . . . H22E H 0.1539 0.6308 0.5526 0.061 Uiso 1 1 calc R . . H22F H 0.2736 0.6579 0.5905 0.061 Uiso 1 1 calc R . . H22G H 0.2121 0.5897 0.5085 0.061 Uiso 1 1 calc R . . C831 C 0.6565(5) 0.9962(4) -0.0009(4) 0.0457(17) Uani 1 1 d . . . C422 C 0.4943(5) 0.5536(4) 0.4011(4) 0.0508(18) Uani 1 1 d . . . H42B H 0.4346 0.5645 0.3702 0.076 Uiso 1 1 calc R . . H42C H 0.5538 0.5876 0.4024 0.076 Uiso 1 1 calc R . . H42D H 0.4997 0.5655 0.4525 0.076 Uiso 1 1 calc R . . C931 C 0.4636(5) 0.6930(5) 0.0461(4) 0.056(2) Uani 1 1 d . . . C463 C 0.3317(5) 0.2312(4) 0.0290(4) 0.057(2) Uani 1 1 d . . . H46E H 0.3984 0.2239 0.0467 0.086 Uiso 1 1 calc R . . H46F H 0.3294 0.2686 0.0016 0.086 Uiso 1 1 calc R . . H46G H 0.2815 0.1791 -0.0047 0.086 Uiso 1 1 calc R . . C423 C 0.5793(5) 0.4438(5) 0.4129(4) 0.071(2) Uani 1 1 d . . . H42E H 0.5681 0.3856 0.3932 0.107 Uiso 1 1 calc R . . H42F H 0.5913 0.4609 0.4659 0.107 Uiso 1 1 calc R . . H42G H 0.6377 0.4720 0.4085 0.107 Uiso 1 1 calc R . . Cl99 Cl 0.66684(12) 1.16494(11) -0.12535(10) 0.0548(5) Uani 1 1 d . . . Cl98 Cl 0.86503(14) 1.18463(13) -0.12484(11) 0.0684(6) Uani 1 1 d . . . F631 F 1.0375(2) 1.20014(19) 0.50522(18) 0.0424(9) Uani 1 1 d . . . F632 F 0.9835(3) 1.1040(2) 0.53609(18) 0.0494(10) Uani 1 1 d . . . F633 F 1.1264(2) 1.1231(2) 0.53377(18) 0.0512(10) Uani 1 1 d . . . C631 C 1.0321(4) 1.1232(4) 0.4969(3) 0.0307(14) Uani 1 1 d . . . C999 C 0.7777(5) 1.1367(4) -0.0962(4) 0.0546(19) Uani 1 1 d . . . H99A H 0.7613 1.0775 -0.1187 0.066 Uiso 1 1 calc R . . H99B H 0.8085 1.1524 -0.0407 0.066 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 Ni2 0.0187(4) 0.0201(4) 0.0364(4) 0.0134(3) 0.0181(3) 0.0139(3) Ni1 0.0191(4) 0.0191(4) 0.0356(4) 0.0131(3) 0.0189(3) 0.0135(3) Cl1 0.0313(7) 0.0264(8) 0.0360(8) 0.0132(6) 0.0170(6) 0.0194(6) N1 0.019(2) 0.020(2) 0.030(2) 0.010(2) 0.0148(19) 0.012(2) N3 0.019(2) 0.019(2) 0.034(3) 0.014(2) 0.018(2) 0.0134(19) C12 0.025(3) 0.019(3) 0.036(3) 0.008(3) 0.018(3) 0.017(2) C5 0.025(3) 0.022(3) 0.045(3) 0.015(3) 0.021(3) 0.017(3) C2 0.015(3) 0.020(3) 0.032(3) 0.010(2) 0.013(2) 0.010(2) C3 0.026(3) 0.021(3) 0.035(3) 0.012(3) 0.018(3) 0.015(3) C1 0.023(3) 0.025(3) 0.034(3) 0.020(3) 0.021(3) 0.014(3) N2 0.017(2) 0.021(3) 0.034(3) 0.012(2) 0.016(2) 0.011(2) C4 0.026(3) 0.015(3) 0.040(3) 0.008(3) 0.017(3) 0.011(2) C11 0.019(3) 0.016(3) 0.030(3) 0.006(2) 0.017(2) 0.014(2) C35 0.025(3) 0.029(3) 0.043(3) 0.021(3) 0.024(3) 0.016(3) C51 0.025(3) 0.022(3) 0.032(3) 0.016(3) 0.019(2) 0.015(2) C56 0.023(3) 0.023(3) 0.029(3) 0.009(3) 0.012(2) 0.009(2) C31 0.016(3) 0.018(3) 0.036(3) 0.016(3) 0.016(2) 0.014(2) C32 0.026(3) 0.019(3) 0.036(3) 0.019(3) 0.015(3) 0.014(2) C16 0.026(3) 0.024(3) 0.036(3) 0.009(3) 0.019(3) 0.016(3) C15 0.035(3) 0.036(4) 0.036(3) 0.012(3) 0.014(3) 0.018(3) C34 0.019(3) 0.030(3) 0.053(4) 0.028(3) 0.022(3) 0.011(3) C52 0.029(3) 0.028(3) 0.046(4) 0.020(3) 0.027(3) 0.020(3) C13 0.026(3) 0.026(3) 0.046(4) 0.012(3) 0.022(3) 0.013(3) C55 0.035(3) 0.029(3) 0.052(4) 0.025(3) 0.030(3) 0.022(3) C36 0.022(3) 0.017(3) 0.036(3) 0.016(3) 0.018(2) 0.014(2) C6 0.025(3) 0.026(3) 0.052(4) 0.021(3) 0.023(3) 0.019(3) C26 0.024(3) 0.020(3) 0.048(4) 0.011(3) 0.022(3) 0.010(3) C321 0.029(3) 0.023(3) 0.037(3) 0.014(3) 0.015(3) 0.010(3) C161 0.032(3) 0.043(4) 0.038(3) 0.021(3) 0.021(3) 0.023(3) C21 0.016(3) 0.014(3) 0.046(4) 0.013(3) 0.015(3) 0.010(2) C53 0.029(3) 0.032(3) 0.053(4) 0.024(3) 0.031(3) 0.021(3) F653 0.040(2) 0.063(3) 0.050(2) 0.021(2) 0.0330(18) 0.0306(19) F652 0.0293(19) 0.056(3) 0.084(3) 0.019(2) 0.0428(19) 0.0142(18) F651 0.068(2) 0.059(3) 0.081(3) 0.046(2) 0.055(2) 0.054(2) C651 0.027(3) 0.033(4) 0.046(4) 0.021(3) 0.020(3) 0.013(3) C84 0.020(3) 0.041(4) 0.050(4) 0.028(3) 0.019(3) 0.009(3) C64 0.018(3) 0.028(3) 0.041(4) 0.022(3) 0.017(3) 0.011(2) C71 0.014(3) 0.023(3) 0.034(3) 0.010(3) 0.013(2) 0.009(2) C65 0.019(3) 0.024(3) 0.041(3) 0.019(3) 0.019(3) 0.013(2) C61 0.017(3) 0.028(3) 0.038(3) 0.024(3) 0.017(2) 0.017(2) N4 0.021(2) 0.020(3) 0.045(3) 0.018(2) 0.022(2) 0.014(2) B1 0.019(3) 0.033(4) 0.035(4) 0.017(3) 0.016(3) 0.014(3) C72 0.018(3) 0.031(3) 0.046(4) 0.018(3) 0.021(3) 0.015(3) C513 0.036(4) 0.035(4) 0.039(4) 0.018(3) 0.012(3) 0.011(3) C362 0.039(3) 0.034(4) 0.040(4) 0.006(3) 0.022(3) 0.015(3) C81 0.014(3) 0.033(3) 0.043(3) 0.021(3) 0.017(3) 0.012(2) C512 0.034(3) 0.021(3) 0.034(3) 0.012(3) 0.017(3) 0.007(3) C63 0.022(3) 0.021(3) 0.036(3) 0.018(3) 0.015(2) 0.010(2) C514 0.021(3) 0.031(4) 0.045(4) 0.015(3) 0.009(3) 0.008(3) C22 0.024(3) 0.022(3) 0.039(3) 0.011(3) 0.015(3) 0.013(2) C62 0.020(3) 0.025(3) 0.042(3) 0.020(3) 0.021(3) 0.014(2) C33 0.022(3) 0.024(3) 0.043(4) 0.020(3) 0.010(3) 0.005(3) C361 0.027(3) 0.023(3) 0.040(3) 0.018(3) 0.024(3) 0.014(3) C515 0.030(3) 0.027(3) 0.047(4) 0.019(3) 0.027(3) 0.016(3) C363 0.022(3) 0.036(4) 0.038(3) 0.014(3) 0.013(3) 0.012(3) C92 0.019(3) 0.047(4) 0.036(3) 0.019(3) 0.020(3) 0.013(3) C162 0.041(4) 0.058(4) 0.041(4) 0.026(3) 0.023(3) 0.034(3) C54 0.039(3) 0.032(3) 0.048(4) 0.026(3) 0.030(3) 0.018(3) C83 0.032(3) 0.037(4) 0.053(4) 0.025(3) 0.031(3) 0.014(3) C85 0.016(3) 0.031(3) 0.043(4) 0.019(3) 0.015(3) 0.012(3) C511 0.030(3) 0.019(3) 0.038(3) 0.013(3) 0.025(3) 0.018(3) C24 0.021(3) 0.041(4) 0.057(4) 0.014(3) 0.010(3) 0.013(3) C86 0.014(3) 0.037(4) 0.037(3) 0.017(3) 0.015(2) 0.009(3) C122 0.046(4) 0.037(4) 0.049(4) 0.027(3) 0.031(3) 0.023(3) C82 0.020(3) 0.036(4) 0.044(4) 0.021(3) 0.019(3) 0.012(3) C50 0.018(3) 0.019(3) 0.036(3) 0.012(3) 0.020(2) 0.015(2) C25 0.016(3) 0.035(4) 0.059(4) 0.017(3) 0.017(3) 0.013(3) C91 0.019(3) 0.035(3) 0.040(3) 0.016(3) 0.024(3) 0.016(3) C14 0.023(3) 0.028(4) 0.055(4) 0.005(3) 0.012(3) 0.008(3) C121 0.025(3) 0.023(3) 0.039(3) 0.010(3) 0.024(3) 0.009(2) C76 0.021(3) 0.023(3) 0.041(3) 0.014(3) 0.015(3) 0.011(2) F851 0.066(3) 0.054(3) 0.143(4) 0.054(3) 0.085(3) 0.042(2) F852 0.055(2) 0.042(2) 0.063(2) 0.016(2) 0.026(2) 0.021(2) F853 0.079(3) 0.048(2) 0.072(3) 0.039(2) 0.039(2) 0.039(2) C74 0.022(3) 0.031(3) 0.052(4) 0.018(3) 0.028(3) 0.015(3) C41 0.024(3) 0.025(3) 0.064(4) 0.028(3) 0.031(3) 0.022(3) C66 0.022(3) 0.025(3) 0.041(3) 0.013(3) 0.020(3) 0.012(2) C516 0.027(3) 0.026(3) 0.033(3) 0.017(3) 0.019(3) 0.014(3) C95 0.016(3) 0.033(4) 0.040(3) 0.010(3) 0.019(3) 0.008(3) C75 0.018(3) 0.027(3) 0.054(4) 0.025(3) 0.023(3) 0.015(3) C43 0.038(4) 0.026(4) 0.078(5) 0.017(3) 0.038(4) 0.009(3) C42 0.021(3) 0.024(3) 0.054(4) 0.018(3) 0.020(3) 0.012(3) C221 0.027(3) 0.036(4) 0.035(3) 0.017(3) 0.021(3) 0.018(3) C46 0.034(3) 0.029(3) 0.068(4) 0.024(3) 0.041(3) 0.018(3) C93 0.021(3) 0.053(4) 0.032(3) 0.007(3) 0.019(3) -0.001(3) C94 0.033(3) 0.034(4) 0.043(4) 0.008(3) 0.026(3) 0.001(3) C851 0.032(3) 0.040(4) 0.058(4) 0.030(4) 0.028(3) 0.018(3) C222 0.046(4) 0.045(4) 0.053(4) 0.011(3) 0.032(3) 0.022(3) C23 0.029(3) 0.033(4) 0.044(4) 0.015(3) 0.014(3) 0.014(3) C163 0.038(4) 0.048(4) 0.049(4) 0.023(3) 0.025(3) 0.029(3) C421 0.021(3) 0.028(4) 0.057(4) 0.019(3) 0.010(3) 0.007(3) C44 0.054(4) 0.037(4) 0.109(6) 0.030(4) 0.062(5) 0.015(4) C322 0.046(4) 0.030(4) 0.040(4) 0.008(3) 0.016(3) 0.017(3) F951 0.0289(18) 0.033(2) 0.063(2) 0.0219(18) 0.0186(17) 0.0110(16) F731 0.036(2) 0.044(2) 0.051(2) 0.0192(18) 0.0175(17) 0.0110(17) F931 0.048(3) 0.125(4) 0.046(2) 0.042(3) 0.003(2) -0.027(3) F932 0.0218(18) 0.078(3) 0.049(2) 0.012(2) 0.0204(16) -0.0060(18) F733 0.079(3) 0.045(3) 0.067(3) 0.039(2) 0.019(2) 0.008(2) F831 0.044(2) 0.071(3) 0.047(2) 0.019(2) 0.0208(18) 0.012(2) F952 0.063(2) 0.067(3) 0.099(3) 0.061(2) 0.061(2) 0.043(2) F832 0.048(2) 0.102(4) 0.072(3) 0.002(3) 0.047(2) 0.001(2) F953 0.044(2) 0.027(2) 0.099(3) 0.008(2) 0.026(2) 0.0163(18) F751 0.050(2) 0.098(3) 0.078(3) 0.026(3) 0.034(2) 0.060(2) F933 0.054(3) 0.140(5) 0.062(3) -0.017(3) 0.031(2) 0.018(3) F732 0.065(3) 0.190(5) 0.067(3) 0.072(3) 0.056(2) 0.088(3) F752 0.098(3) 0.183(5) 0.190(5) 0.167(5) 0.120(4) 0.127(4) F753 0.026(2) 0.056(3) 0.149(4) 0.013(3) 0.001(2) 0.024(2) C731 0.027(3) 0.043(4) 0.058(4) 0.027(3) 0.033(3) 0.019(3) F833 0.222(6) 0.084(4) 0.080(3) 0.061(3) 0.099(4) 0.080(4) C951 0.036(4) 0.026(4) 0.056(4) 0.015(3) 0.028(3) 0.009(3) C73 0.016(3) 0.025(3) 0.039(3) 0.015(3) 0.015(2) 0.008(2) C261 0.024(3) 0.032(4) 0.046(4) 0.011(3) 0.021(3) 0.007(3) C96 0.016(3) 0.028(3) 0.037(3) 0.010(3) 0.015(2) 0.008(2) C461 0.047(4) 0.032(4) 0.056(4) 0.022(3) 0.040(3) 0.023(3) C45 0.062(5) 0.034(4) 0.083(5) 0.026(4) 0.057(4) 0.021(4) C323 0.034(3) 0.026(3) 0.044(4) 0.013(3) 0.017(3) 0.011(3) C751 0.030(3) 0.037(4) 0.075(5) 0.033(4) 0.034(3) 0.028(3) C262 0.034(4) 0.058(5) 0.068(5) 0.023(4) 0.032(3) 0.011(3) C263 0.051(4) 0.055(5) 0.071(5) 0.038(4) 0.040(4) 0.026(4) C123 0.051(4) 0.042(4) 0.044(4) 0.014(3) 0.029(3) 0.031(3) C462 0.051(4) 0.040(4) 0.050(4) 0.020(3) 0.032(3) 0.028(3) C223 0.042(4) 0.047(4) 0.052(4) 0.024(3) 0.032(3) 0.023(3) C831 0.056(4) 0.046(5) 0.048(4) 0.028(4) 0.030(4) 0.016(4) C422 0.048(4) 0.042(4) 0.059(4) 0.015(4) 0.025(3) 0.007(3) C931 0.032(4) 0.079(6) 0.044(4) 0.008(4) 0.021(3) -0.004(4) C463 0.078(5) 0.046(4) 0.075(5) 0.017(4) 0.060(4) 0.033(4) C423 0.043(4) 0.065(6) 0.092(6) 0.042(5) 0.005(4) 0.015(4) Cl99 0.0495(10) 0.0535(12) 0.0673(11) 0.0270(10) 0.0248(9) 0.0210(9) Cl98 0.0580(12) 0.0771(15) 0.0832(14) 0.0291(12) 0.0384(11) 0.0323(11) F631 0.057(2) 0.027(2) 0.048(2) 0.0130(17) 0.0267(18) 0.0154(17) F632 0.052(2) 0.055(2) 0.045(2) 0.0198(19) 0.0284(18) 0.0037(19) F633 0.0292(19) 0.067(3) 0.047(2) 0.011(2) 0.0077(16) 0.0243(19) C631 0.024(3) 0.034(4) 0.048(4) 0.025(3) 0.023(3) 0.013(3) C999 0.044(4) 0.054(5) 0.069(5) 0.026(4) 0.023(4) 0.019(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 Ni2 C50 1.831(5) . ? Ni2 C2 1.893(5) . ? Ni2 Cl1 2.1641(15) . ? Ni2 Ni1 2.4312(10) . ? Ni1 C50 1.958(5) . ? Ni1 C1 1.975(5) . ? Ni1 C51 2.134(5) . ? Ni1 Cl1 2.2244(15) . ? Ni1 C56 2.368(5) . ? N1 C1 1.362(6) . ? N1 C3 1.399(6) . ? N1 C11 1.441(6) . ? N3 C2 1.354(6) . ? N3 C5 1.391(6) . ? N3 C31 1.446(6) . ? C12 C13 1.388(7) . ? C12 C11 1.401(7) . ? C12 C121 1.508(7) . ? C5 C6 1.344(7) . ? C2 N4 1.361(6) . ? C3 C4 1.330(7) . ? C1 N2 1.348(6) . ? N2 C4 1.400(6) . ? N2 C21 1.456(6) . ? C11 C16 1.393(7) . ? C35 C34 1.350(7) . ? C35 C36 1.403(7) . ? C51 C56 1.403(7) . ? C51 C52 1.430(7) . ? C51 C50 1.458(7) . ? C56 C55 1.403(7) . ? C31 C32 1.390(7) . ? C31 C36 1.396(7) . ? C32 C33 1.405(7) . ? C32 C321 1.511(7) . ? C16 C15 1.377(7) . ? C16 C161 1.528(8) . ? C15 C14 1.383(8) . ? C34 C33 1.368(7) . ? C52 C53 1.335(7) . ? C13 C14 1.392(8) . ? C55 C54 1.369(7) . ? C36 C361 1.512(7) . ? C6 N4 1.376(6) . ? C26 C25 1.378(7) . ? C26 C21 1.414(7) . ? C26 C261 1.496(8) . ? C321 C323 1.518(7) . ? C321 C322 1.546(7) . ? C161 C162 1.512(7) . ? C161 C163 1.553(7) . ? C21 C22 1.373(7) . ? C53 C54 1.416(7) . ? F653 C651 1.326(6) . ? F652 C651 1.329(6) . ? F651 C651 1.327(6) . ? C651 C65 1.517(7) . ? C84 C85 1.379(8) . ? C84 C83 1.389(8) . ? C64 C65 1.353(7) . ? C64 C63 1.383(7) . ? C71 C72 1.379(7) . ? C71 C76 1.401(7) . ? C71 B1 1.651(8) . ? C65 C66 1.390(7) . ? C61 C62 1.361(7) . ? C61 C66 1.413(7) . ? C61 B1 1.652(7) . ? N4 C41 1.453(6) . ? B1 C81 1.628(8) . ? B1 C91 1.645(8) . ? C72 C73 1.386(7) . ? C513 C512 1.379(7) . ? C513 C514 1.395(8) . ? C362 C361 1.515(7) . ? C81 C82 1.405(7) . ? C81 C86 1.413(7) . ? C512 C511 1.385(7) . ? C63 C62 1.394(7) . ? C63 C631 1.498(8) . ? C514 C515 1.352(7) . ? C22 C23 1.387(7) . ? C22 C221 1.543(7) . ? C361 C363 1.536(7) . ? C515 C516 1.386(7) . ? C92 C93 1.403(8) . ? C92 C91 1.410(7) . ? C83 C82 1.386(7) . ? C83 C831 1.473(8) . ? C85 C86 1.377(7) . ? C85 C851 1.485(8) . ? C511 C516 1.406(7) . ? C511 C50 1.474(7) . ? C24 C25 1.377(8) . ? C24 C23 1.390(8) . ? C122 C121 1.517(7) . ? C91 C96 1.395(7) . ? C121 C123 1.524(7) . ? C76 C75 1.389(7) . ? F851 C851 1.344(6) . ? F852 C851 1.338(7) . ? F853 C851 1.326(6) . ? C74 C75 1.359(7) . ? C74 C73 1.403(7) . ? C41 C42 1.382(8) . ? C41 C46 1.400(8) . ? C95 C94 1.374(7) . ? C95 C96 1.383(7) . ? C95 C951 1.505(8) . ? C75 C751 1.497(7) . ? C43 C44 1.366(9) . ? C43 C42 1.392(8) . ? C42 C421 1.479(8) . ? C221 C222 1.526(7) . ? C221 C223 1.530(8) . ? C46 C45 1.406(8) . ? C46 C461 1.516(8) . ? C93 C94 1.393(8) . ? C93 C931 1.465(8) . ? C421 C422 1.539(8) . ? C421 C423 1.547(8) . ? C44 C45 1.354(9) . ? F951 C951 1.342(6) . ? F731 C731 1.339(6) . ? F931 C931 1.291(8) . ? F932 C931 1.325(7) . ? F733 C731 1.341(7) . ? F831 C831 1.342(7) . ? F952 C951 1.343(6) . ? F832 C831 1.359(7) . ? F953 C951 1.327(6) . ? F751 C751 1.332(7) . ? F933 C931 1.408(9) . ? F732 C731 1.331(6) . ? F752 C751 1.307(7) . ? F753 C751 1.289(7) . ? C731 C73 1.474(8) . ? F833 C831 1.304(7) . ? C261 C263 1.520(8) . ? C261 C262 1.551(7) . ? C461 C463 1.545(7) . ? C461 C462 1.556(8) . ? Cl99 C999 1.769(6) . ? Cl98 C999 1.798(7) . ? F631 C631 1.338(6) . ? F632 C631 1.330(6) . ? F633 C631 1.344(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 C50 Ni2 C2 117.6(2) . . ? C50 Ni2 Cl1 108.24(15) . . ? C2 Ni2 Cl1 133.63(16) . . ? C50 Ni2 Ni1 52.41(15) . . ? C2 Ni2 Ni1 168.05(15) . . ? Cl1 Ni2 Ni1 57.55(4) . . ? C50 Ni1 C1 152.4(2) . . ? C50 Ni1 C51 41.47(19) . . ? C1 Ni1 C51 125.09(19) . . ? C50 Ni1 Cl1 101.49(15) . . ? C1 Ni1 Cl1 102.37(15) . . ? C51 Ni1 Cl1 128.93(14) . . ? C50 Ni1 C56 68.31(19) . . ? C1 Ni1 C56 90.79(19) . . ? C51 Ni1 C56 35.84(18) . . ? Cl1 Ni1 C56 164.23(13) . . ? C50 Ni1 Ni2 47.82(14) . . ? C1 Ni1 Ni2 157.51(15) . . ? C51 Ni1 Ni2 76.62(13) . . ? Cl1 Ni1 Ni2 55.18(4) . . ? C56 Ni1 Ni2 111.59(13) . . ? Ni2 Cl1 Ni1 67.27(5) . . ? C1 N1 C3 110.6(4) . . ? C1 N1 C11 125.7(4) . . ? C3 N1 C11 123.0(4) . . ? C2 N3 C5 111.6(4) . . ? C2 N3 C31 125.6(4) . . ? C5 N3 C31 122.2(4) . . ? C13 C12 C11 117.4(5) . . ? C13 C12 C121 119.6(5) . . ? C11 C12 C121 122.8(5) . . ? C6 C5 N3 105.8(5) . . ? N3 C2 N4 103.9(4) . . ? N3 C2 Ni2 127.2(3) . . ? N4 C2 Ni2 127.8(4) . . ? C4 C3 N1 106.7(4) . . ? N2 C1 N1 104.7(4) . . ? N2 C1 Ni1 129.8(3) . . ? N1 C1 Ni1 125.4(4) . . ? C1 N2 C4 110.8(4) . . ? C1 N2 C21 125.8(4) . . ? C4 N2 C21 121.1(4) . . ? C3 C4 N2 107.1(5) . . ? C16 C11 C12 122.4(5) . . ? C16 C11 N1 119.6(4) . . ? C12 C11 N1 117.9(4) . . ? C34 C35 C36 122.3(5) . . ? C56 C51 C52 117.9(5) . . ? C56 C51 C50 118.0(4) . . ? C52 C51 C50 123.2(4) . . ? C56 C51 Ni1 81.2(3) . . ? C52 C51 Ni1 118.2(4) . . ? C50 C51 Ni1 62.8(3) . . ? C51 C56 C55 119.7(5) . . ? C51 C56 Ni1 62.9(3) . . ? C55 C56 Ni1 127.1(4) . . ? C32 C31 C36 124.2(4) . . ? C32 C31 N3 117.4(4) . . ? C36 C31 N3 118.4(4) . . ? C31 C32 C33 116.1(5) . . ? C31 C32 C321 122.8(4) . . ? C33 C32 C321 121.1(5) . . ? C15 C16 C11 118.3(5) . . ? C15 C16 C161 119.1(5) . . ? C11 C16 C161 122.5(5) . . ? C16 C15 C14 120.8(5) . . ? C35 C34 C33 120.5(5) . . ? C53 C52 C51 121.1(5) . . ? C12 C13 C14 120.8(5) . . ? C54 C55 C56 121.0(5) . . ? C31 C36 C35 115.5(5) . . ? C31 C36 C361 122.4(4) . . ? C35 C36 C361 122.0(5) . . ? C5 C6 N4 107.5(4) . . ? C25 C26 C21 116.4(5) . . ? C25 C26 C261 122.3(5) . . ? C21 C26 C261 121.2(5) . . ? C32 C321 C323 113.1(4) . . ? C32 C321 C322 111.4(5) . . ? C323 C321 C322 109.7(4) . . ? C162 C161 C16 113.5(5) . . ? C162 C161 C163 108.7(5) . . ? C16 C161 C163 110.5(4) . . ? C22 C21 C26 122.7(5) . . ? C22 C21 N2 117.2(4) . . ? C26 C21 N2 120.0(5) . . ? C52 C53 C54 121.0(5) . . ? F653 C651 F651 106.7(5) . . ? F653 C651 F652 107.5(5) . . ? F651 C651 F652 106.4(4) . . ? F653 C651 C65 112.8(4) . . ? F651 C651 C65 111.5(4) . . ? F652 C651 C65 111.4(5) . . ? C85 C84 C83 118.2(5) . . ? C65 C64 C63 118.3(5) . . ? C72 C71 C76 115.0(5) . . ? C72 C71 B1 122.4(4) . . ? C76 C71 B1 122.6(5) . . ? C64 C65 C66 121.2(5) . . ? C64 C65 C651 119.5(5) . . ? C66 C65 C651 119.2(5) . . ? C62 C61 C66 115.5(5) . . ? C62 C61 B1 126.0(4) . . ? C66 C61 B1 118.6(5) . . ? C2 N4 C6 111.1(4) . . ? C2 N4 C41 125.7(4) . . ? C6 N4 C41 123.0(4) . . ? C81 B1 C91 115.4(5) . . ? C81 B1 C71 110.9(4) . . ? C91 B1 C71 103.1(4) . . ? C81 B1 C61 106.6(4) . . ? C91 B1 C61 108.9(4) . . ? C71 B1 C61 112.1(4) . . ? C71 C72 C73 123.8(5) . . ? C512 C513 C514 120.0(5) . . ? C82 C81 C86 114.2(5) . . ? C82 C81 B1 125.1(5) . . ? C86 C81 B1 120.6(5) . . ? C513 C512 C511 121.5(5) . . ? C64 C63 C62 120.3(5) . . ? C64 C63 C631 120.9(5) . . ? C62 C63 C631 118.8(5) . . ? C515 C514 C513 119.6(5) . . ? C21 C22 C23 118.8(5) . . ? C21 C22 C221 123.5(5) . . ? C23 C22 C221 117.6(5) . . ? C61 C62 C63 122.9(5) . . ? C34 C33 C32 121.3(5) . . ? C36 C361 C362 113.6(4) . . ? C36 C361 C363 109.0(4) . . ? C362 C361 C363 110.0(4) . . ? C514 C515 C516 120.6(5) . . ? C93 C92 C91 121.3(5) . . ? C55 C54 C53 119.1(5) . . ? C82 C83 C84 120.3(5) . . ? C82 C83 C831 120.1(6) . . ? C84 C83 C831 119.6(6) . . ? C86 C85 C84 121.0(5) . . ? C86 C85 C851 118.6(5) . . ? C84 C85 C851 120.4(5) . . ? C512 C511 C516 117.1(5) . . ? C512 C511 C50 122.4(5) . . ? C516 C511 C50 120.5(5) . . ? C25 C24 C23 119.9(5) . . ? C85 C86 C81 123.0(5) . . ? C83 C82 C81 123.2(5) . . ? C51 C50 C511 120.7(4) . . ? C51 C50 Ni2 119.0(4) . . ? C511 C50 Ni2 120.4(4) . . ? C51 C50 Ni1 75.8(3) . . ? C511 C50 Ni1 115.5(3) . . ? Ni2 C50 Ni1 79.8(2) . . ? C24 C25 C26 122.2(5) . . ? C96 C91 C92 116.3(5) . . ? C96 C91 B1 118.9(5) . . ? C92 C91 B1 124.5(5) . . ? C15 C14 C13 120.2(6) . . ? C12 C121 C122 114.8(5) . . ? C12 C121 C123 109.6(4) . . ? C122 C121 C123 109.1(4) . . ? C75 C76 C71 122.2(5) . . ? C75 C74 C73 118.2(5) . . ? C42 C41 C46 124.1(5) . . ? C42 C41 N4 119.6(5) . . ? C46 C41 N4 116.2(5) . . ? C65 C66 C61 121.7(5) . . ? C515 C516 C511 121.1(5) . . ? C94 C95 C96 122.3(6) . . ? C94 C95 C951 118.6(5) . . ? C96 C95 C951 119.0(5) . . ? C74 C75 C76 121.2(5) . . ? C74 C75 C751 120.0(5) . . ? C76 C75 C751 118.8(5) . . ? C44 C43 C42 120.8(6) . . ? C41 C42 C43 116.6(6) . . ? C41 C42 C421 123.3(5) . . ? C43 C42 C421 120.0(6) . . ? C222 C221 C223 111.0(5) . . ? C222 C221 C22 109.9(5) . . ? C223 C221 C22 113.0(4) . . ? C41 C46 C45 115.9(6) . . ? C41 C46 C461 123.1(5) . . ? C45 C46 C461 120.9(6) . . ? C94 C93 C92 121.0(5) . . ? C94 C93 C931 118.8(6) . . ? C92 C93 C931 120.2(6) . . ? C95 C94 C93 117.4(6) . . ? F853 C851 F852 105.2(5) . . ? F853 C851 F851 107.1(5) . . ? F852 C851 F851 105.4(5) . . ? F853 C851 C85 114.0(5) . . ? F852 C851 C85 112.5(5) . . ? F851 C851 C85 112.1(5) . . ? C22 C23 C24 119.9(6) . . ? C42 C421 C422 113.3(5) . . ? C42 C421 C423 108.7(5) . . ? C422 C421 C423 111.8(5) . . ? C45 C44 C43 121.7(6) . . ? F732 C731 F731 104.9(5) . . ? F732 C731 F733 107.8(5) . . ? F731 C731 F733 104.1(4) . . ? F732 C731 C73 113.8(5) . . ? F731 C731 C73 113.4(4) . . ? F733 C731 C73 112.2(5) . . ? F953 C951 F951 106.5(5) . . ? F953 C951 F952 106.0(5) . . ? F951 C951 F952 105.4(5) . . ? F953 C951 C95 114.0(5) . . ? F951 C951 C95 112.8(5) . . ? F952 C951 C95 111.5(5) . . ? C72 C73 C74 119.3(5) . . ? C72 C73 C731 119.4(5) . . ? C74 C73 C731 121.2(5) . . ? C26 C261 C263 111.4(5) . . ? C26 C261 C262 112.1(5) . . ? C263 C261 C262 109.0(5) . . ? C95 C96 C91 121.7(5) . . ? C46 C461 C463 114.2(5) . . ? C46 C461 C462 109.7(5) . . ? C463 C461 C462 108.0(5) . . ? C44 C45 C46 120.8(6) . . ? F753 C751 F752 107.1(6) . . ? F753 C751 F751 102.9(5) . . ? F752 C751 F751 106.4(5) . . ? F753 C751 C75 113.7(5) . . ? F752 C751 C75 113.1(5) . . ? F751 C751 C75 112.8(5) . . ? F833 C831 F831 106.0(6) . . ? F833 C831 F832 106.7(5) . . ? F831 C831 F832 103.1(5) . . ? F833 C831 C83 115.0(6) . . ? F831 C831 C83 112.9(5) . . ? F832 C831 C83 112.2(5) . . ? F931 C931 F932 107.5(6) . . ? F931 C931 F933 104.8(6) . . ? F932 C931 F933 102.9(6) . . ? F931 C931 C93 115.6(6) . . ? F932 C931 C93 114.1(6) . . ? F933 C931 C93 110.8(6) . . ? F632 C631 F631 105.6(4) . . ? F632 C631 F633 105.9(4) . . ? F631 C631 F633 105.8(4) . . ? F632 C631 C63 112.9(4) . . ? F631 C631 C63 113.0(5) . . ? F633 C631 C63 113.0(4) . . ? Cl99 C999 Cl98 110.6(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.192 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.111 data_7 _database_code_depnum_ccdc_archive 'CCDC 791320' #TrackingRef 'Carbene.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H96 B Cl3 F24 N4 Ni2 Si' _chemical_formula_weight 1964.39 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.729(5) _cell_length_b 17.963(6) _cell_length_c 20.822(7) _cell_angle_alpha 69.525(6) _cell_angle_beta 73.169(6) _cell_angle_gamma 82.761(6) _cell_volume 4603(3) _cell_formula_units_Z 2 _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 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.3775 _exptl_absorpt_correction_T_max 0.6215 _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 23070 _diffrn_reflns_av_R_equivalents 0.1402 _diffrn_reflns_av_sigmaI/netI 0.1098 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15798 _reflns_number_gt 11202 _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^)+(0.0604P)^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 15798 _refine_ls_number_parameters 1158 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _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 0.86684(3) 0.66415(2) 0.30044(2) 0.01828(11) Uani 1 1 d . . . Ni2 Ni 0.84498(3) 0.78365(2) 0.33389(2) 0.01825(11) Uani 1 1 d . . . Si1 Si 0.64554(7) 0.69755(5) 0.36989(5) 0.0198(2) Uani 1 1 d . . . Cl1 Cl 0.97056(6) 0.69822(4) 0.34504(5) 0.0284(2) Uani 1 1 d . . . C50 C 0.7635(2) 0.74093(16) 0.29886(16) 0.0162(6) Uani 1 1 d . . . C1 C 0.8433(2) 0.59775(16) 0.25302(16) 0.0171(7) Uani 1 1 d . . . F633 F 0.35864(15) 0.02741(10) 0.01575(10) 0.0294(5) Uani 1 1 d . . . F632 F 0.41159(15) -0.03673(9) 0.10792(10) 0.0308(5) Uani 1 1 d . . . F631 F 0.26436(14) 0.02228(11) 0.11907(11) 0.0357(5) Uani 1 1 d . . . C63 C 0.4072(2) 0.10324(16) 0.07396(16) 0.0192(7) Uani 1 1 d . . . C66 C 0.4989(2) 0.23535(17) 0.06390(16) 0.0208(7) Uani 1 1 d . . . H66A H 0.5309 0.2817 0.0589 0.025 Uiso 1 1 calc R . . C62 C 0.3630(2) 0.14591(16) 0.11919(16) 0.0178(7) Uani 1 1 d . . . H62A H 0.3002 0.1290 0.1535 0.021 Uiso 1 1 calc R . . N4 N 0.77426(19) 0.95381(13) 0.29186(13) 0.0180(6) Uani 1 1 d . . . C61 C 0.4076(2) 0.21364(16) 0.11631(16) 0.0183(7) Uani 1 1 d . . . C96 C 0.1700(2) 0.23472(17) 0.26290(16) 0.0195(7) Uani 1 1 d . . . H96A H 0.1453 0.2853 0.2381 0.023 Uiso 1 1 calc R . . C92 C 0.3037(2) 0.13890(16) 0.27975(16) 0.0201(7) Uani 1 1 d . . . H92A H 0.3727 0.1219 0.2664 0.024 Uiso 1 1 calc R . . C64 C 0.4993(2) 0.12448(17) 0.02328(17) 0.0223(7) Uani 1 1 d . . . H64A H 0.5301 0.0943 -0.0072 0.027 Uiso 1 1 calc R . . C84 C 0.5705(2) 0.35568(17) 0.24692(16) 0.0223(7) Uani 1 1 d . . . H84A H 0.6167 0.3750 0.2633 0.027 Uiso 1 1 calc R . . N1 N 0.82977(18) 0.61094(13) 0.18821(13) 0.0166(5) Uani 1 1 d . . . N2 N 0.85923(19) 0.51743(13) 0.27877(13) 0.0176(6) Uani 1 1 d . . . C86 C 0.5309(2) 0.26467(16) 0.19707(16) 0.0199(7) Uani 1 1 d . . . H86A H 0.5515 0.2204 0.1808 0.024 Uiso 1 1 calc R . . C631 C 0.3596(2) 0.02982(17) 0.07954(17) 0.0210(7) Uani 1 1 d . . . B1 B 0.3518(3) 0.26727(18) 0.16731(18) 0.0174(7) Uani 1 1 d . . . N3 N 0.75639(19) 0.89893(13) 0.40350(13) 0.0181(6) Uani 1 1 d . . . C93 C 0.2377(2) 0.08982(17) 0.33899(16) 0.0216(7) Uani 1 1 d . . . C32 C 0.8617(2) 0.81410(17) 0.47921(16) 0.0212(7) Uani 1 1 d . . . C36 C 0.6754(3) 0.81769(17) 0.52614(16) 0.0225(7) Uani 1 1 d . . . C94 C 0.1369(3) 0.11183(17) 0.36060(17) 0.0226(7) Uani 1 1 d . . . H94A H 0.0918 0.0775 0.4010 0.027 Uiso 1 1 calc R . . C4 C 0.8565(2) 0.48197(17) 0.22979(17) 0.0236(7) Uani 1 1 d . . . H4A H 0.8661 0.4270 0.2353 0.028 Uiso 1 1 calc R . . C6 C 0.7399(2) 1.01224(17) 0.32229(17) 0.0238(7) Uani 1 1 d . . . H6A H 0.7267 1.0665 0.2981 0.029 Uiso 1 1 calc R . . C31 C 0.7639(3) 0.84173(16) 0.47184(16) 0.0220(7) Uani 1 1 d . . . C76 C 0.3338(2) 0.41618(16) 0.08112(15) 0.0173(6) Uani 1 1 d . . . H76A H 0.3973 0.4266 0.0856 0.021 Uiso 1 1 calc R . . C2 C 0.7851(2) 0.88232(16) 0.34175(15) 0.0173(7) Uani 1 1 d . . . C3 C 0.8378(2) 0.54067(17) 0.17310(17) 0.0225(7) Uani 1 1 d . . . H3A H 0.8313 0.5351 0.1308 0.027 Uiso 1 1 calc R . . C12 C 0.7309(3) 0.70598(18) 0.11321(16) 0.0238(7) Uani 1 1 d . . . C91 C 0.2715(2) 0.21342(16) 0.23849(16) 0.0187(7) Uani 1 1 d . . . C81 C 0.4342(2) 0.29964(16) 0.19503(15) 0.0180(7) Uani 1 1 d . . . C75 C 0.2837(2) 0.47687(16) 0.03836(16) 0.0208(7) Uani 1 1 d . . . C83 C 0.4746(2) 0.39042(16) 0.24747(16) 0.0211(7) Uani 1 1 d . . . C322 C 0.9703(3) 0.93493(18) 0.42528(19) 0.0298(8) Uani 1 1 d . . . H32A H 0.9083 0.9671 0.4194 0.045 Uiso 1 1 calc R . . H32B H 1.0285 0.9604 0.3865 0.045 Uiso 1 1 calc R . . H32C H 0.9816 0.9304 0.4709 0.045 Uiso 1 1 calc R . . C321 C 0.9585(2) 0.85146(17) 0.42386(17) 0.0224(7) Uani 1 1 d . . . H32D H 0.9505 0.8578 0.3760 0.027 Uiso 1 1 calc R . . C71 C 0.2940(2) 0.34117(16) 0.11734(15) 0.0176(6) Uani 1 1 d . . . C5 C 0.7284(2) 0.97833(17) 0.39222(17) 0.0225(7) Uani 1 1 d . . . H5A H 0.7056 1.0037 0.4273 0.027 Uiso 1 1 calc R . . C82 C 0.4084(2) 0.36293(16) 0.22179(15) 0.0192(7) Uani 1 1 d . . . H82A H 0.3431 0.3881 0.2225 0.023 Uiso 1 1 calc R . . C21 C 0.8952(2) 0.48064(16) 0.34191(17) 0.0206(7) Uani 1 1 d . . . C11 C 0.8206(2) 0.68814(17) 0.13489(16) 0.0207(7) Uani 1 1 d . . . C33 C 0.8674(3) 0.75422(17) 0.54213(17) 0.0256(8) Uani 1 1 d . . . H33A H 0.9318 0.7315 0.5481 0.031 Uiso 1 1 calc R . . C74 C 0.1906(2) 0.46517(17) 0.03118(16) 0.0237(7) Uani 1 1 d . . . H74A H 0.1547 0.5075 0.0042 0.028 Uiso 1 1 calc R . . Cl2 Cl 0.30369(9) 0.65920(6) 0.33688(6) 0.0566(3) Uani 1 1 d . . . Cl3 Cl 0.31527(9) 0.82857(7) 0.26805(10) 0.0933(6) Uani 1 1 d . . . F831 F 0.40528(16) 0.52067(10) 0.23024(11) 0.0387(5) Uani 1 1 d . . . F731 F 0.03314(16) 0.29938(11) 0.07302(13) 0.0454(6) Uani 1 1 d . . . F931 F 0.37199(16) -0.00380(10) 0.36075(10) 0.0371(5) Uani 1 1 d . . . F951 F -0.01648(15) 0.28309(12) 0.34960(12) 0.0405(5) Uani 1 1 d . . . F651 F 0.64463(17) 0.28586(13) -0.08188(12) 0.0554(7) Uani 1 1 d . . . F732 F -0.02680(15) 0.40073(14) 0.10454(12) 0.0451(6) Uani 1 1 d . . . F851 F 0.72726(16) 0.20350(13) 0.18682(13) 0.0501(6) Uani 1 1 d . . . F733 F 0.03457(16) 0.41466(12) -0.00490(11) 0.0437(6) Uani 1 1 d . . . F832 F 0.36435(19) 0.43867(12) 0.33535(11) 0.0502(6) Uani 1 1 d . . . F852 F 0.70566(17) 0.21044(12) 0.28940(12) 0.0499(6) Uani 1 1 d . . . F833 F 0.51472(17) 0.48519(13) 0.29049(14) 0.0565(7) Uani 1 1 d . . . F932 F 0.24620(19) -0.00472(13) 0.44947(11) 0.0563(7) Uani 1 1 d . . . F751 F 0.40807(17) 0.55177(12) -0.05907(13) 0.0519(6) Uani 1 1 d . . . F933 F 0.23079(19) -0.04876(11) 0.36981(15) 0.0643(8) Uani 1 1 d . . . F652 F 0.71436(16) 0.22090(16) -0.00102(13) 0.0582(7) Uani 1 1 d . . . F952 F -0.06085(16) 0.16310(13) 0.40202(13) 0.0570(7) Uani 1 1 d . . . F853 F 0.77347(16) 0.30679(12) 0.19881(15) 0.0595(7) Uani 1 1 d . . . C72 C 0.2038(2) 0.32854(16) 0.10484(15) 0.0190(7) Uani 1 1 d . . . H72A H 0.1775 0.2765 0.1245 0.023 Uiso 1 1 calc R . . F953 F -0.05213(16) 0.21953(17) 0.29113(13) 0.0609(7) Uani 1 1 d . . . F653 F 0.6839(2) 0.16542(16) -0.06840(17) 0.0841(10) Uani 1 1 d . . . C422 C 0.6012(3) 0.8979(2) 0.17747(19) 0.0336(9) Uani 1 1 d . . . H42A H 0.6479 0.8517 0.1785 0.050 Uiso 1 1 calc R . . H42B H 0.6010 0.9282 0.1282 0.050 Uiso 1 1 calc R . . H42C H 0.5324 0.8798 0.2050 0.050 Uiso 1 1 calc R . . F752 F 0.27186(17) 0.61337(11) -0.02681(13) 0.0563(7) Uani 1 1 d . . . C73 C 0.1510(2) 0.38979(17) 0.06452(16) 0.0205(7) Uani 1 1 d . . . C161 C 1.0038(2) 0.71711(17) 0.12684(17) 0.0222(7) Uani 1 1 d . . . H16A H 0.9870 0.6810 0.1774 0.027 Uiso 1 1 calc R . . F753 F 0.3790(3) 0.57869(13) 0.03522(14) 0.0875(12) Uani 1 1 d . . . C162 C 1.0533(3) 0.79013(19) 0.1247(2) 0.0345(9) Uani 1 1 d . . . H16B H 1.0017 0.8219 0.1482 0.052 Uiso 1 1 calc R . . H16C H 1.0824 0.8223 0.0751 0.052 Uiso 1 1 calc R . . H16D H 1.1073 0.7729 0.1493 0.052 Uiso 1 1 calc R . . C43 C 0.7858(3) 0.99395(17) 0.10241(17) 0.0247(7) Uani 1 1 d . . . H43A H 0.7427 0.9948 0.0738 0.030 Uiso 1 1 calc R . . C24 C 0.9622(3) 0.42435(18) 0.46247(19) 0.0318(9) Uani 1 1 d . . . H24A H 0.9842 0.4078 0.5047 0.038 Uiso 1 1 calc R . . C163 C 1.0765(3) 0.6713(2) 0.08340(19) 0.0324(8) Uani 1 1 d . . . H16E H 1.0455 0.6217 0.0908 0.049 Uiso 1 1 calc R . . H16F H 1.1399 0.6590 0.0983 0.049 Uiso 1 1 calc R . . H16G H 1.0915 0.7035 0.0329 0.049 Uiso 1 1 calc R . . C51 C 0.5461(3) 0.77747(18) 0.37511(17) 0.0263(7) Uani 1 1 d . . . H51A H 0.4847 0.7548 0.4120 0.039 Uiso 1 1 calc R . . H51B H 0.5299 0.8013 0.3292 0.039 Uiso 1 1 calc R . . H51C H 0.5715 0.8184 0.3868 0.039 Uiso 1 1 calc R . . C44 C 0.8858(3) 1.01514(18) 0.07068(17) 0.0269(8) Uani 1 1 d . . . H44A H 0.9109 1.0304 0.0204 0.032 Uiso 1 1 calc R . . C122 C 0.5416(3) 0.70320(19) 0.16804(19) 0.0307(8) Uani 1 1 d . . . H12A H 0.5514 0.7288 0.2002 0.046 Uiso 1 1 calc R . . H12B H 0.4837 0.6678 0.1922 0.046 Uiso 1 1 calc R . . H12C H 0.5282 0.7440 0.1256 0.046 Uiso 1 1 calc R . . C951 C -0.0056(3) 0.2121(2) 0.34114(17) 0.0281(8) Uani 1 1 d . . . C65 C 0.5449(2) 0.19199(17) 0.01874(16) 0.0211(7) Uani 1 1 d . . . C731 C 0.0496(3) 0.37527(18) 0.05981(17) 0.0259(8) Uani 1 1 d . . . C362 C 0.5344(3) 0.9081(2) 0.5639(2) 0.0403(9) Uani 1 1 d . . . H36A H 0.5812 0.9523 0.5447 0.060 Uiso 1 1 calc R . . H36B H 0.5336 0.8795 0.6137 0.060 Uiso 1 1 calc R . . H36C H 0.4658 0.9288 0.5610 0.060 Uiso 1 1 calc R . . C42 C 0.7473(2) 0.97137(16) 0.17578(17) 0.0211(7) Uani 1 1 d . . . C34 C 0.7805(3) 0.72734(18) 0.59606(17) 0.0285(8) Uani 1 1 d . . . H34A H 0.7858 0.6859 0.6384 0.034 Uiso 1 1 calc R . . C222 C 0.6412(3) 0.4247(2) 0.4743(2) 0.0404(10) Uani 1 1 d . . . H22A H 0.6457 0.4751 0.4815 0.061 Uiso 1 1 calc R . . H22B H 0.6526 0.3803 0.5154 0.061 Uiso 1 1 calc R . . H22C H 0.5735 0.4210 0.4691 0.061 Uiso 1 1 calc R . . C41 C 0.8130(2) 0.97193(16) 0.21521(16) 0.0196(7) Uani 1 1 d . . . C23 C 0.8634(3) 0.41191(18) 0.46604(18) 0.0295(8) Uani 1 1 d . . . H23A H 0.8193 0.3839 0.5105 0.035 Uiso 1 1 calc R . . C26 C 0.9975(2) 0.48980(16) 0.33589(17) 0.0235(7) Uani 1 1 d . . . C421 C 0.6361(2) 0.95074(18) 0.20983(17) 0.0259(8) Uani 1 1 d . . . H42D H 0.6286 0.9202 0.2613 0.031 Uiso 1 1 calc R . . C16 C 0.9045(3) 0.73759(17) 0.10527(17) 0.0231(7) Uani 1 1 d . . . C461 C 0.9859(3) 0.99564(18) 0.22841(17) 0.0258(7) Uani 1 1 d . . . H46A H 0.9447 0.9852 0.2787 0.031 Uiso 1 1 calc R . . C15 C 0.8967(3) 0.80660(18) 0.04920(18) 0.0290(8) Uani 1 1 d . . . H15A H 0.9520 0.8418 0.0272 0.035 Uiso 1 1 calc R . . C931 C 0.2731(3) 0.00864(19) 0.37919(19) 0.0324(9) Uani 1 1 d . . . C52 C 0.5901(2) 0.62283(18) 0.34780(17) 0.0236(7) Uani 1 1 d . . . H52A H 0.5372 0.5939 0.3892 0.035 Uiso 1 1 calc R . . H52B H 0.6438 0.5853 0.3347 0.035 Uiso 1 1 calc R . . H52C H 0.5603 0.6500 0.3079 0.035 Uiso 1 1 calc R . . C361 C 0.5698(3) 0.85155(18) 0.52112(18) 0.0264(8) Uani 1 1 d . . . H36D H 0.5731 0.8821 0.4702 0.032 Uiso 1 1 calc R . . C831 C 0.4413(3) 0.45731(19) 0.27586(18) 0.0291(8) Uani 1 1 d . . . C121 C 0.6377(2) 0.65489(18) 0.14641(17) 0.0253(7) Uani 1 1 d . . . H12D H 0.6482 0.6121 0.1902 0.030 Uiso 1 1 calc R . . C46 C 0.9149(2) 0.99342(17) 0.18504(17) 0.0222(7) Uani 1 1 d . . . C95 C 0.1029(2) 0.18504(18) 0.32211(17) 0.0227(7) Uani 1 1 d . . . C323 C 1.0556(3) 0.80175(18) 0.43220(18) 0.0281(8) Uani 1 1 d . . . H32E H 1.0470 0.7479 0.4333 0.042 Uiso 1 1 calc R . . H32F H 1.0693 0.7991 0.4766 0.042 Uiso 1 1 calc R . . H32G H 1.1128 0.8263 0.3920 0.042 Uiso 1 1 calc R . . C223 C 0.7235(3) 0.3386(2) 0.4002(2) 0.0414(10) Uani 1 1 d . . . H22D H 0.7739 0.3377 0.3561 0.062 Uiso 1 1 calc R . . H22E H 0.6562 0.3277 0.3987 0.062 Uiso 1 1 calc R . . H22F H 0.7422 0.2978 0.4408 0.062 Uiso 1 1 calc R . . C13 C 0.7289(3) 0.7759(2) 0.05598(18) 0.0333(9) Uani 1 1 d . . . H13A H 0.6702 0.7895 0.0384 0.040 Uiso 1 1 calc R . . C423 C 0.5690(3) 1.0258(2) 0.2051(2) 0.0376(9) Uani 1 1 d . . . H42E H 0.5880 1.0558 0.2307 0.056 Uiso 1 1 calc R . . H42F H 0.4975 1.0112 0.2264 0.056 Uiso 1 1 calc R . . H42G H 0.5782 1.0587 0.1551 0.056 Uiso 1 1 calc R . . C261 C 1.0729(2) 0.52235(18) 0.26351(19) 0.0292(8) Uani 1 1 d . . . H26A H 1.0344 0.5597 0.2306 0.035 Uiso 1 1 calc R . . C25 C 1.0289(3) 0.46070(18) 0.39800(19) 0.0299(8) Uani 1 1 d . . . H25A H 1.0978 0.4660 0.3960 0.036 Uiso 1 1 calc R . . C262 C 1.1175(3) 0.45518(19) 0.23375(19) 0.0339(8) Uani 1 1 d . . . H26B H 1.0622 0.4278 0.2310 0.051 Uiso 1 1 calc R . . H26C H 1.1558 0.4174 0.2650 0.051 Uiso 1 1 calc R . . H26D H 1.1631 0.4773 0.1861 0.051 Uiso 1 1 calc R . . C651 C 0.6454(3) 0.21509(19) -0.03266(19) 0.0315(8) Uani 1 1 d . . . C85 C 0.5974(2) 0.29233(17) 0.22193(17) 0.0236(7) Uani 1 1 d . . . C45 C 0.9501(3) 1.01446(18) 0.11130(17) 0.0257(7) Uani 1 1 d . . . H45A H 1.0191 1.0285 0.0886 0.031 Uiso 1 1 calc R . . C53 C 0.6811(3) 0.64841(18) 0.45561(17) 0.0260(8) Uani 1 1 d . . . H53A H 0.6208 0.6248 0.4933 0.039 Uiso 1 1 calc R . . H53B H 0.7081 0.6880 0.4681 0.039 Uiso 1 1 calc R . . H53C H 0.7332 0.6067 0.4504 0.039 Uiso 1 1 calc R . . C462 C 1.0681(3) 0.92997(18) 0.22754(18) 0.0293(8) Uani 1 1 d . . . H46B H 1.0361 0.8781 0.2486 0.044 Uiso 1 1 calc R . . H46C H 1.1138 0.9328 0.2550 0.044 Uiso 1 1 calc R . . H46D H 1.1072 0.9369 0.1784 0.044 Uiso 1 1 calc R . . C851 C 0.7007(3) 0.25384(19) 0.2231(2) 0.0320(8) Uani 1 1 d . . . C221 C 0.7209(2) 0.42091(18) 0.40810(18) 0.0281(8) Uani 1 1 d . . . H22G H 0.7011 0.4611 0.3663 0.034 Uiso 1 1 calc R . . C123 C 0.6233(3) 0.6151(2) 0.09561(19) 0.0368(9) Uani 1 1 d . . . H12E H 0.5617 0.5836 0.1177 0.055 Uiso 1 1 calc R . . H12F H 0.6824 0.5802 0.0855 0.055 Uiso 1 1 calc R . . H12G H 0.6167 0.6560 0.0512 0.055 Uiso 1 1 calc R . . C35 C 0.6867(3) 0.75980(18) 0.58910(17) 0.0268(8) Uani 1 1 d . . . H35A H 0.6284 0.7426 0.6279 0.032 Uiso 1 1 calc R . . C22 C 0.8271(2) 0.43982(16) 0.40547(16) 0.0219(7) Uani 1 1 d . . . C751 C 0.3344(3) 0.55522(18) -0.00239(18) 0.0288(8) Uani 1 1 d . . . C263 C 1.1584(3) 0.5684(2) 0.2640(3) 0.0490(11) Uani 1 1 d . . . H26E H 1.1292 0.6123 0.2819 0.073 Uiso 1 1 calc R . . H26F H 1.2020 0.5898 0.2155 0.073 Uiso 1 1 calc R . . H26G H 1.1990 0.5329 0.2948 0.073 Uiso 1 1 calc R . . C463 C 1.0333(3) 1.07750(19) 0.20255(19) 0.0332(8) Uani 1 1 d . . . H46E H 0.9791 1.1180 0.2067 0.050 Uiso 1 1 calc R . . H46F H 1.0727 1.0899 0.1528 0.050 Uiso 1 1 calc R . . H46G H 1.0783 1.0768 0.2317 0.050 Uiso 1 1 calc R . . C999 C 0.2678(3) 0.7405(2) 0.2722(2) 0.0522(11) Uani 1 1 d . . . H99A H 0.1926 0.7448 0.2831 0.063 Uiso 1 1 calc R . . H99B H 0.2939 0.7325 0.2254 0.063 Uiso 1 1 calc R . . C363 C 0.4913(3) 0.7866(2) 0.54799(19) 0.0362(9) Uani 1 1 d . . . H36E H 0.5169 0.7466 0.5246 0.054 Uiso 1 1 calc R . . H36F H 0.4272 0.8103 0.5370 0.054 Uiso 1 1 calc R . . H36G H 0.4795 0.7615 0.5995 0.054 Uiso 1 1 calc R . . C14 C 0.8107(3) 0.8250(2) 0.02492(19) 0.0365(9) Uani 1 1 d . . . H14A H 0.8078 0.8722 -0.0138 0.044 Uiso 1 1 calc R . . H H 0.765(2) 0.7727(18) 0.2490(18) 0.029(9) 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 0.0234(2) 0.01389(19) 0.0192(2) -0.00580(15) -0.00845(19) 0.00139(16) Ni2 0.0232(2) 0.01269(18) 0.0197(2) -0.00543(15) -0.00758(19) 0.00164(16) Si1 0.0222(5) 0.0182(4) 0.0178(5) -0.0044(3) -0.0051(4) -0.0012(4) Cl1 0.0294(5) 0.0254(4) 0.0419(5) -0.0190(3) -0.0203(4) 0.0080(3) C50 0.0187(17) 0.0147(14) 0.0141(16) -0.0055(12) -0.0029(14) 0.0024(12) C1 0.0163(16) 0.0156(14) 0.0185(17) -0.0046(12) -0.0037(14) -0.0027(12) F633 0.0432(12) 0.0233(9) 0.0307(11) -0.0115(8) -0.0203(10) 0.0000(8) F632 0.0456(12) 0.0147(8) 0.0370(12) -0.0048(8) -0.0236(10) 0.0015(8) F631 0.0266(11) 0.0307(10) 0.0506(13) -0.0231(9) 0.0038(11) -0.0092(9) C63 0.0232(18) 0.0152(14) 0.0193(17) -0.0020(12) -0.0104(15) -0.0006(13) C66 0.0237(18) 0.0169(15) 0.0228(18) -0.0062(12) -0.0076(16) -0.0014(13) C62 0.0188(17) 0.0171(14) 0.0149(16) -0.0007(12) -0.0066(14) -0.0001(12) N4 0.0217(14) 0.0142(12) 0.0157(14) -0.0028(10) -0.0054(12) 0.0025(10) C61 0.0235(18) 0.0161(14) 0.0157(16) -0.0040(12) -0.0089(15) 0.0030(13) C96 0.0256(18) 0.0160(14) 0.0191(17) -0.0079(12) -0.0070(15) 0.0002(13) C92 0.0224(17) 0.0198(15) 0.0194(17) -0.0081(12) -0.0063(15) 0.0013(13) C64 0.0254(18) 0.0213(16) 0.0220(17) -0.0088(13) -0.0084(16) 0.0025(14) C84 0.0251(18) 0.0198(15) 0.0213(17) -0.0025(13) -0.0069(15) -0.0087(14) N1 0.0190(14) 0.0138(12) 0.0145(13) -0.0036(10) -0.0032(12) 0.0018(10) N2 0.0217(14) 0.0127(12) 0.0161(13) -0.0036(10) -0.0032(12) 0.0001(10) C86 0.0236(18) 0.0144(14) 0.0177(16) -0.0030(12) -0.0021(15) -0.0015(13) C631 0.0213(18) 0.0189(15) 0.0243(18) -0.0096(13) -0.0076(16) 0.0047(13) B1 0.022(2) 0.0131(16) 0.0171(18) -0.0055(13) -0.0058(17) 0.0011(14) N3 0.0255(15) 0.0132(12) 0.0125(13) -0.0020(10) -0.0034(12) -0.0002(11) C93 0.031(2) 0.0182(15) 0.0172(17) -0.0062(12) -0.0067(16) -0.0030(14) C32 0.0289(19) 0.0174(15) 0.0208(17) -0.0079(12) -0.0089(16) -0.0032(13) C36 0.035(2) 0.0177(15) 0.0161(17) -0.0058(12) -0.0065(16) -0.0072(14) C94 0.0281(19) 0.0204(15) 0.0187(17) -0.0060(13) -0.0027(15) -0.0085(14) C4 0.031(2) 0.0168(15) 0.0256(18) -0.0083(13) -0.0084(16) -0.0029(14) C6 0.0316(19) 0.0123(14) 0.0243(18) -0.0022(12) -0.0084(16) 0.0016(13) C31 0.039(2) 0.0111(14) 0.0168(17) -0.0014(12) -0.0116(16) -0.0045(14) C76 0.0171(16) 0.0194(15) 0.0156(16) -0.0092(12) -0.0009(14) 0.0003(12) C2 0.0195(17) 0.0170(14) 0.0146(16) -0.0015(12) -0.0064(14) -0.0040(12) C3 0.0303(19) 0.0199(15) 0.0199(17) -0.0083(13) -0.0072(16) -0.0034(14) C12 0.0280(19) 0.0254(16) 0.0159(17) -0.0050(13) -0.0050(16) -0.0008(14) C91 0.0264(18) 0.0139(14) 0.0210(17) -0.0072(12) -0.0118(15) -0.0014(13) C81 0.0233(17) 0.0132(14) 0.0123(15) 0.0012(11) -0.0023(14) -0.0040(12) C75 0.0285(19) 0.0161(15) 0.0153(16) -0.0043(12) -0.0025(15) -0.0016(13) C83 0.0286(19) 0.0156(14) 0.0174(17) -0.0024(12) -0.0055(15) -0.0046(13) C322 0.034(2) 0.0243(17) 0.031(2) -0.0083(14) -0.0081(18) -0.0057(15) C321 0.0273(19) 0.0188(15) 0.0216(17) -0.0058(12) -0.0080(16) -0.0012(13) C71 0.0227(17) 0.0163(14) 0.0144(16) -0.0075(12) -0.0035(14) 0.0016(12) C5 0.0257(18) 0.0168(15) 0.0232(18) -0.0083(13) -0.0048(16) 0.0064(13) C82 0.0200(17) 0.0171(15) 0.0163(16) -0.0026(12) -0.0012(15) -0.0021(13) C21 0.0300(19) 0.0127(14) 0.0229(17) -0.0059(12) -0.0148(16) 0.0041(13) C11 0.0273(18) 0.0176(15) 0.0149(16) -0.0031(12) -0.0064(15) 0.0026(13) C33 0.034(2) 0.0209(16) 0.0230(18) -0.0032(13) -0.0134(17) -0.0037(14) C74 0.034(2) 0.0181(15) 0.0186(17) -0.0046(12) -0.0106(16) 0.0061(14) Cl2 0.0659(8) 0.0614(7) 0.0396(6) -0.0108(5) -0.0179(6) 0.0015(6) Cl3 0.0420(7) 0.0558(7) 0.1489(15) 0.0040(8) -0.0190(9) -0.0088(6) F831 0.0498(14) 0.0211(10) 0.0432(13) -0.0129(9) -0.0090(11) 0.0051(9) F731 0.0413(13) 0.0293(11) 0.0749(17) -0.0134(10) -0.0334(13) -0.0019(9) F931 0.0398(13) 0.0269(10) 0.0336(12) 0.0002(8) -0.0092(11) 0.0069(9) F951 0.0312(12) 0.0404(12) 0.0537(14) -0.0250(10) -0.0101(11) 0.0108(9) F651 0.0422(14) 0.0531(14) 0.0441(14) 0.0055(11) 0.0078(12) -0.0146(11) F732 0.0227(11) 0.0728(15) 0.0465(14) -0.0332(12) -0.0031(11) 0.0006(11) F851 0.0355(13) 0.0621(14) 0.0717(17) -0.0438(13) -0.0261(13) 0.0233(11) F733 0.0435(13) 0.0569(13) 0.0303(12) -0.0024(10) -0.0222(11) -0.0051(11) F832 0.0727(17) 0.0346(12) 0.0343(13) -0.0191(9) 0.0117(13) -0.0074(11) F852 0.0510(14) 0.0507(13) 0.0488(14) -0.0106(11) -0.0312(13) 0.0214(11) F833 0.0541(15) 0.0536(14) 0.096(2) -0.0552(14) -0.0385(15) 0.0098(12) F932 0.0620(16) 0.0526(14) 0.0227(12) 0.0101(10) 0.0016(12) 0.0139(12) F751 0.0433(14) 0.0281(11) 0.0575(16) -0.0038(10) 0.0164(13) -0.0071(10) F933 0.0709(17) 0.0172(10) 0.109(2) -0.0077(12) -0.0450(17) -0.0045(11) F652 0.0275(12) 0.0969(19) 0.0442(14) -0.0152(13) -0.0043(12) -0.0165(13) F952 0.0334(13) 0.0486(14) 0.0552(16) 0.0014(11) 0.0162(12) -0.0022(11) F853 0.0259(12) 0.0364(12) 0.109(2) -0.0119(13) -0.0222(14) -0.0001(10) C72 0.0254(18) 0.0150(14) 0.0147(16) -0.0054(12) -0.0021(15) 0.0005(13) F953 0.0313(13) 0.117(2) 0.0588(17) -0.0569(15) -0.0203(13) 0.0118(13) F653 0.0629(18) 0.0754(18) 0.112(2) -0.0765(18) 0.0536(17) -0.0430(15) C422 0.032(2) 0.0372(19) 0.031(2) -0.0039(15) -0.0146(18) -0.0064(16) F752 0.0432(14) 0.0192(10) 0.0759(18) 0.0114(10) -0.0059(13) 0.0052(10) C73 0.0250(18) 0.0217(15) 0.0157(16) -0.0082(12) -0.0053(15) 0.0022(13) C161 0.0217(18) 0.0192(15) 0.0205(17) -0.0006(12) -0.0040(15) -0.0034(13) F753 0.174(3) 0.0402(13) 0.0620(17) 0.0159(12) -0.069(2) -0.0603(18) C162 0.040(2) 0.0263(18) 0.039(2) -0.0082(15) -0.0133(19) -0.0060(16) C43 0.032(2) 0.0225(16) 0.0185(17) -0.0024(13) -0.0102(16) -0.0006(14) C24 0.047(2) 0.0240(17) 0.029(2) -0.0073(14) -0.023(2) 0.0075(16) C163 0.027(2) 0.0368(19) 0.038(2) -0.0172(16) -0.0115(18) 0.0041(16) C51 0.0270(19) 0.0267(17) 0.0222(18) -0.0073(13) -0.0036(16) 0.0004(14) C44 0.037(2) 0.0263(17) 0.0118(16) -0.0030(13) -0.0009(16) -0.0024(15) C122 0.0258(19) 0.0328(18) 0.029(2) -0.0052(15) -0.0049(17) -0.0038(15) C951 0.0269(19) 0.0346(19) 0.0212(18) -0.0102(14) -0.0014(17) -0.0046(15) C65 0.0213(18) 0.0200(15) 0.0200(17) -0.0054(12) -0.0037(15) -0.0011(13) C731 0.029(2) 0.0277(17) 0.0209(18) -0.0076(14) -0.0080(17) 0.0026(15) C362 0.042(2) 0.039(2) 0.038(2) -0.0134(17) -0.006(2) 0.0002(18) C42 0.0223(18) 0.0153(14) 0.0216(17) -0.0017(12) -0.0056(15) 0.0003(13) C34 0.047(2) 0.0212(16) 0.0184(18) -0.0013(13) -0.0151(18) -0.0066(16) C222 0.036(2) 0.035(2) 0.037(2) -0.0013(16) -0.002(2) -0.0022(17) C41 0.0267(18) 0.0122(14) 0.0149(16) -0.0003(11) -0.0041(15) 0.0017(13) C23 0.039(2) 0.0216(16) 0.0213(18) -0.0026(13) -0.0059(18) 0.0038(15) C26 0.0306(19) 0.0129(14) 0.0285(19) -0.0065(13) -0.0126(17) 0.0043(13) C421 0.0262(19) 0.0290(17) 0.0185(17) -0.0025(13) -0.0064(16) -0.0008(14) C16 0.0303(19) 0.0183(15) 0.0184(17) -0.0031(12) -0.0063(16) -0.0013(14) C461 0.0274(19) 0.0270(17) 0.0200(17) -0.0051(13) -0.0038(16) -0.0042(14) C15 0.0247(19) 0.0242(17) 0.0267(19) 0.0009(14) -0.0009(17) -0.0018(14) C931 0.032(2) 0.0251(18) 0.032(2) -0.0001(15) -0.0071(18) -0.0027(16) C52 0.0197(17) 0.0265(16) 0.0223(18) -0.0080(13) -0.0012(15) -0.0030(14) C361 0.0293(19) 0.0264(17) 0.0207(18) -0.0069(13) -0.0031(16) -0.0017(15) C831 0.034(2) 0.0284(18) 0.027(2) -0.0108(14) -0.0071(18) -0.0040(16) C121 0.0251(19) 0.0286(17) 0.0203(17) -0.0051(13) -0.0067(16) -0.0013(14) C46 0.0290(19) 0.0155(14) 0.0218(18) -0.0057(12) -0.0070(16) 0.0001(13) C95 0.0267(18) 0.0252(16) 0.0207(17) -0.0120(13) -0.0064(16) -0.0033(14) C323 0.032(2) 0.0260(17) 0.030(2) -0.0105(14) -0.0132(18) 0.0006(15) C223 0.040(2) 0.037(2) 0.046(2) -0.0092(17) -0.010(2) -0.0123(18) C13 0.029(2) 0.039(2) 0.0234(19) 0.0024(15) -0.0119(17) 0.0029(16) C423 0.031(2) 0.042(2) 0.036(2) -0.0127(17) -0.0080(19) 0.0080(17) C261 0.0219(18) 0.0208(16) 0.037(2) -0.0018(14) -0.0074(17) 0.0032(14) C25 0.033(2) 0.0216(16) 0.041(2) -0.0111(15) -0.0193(19) 0.0042(15) C262 0.036(2) 0.0285(18) 0.032(2) -0.0058(15) -0.0085(18) 0.0062(16) C651 0.035(2) 0.0277(18) 0.033(2) -0.0154(15) -0.0004(18) -0.0078(16) C85 0.0290(19) 0.0176(15) 0.0212(17) -0.0003(12) -0.0093(16) -0.0020(14) C45 0.0251(19) 0.0261(17) 0.0197(17) -0.0038(13) 0.0007(16) -0.0049(14) C53 0.033(2) 0.0222(16) 0.0202(17) -0.0034(13) -0.0070(16) -0.0035(14) C462 0.030(2) 0.0278(17) 0.0281(19) -0.0052(14) -0.0080(17) -0.0054(15) C851 0.030(2) 0.0271(18) 0.043(2) -0.0118(16) -0.0171(19) 0.0009(16) C221 0.0260(19) 0.0268(17) 0.0217(18) 0.0013(14) -0.0025(17) -0.0020(15) C123 0.033(2) 0.052(2) 0.030(2) -0.0207(17) -0.0065(19) -0.0024(18) C35 0.039(2) 0.0237(16) 0.0158(17) -0.0032(13) -0.0041(17) -0.0119(15) C22 0.0298(19) 0.0136(14) 0.0197(17) -0.0034(12) -0.0067(16) 0.0028(13) C751 0.037(2) 0.0207(16) 0.0248(19) -0.0026(14) -0.0080(19) -0.0005(15) C263 0.030(2) 0.036(2) 0.078(3) -0.027(2) 0.001(2) -0.0026(18) C463 0.041(2) 0.0288(18) 0.033(2) -0.0115(15) -0.0091(19) -0.0068(16) C999 0.047(3) 0.065(3) 0.040(3) -0.012(2) -0.013(2) 0.004(2) C363 0.035(2) 0.040(2) 0.028(2) -0.0057(16) -0.0036(18) -0.0080(17) C14 0.034(2) 0.0326(19) 0.025(2) 0.0077(15) -0.0059(18) 0.0058(16) _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 C50 1.849(3) . ? Ni1 C1 1.899(3) . ? Ni1 Cl1 2.1559(9) . ? Ni1 Ni2 2.4385(9) . ? Ni2 C50 1.858(3) . ? Ni2 C2 1.898(3) . ? Ni2 Cl1 2.1672(10) . ? Si1 C51 1.861(3) . ? Si1 C52 1.866(3) . ? Si1 C53 1.870(3) . ? Si1 C50 1.882(3) . ? C1 N1 1.350(4) . ? C1 N2 1.365(4) . ? F633 C631 1.348(3) . ? F632 C631 1.350(3) . ? F631 C631 1.323(4) . ? C63 C62 1.378(4) . ? C63 C64 1.387(4) . ? C63 C631 1.499(4) . ? C66 C65 1.391(4) . ? C66 C61 1.396(4) . ? C62 C61 1.405(4) . ? N4 C2 1.363(3) . ? N4 C6 1.376(4) . ? N4 C41 1.457(4) . ? C61 B1 1.644(5) . ? C96 C91 1.392(4) . ? C96 C95 1.394(4) . ? C92 C93 1.383(4) . ? C92 C91 1.411(4) . ? C64 C65 1.396(4) . ? C84 C85 1.378(4) . ? C84 C83 1.383(5) . ? N1 C3 1.388(4) . ? N1 C11 1.460(3) . ? N2 C4 1.389(4) . ? N2 C21 1.448(4) . ? C86 C85 1.385(4) . ? C86 C81 1.401(4) . ? B1 C91 1.633(5) . ? B1 C71 1.649(4) . ? B1 C81 1.652(4) . ? N3 C2 1.357(4) . ? N3 C5 1.384(4) . ? N3 C31 1.458(3) . ? C93 C94 1.378(5) . ? C93 C931 1.505(4) . ? C32 C33 1.390(4) . ? C32 C31 1.404(4) . ? C32 C321 1.530(4) . ? C36 C31 1.392(5) . ? C36 C35 1.396(4) . ? C36 C361 1.518(5) . ? C94 C95 1.383(4) . ? C4 C3 1.344(4) . ? C6 C5 1.337(4) . ? C76 C71 1.385(4) . ? C76 C75 1.394(4) . ? C12 C11 1.394(4) . ? C12 C13 1.400(4) . ? C12 C121 1.516(4) . ? C81 C82 1.398(4) . ? C75 C74 1.379(4) . ? C75 C751 1.502(4) . ? C83 C82 1.392(4) . ? C83 C831 1.485(5) . ? C322 C321 1.540(4) . ? C321 C323 1.526(4) . ? C71 C72 1.398(4) . ? C21 C22 1.393(4) . ? C21 C26 1.399(4) . ? C11 C16 1.400(4) . ? C33 C34 1.381(5) . ? C74 C73 1.386(4) . ? Cl2 C999 1.737(4) . ? Cl3 C999 1.752(4) . ? F831 C831 1.348(4) . ? F731 C731 1.328(4) . ? F931 C931 1.312(4) . ? F951 C951 1.333(4) . ? F651 C651 1.326(4) . ? F732 C731 1.337(4) . ? F851 C851 1.325(4) . ? F733 C731 1.348(4) . ? F832 C831 1.343(4) . ? F852 C851 1.344(4) . ? F833 C831 1.331(4) . ? F932 C931 1.341(4) . ? F751 C751 1.328(4) . ? F933 C931 1.340(4) . ? F652 C651 1.333(4) . ? F952 C951 1.337(4) . ? F853 C851 1.330(4) . ? C72 C73 1.395(4) . ? F953 C951 1.333(4) . ? F653 C651 1.322(4) . ? C422 C421 1.528(4) . ? F752 C751 1.320(4) . ? C73 C731 1.485(4) . ? C161 C163 1.511(5) . ? C161 C16 1.519(4) . ? C161 C162 1.532(4) . ? F753 C751 1.319(4) . ? C43 C44 1.377(4) . ? C43 C42 1.390(4) . ? C24 C25 1.376(5) . ? C24 C23 1.379(5) . ? C44 C45 1.384(4) . ? C122 C121 1.529(5) . ? C951 C95 1.491(5) . ? C65 C651 1.483(5) . ? C362 C361 1.523(5) . ? C42 C41 1.387(4) . ? C42 C421 1.518(4) . ? C34 C35 1.370(5) . ? C222 C221 1.509(5) . ? C41 C46 1.400(4) . ? C23 C22 1.396(4) . ? C26 C25 1.388(4) . ? C26 C261 1.522(5) . ? C421 C423 1.525(5) . ? C16 C15 1.392(4) . ? C461 C46 1.521(4) . ? C461 C462 1.527(5) . ? C461 C463 1.536(4) . ? C15 C14 1.375(5) . ? C361 C363 1.531(4) . ? C121 C123 1.535(4) . ? C46 C45 1.394(5) . ? C223 C221 1.539(5) . ? C13 C14 1.374(5) . ? C261 C263 1.523(5) . ? C261 C262 1.527(5) . ? C85 C851 1.500(5) . ? C221 C22 1.520(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C50 Ni1 C1 107.42(13) . . ? C50 Ni1 Cl1 104.87(9) . . ? C1 Ni1 Cl1 147.11(10) . . ? C50 Ni1 Ni2 49.04(9) . . ? C1 Ni1 Ni2 155.22(9) . . ? Cl1 Ni1 Ni2 55.88(3) . . ? C50 Ni2 C2 108.27(12) . . ? C50 Ni2 Cl1 104.10(10) . . ? C2 Ni2 Cl1 147.59(8) . . ? C50 Ni2 Ni1 48.71(9) . . ? C2 Ni2 Ni1 156.71(8) . . ? Cl1 Ni2 Ni1 55.44(3) . . ? C51 Si1 C52 106.21(15) . . ? C51 Si1 C53 112.41(16) . . ? C52 Si1 C53 109.41(14) . . ? C51 Si1 C50 109.52(14) . . ? C52 Si1 C50 111.14(14) . . ? C53 Si1 C50 108.17(14) . . ? Ni1 Cl1 Ni2 68.67(3) . . ? Ni1 C50 Ni2 82.25(12) . . ? Ni1 C50 Si1 109.51(14) . . ? Ni2 C50 Si1 111.16(16) . . ? N1 C1 N2 104.3(2) . . ? N1 C1 Ni1 134.2(2) . . ? N2 C1 Ni1 120.3(2) . . ? C62 C63 C64 121.7(3) . . ? C62 C63 C631 121.1(3) . . ? C64 C63 C631 117.2(3) . . ? C65 C66 C61 122.8(3) . . ? C63 C62 C61 122.2(3) . . ? C2 N4 C6 111.3(2) . . ? C2 N4 C41 125.4(3) . . ? C6 N4 C41 122.2(2) . . ? C66 C61 C62 115.4(3) . . ? C66 C61 B1 122.3(2) . . ? C62 C61 B1 122.2(3) . . ? C91 C96 C95 122.9(3) . . ? C93 C92 C91 121.9(3) . . ? C63 C64 C65 117.4(3) . . ? C85 C84 C83 118.3(3) . . ? C1 N1 C3 111.3(2) . . ? C1 N1 C11 126.6(2) . . ? C3 N1 C11 121.6(2) . . ? C1 N2 C4 111.0(2) . . ? C1 N2 C21 121.4(2) . . ? C4 N2 C21 126.3(2) . . ? C85 C86 C81 122.3(3) . . ? F631 C631 F633 106.7(2) . . ? F631 C631 F632 107.1(2) . . ? F633 C631 F632 105.1(2) . . ? F631 C631 C63 112.9(3) . . ? F633 C631 C63 112.7(2) . . ? F632 C631 C63 111.7(2) . . ? C91 B1 C61 110.0(2) . . ? C91 B1 C71 112.0(3) . . ? C61 B1 C71 104.7(2) . . ? C91 B1 C81 106.5(2) . . ? C61 B1 C81 112.0(3) . . ? C71 B1 C81 111.8(2) . . ? C2 N3 C5 111.6(2) . . ? C2 N3 C31 123.7(2) . . ? C5 N3 C31 124.4(3) . . ? C94 C93 C92 121.2(3) . . ? C94 C93 C931 118.2(3) . . ? C92 C93 C931 120.5(3) . . ? C33 C32 C31 116.8(3) . . ? C33 C32 C321 120.6(3) . . ? C31 C32 C321 122.4(3) . . ? C31 C36 C35 116.7(3) . . ? C31 C36 C361 124.1(3) . . ? C35 C36 C361 119.1(3) . . ? C93 C94 C95 118.4(3) . . ? C3 C4 N2 106.6(3) . . ? C5 C6 N4 107.2(3) . . ? C36 C31 C32 123.4(3) . . ? C36 C31 N3 119.2(3) . . ? C32 C31 N3 117.4(3) . . ? C71 C76 C75 122.0(3) . . ? N3 C2 N4 103.5(2) . . ? N3 C2 Ni2 123.8(2) . . ? N4 C2 Ni2 132.0(2) . . ? C4 C3 N1 106.9(3) . . ? C11 C12 C13 116.6(3) . . ? C11 C12 C121 124.7(3) . . ? C13 C12 C121 118.6(3) . . ? C96 C91 C92 115.3(3) . . ? C96 C91 B1 124.9(3) . . ? C92 C91 B1 119.7(3) . . ? C82 C81 C86 115.3(3) . . ? C82 C81 B1 120.8(3) . . ? C86 C81 B1 123.8(3) . . ? C74 C75 C76 121.2(3) . . ? C74 C75 C751 119.9(3) . . ? C76 C75 C751 118.9(3) . . ? C84 C83 C82 120.5(3) . . ? C84 C83 C831 120.1(3) . . ? C82 C83 C831 119.4(3) . . ? C323 C321 C32 114.2(2) . . ? C323 C321 C322 109.5(2) . . ? C32 C321 C322 110.2(3) . . ? C76 C71 C72 115.9(3) . . ? C76 C71 B1 123.6(2) . . ? C72 C71 B1 120.3(2) . . ? C6 C5 N3 106.5(3) . . ? C83 C82 C81 122.5(3) . . ? C22 C21 C26 123.2(3) . . ? C22 C21 N2 119.2(3) . . ? C26 C21 N2 117.5(3) . . ? C12 C11 C16 123.8(3) . . ? C12 C11 N1 117.8(3) . . ? C16 C11 N1 118.3(3) . . ? C34 C33 C32 120.9(3) . . ? C75 C74 C73 117.9(3) . . ? C73 C72 C71 122.2(3) . . ? C74 C73 C72 120.5(3) . . ? C74 C73 C731 119.6(3) . . ? C72 C73 C731 119.9(3) . . ? C163 C161 C16 111.2(3) . . ? C163 C161 C162 111.8(3) . . ? C16 C161 C162 112.7(3) . . ? C44 C43 C42 120.8(3) . . ? C25 C24 C23 120.3(3) . . ? C43 C44 C45 120.6(3) . . ? F951 C951 F953 105.2(3) . . ? F951 C951 F952 105.4(3) . . ? F953 C951 F952 107.0(3) . . ? F951 C951 C95 113.0(3) . . ? F953 C951 C95 112.4(3) . . ? F952 C951 C95 113.2(3) . . ? C66 C65 C64 120.5(3) . . ? C66 C65 C651 120.2(3) . . ? C64 C65 C651 119.3(3) . . ? F731 C731 F732 106.6(3) . . ? F731 C731 F733 105.9(2) . . ? F732 C731 F733 104.5(3) . . ? F731 C731 C73 114.1(3) . . ? F732 C731 C73 112.4(3) . . ? F733 C731 C73 112.5(3) . . ? C41 C42 C43 117.5(3) . . ? C41 C42 C421 122.3(3) . . ? C43 C42 C421 120.2(3) . . ? C35 C34 C33 120.7(3) . . ? C42 C41 C46 123.5(3) . . ? C42 C41 N4 119.4(3) . . ? C46 C41 N4 117.0(2) . . ? C24 C23 C22 121.1(3) . . ? C25 C26 C21 117.0(3) . . ? C25 C26 C261 121.5(3) . . ? C21 C26 C261 121.1(3) . . ? C42 C421 C423 110.8(3) . . ? C42 C421 C422 111.8(3) . . ? C423 C421 C422 111.0(3) . . ? C15 C16 C11 116.3(3) . . ? C15 C16 C161 119.4(3) . . ? C11 C16 C161 124.1(2) . . ? C46 C461 C462 110.5(3) . . ? C46 C461 C463 111.7(2) . . ? C462 C461 C463 111.1(3) . . ? C14 C15 C16 121.5(3) . . ? F931 C931 F933 106.6(3) . . ? F931 C931 F932 106.7(3) . . ? F933 C931 F932 106.0(3) . . ? F931 C931 C93 114.1(3) . . ? F933 C931 C93 111.2(3) . . ? F932 C931 C93 111.7(3) . . ? C36 C361 C362 110.2(3) . . ? C36 C361 C363 112.4(3) . . ? C362 C361 C363 108.8(3) . . ? F833 C831 F832 106.7(3) . . ? F833 C831 F831 105.2(3) . . ? F832 C831 F831 104.3(3) . . ? F833 C831 C83 114.2(3) . . ? F832 C831 C83 113.0(3) . . ? F831 C831 C83 112.6(3) . . ? C12 C121 C122 111.5(3) . . ? C12 C121 C123 111.0(3) . . ? C122 C121 C123 109.8(3) . . ? C45 C46 C41 116.7(3) . . ? C45 C46 C461 120.0(3) . . ? C41 C46 C461 123.3(3) . . ? C94 C95 C96 120.1(3) . . ? C94 C95 C951 121.5(3) . . ? C96 C95 C951 118.3(3) . . ? C14 C13 C12 120.9(3) . . ? C26 C261 C263 113.8(3) . . ? C26 C261 C262 110.3(3) . . ? C263 C261 C262 110.0(3) . . ? C24 C25 C26 121.3(3) . . ? F653 C651 F651 105.1(3) . . ? F653 C651 F652 107.1(3) . . ? F651 C651 F652 104.0(3) . . ? F653 C651 C65 113.9(3) . . ? F651 C651 C65 114.0(3) . . ? F652 C651 C65 111.9(3) . . ? C84 C85 C86 121.0(3) . . ? C84 C85 C851 117.9(3) . . ? C86 C85 C851 121.1(3) . . ? C44 C45 C46 120.9(3) . . ? F851 C851 F853 108.1(3) . . ? F851 C851 F852 104.8(3) . . ? F853 C851 F852 105.4(3) . . ? F851 C851 C85 113.7(3) . . ? F853 C851 C85 112.4(3) . . ? F852 C851 C85 111.8(3) . . ? C222 C221 C22 113.7(3) . . ? C222 C221 C223 110.5(3) . . ? C22 C221 C223 109.3(3) . . ? C34 C35 C36 121.2(3) . . ? C21 C22 C23 116.8(3) . . ? C21 C22 C221 121.8(3) . . ? C23 C22 C221 121.2(3) . . ? F753 C751 F752 107.4(3) . . ? F753 C751 F751 105.0(3) . . ? F752 C751 F751 105.5(3) . . ? F753 C751 C75 112.8(3) . . ? F752 C751 C75 113.5(3) . . ? F751 C751 C75 111.9(3) . . ? Cl2 C999 Cl3 111.1(2) . . ? C13 C14 C15 120.8(3) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.961 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.096 data_8 _database_code_depnum_ccdc_archive 'CCDC 791321' #TrackingRef 'Carbene.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H84 B Cl F24 N4 Ni2 O2' _chemical_formula_weight 1849.27 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5310(11) _cell_length_b 17.5339(15) _cell_length_c 21.5138(18) _cell_angle_alpha 106.6720(10) _cell_angle_beta 104.999(2) _cell_angle_gamma 91.050(2) _cell_volume 4352.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brick _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 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7284 _exptl_absorpt_correction_T_max 0.8956 _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 42603 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15284 _reflns_number_gt 11728 _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^)+(0.0509P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15284 _refine_ls_number_parameters 1115 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 0.40652(3) 0.29038(2) 0.338210(17) 0.01698(10) Uani 1 1 d . . . Ni2 Ni 0.41845(3) 0.30539(2) 0.228189(17) 0.01771(10) Uani 1 1 d . . . Cl1 Cl 0.45772(6) 0.20372(4) 0.26268(3) 0.02461(17) Uani 1 1 d . . . N3 N 0.48474(17) 0.22505(13) 0.10269(11) 0.0169(5) Uani 1 1 d . . . N2 N 0.48088(17) 0.19145(12) 0.43089(11) 0.0165(5) Uani 1 1 d . . . N1 N 0.33466(17) 0.24697(12) 0.44639(10) 0.0157(5) Uani 1 1 d . . . C13 C 0.0620(2) 0.31286(18) 0.37778(15) 0.0275(7) Uani 1 1 d . . . H13A H 0.0001 0.2968 0.3389 0.033 Uiso 1 1 calc R . . C11 C 0.2399(2) 0.29261(16) 0.44071(13) 0.0183(6) Uani 1 1 d . . . C12 C 0.1501(2) 0.26506(17) 0.38309(14) 0.0218(6) Uani 1 1 d . . . C16 C 0.2424(2) 0.36231(16) 0.49382(14) 0.0204(6) Uani 1 1 d . . . C14 C 0.0633(2) 0.38242(18) 0.42767(16) 0.0292(7) Uani 1 1 d . . . H14A H 0.0032 0.4144 0.4225 0.035 Uiso 1 1 calc R . . C15 C 0.1511(2) 0.40628(17) 0.48521(15) 0.0240(7) Uani 1 1 d . . . H15A H 0.1493 0.4538 0.5198 0.029 Uiso 1 1 calc R . . C24 C 0.7560(2) 0.10642(18) 0.36646(15) 0.0269(7) Uani 1 1 d . . . H24A H 0.8185 0.0867 0.3521 0.032 Uiso 1 1 calc R . . C21 C 0.5754(2) 0.16346(16) 0.40693(13) 0.0185(6) Uani 1 1 d . . . C25 C 0.6597(2) 0.05686(18) 0.34776(14) 0.0249(7) Uani 1 1 d . . . H25A H 0.6571 0.0028 0.3213 0.030 Uiso 1 1 calc R . . C22 C 0.6725(2) 0.21544(16) 0.42786(13) 0.0208(6) Uani 1 1 d . . . C26 C 0.5660(2) 0.08402(16) 0.36671(13) 0.0199(6) Uani 1 1 d . . . C23 C 0.7627(2) 0.18530(18) 0.40616(14) 0.0250(7) Uani 1 1 d . . . H23A H 0.8298 0.2190 0.4186 0.030 Uiso 1 1 calc R . . C6 C 0.4244(2) 0.29308(16) 0.03191(13) 0.0212(6) Uani 1 1 d . . . H6A H 0.4069 0.3114 -0.0067 0.025 Uiso 1 1 calc R . . C2 C 0.4340(2) 0.28457(15) 0.13672(13) 0.0156(6) Uani 1 1 d . . . C4 C 0.4521(2) 0.16694(16) 0.48072(13) 0.0191(6) Uani 1 1 d . . . H4A H 0.4904 0.1326 0.5040 0.023 Uiso 1 1 calc R . . C3 C 0.3604(2) 0.20059(15) 0.48995(13) 0.0183(6) Uani 1 1 d . . . H3A H 0.3205 0.1941 0.5204 0.022 Uiso 1 1 calc R . . C5 C 0.4803(2) 0.23036(16) 0.03897(13) 0.0208(6) Uani 1 1 d . . . H5A H 0.5110 0.1961 0.0066 0.025 Uiso 1 1 calc R . . C1 C 0.4086(2) 0.24131(15) 0.40878(13) 0.0162(6) Uani 1 1 d . . . C161 C 0.3390(2) 0.38870(17) 0.55740(14) 0.0241(7) Uani 1 1 d . . . H16A H 0.3641 0.3393 0.5688 0.029 Uiso 1 1 calc R . . C162 C 0.4380(3) 0.43061(19) 0.54684(15) 0.0359(8) Uani 1 1 d . . . H16B H 0.4602 0.3954 0.5089 0.054 Uiso 1 1 calc R . . H16C H 0.5002 0.4428 0.5878 0.054 Uiso 1 1 calc R . . H16D H 0.4170 0.4804 0.5371 0.054 Uiso 1 1 calc R . . C222 C 0.7174(3) 0.2986(2) 0.54882(16) 0.0444(9) Uani 1 1 d . . . H22A H 0.6646 0.2621 0.5558 0.067 Uiso 1 1 calc R . . H22B H 0.7190 0.3526 0.5790 0.067 Uiso 1 1 calc R . . H22C H 0.7917 0.2803 0.5586 0.067 Uiso 1 1 calc R . . C221 C 0.6817(2) 0.29963(17) 0.47552(15) 0.0259(7) Uani 1 1 d . . . H22D H 0.6060 0.3186 0.4672 0.031 Uiso 1 1 calc R . . C34 C 0.6250(2) 0.04572(16) 0.17942(14) 0.0210(6) Uani 1 1 d . . . H34A H 0.6554 0.0059 0.1988 0.025 Uiso 1 1 calc R . . C35 C 0.5183(2) 0.03112(16) 0.13673(13) 0.0211(6) Uani 1 1 d . . . H35A H 0.4774 -0.0193 0.1260 0.025 Uiso 1 1 calc R . . C36 C 0.4702(2) 0.08931(16) 0.10932(13) 0.0185(6) Uani 1 1 d . . . C31 C 0.5350(2) 0.16203(16) 0.12751(13) 0.0180(6) Uani 1 1 d . . . C33 C 0.6877(2) 0.11707(16) 0.19415(14) 0.0222(7) Uani 1 1 d . . . H33A H 0.7618 0.1252 0.2223 0.027 Uiso 1 1 calc R . . C32 C 0.6437(2) 0.17777(16) 0.16815(14) 0.0202(6) Uani 1 1 d . . . C361 C 0.3517(2) 0.07285(16) 0.06293(14) 0.0208(6) Uani 1 1 d . . . H36A H 0.3371 0.1183 0.0435 0.025 Uiso 1 1 calc R . . C321 C 0.7128(2) 0.25644(17) 0.18554(15) 0.0270(7) Uani 1 1 d . . . H32A H 0.6681 0.2902 0.1602 0.032 Uiso 1 1 calc R . . C322 C 0.8196(3) 0.24404(19) 0.16332(18) 0.0402(9) Uani 1 1 d . . . H32B H 0.8006 0.2183 0.1145 0.060 Uiso 1 1 calc R . . H32C H 0.8642 0.2100 0.1866 0.060 Uiso 1 1 calc R . . H32D H 0.8621 0.2960 0.1747 0.060 Uiso 1 1 calc R . . C121 C 0.1438(2) 0.18715(18) 0.32793(14) 0.0264(7) Uani 1 1 d . . . H12A H 0.2128 0.1611 0.3411 0.032 Uiso 1 1 calc R . . C122 C 0.0442(3) 0.13010(19) 0.32086(15) 0.0362(8) Uani 1 1 d . . . H12B H 0.0495 0.1208 0.3643 0.054 Uiso 1 1 calc R . . H12C H 0.0440 0.0791 0.2867 0.054 Uiso 1 1 calc R . . H12D H -0.0247 0.1540 0.3070 0.054 Uiso 1 1 calc R . . N4 N 0.39733(18) 0.32582(13) 0.09148(11) 0.0168(5) Uani 1 1 d . . . C41 C 0.3324(2) 0.39342(16) 0.10263(13) 0.0181(6) Uani 1 1 d . . . C43 C 0.1612(2) 0.44374(17) 0.11143(14) 0.0265(7) Uani 1 1 d . . . H43A H 0.0849 0.4359 0.1092 0.032 Uiso 1 1 calc R . . C42 C 0.2205(2) 0.37783(16) 0.09760(13) 0.0212(6) Uani 1 1 d . . . C46 C 0.3845(2) 0.46956(16) 0.11653(13) 0.0196(6) Uani 1 1 d . . . C45 C 0.3204(2) 0.53294(17) 0.13030(14) 0.0252(7) Uani 1 1 d . . . H45A H 0.3529 0.5862 0.1413 0.030 Uiso 1 1 calc R . . C461 C 0.5051(2) 0.48353(16) 0.11785(14) 0.0242(7) Uani 1 1 d . . . H46A H 0.5215 0.4366 0.0835 0.029 Uiso 1 1 calc R . . C462 C 0.5837(3) 0.4875(2) 0.18662(16) 0.0388(8) Uani 1 1 d . . . H46B H 0.5714 0.4377 0.1970 0.058 Uiso 1 1 calc R . . H46C H 0.5693 0.5328 0.2215 0.058 Uiso 1 1 calc R . . H46D H 0.6608 0.4946 0.1853 0.058 Uiso 1 1 calc R . . C463 C 0.5285(3) 0.55848(18) 0.09883(18) 0.0411(9) Uani 1 1 d . . . H46E H 0.6032 0.5598 0.0926 0.062 Uiso 1 1 calc R . . H46F H 0.5237 0.6062 0.1350 0.062 Uiso 1 1 calc R . . H46G H 0.4737 0.5576 0.0568 0.062 Uiso 1 1 calc R . . C421 C 0.1625(2) 0.29361(17) 0.07405(15) 0.0258(7) Uani 1 1 d . . . H42A H 0.2208 0.2559 0.0792 0.031 Uiso 1 1 calc R . . C422 C 0.0844(3) 0.2828(2) 0.11518(18) 0.0554(11) Uani 1 1 d . . . H42B H 0.1246 0.3002 0.1633 0.083 Uiso 1 1 calc R . . H42C H 0.0563 0.2262 0.1016 0.083 Uiso 1 1 calc R . . H42D H 0.0220 0.3149 0.1072 0.083 Uiso 1 1 calc R . . C323 C 0.7390(3) 0.30158(19) 0.26101(16) 0.0404(9) Uani 1 1 d . . . H32E H 0.6695 0.3097 0.2738 0.061 Uiso 1 1 calc R . . H32F H 0.7799 0.3536 0.2703 0.061 Uiso 1 1 calc R . . H32G H 0.7842 0.2703 0.2871 0.061 Uiso 1 1 calc R . . C362 C 0.3365(3) -0.00382(18) 0.00445(15) 0.0350(8) Uani 1 1 d . . . H36B H 0.3882 0.0004 -0.0219 0.053 Uiso 1 1 calc R . . H36C H 0.2601 -0.0118 -0.0245 0.053 Uiso 1 1 calc R . . H36D H 0.3514 -0.0493 0.0222 0.053 Uiso 1 1 calc R . . C223 C 0.7596(3) 0.3595(2) 0.46504(18) 0.0486(10) Uani 1 1 d . . . H22E H 0.7384 0.3579 0.4175 0.073 Uiso 1 1 calc R . . H22F H 0.8360 0.3457 0.4775 0.073 Uiso 1 1 calc R . . H22G H 0.7545 0.4134 0.4933 0.073 Uiso 1 1 calc R . . C261 C 0.4604(2) 0.02734(16) 0.34472(14) 0.0232(7) Uani 1 1 d . . . H26A H 0.4023 0.0579 0.3623 0.028 Uiso 1 1 calc R . . C262 C 0.4156(3) -0.0062(2) 0.26747(16) 0.0419(9) Uani 1 1 d . . . H26B H 0.4029 0.0381 0.2481 0.063 Uiso 1 1 calc R . . H26C H 0.3455 -0.0397 0.2558 0.063 Uiso 1 1 calc R . . H26D H 0.4698 -0.0385 0.2493 0.063 Uiso 1 1 calc R . . C123 C 0.1385(3) 0.20160(19) 0.26023(14) 0.0340(8) Uani 1 1 d . . . H12E H 0.2028 0.2379 0.2656 0.051 Uiso 1 1 calc R . . H12F H 0.0701 0.2256 0.2455 0.051 Uiso 1 1 calc R . . H12G H 0.1390 0.1505 0.2264 0.051 Uiso 1 1 calc R . . C163 C 0.3074(3) 0.44255(19) 0.61853(15) 0.0375(8) Uani 1 1 d . . . H16E H 0.2429 0.4164 0.6248 0.056 Uiso 1 1 calc R . . H16F H 0.2892 0.4938 0.6109 0.056 Uiso 1 1 calc R . . H16G H 0.3700 0.4518 0.6590 0.056 Uiso 1 1 calc R . . C51 C 0.3573(2) 0.38300(18) 0.37014(14) 0.0208(6) Uani 1 1 d . . . C52 C 0.3852(2) 0.40457(19) 0.24953(14) 0.0260(7) Uani 1 1 d . . . O51 O 0.32506(17) 0.44236(12) 0.39075(10) 0.0291(5) Uani 1 1 d . . . O52 O 0.3687(2) 0.47035(12) 0.26568(10) 0.0391(6) Uani 1 1 d . . . B1 B 0.9416(3) 0.24656(18) 0.76174(16) 0.0183(7) Uani 1 1 d . . . C64 C 0.9275(2) 0.11614(17) 0.54707(14) 0.0244(7) Uani 1 1 d . . . H64A H 0.9255 0.0879 0.5019 0.029 Uiso 1 1 calc R . . C63 C 1.0004(2) 0.18338(17) 0.58275(14) 0.0225(7) Uani 1 1 d . . . C61 C 0.9311(2) 0.20209(15) 0.68198(13) 0.0167(6) Uani 1 1 d . . . C66 C 0.8592(2) 0.13318(16) 0.64459(14) 0.0203(6) Uani 1 1 d . . . H66A H 0.8097 0.1145 0.6650 0.024 Uiso 1 1 calc R . . C62 C 1.0019(2) 0.22507(16) 0.64871(14) 0.0209(6) Uani 1 1 d . . . H62A H 1.0534 0.2712 0.6720 0.025 Uiso 1 1 calc R . . C65 C 0.8570(2) 0.09072(16) 0.57891(14) 0.0232(7) Uani 1 1 d . . . C71 C 0.9903(2) 0.34071(16) 0.78451(13) 0.0172(6) Uani 1 1 d . . . C73 C 0.9990(2) 0.46700(16) 0.75832(14) 0.0216(6) Uani 1 1 d . . . C72 C 0.9591(2) 0.38776(16) 0.74087(14) 0.0195(6) Uani 1 1 d . . . H72A H 0.9085 0.3640 0.6977 0.023 Uiso 1 1 calc R . . C81 C 0.8210(2) 0.24697(15) 0.77836(13) 0.0161(6) Uani 1 1 d . . . C82 C 0.7240(2) 0.25549(15) 0.73261(13) 0.0186(6) Uani 1 1 d . . . H82A H 0.7278 0.2586 0.6899 0.022 Uiso 1 1 calc R . . C86 C 0.8101(2) 0.24529(15) 0.84125(13) 0.0170(6) Uani 1 1 d . . . H86A H 0.8748 0.2429 0.8751 0.020 Uiso 1 1 calc R . . C85 C 0.7086(2) 0.24703(15) 0.85589(13) 0.0174(6) Uani 1 1 d . . . C83 C 0.6215(2) 0.25958(15) 0.74701(13) 0.0185(6) Uani 1 1 d . . . C84 C 0.6131(2) 0.25376(15) 0.80870(13) 0.0184(6) Uani 1 1 d . . . H84A H 0.5432 0.2544 0.8183 0.022 Uiso 1 1 calc R . . C851 C 0.6999(2) 0.24025(17) 0.92213(14) 0.0237(7) Uani 1 1 d . . . F851 F 0.79566(14) 0.25973(12) 0.97016(8) 0.0435(5) Uani 1 1 d . . . F852 F 0.62751(15) 0.28682(11) 0.94607(9) 0.0429(5) Uani 1 1 d . . . C651 C 0.7764(3) 0.01904(19) 0.54261(17) 0.0377(8) Uani 1 1 d . . . F651 F 0.79704(19) -0.02643(12) 0.48651(10) 0.0663(7) Uani 1 1 d . . . F653 F 0.77042(17) -0.02797(11) 0.58077(10) 0.0527(6) Uani 1 1 d . . . F652 F 0.67262(17) 0.03857(13) 0.52209(11) 0.0649(7) Uani 1 1 d . . . C631 C 1.0747(3) 0.2158(2) 0.55067(16) 0.0359(8) Uani 1 1 d . . . F631 F 1.07437(19) 0.16824(13) 0.49025(10) 0.0655(7) Uani 1 1 d . . . F632 F 1.17942(16) 0.23010(14) 0.58710(10) 0.0598(6) Uani 1 1 d . . . F633 F 1.0457(2) 0.28533(14) 0.54140(14) 0.0782(8) Uani 1 1 d . . . C91 C 1.0275(2) 0.19489(15) 0.80072(13) 0.0160(6) Uani 1 1 d . . . C93 C 1.2168(2) 0.16132(15) 0.83855(13) 0.0171(6) Uani 1 1 d . . . C92 C 1.1416(2) 0.20746(16) 0.80987(13) 0.0178(6) Uani 1 1 d . . . H92A H 1.1688 0.2490 0.7960 0.021 Uiso 1 1 calc R . . C95 C 1.0683(2) 0.08563(15) 0.84983(13) 0.0177(6) Uani 1 1 d . . . C96 C 0.9933(2) 0.13077(15) 0.82023(13) 0.0178(6) Uani 1 1 d . . . H96A H 0.9162 0.1179 0.8129 0.021 Uiso 1 1 calc R . . C731 C 0.9677(3) 0.51246(18) 0.70893(16) 0.0328(8) Uani 1 1 d . . . F732 F 0.8911(2) 0.47870(13) 0.65552(12) 0.0920(10) Uani 1 1 d . . . F731 F 0.9407(4) 0.58235(16) 0.73352(13) 0.1535(18) Uani 1 1 d . . . C74 C 1.0723(2) 0.50413(16) 0.82148(14) 0.0216(6) Uani 1 1 d . . . H74A H 1.1020 0.5582 0.8334 0.026 Uiso 1 1 calc R . . C76 C 1.0608(2) 0.38079(16) 0.84808(13) 0.0188(6) Uani 1 1 d . . . H76A H 1.0821 0.3522 0.8800 0.023 Uiso 1 1 calc R . . C75 C 1.1010(2) 0.46035(16) 0.86654(13) 0.0195(6) Uani 1 1 d . . . C751 C 1.1728(2) 0.50123(18) 0.93592(15) 0.0274(7) Uani 1 1 d . . . C831 C 0.5229(2) 0.27465(18) 0.69761(15) 0.0260(7) Uani 1 1 d . . . F833 F 0.51216(17) 0.23137(13) 0.63530(9) 0.0605(6) Uani 1 1 d . . . F831 F 0.52736(19) 0.34889(12) 0.69638(12) 0.0836(9) Uani 1 1 d . . . F832 F 0.42933(16) 0.2614(2) 0.70995(12) 0.1030(11) Uani 1 1 d . . . F853 F 0.66431(17) 0.16600(11) 0.91737(9) 0.0490(5) Uani 1 1 d . . . C44 C 0.2108(3) 0.52004(17) 0.12835(14) 0.0276(7) Uani 1 1 d . . . H44A H 0.1691 0.5643 0.1388 0.033 Uiso 1 1 calc R . . C423 C 0.0988(3) 0.27113(19) -0.00037(16) 0.0445(9) Uani 1 1 d . . . H42E H 0.1505 0.2743 -0.0271 0.067 Uiso 1 1 calc R . . H42F H 0.0424 0.3082 -0.0069 0.067 Uiso 1 1 calc R . . H42G H 0.0627 0.2164 -0.0150 0.067 Uiso 1 1 calc R . . C363 C 0.2673(3) 0.0696(2) 0.10214(16) 0.0461(10) Uani 1 1 d . . . H36E H 0.1921 0.0609 0.0716 0.069 Uiso 1 1 calc R . . H36F H 0.2757 0.1202 0.1382 0.069 Uiso 1 1 calc R . . H36G H 0.2799 0.0255 0.1219 0.069 Uiso 1 1 calc R . . C951 C 1.0281(2) 0.02141(17) 0.87387(14) 0.0241(7) Uani 1 1 d . . . F951 F 1.08066(13) -0.04492(9) 0.86028(9) 0.0328(4) Uani 1 1 d . . . F952 F 0.92005(13) -0.00189(10) 0.84611(10) 0.0384(5) Uani 1 1 d . . . F953 F 1.04449(16) 0.04498(10) 0.94109(9) 0.0443(5) Uani 1 1 d . . . C94 C 1.1814(2) 0.10061(15) 0.85970(13) 0.0190(6) Uani 1 1 d . . . H94A H 1.2328 0.0700 0.8804 0.023 Uiso 1 1 calc R . . C931 C 1.3362(2) 0.17709(16) 0.84291(14) 0.0214(6) Uani 1 1 d . . . F933 F 1.40492(12) 0.14558(9) 0.88628(8) 0.0282(4) Uani 1 1 d . . . F932 F 1.35806(13) 0.14596(10) 0.78298(8) 0.0305(4) Uani 1 1 d . . . F931 F 1.37055(13) 0.25556(9) 0.86289(8) 0.0289(4) Uani 1 1 d . . . F751 F 1.22849(14) 0.45026(10) 0.96536(8) 0.0336(4) Uani 1 1 d . . . F752 F 1.11535(15) 0.54052(11) 0.97738(9) 0.0469(5) Uani 1 1 d . . . F753 F 1.25064(15) 0.55600(10) 0.93701(9) 0.0420(5) Uani 1 1 d . . . F733 F 1.0504(2) 0.5294(2) 0.68726(17) 0.1358(16) Uani 1 1 d . . . C263 C 0.4794(3) -0.04221(19) 0.37424(18) 0.0442(9) Uani 1 1 d . . . H26E H 0.5055 -0.0214 0.4236 0.066 Uiso 1 1 calc R . . H26F H 0.5354 -0.0735 0.3571 0.066 Uiso 1 1 calc R . . H26G H 0.4096 -0.0765 0.3610 0.066 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 0.0192(2) 0.0200(2) 0.01388(19) 0.00705(15) 0.00606(15) 0.00301(15) Ni2 0.0216(2) 0.0201(2) 0.01414(19) 0.00737(15) 0.00685(15) 0.00449(15) Cl1 0.0370(4) 0.0246(4) 0.0190(4) 0.0110(3) 0.0137(3) 0.0131(3) N3 0.0184(12) 0.0190(12) 0.0157(12) 0.0071(10) 0.0067(10) 0.0036(10) N2 0.0182(12) 0.0180(12) 0.0158(12) 0.0070(10) 0.0068(10) 0.0037(10) N1 0.0174(12) 0.0198(12) 0.0112(11) 0.0061(10) 0.0045(10) 0.0016(10) C13 0.0186(16) 0.042(2) 0.0249(17) 0.0187(15) 0.0022(13) 0.0011(14) C11 0.0169(15) 0.0245(16) 0.0197(15) 0.0133(13) 0.0082(12) 0.0049(12) C12 0.0194(16) 0.0293(17) 0.0197(15) 0.0112(13) 0.0066(13) -0.0015(13) C16 0.0271(16) 0.0207(15) 0.0194(15) 0.0114(13) 0.0109(13) 0.0030(13) C14 0.0257(17) 0.0382(19) 0.0370(19) 0.0242(16) 0.0163(15) 0.0123(14) C15 0.0286(17) 0.0259(16) 0.0261(17) 0.0135(14) 0.0161(14) 0.0057(13) C24 0.0232(17) 0.0366(19) 0.0281(17) 0.0146(15) 0.0134(14) 0.0110(14) C21 0.0188(15) 0.0263(16) 0.0149(14) 0.0118(13) 0.0057(12) 0.0068(12) C25 0.0310(18) 0.0278(17) 0.0205(16) 0.0109(13) 0.0104(14) 0.0099(14) C22 0.0208(16) 0.0282(16) 0.0169(15) 0.0131(13) 0.0040(12) 0.0038(13) C26 0.0234(16) 0.0244(16) 0.0162(15) 0.0112(13) 0.0070(12) 0.0058(12) C23 0.0180(15) 0.0347(18) 0.0248(16) 0.0144(14) 0.0043(13) 0.0003(13) C6 0.0286(17) 0.0241(16) 0.0152(15) 0.0081(13) 0.0107(13) 0.0047(13) C2 0.0140(14) 0.0169(14) 0.0174(14) 0.0068(12) 0.0050(12) 0.0011(11) C4 0.0247(16) 0.0207(15) 0.0148(14) 0.0098(12) 0.0049(12) 0.0038(12) C3 0.0223(16) 0.0215(15) 0.0126(14) 0.0079(12) 0.0049(12) -0.0011(12) C5 0.0256(16) 0.0240(16) 0.0170(15) 0.0071(13) 0.0118(13) 0.0065(13) C1 0.0145(14) 0.0179(15) 0.0141(14) 0.0027(12) 0.0029(12) -0.0016(11) C161 0.0312(17) 0.0227(16) 0.0178(15) 0.0060(13) 0.0055(13) 0.0056(13) C162 0.0335(19) 0.041(2) 0.0241(18) 0.0030(15) 0.0005(15) -0.0058(15) C222 0.062(2) 0.036(2) 0.0280(19) 0.0032(16) 0.0066(17) -0.0055(18) C221 0.0207(16) 0.0269(17) 0.0282(17) 0.0089(14) 0.0031(13) 0.0015(13) C34 0.0262(17) 0.0200(15) 0.0216(16) 0.0091(13) 0.0109(13) 0.0111(13) C35 0.0256(16) 0.0196(15) 0.0202(15) 0.0041(12) 0.0121(13) 0.0052(12) C36 0.0214(15) 0.0188(15) 0.0185(15) 0.0058(12) 0.0108(12) 0.0062(12) C31 0.0218(16) 0.0199(15) 0.0159(14) 0.0073(12) 0.0091(12) 0.0090(12) C33 0.0182(15) 0.0305(17) 0.0192(15) 0.0083(13) 0.0064(12) 0.0075(13) C32 0.0213(16) 0.0216(16) 0.0215(15) 0.0068(13) 0.0114(13) 0.0067(12) C361 0.0204(15) 0.0218(15) 0.0223(16) 0.0092(13) 0.0065(13) 0.0045(12) C321 0.0228(17) 0.0265(17) 0.0312(18) 0.0106(14) 0.0047(14) 0.0032(13) C322 0.0330(19) 0.037(2) 0.056(2) 0.0160(18) 0.0191(17) -0.0022(15) C121 0.0229(16) 0.0356(18) 0.0180(16) 0.0072(14) 0.0022(13) -0.0022(14) C122 0.040(2) 0.042(2) 0.0226(17) 0.0094(15) 0.0033(15) -0.0095(16) N4 0.0202(13) 0.0191(12) 0.0140(12) 0.0075(10) 0.0066(10) 0.0050(10) C41 0.0267(16) 0.0192(15) 0.0104(14) 0.0069(12) 0.0056(12) 0.0083(12) C43 0.0225(16) 0.0346(18) 0.0273(17) 0.0131(14) 0.0108(14) 0.0105(14) C42 0.0242(16) 0.0260(16) 0.0154(15) 0.0094(13) 0.0054(12) 0.0042(13) C46 0.0276(16) 0.0202(15) 0.0120(14) 0.0062(12) 0.0057(12) 0.0033(13) C45 0.0372(19) 0.0195(16) 0.0187(16) 0.0054(13) 0.0078(14) 0.0032(14) C461 0.0301(17) 0.0188(15) 0.0226(16) 0.0047(13) 0.0073(13) -0.0002(13) C462 0.0287(19) 0.051(2) 0.0326(19) 0.0111(17) 0.0031(15) -0.0035(16) C463 0.046(2) 0.0288(19) 0.060(2) 0.0210(17) 0.0269(19) 0.0042(16) C421 0.0218(16) 0.0285(17) 0.0301(17) 0.0134(14) 0.0071(14) 0.0049(13) C422 0.075(3) 0.050(2) 0.043(2) 0.0073(19) 0.030(2) -0.021(2) C323 0.039(2) 0.034(2) 0.040(2) 0.0029(16) 0.0083(17) -0.0076(16) C362 0.0345(19) 0.041(2) 0.0235(17) 0.0056(15) 0.0025(15) 0.0081(15) C223 0.063(3) 0.036(2) 0.049(2) 0.0109(18) 0.022(2) -0.0059(18) C261 0.0245(16) 0.0228(16) 0.0232(16) 0.0056(13) 0.0095(13) 0.0030(13) C262 0.047(2) 0.044(2) 0.0291(19) 0.0086(16) 0.0036(16) -0.0117(17) C123 0.0307(18) 0.048(2) 0.0201(17) 0.0084(15) 0.0040(14) -0.0096(15) C163 0.052(2) 0.0357(19) 0.0227(18) 0.0045(15) 0.0114(16) 0.0087(16) C51 0.0212(16) 0.0282(17) 0.0161(15) 0.0123(13) 0.0047(12) -0.0026(13) C52 0.0339(18) 0.0339(19) 0.0132(15) 0.0109(14) 0.0076(13) 0.0008(15) O51 0.0422(13) 0.0232(12) 0.0292(12) 0.0112(10) 0.0183(10) 0.0105(10) O52 0.0785(18) 0.0217(12) 0.0248(12) 0.0104(10) 0.0229(12) 0.0157(12) B1 0.0189(17) 0.0200(17) 0.0184(17) 0.0084(14) 0.0060(14) 0.0023(14) C64 0.0297(17) 0.0299(17) 0.0164(15) 0.0078(13) 0.0097(13) 0.0108(14) C63 0.0226(16) 0.0291(17) 0.0207(16) 0.0117(13) 0.0096(13) 0.0060(13) C61 0.0152(14) 0.0193(15) 0.0198(15) 0.0118(12) 0.0051(12) 0.0050(12) C66 0.0212(15) 0.0218(15) 0.0232(16) 0.0109(13) 0.0105(13) 0.0043(12) C62 0.0215(16) 0.0221(16) 0.0207(16) 0.0087(13) 0.0062(13) 0.0042(12) C65 0.0258(16) 0.0210(16) 0.0222(16) 0.0061(13) 0.0055(13) 0.0044(13) C71 0.0135(14) 0.0224(15) 0.0185(15) 0.0070(12) 0.0083(12) 0.0040(12) C73 0.0225(16) 0.0216(16) 0.0230(16) 0.0099(13) 0.0067(13) 0.0012(12) C72 0.0193(15) 0.0215(15) 0.0156(15) 0.0051(12) 0.0021(12) 0.0013(12) C81 0.0189(15) 0.0136(14) 0.0168(14) 0.0061(12) 0.0050(12) 0.0002(11) C82 0.0258(16) 0.0182(15) 0.0137(14) 0.0056(12) 0.0077(12) 0.0026(12) C86 0.0145(14) 0.0170(14) 0.0193(15) 0.0073(12) 0.0023(12) 0.0012(11) C85 0.0236(16) 0.0126(14) 0.0174(15) 0.0039(12) 0.0087(12) 0.0026(12) C83 0.0175(15) 0.0166(15) 0.0196(15) 0.0045(12) 0.0034(12) 0.0013(12) C84 0.0179(15) 0.0165(15) 0.0204(15) 0.0022(12) 0.0086(12) -0.0007(12) C851 0.0219(16) 0.0304(17) 0.0232(16) 0.0115(14) 0.0098(14) 0.0055(13) F851 0.0260(10) 0.0862(15) 0.0207(10) 0.0223(10) 0.0042(8) 0.0002(10) F852 0.0467(12) 0.0655(13) 0.0316(11) 0.0217(10) 0.0275(9) 0.0264(10) C651 0.045(2) 0.0321(19) 0.0312(19) -0.0010(16) 0.0137(17) -0.0025(16) F651 0.0915(18) 0.0445(13) 0.0480(14) -0.0202(11) 0.0336(13) -0.0179(12) F653 0.0700(15) 0.0315(11) 0.0495(13) 0.0074(10) 0.0119(11) -0.0218(10) F652 0.0377(13) 0.0656(15) 0.0639(15) 0.0005(12) -0.0105(11) -0.0107(11) C631 0.037(2) 0.045(2) 0.0319(19) 0.0127(17) 0.0188(17) 0.0057(17) F631 0.0814(16) 0.0847(17) 0.0323(12) 0.0024(11) 0.0380(12) -0.0200(13) F632 0.0352(12) 0.1105(19) 0.0380(12) 0.0228(12) 0.0185(10) -0.0125(12) F633 0.0886(18) 0.0755(17) 0.127(2) 0.0746(17) 0.0756(17) 0.0286(14) C91 0.0186(15) 0.0165(14) 0.0123(14) 0.0023(11) 0.0055(12) 0.0015(11) C93 0.0175(15) 0.0175(15) 0.0151(14) 0.0004(12) 0.0072(12) 0.0027(12) C92 0.0224(16) 0.0185(15) 0.0153(14) 0.0051(12) 0.0102(12) 0.0014(12) C95 0.0223(16) 0.0179(15) 0.0142(14) 0.0048(12) 0.0071(12) 0.0008(12) C96 0.0146(14) 0.0216(15) 0.0163(15) 0.0040(12) 0.0047(12) 0.0012(12) C731 0.041(2) 0.0228(18) 0.0316(19) 0.0150(15) -0.0025(16) -0.0064(15) F732 0.115(2) 0.0622(16) 0.0705(17) 0.0530(14) -0.0557(15) -0.0408(14) F731 0.355(6) 0.0624(18) 0.0480(17) 0.0355(14) 0.038(2) 0.102(3) C74 0.0226(16) 0.0172(15) 0.0261(16) 0.0074(13) 0.0078(13) 0.0008(12) C76 0.0192(15) 0.0227(16) 0.0192(15) 0.0105(12) 0.0084(12) 0.0081(12) C75 0.0170(15) 0.0230(16) 0.0194(15) 0.0064(13) 0.0063(12) 0.0047(12) C751 0.0247(17) 0.0278(17) 0.0273(17) 0.0072(14) 0.0042(14) 0.0069(14) C831 0.0232(17) 0.0323(18) 0.0227(17) 0.0087(14) 0.0061(13) 0.0033(14) F833 0.0641(14) 0.0719(15) 0.0237(11) 0.0005(10) -0.0115(10) 0.0362(12) F831 0.0810(17) 0.0380(13) 0.0948(19) 0.0244(13) -0.0440(14) 0.0131(12) F832 0.0192(12) 0.250(4) 0.0768(18) 0.109(2) 0.0098(12) 0.0250(16) F853 0.0801(15) 0.0365(11) 0.0404(12) 0.0211(9) 0.0237(11) -0.0069(10) C44 0.0384(19) 0.0252(17) 0.0236(17) 0.0091(14) 0.0133(14) 0.0158(15) C423 0.057(2) 0.036(2) 0.032(2) 0.0031(16) 0.0066(18) -0.0087(17) C363 0.0214(18) 0.080(3) 0.0293(19) 0.0063(19) 0.0057(15) -0.0017(18) C951 0.0250(17) 0.0229(16) 0.0255(17) 0.0085(13) 0.0076(14) 0.0034(13) F951 0.0350(10) 0.0209(9) 0.0489(12) 0.0170(8) 0.0149(9) 0.0070(8) F952 0.0245(10) 0.0371(11) 0.0646(13) 0.0322(10) 0.0122(9) -0.0005(8) F953 0.0761(14) 0.0369(11) 0.0291(11) 0.0152(9) 0.0248(10) 0.0004(10) C94 0.0231(16) 0.0186(15) 0.0141(14) 0.0049(12) 0.0028(12) 0.0053(12) C931 0.0214(16) 0.0190(16) 0.0220(16) 0.0036(13) 0.0058(13) 0.0047(12) F933 0.0194(9) 0.0301(10) 0.0329(10) 0.0108(8) 0.0019(8) 0.0047(7) F932 0.0258(9) 0.0394(10) 0.0272(10) 0.0038(8) 0.0158(8) 0.0038(8) F931 0.0225(9) 0.0199(9) 0.0432(11) 0.0065(8) 0.0106(8) -0.0003(7) F751 0.0358(10) 0.0350(10) 0.0237(9) 0.0094(8) -0.0031(8) 0.0064(8) F752 0.0448(12) 0.0591(13) 0.0230(10) -0.0053(9) 0.0047(9) 0.0194(10) F753 0.0415(11) 0.0342(11) 0.0372(11) 0.0084(9) -0.0078(9) -0.0137(9) F733 0.0668(19) 0.245(4) 0.166(3) 0.186(3) 0.0129(19) 0.002(2) C263 0.039(2) 0.039(2) 0.053(2) 0.0225(18) 0.0017(18) -0.0077(16) _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 C51 1.762(3) . ? Ni1 C1 1.943(3) . ? Ni1 Cl1 2.1260(7) . ? Ni1 Ni2 2.4967(5) . ? Ni2 C52 1.754(3) . ? Ni2 C2 1.958(3) . ? Ni2 Cl1 2.1383(8) . ? N3 C2 1.362(3) . ? N3 C5 1.387(3) . ? N3 C31 1.447(3) . ? N2 C1 1.362(3) . ? N2 C4 1.387(3) . ? N2 C21 1.450(3) . ? N1 C1 1.367(3) . ? N1 C3 1.391(3) . ? N1 C11 1.443(3) . ? C13 C14 1.371(4) . ? C13 C12 1.400(4) . ? C11 C12 1.396(4) . ? C11 C16 1.407(4) . ? C12 C121 1.516(4) . ? C16 C15 1.393(4) . ? C16 C161 1.520(4) . ? C14 C15 1.378(4) . ? C24 C25 1.372(4) . ? C24 C23 1.389(4) . ? C21 C26 1.397(4) . ? C21 C22 1.397(4) . ? C25 C26 1.389(4) . ? C22 C23 1.389(4) . ? C22 C221 1.519(4) . ? C26 C261 1.523(4) . ? C6 C5 1.338(4) . ? C6 N4 1.378(3) . ? C2 N4 1.366(3) . ? C4 C3 1.335(4) . ? C161 C162 1.529(4) . ? C161 C163 1.532(4) . ? C222 C221 1.529(4) . ? C221 C223 1.522(4) . ? C34 C33 1.375(4) . ? C34 C35 1.384(4) . ? C35 C36 1.392(4) . ? C36 C31 1.396(4) . ? C36 C361 1.528(4) . ? C31 C32 1.389(4) . ? C33 C32 1.397(4) . ? C32 C321 1.511(4) . ? C361 C363 1.523(4) . ? C361 C362 1.524(4) . ? C321 C323 1.532(4) . ? C321 C322 1.532(4) . ? C121 C122 1.533(4) . ? C121 C123 1.533(4) . ? N4 C41 1.448(3) . ? C41 C46 1.391(4) . ? C41 C42 1.395(4) . ? C43 C44 1.372(4) . ? C43 C42 1.387(4) . ? C42 C421 1.519(4) . ? C46 C45 1.391(4) . ? C46 C461 1.519(4) . ? C45 C44 1.376(4) . ? C461 C463 1.529(4) . ? C461 C462 1.532(4) . ? C421 C422 1.521(4) . ? C421 C423 1.523(4) . ? C261 C263 1.524(4) . ? C261 C262 1.539(4) . ? C51 O51 1.134(3) . ? C52 O52 1.145(3) . ? B1 C61 1.638(4) . ? B1 C71 1.638(4) . ? B1 C91 1.639(4) . ? B1 C81 1.640(4) . ? C64 C63 1.376(4) . ? C64 C65 1.386(4) . ? C63 C62 1.393(4) . ? C63 C631 1.484(4) . ? C61 C62 1.394(4) . ? C61 C66 1.395(4) . ? C66 C65 1.388(4) . ? C65 C651 1.480(4) . ? C71 C76 1.395(4) . ? C71 C72 1.407(4) . ? C73 C72 1.378(4) . ? C73 C74 1.392(4) . ? C73 C731 1.483(4) . ? C81 C82 1.393(4) . ? C81 C86 1.403(3) . ? C82 C83 1.396(4) . ? C86 C85 1.386(4) . ? C85 C84 1.386(4) . ? C85 C851 1.495(4) . ? C83 C84 1.390(4) . ? C83 C831 1.490(4) . ? C851 F851 1.329(3) . ? C851 F852 1.335(3) . ? C851 F853 1.335(3) . ? C651 F651 1.333(3) . ? C651 F653 1.333(4) . ? C651 F652 1.345(4) . ? C631 F632 1.320(4) . ? C631 F631 1.327(4) . ? C631 F633 1.334(4) . ? C91 C92 1.396(4) . ? C91 C96 1.403(4) . ? C93 C94 1.379(4) . ? C93 C92 1.392(4) . ? C93 C931 1.490(4) . ? C95 C94 1.385(4) . ? C95 C96 1.386(4) . ? C95 C951 1.496(4) . ? C731 F732 1.269(3) . ? C731 F731 1.278(4) . ? C731 F733 1.303(4) . ? C74 C75 1.384(4) . ? C76 C75 1.382(4) . ? C75 C751 1.490(4) . ? C751 F752 1.337(3) . ? C751 F751 1.344(3) . ? C751 F753 1.347(3) . ? C831 F832 1.299(3) . ? C831 F833 1.308(3) . ? C831 F831 1.310(3) . ? C951 F952 1.334(3) . ? C951 F951 1.343(3) . ? C951 F953 1.343(3) . ? C931 F931 1.344(3) . ? C931 F933 1.347(3) . ? C931 F932 1.349(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 C51 Ni1 C1 101.47(11) . . ? C51 Ni1 Cl1 152.82(9) . . ? C1 Ni1 Cl1 105.62(8) . . ? C51 Ni1 Ni2 98.44(9) . . ? C1 Ni1 Ni2 159.89(8) . . ? Cl1 Ni1 Ni2 54.39(2) . . ? C52 Ni2 C2 104.06(12) . . ? C52 Ni2 Cl1 145.96(9) . . ? C2 Ni2 Cl1 109.82(8) . . ? C52 Ni2 Ni1 92.35(9) . . ? C2 Ni2 Ni1 163.53(8) . . ? Cl1 Ni2 Ni1 53.93(2) . . ? Ni1 Cl1 Ni2 71.67(3) . . ? C2 N3 C5 111.5(2) . . ? C2 N3 C31 125.6(2) . . ? C5 N3 C31 122.9(2) . . ? C1 N2 C4 111.1(2) . . ? C1 N2 C21 127.3(2) . . ? C4 N2 C21 121.6(2) . . ? C1 N1 C3 111.1(2) . . ? C1 N1 C11 125.1(2) . . ? C3 N1 C11 123.8(2) . . ? C14 C13 C12 121.2(3) . . ? C12 C11 C16 123.4(2) . . ? C12 C11 N1 118.4(2) . . ? C16 C11 N1 118.2(2) . . ? C11 C12 C13 116.8(3) . . ? C11 C12 C121 123.6(3) . . ? C13 C12 C121 119.6(3) . . ? C15 C16 C11 116.4(3) . . ? C15 C16 C161 121.4(2) . . ? C11 C16 C161 122.2(2) . . ? C13 C14 C15 120.5(3) . . ? C14 C15 C16 121.5(3) . . ? C25 C24 C23 120.5(3) . . ? C26 C21 C22 123.5(3) . . ? C26 C21 N2 117.6(2) . . ? C22 C21 N2 118.8(2) . . ? C24 C25 C26 121.4(3) . . ? C23 C22 C21 117.0(3) . . ? C23 C22 C221 121.1(3) . . ? C21 C22 C221 121.8(2) . . ? C25 C26 C21 116.8(3) . . ? C25 C26 C261 119.9(3) . . ? C21 C26 C261 123.3(2) . . ? C22 C23 C24 120.8(3) . . ? C5 C6 N4 106.7(2) . . ? N3 C2 N4 103.0(2) . . ? N3 C2 Ni2 128.18(19) . . ? N4 C2 Ni2 128.83(19) . . ? C3 C4 N2 107.2(2) . . ? C4 C3 N1 106.8(2) . . ? C6 C5 N3 106.8(2) . . ? N2 C1 N1 103.8(2) . . ? N2 C1 Ni1 128.62(19) . . ? N1 C1 Ni1 127.57(19) . . ? C16 C161 C162 112.2(2) . . ? C16 C161 C163 113.3(2) . . ? C162 C161 C163 109.3(2) . . ? C22 C221 C223 113.9(3) . . ? C22 C221 C222 110.2(2) . . ? C223 C221 C222 110.0(3) . . ? C33 C34 C35 120.9(3) . . ? C34 C35 C36 120.8(3) . . ? C35 C36 C31 116.4(2) . . ? C35 C36 C361 120.4(2) . . ? C31 C36 C361 123.2(2) . . ? C32 C31 C36 124.3(2) . . ? C32 C31 N3 118.2(2) . . ? C36 C31 N3 117.5(2) . . ? C34 C33 C32 120.7(3) . . ? C31 C32 C33 116.7(2) . . ? C31 C32 C321 123.1(2) . . ? C33 C32 C321 120.3(2) . . ? C363 C361 C362 110.3(2) . . ? C363 C361 C36 111.2(2) . . ? C362 C361 C36 111.9(2) . . ? C32 C321 C323 111.3(2) . . ? C32 C321 C322 111.2(2) . . ? C323 C321 C322 110.9(3) . . ? C12 C121 C122 110.8(2) . . ? C12 C121 C123 111.5(2) . . ? C122 C121 C123 110.5(2) . . ? C2 N4 C6 112.0(2) . . ? C2 N4 C41 124.6(2) . . ? C6 N4 C41 123.3(2) . . ? C46 C41 C42 123.9(2) . . ? C46 C41 N4 118.4(2) . . ? C42 C41 N4 117.7(2) . . ? C44 C43 C42 121.2(3) . . ? C43 C42 C41 116.6(3) . . ? C43 C42 C421 120.5(3) . . ? C41 C42 C421 122.8(2) . . ? C45 C46 C41 116.3(3) . . ? C45 C46 C461 121.4(2) . . ? C41 C46 C461 122.3(2) . . ? C44 C45 C46 121.3(3) . . ? C46 C461 C463 112.6(2) . . ? C46 C461 C462 111.5(2) . . ? C463 C461 C462 110.1(3) . . ? C42 C421 C422 112.9(3) . . ? C42 C421 C423 110.4(2) . . ? C422 C421 C423 109.7(3) . . ? C26 C261 C263 111.0(2) . . ? C26 C261 C262 112.5(2) . . ? C263 C261 C262 108.9(2) . . ? O51 C51 Ni1 179.5(3) . . ? O52 C52 Ni2 176.6(3) . . ? C61 B1 C71 111.6(2) . . ? C61 B1 C91 103.2(2) . . ? C71 B1 C91 111.6(2) . . ? C61 B1 C81 112.3(2) . . ? C71 B1 C81 105.7(2) . . ? C91 B1 C81 112.7(2) . . ? C63 C64 C65 118.2(3) . . ? C64 C63 C62 120.6(3) . . ? C64 C63 C631 120.9(3) . . ? C62 C63 C631 118.4(3) . . ? C62 C61 C66 115.0(2) . . ? C62 C61 B1 122.3(2) . . ? C66 C61 B1 122.4(2) . . ? C65 C66 C61 122.9(3) . . ? C63 C62 C61 122.8(3) . . ? C64 C65 C66 120.5(3) . . ? C64 C65 C651 120.3(3) . . ? C66 C65 C651 119.2(3) . . ? C76 C71 C72 115.3(2) . . ? C76 C71 B1 123.5(2) . . ? C72 C71 B1 121.2(2) . . ? C72 C73 C74 120.3(3) . . ? C72 C73 C731 120.2(3) . . ? C74 C73 C731 119.5(3) . . ? C73 C72 C71 122.6(3) . . ? C82 C81 C86 115.7(2) . . ? C82 C81 B1 121.8(2) . . ? C86 C81 B1 122.3(2) . . ? C81 C82 C83 122.7(2) . . ? C85 C86 C81 122.5(2) . . ? C86 C85 C84 120.4(2) . . ? C86 C85 C851 120.7(2) . . ? C84 C85 C851 118.9(2) . . ? C84 C83 C82 119.9(2) . . ? C84 C83 C831 120.3(2) . . ? C82 C83 C831 119.7(2) . . ? C85 C84 C83 118.7(2) . . ? F851 C851 F852 106.4(2) . . ? F851 C851 F853 106.6(2) . . ? F852 C851 F853 105.5(2) . . ? F851 C851 C85 113.3(2) . . ? F852 C851 C85 112.7(2) . . ? F853 C851 C85 111.9(2) . . ? F651 C651 F653 107.2(3) . . ? F651 C651 F652 104.7(3) . . ? F653 C651 F652 105.6(3) . . ? F651 C651 C65 113.8(3) . . ? F653 C651 C65 112.8(3) . . ? F652 C651 C65 111.9(3) . . ? F632 C631 F631 106.3(3) . . ? F632 C631 F633 105.6(3) . . ? F631 C631 F633 105.6(3) . . ? F632 C631 C63 113.3(3) . . ? F631 C631 C63 113.8(3) . . ? F633 C631 C63 111.7(3) . . ? C92 C91 C96 115.5(2) . . ? C92 C91 B1 120.4(2) . . ? C96 C91 B1 123.8(2) . . ? C94 C93 C92 121.0(2) . . ? C94 C93 C931 121.0(2) . . ? C92 C93 C931 118.0(2) . . ? C93 C92 C91 122.3(2) . . ? C94 C95 C96 121.0(2) . . ? C94 C95 C951 118.9(2) . . ? C96 C95 C951 120.1(2) . . ? C95 C96 C91 122.2(2) . . ? F732 C731 F731 106.7(3) . . ? F732 C731 F733 104.3(3) . . ? F731 C731 F733 101.0(3) . . ? F732 C731 C73 116.4(3) . . ? F731 C731 C73 114.1(3) . . ? F733 C731 C73 112.8(3) . . ? C75 C74 C73 118.4(3) . . ? C75 C76 C71 122.8(3) . . ? C76 C75 C74 120.5(3) . . ? C76 C75 C751 120.7(3) . . ? C74 C75 C751 118.8(3) . . ? F752 C751 F751 106.6(2) . . ? F752 C751 F753 105.8(2) . . ? F751 C751 F753 105.8(2) . . ? F752 C751 C75 112.6(2) . . ? F751 C751 C75 112.7(2) . . ? F753 C751 C75 112.7(2) . . ? F832 C831 F833 106.0(3) . . ? F832 C831 F831 105.7(3) . . ? F833 C831 F831 105.0(3) . . ? F832 C831 C83 113.7(2) . . ? F833 C831 C83 113.6(2) . . ? F831 C831 C83 112.2(2) . . ? C43 C44 C45 120.6(3) . . ? F952 C951 F951 106.2(2) . . ? F952 C951 F953 106.9(2) . . ? F951 C951 F953 105.5(2) . . ? F952 C951 C95 112.8(2) . . ? F951 C951 C95 112.9(2) . . ? F953 C951 C95 112.0(2) . . ? C93 C94 C95 117.9(2) . . ? F931 C931 F933 106.2(2) . . ? F931 C931 F932 106.0(2) . . ? F933 C931 F932 105.7(2) . . ? F931 C931 C93 112.8(2) . . ? F933 C931 C93 113.3(2) . . ? F932 C931 C93 112.2(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.995 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.066 data_9 _database_code_depnum_ccdc_archive 'CCDC 791322' #TrackingRef 'Carbene.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H69 B F24 N5 Ni' _chemical_formula_weight 1553.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 20.610(3) _cell_length_b 12.8020(15) _cell_length_c 30.984(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.837(2) _cell_angle_gamma 90.00 _cell_volume 8132.8(17) _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 yellow _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 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3188 _exptl_absorpt_coefficient_mu 0.335 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8244 _exptl_absorpt_correction_T_max 0.9361 _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 ? _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 77481 _diffrn_reflns_av_R_equivalents 0.1713 _diffrn_reflns_av_sigmaI/netI 0.0975 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14312 _reflns_number_gt 10220 _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^)+(0.0666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14312 _refine_ls_number_parameters 981 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.257199(18) 0.26372(3) 0.840613(11) 0.02287(12) Uani 1 1 d . . . C1 C 0.20632(13) 0.1316(2) 0.84048(8) 0.0215(6) Uani 1 1 d . . . C2 C 0.14866(15) -0.0054(2) 0.86399(9) 0.0288(7) Uani 1 1 d . . . H2A H 0.1221 -0.0454 0.8811 0.035 Uiso 1 1 calc R . . C3 C 0.17501(15) -0.0372(2) 0.82829(9) 0.0299(7) Uani 1 1 d . . . H3A H 0.1706 -0.1043 0.8152 0.036 Uiso 1 1 calc R . . C14 C 0.10780(17) 0.2518(2) 0.97802(10) 0.0353(8) Uani 1 1 d . . . H14A H 0.0934 0.2844 1.0029 0.042 Uiso 1 1 calc R . . C15 C 0.06610(16) 0.2456(2) 0.94028(10) 0.0332(8) Uani 1 1 d . . . H15A H 0.0237 0.2753 0.9393 0.040 Uiso 1 1 calc R . . C13 C 0.16974(16) 0.2114(2) 0.98007(10) 0.0322(7) Uani 1 1 d . . . H13A H 0.1979 0.2177 1.0062 0.039 Uiso 1 1 calc R . . C11 C 0.14861(14) 0.1555(2) 0.90703(9) 0.0232(6) Uani 1 1 d . . . C12 C 0.19181(14) 0.1617(2) 0.94465(9) 0.0260(7) Uani 1 1 d . . . C121 C 0.26000(15) 0.1144(2) 0.94722(9) 0.0309(7) Uani 1 1 d . . . H12A H 0.2711 0.1037 0.9169 0.037 Uiso 1 1 calc R . . C42 C 0.28317(15) 0.2813(2) 0.78328(10) 0.0268(7) Uani 1 1 d . . . C41 C 0.21231(14) 0.3658(2) 0.87193(9) 0.0277(7) Uani 1 1 d . . . N41 N 0.19457(12) 0.43619(19) 0.89120(8) 0.0292(6) Uani 1 1 d . . . N42 N 0.30592(12) 0.30202(19) 0.75198(8) 0.0289(6) Uani 1 1 d . . . C52 C 0.33816(16) 0.3398(3) 0.71495(10) 0.0362(8) Uani 1 1 d . . . C44 C 0.17917(16) 0.5286(2) 0.91597(10) 0.0329(8) Uani 1 1 d . . . N2 N 0.20964(12) 0.04621(17) 0.81426(7) 0.0241(5) Uani 1 1 d . . . N1 N 0.16790(11) 0.09653(17) 0.87075(7) 0.0226(5) Uani 1 1 d . . . C16 C 0.08552(14) 0.1963(2) 0.90387(10) 0.0271(7) Uani 1 1 d . . . C122 C 0.31192(16) 0.1858(3) 0.97011(11) 0.0460(9) Uani 1 1 d . . . H12B H 0.3083 0.2556 0.9571 0.069 Uiso 1 1 calc R . . H12C H 0.3553 0.1572 0.9670 0.069 Uiso 1 1 calc R . . H12D H 0.3055 0.1906 1.0010 0.069 Uiso 1 1 calc R . . C123 C 0.26105(18) 0.0070(3) 0.96931(13) 0.0529(10) Uani 1 1 d . . . H12E H 0.3045 -0.0239 0.9693 0.079 Uiso 1 1 calc R . . H12F H 0.2288 -0.0387 0.9535 0.079 Uiso 1 1 calc R . . H12G H 0.2505 0.0151 0.9993 0.079 Uiso 1 1 calc R . . C23 C 0.34464(18) -0.0015(2) 0.74651(10) 0.0402(8) Uani 1 1 d . . . H23A H 0.3903 -0.0139 0.7495 0.048 Uiso 1 1 calc R . . C26 C 0.21048(17) 0.0400(2) 0.73546(9) 0.0339(8) Uani 1 1 d . . . C25 C 0.2448(2) 0.0182(2) 0.70021(10) 0.0412(9) Uani 1 1 d . . . H25A H 0.2225 0.0180 0.6718 0.049 Uiso 1 1 calc R . . C21 C 0.24550(15) 0.0369(2) 0.77663(9) 0.0270(7) Uani 1 1 d . . . C24 C 0.3101(2) -0.0027(2) 0.70564(11) 0.0440(9) Uani 1 1 d . . . H24A H 0.3323 -0.0184 0.6810 0.053 Uiso 1 1 calc R . . C22 C 0.31262(16) 0.0179(2) 0.78338(9) 0.0305(7) Uani 1 1 d . . . C43 C 0.34035(16) 0.3056(2) 0.86783(10) 0.0312(7) Uani 1 1 d . . . N43 N 0.39041(12) 0.3367(2) 0.88348(8) 0.0338(6) Uani 1 1 d . . . C48 C 0.45129(15) 0.3834(3) 0.90233(11) 0.0436(9) Uani 1 1 d . . . C49 C 0.45039(18) 0.3841(3) 0.95147(11) 0.0554(10) Uani 1 1 d . . . H49A H 0.4468 0.3123 0.9619 0.083 Uiso 1 1 calc R . . H49B H 0.4130 0.4249 0.9591 0.083 Uiso 1 1 calc R . . H49C H 0.4908 0.4156 0.9650 0.083 Uiso 1 1 calc R . . C45 C 0.10585(17) 0.5340(3) 0.91601(13) 0.0536(10) Uani 1 1 d . . . H45A H 0.0902 0.4704 0.9292 0.080 Uiso 1 1 calc R . . H45B H 0.0855 0.5400 0.8861 0.080 Uiso 1 1 calc R . . H45C H 0.0943 0.5950 0.9327 0.080 Uiso 1 1 calc R . . B1 B 0.25956(15) 0.7722(2) 0.09634(10) 0.0215(7) Uani 1 1 d . . . C65 C 0.27007(13) 0.4655(2) 0.08073(8) 0.0210(6) Uani 1 1 d . . . C63 C 0.15754(13) 0.5107(2) 0.07732(8) 0.0212(6) Uani 1 1 d . . . C62 C 0.17404(13) 0.6148(2) 0.08358(8) 0.0221(6) Uani 1 1 d . . . H62A H 0.1402 0.6647 0.0850 0.027 Uiso 1 1 calc R . . C61 C 0.23921(13) 0.6491(2) 0.08793(8) 0.0200(6) Uani 1 1 d . . . C66 C 0.28635(13) 0.5705(2) 0.08698(8) 0.0212(6) Uani 1 1 d . . . H66A H 0.3311 0.5895 0.0907 0.025 Uiso 1 1 calc R . . C64 C 0.20514(14) 0.4345(2) 0.07572(8) 0.0217(6) Uani 1 1 d . . . H64A H 0.1936 0.3632 0.0713 0.026 Uiso 1 1 calc R . . C72 C 0.33620(14) 0.7546(2) 0.03174(9) 0.0238(6) Uani 1 1 d . . . H72A H 0.3116 0.6948 0.0221 0.029 Uiso 1 1 calc R . . C71 C 0.32104(13) 0.8054(2) 0.06920(9) 0.0215(6) Uani 1 1 d . . . C75 C 0.40811(14) 0.9290(2) 0.05720(9) 0.0269(7) Uani 1 1 d . . . C74 C 0.42252(14) 0.8750(2) 0.02034(10) 0.0303(7) Uani 1 1 d . . . H74A H 0.4567 0.8975 0.0042 0.036 Uiso 1 1 calc R . . C73 C 0.38571(14) 0.7879(2) 0.00793(9) 0.0274(7) Uani 1 1 d . . . C76 C 0.35826(13) 0.8952(2) 0.08058(9) 0.0241(6) Uani 1 1 d . . . H76A H 0.3488 0.9343 0.1053 0.029 Uiso 1 1 calc R . . C83 C 0.13969(13) 1.0137(2) 0.07838(9) 0.0229(6) Uani 1 1 d . . . C81 C 0.20108(13) 0.8512(2) 0.07711(9) 0.0203(6) Uani 1 1 d . . . C82 C 0.18665(13) 0.9441(2) 0.09715(9) 0.0216(6) Uani 1 1 d . . . H82A H 0.2094 0.9610 0.1245 0.026 Uiso 1 1 calc R . . C85 C 0.11949(13) 0.9002(2) 0.01803(9) 0.0215(6) Uani 1 1 d . . . C84 C 0.10524(13) 0.9925(2) 0.03830(9) 0.0228(6) Uani 1 1 d . . . H84A H 0.0733 1.0394 0.0254 0.027 Uiso 1 1 calc R . . C651 C 0.32403(15) 0.3888(2) 0.07772(10) 0.0282(7) Uani 1 1 d . . . F652 F 0.30437(9) 0.28985(13) 0.07814(7) 0.0468(5) Uani 1 1 d . . . F651 F 0.35330(10) 0.40049(15) 0.04148(6) 0.0513(5) Uani 1 1 d . . . F632 F 0.07534(8) 0.38200(13) 0.07879(6) 0.0451(5) Uani 1 1 d . . . F631 F 0.06328(10) 0.49467(18) 0.02862(7) 0.0615(6) Uani 1 1 d . . . C631 C 0.08712(14) 0.4814(2) 0.07004(10) 0.0294(7) Uani 1 1 d . . . C751 C 0.44541(15) 1.0260(2) 0.06998(10) 0.0342(8) Uani 1 1 d . . . F751 F 0.42845(11) 1.10645(14) 0.04422(8) 0.0682(7) Uani 1 1 d . . . C831 C 0.12679(15) 1.1127(2) 0.10169(10) 0.0315(7) Uani 1 1 d . . . F832 F 0.07057(9) 1.15785(14) 0.08764(7) 0.0540(6) Uani 1 1 d . . . F831 F 0.17362(9) 1.18470(13) 0.09751(6) 0.0452(5) Uani 1 1 d . . . C851 C 0.08221(14) 0.8712(2) -0.02419(9) 0.0281(7) Uani 1 1 d . . . F852 F 0.05524(9) 0.95362(13) -0.04586(5) 0.0382(5) Uani 1 1 d . . . F851 F 0.11965(9) 0.82392(14) -0.05157(5) 0.0386(4) Uani 1 1 d . . . F853 F 0.03337(9) 0.80439(15) -0.01917(6) 0.0467(5) Uani 1 1 d . . . F833 F 0.12622(9) 1.09766(13) 0.14452(6) 0.0419(5) Uani 1 1 d . . . F633 F 0.04939(9) 0.53922(14) 0.09288(7) 0.0543(6) Uani 1 1 d . . . F653 F 0.37161(9) 0.39884(14) 0.11036(6) 0.0451(5) Uani 1 1 d . . . C91 C 0.27715(13) 0.78270(19) 0.14885(9) 0.0204(6) Uani 1 1 d . . . C92 C 0.22788(14) 0.7919(2) 0.17663(9) 0.0251(7) Uani 1 1 d . . . H92A H 0.1838 0.7951 0.1644 0.030 Uiso 1 1 calc R . . C93 C 0.24132(15) 0.7966(2) 0.22143(10) 0.0291(7) Uani 1 1 d . . . C96 C 0.34076(14) 0.7754(2) 0.16923(9) 0.0227(6) Uani 1 1 d . . . H96A H 0.3758 0.7684 0.1518 0.027 Uiso 1 1 calc R . . C221 C 0.34967(15) 0.0157(2) 0.82817(10) 0.0345(8) Uani 1 1 d . . . H22A H 0.3240 0.0577 0.8477 0.041 Uiso 1 1 calc R . . C223 C 0.3551(2) -0.0951(3) 0.84666(13) 0.0608(11) Uani 1 1 d . . . H22B H 0.3113 -0.1252 0.8467 0.091 Uiso 1 1 calc R . . H22C H 0.3763 -0.0928 0.8764 0.091 Uiso 1 1 calc R . . H22D H 0.3810 -0.1383 0.8287 0.091 Uiso 1 1 calc R . . C222 C 0.41699(17) 0.0664(3) 0.82916(12) 0.0481(9) Uani 1 1 d . . . H22E H 0.4128 0.1351 0.8152 0.072 Uiso 1 1 calc R . . H22F H 0.4455 0.0220 0.8135 0.072 Uiso 1 1 calc R . . H22G H 0.4358 0.0745 0.8593 0.072 Uiso 1 1 calc R . . C261 C 0.13886(17) 0.0675(3) 0.72928(11) 0.0445(9) Uani 1 1 d . . . H26A H 0.1224 0.0712 0.7585 0.053 Uiso 1 1 calc R . . C263 C 0.0986(3) -0.0116(5) 0.7026(2) 0.136(3) Uani 1 1 d . . . H26B H 0.1082 -0.0817 0.7142 0.204 Uiso 1 1 calc R . . H26C H 0.1091 -0.0084 0.6724 0.204 Uiso 1 1 calc R . . H26D H 0.0522 0.0038 0.7036 0.204 Uiso 1 1 calc R . . C262 C 0.1293(2) 0.1725(4) 0.7081(3) 0.155(3) Uani 1 1 d . . . H26E H 0.1471 0.2269 0.7282 0.233 Uiso 1 1 calc R . . H26F H 0.0827 0.1849 0.7004 0.233 Uiso 1 1 calc R . . H26G H 0.1520 0.1744 0.6818 0.233 Uiso 1 1 calc R . . C161 C 0.04010(14) 0.1894(2) 0.86202(10) 0.0314(7) Uani 1 1 d . . . H16A H 0.0582 0.1353 0.8433 0.038 Uiso 1 1 calc R . . C162 C 0.0381(2) 0.2925(3) 0.83734(12) 0.0653(12) Uani 1 1 d . . . H16B H 0.0823 0.3113 0.8312 0.098 Uiso 1 1 calc R . . H16C H 0.0207 0.3473 0.8550 0.098 Uiso 1 1 calc R . . H16D H 0.0101 0.2851 0.8100 0.098 Uiso 1 1 calc R . . C163 C -0.02811(19) 0.1550(4) 0.87019(14) 0.0886(17) Uani 1 1 d . . . H16E H -0.0255 0.0900 0.8870 0.133 Uiso 1 1 calc R . . H16F H -0.0543 0.1434 0.8424 0.133 Uiso 1 1 calc R . . H16G H -0.0486 0.2095 0.8865 0.133 Uiso 1 1 calc R . . C46 C 0.2123(2) 0.5148(3) 0.96170(11) 0.0526(10) Uani 1 1 d . . . H46A H 0.1961 0.4509 0.9744 0.079 Uiso 1 1 calc R . . H46B H 0.2024 0.5750 0.9795 0.079 Uiso 1 1 calc R . . H46C H 0.2595 0.5096 0.9608 0.079 Uiso 1 1 calc R . . C51 C 0.50651(18) 0.3146(4) 0.88918(15) 0.0771(15) Uani 1 1 d . . . H51A H 0.5001 0.2428 0.8987 0.116 Uiso 1 1 calc R . . H51B H 0.5483 0.3410 0.9028 0.116 Uiso 1 1 calc R . . H51C H 0.5066 0.3160 0.8576 0.116 Uiso 1 1 calc R . . C50 C 0.4539(2) 0.4934(3) 0.88459(13) 0.0645(12) Uani 1 1 d . . . H50A H 0.4150 0.5320 0.8911 0.097 Uiso 1 1 calc R . . H50B H 0.4555 0.4906 0.8531 0.097 Uiso 1 1 calc R . . H50C H 0.4930 0.5288 0.8981 0.097 Uiso 1 1 calc R . . C54 C 0.3903(2) 0.2640(3) 0.70650(16) 0.0775(14) Uani 1 1 d . . . H54A H 0.4224 0.2597 0.7321 0.116 Uiso 1 1 calc R . . H54B H 0.4120 0.2875 0.6815 0.116 Uiso 1 1 calc R . . H54C H 0.3709 0.1950 0.7004 0.116 Uiso 1 1 calc R . . C95 C 0.35463(14) 0.7782(2) 0.21434(10) 0.0268(7) Uani 1 1 d . . . C94 C 0.30501(15) 0.7893(2) 0.24061(9) 0.0297(7) Uani 1 1 d . . . H94A H 0.3142 0.7919 0.2713 0.036 Uiso 1 1 calc R . . C931 C 0.18759(19) 0.8144(3) 0.24887(11) 0.0492(10) Uani 1 1 d . . . F931 F 0.19882(11) 0.77935(17) 0.28862(6) 0.0597(6) Uani 1 1 d . . . F932 F 0.1757(2) 0.9132(3) 0.25403(13) 0.164(2) Uani 1 1 d . . . F933 F 0.13298(13) 0.7735(5) 0.23448(9) 0.185(3) Uani 1 1 d . . . C951 C 0.42392(16) 0.7716(3) 0.23280(11) 0.0383(8) Uani 1 1 d . . . F952 F 0.46137(9) 0.84418(16) 0.21778(7) 0.0608(6) Uani 1 1 d . . . F951 F 0.45195(9) 0.68176(17) 0.22319(8) 0.0673(7) Uani 1 1 d . . . F753 F 0.50977(9) 1.01388(15) 0.06747(6) 0.0460(5) Uani 1 1 d . . . F752 F 0.44031(11) 1.05533(15) 0.11090(7) 0.0606(6) Uani 1 1 d . . . C731 C 0.39845(17) 0.7285(3) -0.03187(11) 0.0396(8) Uani 1 1 d . . . F731 F 0.39766(12) 0.62585(14) -0.02577(7) 0.0606(6) Uani 1 1 d . . . F733 F 0.35248(13) 0.74568(19) -0.06476(7) 0.0751(7) Uani 1 1 d . . . F732 F 0.45469(12) 0.74969(18) -0.04636(8) 0.0843(9) Uani 1 1 d . . . C86 C 0.16624(13) 0.8321(2) 0.03676(9) 0.0220(6) Uani 1 1 d . . . H86A H 0.1750 0.7699 0.0216 0.026 Uiso 1 1 calc R . . C47 C 0.20693(19) 0.6222(2) 0.89420(12) 0.0516(10) Uani 1 1 d . . . H47A H 0.2543 0.6142 0.8946 0.077 Uiso 1 1 calc R . . H47B H 0.1972 0.6859 0.9098 0.077 Uiso 1 1 calc R . . H47C H 0.1872 0.6269 0.8641 0.077 Uiso 1 1 calc R . . F953 F 0.43149(11) 0.7791(3) 0.27563(7) 0.0992(10) Uani 1 1 d . . . C53 C 0.2876(4) 0.3121(13) 0.6735(2) 0.052(4) Uani 0.55(3) 1 d P . . C55 C 0.3477(12) 0.4495(6) 0.7168(4) 0.051(6) Uani 0.47(3) 1 d P . . C57 C 0.2925(6) 0.398(3) 0.6858(6) 0.104(13) Uani 0.45(3) 1 d P . . C58 C 0.3887(10) 0.4321(9) 0.7370(7) 0.072(6) Uani 0.53(3) 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 0.0209(2) 0.0249(2) 0.0230(2) -0.00241(15) 0.00321(16) -0.00029(16) C1 0.0177(15) 0.0258(15) 0.0203(14) 0.0002(12) -0.0013(12) 0.0040(12) C2 0.0311(18) 0.0255(16) 0.0300(17) -0.0002(13) 0.0049(14) -0.0042(13) C3 0.0384(19) 0.0231(16) 0.0287(17) -0.0038(13) 0.0058(15) -0.0051(14) C14 0.050(2) 0.0298(18) 0.0291(18) -0.0046(14) 0.0167(16) -0.0031(15) C15 0.0343(19) 0.0287(17) 0.0396(19) 0.0023(14) 0.0190(16) 0.0023(14) C13 0.041(2) 0.0326(18) 0.0235(16) 0.0010(13) 0.0065(14) -0.0042(15) C11 0.0263(17) 0.0205(15) 0.0236(15) -0.0005(12) 0.0071(13) -0.0023(12) C12 0.0311(17) 0.0262(16) 0.0213(15) 0.0021(12) 0.0053(13) -0.0047(13) C121 0.0298(18) 0.0395(18) 0.0228(16) 0.0006(13) 0.0003(13) -0.0010(14) C42 0.0262(17) 0.0288(16) 0.0249(16) -0.0003(13) -0.0006(14) -0.0007(13) C41 0.0229(17) 0.0311(17) 0.0288(17) 0.0034(14) 0.0012(13) -0.0042(14) N41 0.0286(15) 0.0293(14) 0.0305(14) -0.0027(12) 0.0069(12) 0.0002(12) N42 0.0263(14) 0.0318(14) 0.0284(15) 0.0031(11) 0.0018(12) 0.0024(11) C52 0.038(2) 0.043(2) 0.0295(17) 0.0123(15) 0.0135(15) 0.0068(16) C44 0.0356(19) 0.0245(16) 0.0407(19) -0.0094(14) 0.0145(15) -0.0006(14) N2 0.0305(15) 0.0216(12) 0.0204(12) -0.0032(10) 0.0035(11) -0.0014(11) N1 0.0216(13) 0.0245(13) 0.0218(12) -0.0009(10) 0.0028(10) -0.0017(10) C16 0.0244(17) 0.0244(16) 0.0333(17) 0.0055(13) 0.0066(14) -0.0028(13) C122 0.034(2) 0.058(2) 0.045(2) -0.0022(18) -0.0035(17) -0.0066(18) C123 0.040(2) 0.047(2) 0.071(3) 0.0156(19) 0.003(2) 0.0067(18) C23 0.053(2) 0.0294(18) 0.042(2) 0.0025(15) 0.0234(18) 0.0110(16) C26 0.051(2) 0.0273(17) 0.0241(16) -0.0017(13) 0.0047(15) -0.0084(15) C25 0.069(3) 0.0333(19) 0.0211(17) -0.0022(14) 0.0053(17) -0.0106(18) C21 0.0389(19) 0.0194(15) 0.0237(16) -0.0040(12) 0.0084(14) 0.0012(13) C24 0.075(3) 0.0304(18) 0.0306(19) -0.0012(14) 0.0256(19) -0.0005(18) C22 0.043(2) 0.0206(15) 0.0291(17) 0.0000(13) 0.0115(15) 0.0022(14) C43 0.0291(19) 0.0331(17) 0.0324(18) -0.0005(14) 0.0078(15) 0.0088(15) N43 0.0217(15) 0.0395(16) 0.0394(16) -0.0083(12) -0.0003(12) 0.0025(12) C48 0.0210(18) 0.058(2) 0.052(2) -0.0187(18) 0.0004(16) -0.0006(16) C49 0.044(2) 0.067(3) 0.052(2) -0.018(2) -0.0089(19) -0.006(2) C45 0.042(2) 0.043(2) 0.080(3) -0.0155(19) 0.021(2) 0.0027(18) B1 0.0176(17) 0.0207(17) 0.0265(18) 0.0006(14) 0.0032(14) -0.0013(14) C65 0.0218(16) 0.0229(15) 0.0187(14) 0.0023(12) 0.0038(12) 0.0025(12) C63 0.0197(15) 0.0231(15) 0.0210(15) 0.0023(12) 0.0033(12) -0.0022(12) C62 0.0192(15) 0.0235(15) 0.0245(15) 0.0032(12) 0.0058(12) 0.0036(12) C61 0.0191(15) 0.0231(15) 0.0181(14) 0.0013(11) 0.0027(12) -0.0017(12) C66 0.0163(15) 0.0276(16) 0.0196(14) 0.0038(12) 0.0016(12) -0.0029(12) C64 0.0271(17) 0.0203(15) 0.0181(14) -0.0012(11) 0.0046(12) -0.0019(12) C72 0.0226(16) 0.0216(15) 0.0267(16) 0.0013(12) 0.0003(13) -0.0023(12) C71 0.0169(15) 0.0224(15) 0.0245(15) 0.0039(12) -0.0009(12) 0.0007(12) C75 0.0240(17) 0.0254(16) 0.0319(17) 0.0055(13) 0.0049(13) -0.0048(13) C74 0.0248(17) 0.0334(17) 0.0343(17) 0.0067(14) 0.0100(14) -0.0048(14) C73 0.0265(17) 0.0292(17) 0.0273(16) 0.0013(13) 0.0072(13) 0.0005(13) C76 0.0231(16) 0.0231(15) 0.0261(16) 0.0019(12) 0.0033(13) 0.0022(13) C83 0.0199(16) 0.0183(14) 0.0305(16) 0.0034(12) 0.0026(13) -0.0032(12) C81 0.0154(14) 0.0217(15) 0.0248(15) 0.0024(12) 0.0071(12) -0.0040(12) C82 0.0176(15) 0.0189(14) 0.0277(15) 0.0046(12) 0.0000(12) -0.0039(12) C85 0.0180(15) 0.0234(15) 0.0234(15) 0.0043(12) 0.0033(12) -0.0035(12) C84 0.0192(15) 0.0214(15) 0.0282(16) 0.0050(12) 0.0037(13) -0.0001(12) C651 0.0266(17) 0.0255(17) 0.0329(17) 0.0010(13) 0.0043(14) 0.0007(13) F652 0.0360(11) 0.0239(10) 0.0813(15) -0.0006(9) 0.0095(10) 0.0063(8) F651 0.0547(13) 0.0577(13) 0.0463(12) 0.0103(10) 0.0288(10) 0.0251(10) F632 0.0282(10) 0.0273(10) 0.0797(14) 0.0044(9) 0.0050(10) -0.0093(8) F631 0.0353(12) 0.0921(16) 0.0527(13) 0.0195(12) -0.0163(10) -0.0195(11) C631 0.0253(17) 0.0249(17) 0.0379(18) 0.0002(14) 0.0031(15) 0.0001(13) C751 0.0292(19) 0.0363(19) 0.0377(19) 0.0034(15) 0.0058(15) -0.0105(15) F751 0.0652(15) 0.0314(11) 0.0988(17) 0.0242(11) -0.0364(13) -0.0201(10) C831 0.0274(18) 0.0237(16) 0.042(2) -0.0021(14) -0.0031(15) 0.0016(14) F832 0.0419(12) 0.0385(11) 0.0759(14) -0.0216(10) -0.0223(11) 0.0207(9) F831 0.0540(13) 0.0247(10) 0.0557(12) -0.0014(9) -0.0009(10) -0.0140(9) C851 0.0239(17) 0.0304(17) 0.0300(17) 0.0044(14) 0.0020(14) 0.0009(14) F852 0.0438(11) 0.0402(10) 0.0282(9) 0.0064(8) -0.0072(8) 0.0110(9) F851 0.0401(11) 0.0477(11) 0.0277(9) -0.0067(8) 0.0013(8) 0.0106(9) F853 0.0397(11) 0.0609(13) 0.0371(11) 0.0080(9) -0.0075(9) -0.0257(10) F833 0.0560(13) 0.0305(10) 0.0402(11) -0.0080(8) 0.0096(9) 0.0043(9) F633 0.0235(11) 0.0456(12) 0.0966(17) -0.0276(11) 0.0197(11) -0.0072(9) F653 0.0336(11) 0.0471(11) 0.0519(12) -0.0096(9) -0.0090(9) 0.0184(9) C91 0.0183(15) 0.0152(14) 0.0279(15) 0.0040(12) 0.0034(12) -0.0020(11) C92 0.0189(15) 0.0264(16) 0.0301(16) 0.0054(13) 0.0027(13) 0.0007(12) C93 0.0276(17) 0.0297(17) 0.0313(17) 0.0061(13) 0.0088(14) 0.0007(13) C96 0.0210(15) 0.0179(14) 0.0298(16) 0.0035(12) 0.0049(13) 0.0001(12) C221 0.0328(19) 0.0372(18) 0.0345(18) 0.0030(14) 0.0078(15) 0.0113(15) C223 0.062(3) 0.057(3) 0.061(3) 0.025(2) -0.008(2) -0.004(2) C222 0.038(2) 0.056(2) 0.052(2) 0.0056(18) 0.0074(18) 0.0070(18) C261 0.042(2) 0.058(2) 0.0311(18) 0.0035(16) -0.0086(16) -0.0107(18) C263 0.073(4) 0.159(6) 0.170(6) -0.100(5) -0.013(4) -0.034(4) C262 0.048(3) 0.084(4) 0.322(10) 0.087(5) -0.035(5) 0.002(3) C161 0.0229(17) 0.0347(18) 0.0374(18) 0.0000(14) 0.0068(14) 0.0009(14) C162 0.084(3) 0.054(2) 0.051(2) 0.0080(19) -0.026(2) -0.005(2) C163 0.038(2) 0.160(5) 0.065(3) 0.019(3) -0.006(2) -0.044(3) C46 0.065(3) 0.053(2) 0.041(2) -0.0145(18) 0.0102(19) -0.004(2) C51 0.028(2) 0.119(4) 0.082(3) -0.039(3) -0.007(2) 0.014(2) C50 0.049(3) 0.077(3) 0.068(3) -0.010(2) 0.006(2) -0.031(2) C54 0.082(3) 0.072(3) 0.089(3) 0.021(2) 0.056(3) 0.019(3) C95 0.0238(16) 0.0232(15) 0.0323(17) 0.0039(13) -0.0018(14) -0.0014(13) C94 0.0370(19) 0.0319(17) 0.0196(15) 0.0051(13) -0.0005(14) -0.0048(14) C931 0.045(2) 0.068(3) 0.037(2) 0.0088(19) 0.0134(18) 0.011(2) F931 0.0711(16) 0.0775(15) 0.0343(11) 0.0127(10) 0.0239(11) 0.0120(12) F932 0.215(4) 0.106(2) 0.203(4) 0.092(3) 0.178(4) 0.109(3) F933 0.0366(16) 0.470(8) 0.0538(18) -0.065(3) 0.0279(14) -0.053(3) C951 0.0275(18) 0.049(2) 0.038(2) 0.0095(16) -0.0035(15) -0.0049(17) F952 0.0309(11) 0.0541(13) 0.0931(17) 0.0224(12) -0.0149(11) -0.0165(10) F951 0.0273(11) 0.0528(14) 0.117(2) 0.0175(13) -0.0151(12) 0.0063(10) F753 0.0286(11) 0.0567(12) 0.0515(12) -0.0005(10) -0.0017(9) -0.0168(9) F752 0.0669(15) 0.0590(13) 0.0607(14) -0.0253(11) 0.0300(12) -0.0376(11) C731 0.042(2) 0.041(2) 0.038(2) -0.0009(16) 0.0171(17) -0.0109(16) F731 0.1005(18) 0.0340(12) 0.0527(13) -0.0071(10) 0.0339(12) 0.0002(11) F733 0.0924(19) 0.0983(19) 0.0327(12) -0.0116(11) -0.0026(13) 0.0217(15) F732 0.0814(18) 0.0947(19) 0.0889(18) -0.0528(14) 0.0676(15) -0.0485(15) C86 0.0224(15) 0.0204(15) 0.0243(15) -0.0003(12) 0.0077(12) -0.0009(12) C47 0.073(3) 0.0318(19) 0.055(2) -0.0070(17) 0.029(2) -0.0059(18) F953 0.0371(13) 0.227(3) 0.0310(13) 0.0061(16) -0.0106(11) -0.0101(17) C53 0.057(5) 0.074(9) 0.024(4) 0.008(4) -0.007(3) -0.012(5) C55 0.095(15) 0.023(4) 0.037(6) -0.006(4) 0.014(8) -0.020(5) C57 0.065(8) 0.18(3) 0.074(12) 0.102(17) 0.014(8) 0.024(11) C58 0.075(11) 0.063(6) 0.083(11) -0.010(6) 0.031(10) -0.040(6) _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 C43 1.908(3) . ? Ni1 C42 1.920(3) . ? Ni1 C41 1.921(3) . ? Ni1 C1 1.990(3) . ? C1 N1 1.364(3) . ? C1 N2 1.368(3) . ? C2 C3 1.344(4) . ? C2 N1 1.374(3) . ? C3 N2 1.379(4) . ? C14 C13 1.373(5) . ? C14 C15 1.381(5) . ? C15 C16 1.387(4) . ? C13 C12 1.385(4) . ? C11 C16 1.395(4) . ? C11 C12 1.395(4) . ? C11 N1 1.443(3) . ? C12 C121 1.525(4) . ? C121 C122 1.526(4) . ? C121 C123 1.535(4) . ? C42 N42 1.150(4) . ? C41 N41 1.160(4) . ? N41 C44 1.463(4) . ? N42 C52 1.465(4) . ? C52 C55 1.419(8) . ? C52 C57 1.444(10) . ? C52 C54 1.490(5) . ? C52 C53 1.609(8) . ? C52 C58 1.675(15) . ? C44 C45 1.513(5) . ? C44 C47 1.515(4) . ? C44 C46 1.519(5) . ? N2 C21 1.447(4) . ? C16 C161 1.523(4) . ? C23 C24 1.388(5) . ? C23 C22 1.398(4) . ? C26 C25 1.389(5) . ? C26 C21 1.401(4) . ? C26 C261 1.511(5) . ? C25 C24 1.366(5) . ? C21 C22 1.399(4) . ? C22 C221 1.515(4) . ? C43 N43 1.165(4) . ? N43 C48 1.457(4) . ? C48 C50 1.515(5) . ? C48 C49 1.525(5) . ? C48 C51 1.526(5) . ? B1 C91 1.636(4) . ? B1 C81 1.638(4) . ? B1 C61 1.645(4) . ? B1 C71 1.646(4) . ? C65 C64 1.389(4) . ? C65 C66 1.394(4) . ? C65 C651 1.493(4) . ? C63 C62 1.383(4) . ? C63 C64 1.388(4) . ? C63 C631 1.494(4) . ? C62 C61 1.407(4) . ? C61 C66 1.401(4) . ? C72 C73 1.385(4) . ? C72 C71 1.393(4) . ? C71 C76 1.408(4) . ? C75 C76 1.385(4) . ? C75 C74 1.392(4) . ? C75 C751 1.492(4) . ? C74 C73 1.382(4) . ? C73 C731 1.494(4) . ? C83 C84 1.393(4) . ? C83 C82 1.398(4) . ? C83 C831 1.495(4) . ? C81 C82 1.389(4) . ? C81 C86 1.398(4) . ? C85 C86 1.383(4) . ? C85 C84 1.384(4) . ? C85 C851 1.495(4) . ? C651 F652 1.331(3) . ? C651 F651 1.336(3) . ? C651 F653 1.341(3) . ? F632 C631 1.329(3) . ? F631 C631 1.338(3) . ? C631 F633 1.328(3) . ? C751 F751 1.328(3) . ? C751 F752 1.337(4) . ? C751 F753 1.346(4) . ? C831 F832 1.328(3) . ? C831 F833 1.342(3) . ? C831 F831 1.351(3) . ? C851 F852 1.340(3) . ? C851 F853 1.342(3) . ? C851 F851 1.347(3) . ? C91 C96 1.399(4) . ? C91 C92 1.401(4) . ? C92 C93 1.389(4) . ? C93 C94 1.388(4) . ? C93 C931 1.481(5) . ? C96 C95 1.398(4) . ? C221 C223 1.529(4) . ? C221 C222 1.529(5) . ? C261 C262 1.502(6) . ? C261 C263 1.503(5) . ? C161 C163 1.519(5) . ? C161 C162 1.524(5) . ? C95 C94 1.378(4) . ? C95 C951 1.486(4) . ? C931 F933 1.280(5) . ? C931 F932 1.301(5) . ? C931 F931 1.309(4) . ? C951 F952 1.322(4) . ? C951 F953 1.324(4) . ? C951 F951 1.335(4) . ? C731 F732 1.313(4) . ? C731 F731 1.328(4) . ? C731 F733 1.337(4) . ? C53 C57 1.17(3) . ? C55 C58 1.023(12) . ? C55 C57 1.56(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 C43 Ni1 C42 93.08(13) . . ? C43 Ni1 C41 92.44(12) . . ? C42 Ni1 C41 125.57(12) . . ? C43 Ni1 C1 133.56(12) . . ? C42 Ni1 C1 107.09(12) . . ? C41 Ni1 C1 107.38(12) . . ? N1 C1 N2 102.3(2) . . ? N1 C1 Ni1 128.41(19) . . ? N2 C1 Ni1 128.5(2) . . ? C3 C2 N1 106.2(3) . . ? C2 C3 N2 106.9(3) . . ? C13 C14 C15 120.9(3) . . ? C14 C15 C16 120.6(3) . . ? C14 C13 C12 121.0(3) . . ? C16 C11 C12 123.3(3) . . ? C16 C11 N1 118.0(2) . . ? C12 C11 N1 118.5(2) . . ? C13 C12 C11 117.1(3) . . ? C13 C12 C121 121.1(3) . . ? C11 C12 C121 121.8(3) . . ? C12 C121 C122 112.7(3) . . ? C12 C121 C123 110.5(3) . . ? C122 C121 C123 110.6(3) . . ? N42 C42 Ni1 169.4(3) . . ? N41 C41 Ni1 169.0(3) . . ? C41 N41 C44 174.1(3) . . ? C42 N42 C52 173.0(3) . . ? C55 C52 C57 65.9(17) . . ? C55 C52 N42 111.6(4) . . ? C57 C52 N42 110.0(5) . . ? C55 C52 C54 123.4(9) . . ? C57 C52 C54 131.4(11) . . ? N42 C52 C54 108.4(3) . . ? C55 C52 C53 109.0(10) . . ? C57 C52 C53 44.5(10) . . ? N42 C52 C53 104.1(4) . . ? C54 C52 C53 97.9(6) . . ? C55 C52 C58 37.5(5) . . ? C57 C52 C58 103.2(16) . . ? N42 C52 C58 103.1(6) . . ? C54 C52 C58 95.8(7) . . ? C53 C52 C58 143.7(10) . . ? N41 C44 C45 107.9(3) . . ? N41 C44 C47 107.1(2) . . ? C45 C44 C47 112.8(3) . . ? N41 C44 C46 107.1(3) . . ? C45 C44 C46 111.0(3) . . ? C47 C44 C46 110.7(3) . . ? C1 N2 C3 111.9(2) . . ? C1 N2 C21 127.2(2) . . ? C3 N2 C21 120.8(2) . . ? C1 N1 C2 112.8(2) . . ? C1 N1 C11 126.1(2) . . ? C2 N1 C11 121.2(2) . . ? C15 C16 C11 117.2(3) . . ? C15 C16 C161 121.0(3) . . ? C11 C16 C161 121.7(3) . . ? C24 C23 C22 120.5(3) . . ? C25 C26 C21 117.0(3) . . ? C25 C26 C261 121.1(3) . . ? C21 C26 C261 121.9(3) . . ? C24 C25 C26 121.2(3) . . ? C22 C21 C26 123.4(3) . . ? C22 C21 N2 118.2(2) . . ? C26 C21 N2 118.2(3) . . ? C25 C24 C23 121.1(3) . . ? C23 C22 C21 116.8(3) . . ? C23 C22 C221 120.6(3) . . ? C21 C22 C221 122.6(3) . . ? N43 C43 Ni1 176.2(3) . . ? C43 N43 C48 175.8(3) . . ? N43 C48 C50 107.3(3) . . ? N43 C48 C49 107.8(3) . . ? C50 C48 C49 111.2(3) . . ? N43 C48 C51 107.0(3) . . ? C50 C48 C51 112.6(3) . . ? C49 C48 C51 110.8(3) . . ? C91 B1 C81 113.1(2) . . ? C91 B1 C61 105.3(2) . . ? C81 B1 C61 111.5(2) . . ? C91 B1 C71 112.5(2) . . ? C81 B1 C71 103.4(2) . . ? C61 B1 C71 111.3(2) . . ? C64 C65 C66 120.4(2) . . ? C64 C65 C651 121.4(2) . . ? C66 C65 C651 118.2(2) . . ? C62 C63 C64 121.1(3) . . ? C62 C63 C631 118.9(2) . . ? C64 C63 C631 119.9(2) . . ? C63 C62 C61 122.2(3) . . ? C66 C61 C62 115.5(2) . . ? C66 C61 B1 121.7(2) . . ? C62 C61 B1 122.7(2) . . ? C65 C66 C61 122.5(3) . . ? C63 C64 C65 118.2(2) . . ? C73 C72 C71 122.7(3) . . ? C72 C71 C76 115.3(3) . . ? C72 C71 B1 123.7(2) . . ? C76 C71 B1 120.7(2) . . ? C76 C75 C74 120.3(3) . . ? C76 C75 C751 120.7(3) . . ? C74 C75 C751 118.9(3) . . ? C73 C74 C75 118.2(3) . . ? C74 C73 C72 120.9(3) . . ? C74 C73 C731 120.2(3) . . ? C72 C73 C731 118.9(3) . . ? C75 C76 C71 122.6(3) . . ? C84 C83 C82 121.0(3) . . ? C84 C83 C831 119.8(2) . . ? C82 C83 C831 119.2(2) . . ? C82 C81 C86 115.8(2) . . ? C82 C81 B1 123.3(2) . . ? C86 C81 B1 120.6(2) . . ? C81 C82 C83 122.1(3) . . ? C86 C85 C84 121.3(3) . . ? C86 C85 C851 119.0(2) . . ? C84 C85 C851 119.7(3) . . ? C85 C84 C83 117.3(3) . . ? F652 C651 F651 106.2(2) . . ? F652 C651 F653 106.5(2) . . ? F651 C651 F653 105.4(2) . . ? F652 C651 C65 113.3(2) . . ? F651 C651 C65 112.5(2) . . ? F653 C651 C65 112.5(2) . . ? F633 C631 F632 107.2(2) . . ? F633 C631 F631 105.2(3) . . ? F632 C631 F631 105.1(2) . . ? F633 C631 C63 113.1(2) . . ? F632 C631 C63 113.9(2) . . ? F631 C631 C63 111.7(2) . . ? F751 C751 F752 108.1(3) . . ? F751 C751 F753 104.8(2) . . ? F752 C751 F753 105.1(2) . . ? F751 C751 C75 112.9(3) . . ? F752 C751 C75 113.4(2) . . ? F753 C751 C75 111.9(3) . . ? F832 C831 F833 106.9(3) . . ? F832 C831 F831 106.2(2) . . ? F833 C831 F831 105.7(2) . . ? F832 C831 C83 113.7(2) . . ? F833 C831 C83 112.1(2) . . ? F831 C831 C83 111.6(3) . . ? F852 C851 F853 106.4(2) . . ? F852 C851 F851 105.9(2) . . ? F853 C851 F851 105.7(2) . . ? F852 C851 C85 113.2(2) . . ? F853 C851 C85 112.4(2) . . ? F851 C851 C85 112.7(2) . . ? C96 C91 C92 115.6(3) . . ? C96 C91 B1 123.1(2) . . ? C92 C91 B1 121.1(2) . . ? C93 C92 C91 122.3(3) . . ? C94 C93 C92 120.6(3) . . ? C94 C93 C931 119.6(3) . . ? C92 C93 C931 119.7(3) . . ? C95 C96 C91 122.4(3) . . ? C22 C221 C223 111.8(3) . . ? C22 C221 C222 112.5(3) . . ? C223 C221 C222 110.8(3) . . ? C262 C261 C263 108.8(4) . . ? C262 C261 C26 110.3(3) . . ? C263 C261 C26 113.0(4) . . ? C163 C161 C16 112.0(3) . . ? C163 C161 C162 110.9(3) . . ? C16 C161 C162 111.1(3) . . ? C94 C95 C96 120.3(3) . . ? C94 C95 C951 121.4(3) . . ? C96 C95 C951 118.3(3) . . ? C95 C94 C93 118.7(3) . . ? F933 C931 F932 105.7(4) . . ? F933 C931 F931 104.6(3) . . ? F932 C931 F931 103.6(3) . . ? F933 C931 C93 114.8(3) . . ? F932 C931 C93 112.5(3) . . ? F931 C931 C93 114.6(3) . . ? F952 C951 F953 106.8(3) . . ? F952 C951 F951 104.2(3) . . ? F953 C951 F951 106.1(3) . . ? F952 C951 C95 113.4(3) . . ? F953 C951 C95 113.1(3) . . ? F951 C951 C95 112.6(3) . . ? F732 C731 F731 106.1(3) . . ? F732 C731 F733 106.7(3) . . ? F731 C731 F733 104.7(3) . . ? F732 C731 C73 114.3(3) . . ? F731 C731 C73 112.3(3) . . ? F733 C731 C73 112.0(3) . . ? C85 C86 C81 122.5(3) . . ? C57 C53 C52 60.2(6) . . ? C58 C55 C52 85.0(11) . . ? C58 C55 C57 142.3(14) . . ? C52 C55 C57 57.8(10) . . ? C53 C57 C52 75.3(11) . . ? C53 C57 C55 129.4(12) . . ? C52 C57 C55 56.2(8) . . ? C55 C58 C52 57.5(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.604 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.066