Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Gregory L. Hillhouse' _publ_contact_author_address ; Searle Chemistry Laboratory Department of Chemistry The University of Chicago 5735 S. Ellis Ave. Chicago, IL 60637 ; _publ_contact_author_email g-hillhouse@uchicago.edu loop_ _publ_author_name _publ_author_address V.M.Iluc ;Searle Chemistry Laboratory Department of Chemistry The University of Chicago 5735 S. Ellis Ave. Chicago, IL 60637 ; G.L.Hillhouse ;Searle Chemistry Laboratory Department of Chemistry The University of Chicago 5735 S. Ellis Ave. Chicago, IL 60637 ; A.J.M.Miller ;Searle Chemistry Laboratory Department of Chemistry The University of Chicago 5735 S. Ellis Ave. Chicago, IL 60637 ; _publ_section_title ; Synthesis and Characterization of Side-Bound Aryldiazo and End-Bound Nitrosyl Complexes of Nickel ; data_vlad38m _database_code_depnum_ccdc_archive 'CCDC 279076' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H47 F6 N2 Ni O1 P3, C2 O0.5' _chemical_formula_sum 'C27 H47 F6 N2 Ni O1.50 P3' _chemical_formula_weight 689.29 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6973(9) _cell_length_b 12.4144(10) _cell_length_c 13.2900(11) _cell_angle_alpha 88.4960(10) _cell_angle_beta 75.1410(10) _cell_angle_gamma 79.4050(10) _cell_volume 1676.4(2) _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 red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.2845 _exptl_absorpt_correction_T_max 0.3994 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10764 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7554 _reflns_number_gt 6423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+0.0348P] 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 7554 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Ni Ni 0.51875(3) 0.25947(2) 0.40734(2) 0.01496(10) Uani 1 1 d . . . N1 N 0.41006(19) 0.26263(15) 0.54165(14) 0.0179(4) Uani 1 1 d . . . P1 P 0.73536(6) 0.24241(5) 0.36703(4) 0.01601(14) Uani 1 1 d . . . N2 N 0.3430(2) 0.26779(17) 0.47905(15) 0.0214(4) Uani 1 1 d . . . P2 P 0.51615(6) 0.24910(5) 0.24406(4) 0.01587(14) Uani 1 1 d . . . O O 0.25451(18) 0.20132(18) 0.96620(13) 0.0325(4) Uani 1 1 d . . . P3 P 0.81121(6) 0.19081(6) 0.82501(5) 0.02580(16) Uani 1 1 d . . . C6 C 0.4353(2) 0.13350(18) 0.21914(17) 0.0195(5) Uani 1 1 d . . . C4 C 0.8218(2) 0.10628(19) 0.40019(19) 0.0222(5) Uani 1 1 d . . . F5 F 0.69532(18) 0.16138(19) 0.91658(13) 0.0525(5) Uani 1 1 d . . . C71 C 0.3651(2) 0.25499(18) 0.65203(17) 0.0181(4) Uani 1 1 d . . . C76 C 0.2343(2) 0.2480(2) 0.69691(18) 0.0221(5) Uani 1 1 d . . . H76A H 0.1732 0.2549 0.6552 0.026 Uiso 1 1 calc R . . C5 C 0.4455(2) 0.38055(19) 0.18991(18) 0.0222(5) Uani 1 1 d . . . C3 C 0.8021(2) 0.35634(19) 0.41339(18) 0.0218(5) Uani 1 1 d . . . C73 C 0.4130(2) 0.2359(2) 0.81817(17) 0.0218(5) Uani 1 1 d . . . H73A H 0.4726 0.2343 0.8605 0.026 Uiso 1 1 calc R . . F3 F 0.92783(18) 0.2158(2) 0.73173(15) 0.0614(6) Uani 1 1 d . . . C74 C 0.2837(2) 0.2230(2) 0.86273(18) 0.0238(5) Uani 1 1 d . . . C75 C 0.1936(2) 0.2309(2) 0.80273(18) 0.0242(5) Uani 1 1 d . . . H75A H 0.1050 0.2246 0.8340 0.029 Uiso 1 1 calc R . . C63 C 0.2861(2) 0.1673(2) 0.2525(2) 0.0255(5) Uani 1 1 d . . . H63A H 0.2455 0.1064 0.2392 0.038 Uiso 1 1 calc R . . H63B H 0.2587 0.2310 0.2128 0.038 Uiso 1 1 calc R . . H63C H 0.2582 0.1865 0.3270 0.038 Uiso 1 1 calc R . . C2 C 0.6896(2) 0.2104(2) 0.17009(17) 0.0225(5) Uani 1 1 d . . . H2B H 0.7125 0.1296 0.1616 0.027 Uiso 1 1 calc R . . H2C H 0.7004 0.2417 0.0998 0.027 Uiso 1 1 calc R . . C53 C 0.3129(3) 0.4303(2) 0.2628(2) 0.0318(6) Uani 1 1 d . . . H53A H 0.2765 0.4989 0.2341 0.048 Uiso 1 1 calc R . . H53B H 0.3250 0.4451 0.3314 0.048 Uiso 1 1 calc R . . H53C H 0.2521 0.3788 0.2697 0.048 Uiso 1 1 calc R . . F4 F 0.7132(2) 0.28405(19) 0.7880(2) 0.0804(8) Uani 1 1 d . . . C72 C 0.4543(2) 0.25104(19) 0.71208(18) 0.0209(5) Uani 1 1 d . . . H72A H 0.5426 0.2586 0.6808 0.025 Uiso 1 1 calc R . . F2 F 0.9109(2) 0.0938(3) 0.8571(2) 0.0996(11) Uani 1 1 d . . . C62 C 0.4785(3) 0.0903(2) 0.10604(18) 0.0263(5) Uani 1 1 d . . . H62A H 0.4325 0.0306 0.0992 0.040 Uiso 1 1 calc R . . H62B H 0.5737 0.0630 0.0868 0.040 Uiso 1 1 calc R . . H62C H 0.4569 0.1498 0.0599 0.040 Uiso 1 1 calc R . . C61 C 0.4733(3) 0.0384(2) 0.28804(19) 0.0250(5) Uani 1 1 d . . . H61A H 0.4326 -0.0234 0.2770 0.038 Uiso 1 1 calc R . . H61B H 0.4423 0.0623 0.3613 0.038 Uiso 1 1 calc R . . H61C H 0.5692 0.0155 0.2698 0.038 Uiso 1 1 calc R . . C43 C 0.9693(2) 0.0984(2) 0.3881(2) 0.0299(6) Uani 1 1 d . . . H43A H 1.0069 0.0249 0.4068 0.045 Uiso 1 1 calc R . . H43B H 0.9831 0.1531 0.4341 0.045 Uiso 1 1 calc R . . H43C H 1.0124 0.1122 0.3157 0.045 Uiso 1 1 calc R . . C33 C 0.9431(3) 0.3634(2) 0.3539(2) 0.0308(6) Uani 1 1 d . . . H33A H 0.9709 0.4243 0.3825 0.046 Uiso 1 1 calc R . . H33B H 0.9469 0.3756 0.2801 0.046 Uiso 1 1 calc R . . H33C H 1.0019 0.2947 0.3610 0.046 Uiso 1 1 calc R . . C52 C 0.4322(3) 0.3687(2) 0.07882(19) 0.0293(6) Uani 1 1 d . . . H52A H 0.3949 0.4401 0.0555 0.044 Uiso 1 1 calc R . . H52B H 0.3741 0.3165 0.0777 0.044 Uiso 1 1 calc R . . H52C H 0.5191 0.3419 0.0322 0.044 Uiso 1 1 calc R . . C1 C 0.7855(2) 0.2503(2) 0.22348(17) 0.0228(5) Uani 1 1 d . . . H1A H 0.7911 0.3271 0.2042 0.027 Uiso 1 1 calc R . . H1B H 0.8742 0.2052 0.1973 0.027 Uiso 1 1 calc R . . C51 C 0.5402(3) 0.4604(2) 0.1879(2) 0.0341(6) Uani 1 1 d . . . H51A H 0.5067 0.5305 0.1599 0.051 Uiso 1 1 calc R . . H51B H 0.6273 0.4294 0.1437 0.051 Uiso 1 1 calc R . . H51C H 0.5470 0.4722 0.2588 0.051 Uiso 1 1 calc R . . F6 F 0.7736(2) 0.1105(2) 0.75227(17) 0.0777(8) Uani 1 1 d . . . C42 C 0.7536(3) 0.0788(2) 0.5113(2) 0.0374(7) Uani 1 1 d . . . H42A H 0.7981 0.0076 0.5296 0.056 Uiso 1 1 calc R . . H42B H 0.6615 0.0758 0.5158 0.056 Uiso 1 1 calc R . . H42C H 0.7576 0.1355 0.5598 0.056 Uiso 1 1 calc R . . C32 C 0.7946(3) 0.3454(2) 0.5304(2) 0.0324(6) Uani 1 1 d . . . H32A H 0.8296 0.4052 0.5537 0.049 Uiso 1 1 calc R . . H32B H 0.8467 0.2749 0.5423 0.049 Uiso 1 1 calc R . . H32C H 0.7028 0.3492 0.5695 0.049 Uiso 1 1 calc R . . C41 C 0.8065(3) 0.0195(2) 0.3268(3) 0.0424(8) Uani 1 1 d . . . H41A H 0.8512 -0.0527 0.3428 0.064 Uiso 1 1 calc R . . H41B H 0.8456 0.0371 0.2546 0.064 Uiso 1 1 calc R . . H41C H 0.7129 0.0184 0.3360 0.064 Uiso 1 1 calc R . . C31 C 0.7129(3) 0.4638(2) 0.3992(2) 0.0343(6) Uani 1 1 d . . . H31A H 0.7447 0.5254 0.4227 0.051 Uiso 1 1 calc R . . H31B H 0.6228 0.4629 0.4403 0.051 Uiso 1 1 calc R . . H31C H 0.7140 0.4720 0.3254 0.051 Uiso 1 1 calc R . . C8 C 0.1323(3) 0.1635(3) 1.0097(2) 0.0494(9) Uani 1 1 d . . . H8A H 0.1223 0.1508 1.0842 0.074 Uiso 1 1 calc R . . H8B H 0.1331 0.0950 0.9744 0.074 Uiso 1 1 calc R . . H8C H 0.0587 0.2191 1.0000 0.074 Uiso 1 1 calc R . . F1 F 0.8512(3) 0.2642(3) 0.8989(2) 0.1193(14) Uani 1 1 d . . . C90 C 1.0365(4) 0.4839(4) 0.0807(3) 0.0604(10) Uani 1 1 d . . . O90 O 0.9371(5) 0.4372(4) 0.0839(4) 0.0483(11) Uani 0.50 1 d P . . C91 C 0.8841(5) 0.4863(3) 0.0208(3) 0.0668(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01400(17) 0.01830(16) 0.00982(15) -0.00020(11) 0.00042(11) -0.00079(11) N1 0.0180(10) 0.0163(9) 0.0164(9) 0.0004(7) -0.0003(7) -0.0012(7) P1 0.0146(3) 0.0186(3) 0.0124(3) 0.0001(2) -0.0004(2) -0.0011(2) N2 0.0199(10) 0.0266(10) 0.0149(9) -0.0004(8) -0.0001(8) -0.0031(8) P2 0.0154(3) 0.0198(3) 0.0108(3) 0.0006(2) -0.0006(2) -0.0035(2) O 0.0253(10) 0.0606(13) 0.0125(8) 0.0047(8) -0.0006(7) -0.0171(9) P3 0.0181(3) 0.0398(4) 0.0197(3) 0.0009(3) -0.0032(2) -0.0083(3) C6 0.0215(12) 0.0211(11) 0.0154(10) -0.0015(8) -0.0025(9) -0.0056(9) C4 0.0172(12) 0.0200(11) 0.0272(12) 0.0018(9) -0.0052(10) 0.0013(9) F5 0.0324(10) 0.0958(16) 0.0277(9) 0.0090(9) 0.0024(7) -0.0228(10) C71 0.0192(11) 0.0201(11) 0.0119(10) -0.0012(8) 0.0008(8) -0.0023(8) C76 0.0182(12) 0.0296(12) 0.0177(11) -0.0014(9) -0.0020(9) -0.0059(9) C5 0.0251(13) 0.0224(11) 0.0201(11) 0.0056(9) -0.0075(10) -0.0049(9) C3 0.0225(12) 0.0221(11) 0.0214(11) -0.0008(9) -0.0053(10) -0.0059(9) C73 0.0202(12) 0.0313(13) 0.0142(10) -0.0014(9) -0.0029(9) -0.0078(10) F3 0.0264(10) 0.1081(18) 0.0483(11) 0.0372(11) -0.0044(8) -0.0210(10) C74 0.0243(13) 0.0326(13) 0.0134(11) -0.0020(9) -0.0008(9) -0.0082(10) C75 0.0186(12) 0.0357(13) 0.0165(11) -0.0019(10) 0.0011(9) -0.0080(10) C63 0.0218(13) 0.0285(13) 0.0257(12) -0.0003(10) -0.0030(10) -0.0074(10) C2 0.0192(12) 0.0342(13) 0.0119(10) -0.0025(9) 0.0007(9) -0.0052(10) C53 0.0344(15) 0.0257(13) 0.0316(14) 0.0027(11) -0.0079(12) 0.0031(11) F4 0.0302(11) 0.0615(14) 0.135(2) 0.0463(14) -0.0063(13) -0.0001(9) C72 0.0187(12) 0.0243(12) 0.0178(11) -0.0017(9) -0.0010(9) -0.0041(9) F2 0.0409(13) 0.127(2) 0.115(2) 0.0779(19) -0.0115(14) 0.0021(14) C62 0.0248(13) 0.0347(14) 0.0186(11) -0.0061(10) -0.0027(10) -0.0063(10) C61 0.0274(13) 0.0230(12) 0.0246(12) 0.0011(9) -0.0052(10) -0.0065(10) C43 0.0181(13) 0.0349(14) 0.0328(14) 0.0025(11) -0.0051(11) 0.0025(10) C33 0.0271(14) 0.0366(14) 0.0317(14) 0.0025(11) -0.0079(11) -0.0131(11) C52 0.0348(15) 0.0340(14) 0.0217(12) 0.0085(10) -0.0111(11) -0.0085(11) C1 0.0158(11) 0.0361(13) 0.0141(10) 0.0000(9) 0.0016(9) -0.0060(10) C51 0.0400(16) 0.0280(13) 0.0407(16) 0.0110(11) -0.0185(13) -0.0122(12) F6 0.0791(17) 0.0952(19) 0.0597(14) -0.0352(13) -0.0001(13) -0.0379(15) C42 0.0246(14) 0.0404(16) 0.0413(16) 0.0236(13) -0.0039(12) -0.0003(11) C32 0.0357(16) 0.0387(15) 0.0232(13) -0.0088(11) -0.0063(11) -0.0081(12) C41 0.0451(18) 0.0221(13) 0.065(2) -0.0078(13) -0.0311(17) 0.0066(12) C31 0.0331(15) 0.0222(13) 0.0512(18) -0.0043(12) -0.0178(13) -0.0035(11) C8 0.0398(18) 0.095(3) 0.0201(14) 0.0142(15) -0.0027(12) -0.0387(19) F1 0.088(2) 0.203(4) 0.0798(18) -0.077(2) 0.0059(16) -0.086(2) C90 0.053(2) 0.079(3) 0.047(2) 0.0284(19) -0.0087(17) -0.015(2) O90 0.043(3) 0.061(3) 0.042(3) 0.018(2) -0.006(2) -0.021(2) C91 0.087(3) 0.063(2) 0.044(2) 0.0001(18) 0.014(2) -0.041(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N1 1.8607(19) . ? Ni N2 1.863(2) . ? Ni P2 2.1848(6) . ? Ni P1 2.2113(7) . ? N1 N2 1.224(3) . ? N1 C71 1.428(3) . ? P1 C1 1.850(2) . ? P1 C4 1.871(2) . ? P1 C3 1.880(2) . ? P2 C2 1.845(2) . ? P2 C5 1.875(2) . ? P2 C6 1.883(2) . ? O C74 1.361(3) . ? O C8 1.445(3) . ? P3 F1 1.543(2) . ? P3 F4 1.571(2) . ? P3 F6 1.577(2) . ? P3 F2 1.582(2) . ? P3 F3 1.5870(18) . ? P3 F5 1.5878(17) . ? C6 C63 1.524(3) . ? C6 C62 1.535(3) . ? C6 C61 1.535(3) . ? C4 C43 1.529(3) . ? C4 C41 1.530(4) . ? C4 C42 1.531(4) . ? C71 C72 1.386(3) . ? C71 C76 1.391(3) . ? C76 C75 1.384(3) . ? C5 C53 1.528(4) . ? C5 C52 1.532(3) . ? C5 C51 1.538(3) . ? C3 C31 1.529(3) . ? C3 C33 1.530(3) . ? C3 C32 1.540(3) . ? C73 C72 1.384(3) . ? C73 C74 1.396(3) . ? C74 C75 1.389(3) . ? C2 C1 1.542(3) . ? C90 O90 1.293(6) . ? C90 C91 1.476(5) 2_765 ? O90 C91 1.219(6) . ? C91 C90 1.476(5) 2_765 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni N2 38.38(8) . . ? N1 Ni P2 141.76(6) . . ? N2 Ni P2 103.57(6) . . ? N1 Ni P1 125.46(6) . . ? N2 Ni P1 163.76(6) . . ? P2 Ni P1 92.38(2) . . ? N2 N1 C71 126.4(2) . . ? N2 N1 Ni 70.90(12) . . ? C71 N1 Ni 162.21(17) . . ? C1 P1 C4 106.21(12) . . ? C1 P1 C3 103.92(11) . . ? C4 P1 C3 110.36(11) . . ? C1 P1 Ni 105.10(8) . . ? C4 P1 Ni 113.73(8) . . ? C3 P1 Ni 116.35(8) . . ? N1 N2 Ni 70.72(13) . . ? C2 P2 C5 107.53(11) . . ? C2 P2 C6 105.02(11) . . ? C5 P2 C6 111.14(11) . . ? C2 P2 Ni 105.94(8) . . ? C5 P2 Ni 114.79(8) . . ? C6 P2 Ni 111.71(7) . . ? C74 O C8 117.0(2) . . ? F1 P3 F4 96.20(19) . . ? F1 P3 F6 177.05(19) . . ? F4 P3 F6 86.66(16) . . ? F1 P3 F2 86.3(2) . . ? F4 P3 F2 177.19(19) . . ? F6 P3 F2 90.84(17) . . ? F1 P3 F3 90.26(14) . . ? F4 P3 F3 89.95(11) . . ? F6 P3 F3 90.48(13) . . ? F2 P3 F3 88.79(12) . . ? F1 P3 F5 91.49(13) . . ? F4 P3 F5 91.04(12) . . ? F6 P3 F5 87.72(12) . . ? F2 P3 F5 90.14(12) . . ? F3 P3 F5 177.89(13) . . ? C63 C6 C62 109.8(2) . . ? C63 C6 C61 107.22(19) . . ? C62 C6 C61 107.6(2) . . ? C63 C6 P2 110.43(16) . . ? C62 C6 P2 114.24(16) . . ? C61 C6 P2 107.31(16) . . ? C43 C4 C41 107.1(2) . . ? C43 C4 C42 110.4(2) . . ? C41 C4 C42 107.7(2) . . ? C43 C4 P1 114.64(17) . . ? C41 C4 P1 108.08(17) . . ? C42 C4 P1 108.73(17) . . ? C72 C71 C76 121.3(2) . . ? C72 C71 N1 119.0(2) . . ? C76 C71 N1 119.7(2) . . ? C75 C76 C71 119.5(2) . . ? C53 C5 C52 110.6(2) . . ? C53 C5 C51 107.5(2) . . ? C52 C5 C51 107.9(2) . . ? C53 C5 P2 109.90(16) . . ? C52 C5 P2 113.79(17) . . ? C51 C5 P2 106.85(17) . . ? C31 C3 C33 108.1(2) . . ? C31 C3 C32 107.7(2) . . ? C33 C3 C32 109.3(2) . . ? C31 C3 P1 107.09(16) . . ? C33 C3 P1 114.28(17) . . ? C32 C3 P1 110.15(17) . . ? C72 C73 C74 119.8(2) . . ? O C74 C75 123.6(2) . . ? O C74 C73 115.6(2) . . ? C75 C74 C73 120.7(2) . . ? C76 C75 C74 119.4(2) . . ? C1 C2 P2 112.80(16) . . ? C73 C72 C71 119.1(2) . . ? C2 C1 P1 113.03(16) . . ? O90 C90 C91 119.5(4) . 2_765 ? O90 C90 C91 36.5(2) . . ? C91 C90 C91 90.5(3) 2_765 . ? C91 O90 C90 104.4(4) . . ? O90 C91 C90 120.6(4) . 2_765 ? O90 C91 C90 39.1(3) . . ? C90 C91 C90 89.5(3) 2_765 . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.066 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.101 #===END data_alexNO37 _database_code_depnum_ccdc_archive 'CCDC 279077' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106 H109 B2 Cl F48 N2 Ni2 O2 P4' _chemical_formula_weight 2653.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.385(16) _cell_length_b 35.42(3) _cell_length_c 18.986(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.651(18) _cell_angle_gamma 90.00 _cell_volume 11668(18) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5400 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8798 _exptl_absorpt_correction_T_max 0.9493 _exptl_absorpt_process_details ? _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 83543 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.03 _reflns_number_total 20594 _reflns_number_gt 17064 _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+32.0442P] 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 20594 _refine_ls_number_parameters 1504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0942 _refine_ls_wR_factor_ref 0.2250 _refine_ls_wR_factor_gt 0.2145 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _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 B1 B 0.7975(3) 0.15797(17) 0.2983(3) 0.0208(13) Uani 1 1 d . . . B2 B 0.2276(3) 0.90720(17) 0.2171(3) 0.0206(12) Uani 1 1 d . . . C1 C 0.2602(3) 0.09360(16) 0.1721(4) 0.0341(14) Uani 1 1 d . . . C2 C 0.3482(4) 0.08852(18) 0.1830(4) 0.0449(18) Uani 1 1 d . . . H2A H 0.3627 0.0637 0.1654 0.067 Uiso 1 1 calc R . . H2B H 0.3638 0.0904 0.2334 0.067 Uiso 1 1 calc R . . H2C H 0.3742 0.1083 0.1572 0.067 Uiso 1 1 calc R . . C3 C 0.2391(4) 0.09205(19) 0.0935(4) 0.0422(16) Uani 1 1 d . . . H3A H 0.2503 0.0668 0.0756 0.063 Uiso 1 1 calc R . . H3B H 0.2693 0.1109 0.0693 0.063 Uiso 1 1 calc R . . H3C H 0.1840 0.0975 0.0847 0.063 Uiso 1 1 calc R . . C4 C 0.2204(4) 0.06141(17) 0.2104(4) 0.0469(18) Uani 1 1 d . . . H4A H 0.2337 0.0372 0.1895 0.070 Uiso 1 1 calc R . . H4B H 0.1644 0.0650 0.2055 0.070 Uiso 1 1 calc R . . H4C H 0.2378 0.0616 0.2605 0.070 Uiso 1 1 calc R . . C5 C 0.1385(3) 0.15727(16) 0.1804(3) 0.0259(12) Uani 1 1 d . . . C6 C 0.1390(4) 0.17551(18) 0.1065(3) 0.0356(14) Uani 1 1 d . . . H6A H 0.0868 0.1839 0.0914 0.053 Uiso 1 1 calc R . . H6B H 0.1566 0.1570 0.0728 0.053 Uiso 1 1 calc R . . H6C H 0.1740 0.1973 0.1085 0.053 Uiso 1 1 calc R . . C7 C 0.0787(3) 0.12557(18) 0.1816(4) 0.0369(15) Uani 1 1 d . . . H7A H 0.0276 0.1356 0.1671 0.055 Uiso 1 1 calc R . . H7B H 0.0781 0.1153 0.2295 0.055 Uiso 1 1 calc R . . H7C H 0.0922 0.1055 0.1490 0.055 Uiso 1 1 calc R . . C8 C 0.1159(3) 0.18806(18) 0.2327(3) 0.0350(14) Uani 1 1 d . . . H8A H 0.0633 0.1967 0.2198 0.052 Uiso 1 1 calc R . . H8B H 0.1517 0.2094 0.2308 0.052 Uiso 1 1 calc R . . H8C H 0.1183 0.1776 0.2806 0.052 Uiso 1 1 calc R . . C9 C 0.2480(3) 0.13731(16) 0.3045(3) 0.0254(12) Uani 1 1 d . . . H9A H 0.1968 0.1309 0.3212 0.031 Uiso 1 1 calc R . . H9B H 0.2833 0.1162 0.3175 0.031 Uiso 1 1 calc R . . C10 C 0.2780(3) 0.17331(17) 0.3430(3) 0.0274(12) Uani 1 1 d . . . H10A H 0.2945 0.1669 0.3924 0.033 Uiso 1 1 calc R . . H10B H 0.2355 0.1918 0.3441 0.033 Uiso 1 1 calc R . . C11 C 0.3489(3) 0.24733(16) 0.3150(3) 0.0306(13) Uani 1 1 d . . . C12 C 0.2795(3) 0.25947(17) 0.2657(4) 0.0353(14) Uani 1 1 d . . . H12A H 0.2708 0.2866 0.2709 0.053 Uiso 1 1 calc R . . H12B H 0.2335 0.2456 0.2782 0.053 Uiso 1 1 calc R . . H12C H 0.2900 0.2539 0.2167 0.053 Uiso 1 1 calc R . . C13 C 0.3325(4) 0.2583(2) 0.3906(4) 0.0472(18) Uani 1 1 d . . . H13A H 0.3278 0.2858 0.3939 0.071 Uiso 1 1 calc R . . H13B H 0.3749 0.2497 0.4232 0.071 Uiso 1 1 calc R . . H13C H 0.2843 0.2465 0.4033 0.071 Uiso 1 1 calc R . . C14 C 0.4209(4) 0.26793(17) 0.2920(4) 0.0394(16) Uani 1 1 d . . . H14A H 0.4153 0.2951 0.2998 0.059 Uiso 1 1 calc R . . H14B H 0.4269 0.2631 0.2419 0.059 Uiso 1 1 calc R . . H14C H 0.4665 0.2587 0.3199 0.059 Uiso 1 1 calc R . . C15 C 0.4490(3) 0.17556(16) 0.3479(3) 0.0257(12) Uani 1 1 d . . . C16 C 0.4629(4) 0.19154(19) 0.4228(3) 0.0355(14) Uani 1 1 d . . . H16A H 0.5100 0.1805 0.4452 0.053 Uiso 1 1 calc R . . H16B H 0.4190 0.1854 0.4505 0.053 Uiso 1 1 calc R . . H16C H 0.4687 0.2190 0.4203 0.053 Uiso 1 1 calc R . . C17 C 0.5189(3) 0.18408(17) 0.3048(3) 0.0313(13) Uani 1 1 d . . . H17A H 0.5657 0.1739 0.3294 0.047 Uiso 1 1 calc R . . H17B H 0.5243 0.2114 0.2994 0.047 Uiso 1 1 calc R . . H17C H 0.5114 0.1723 0.2582 0.047 Uiso 1 1 calc R . . C18 C 0.4401(3) 0.13279(16) 0.3531(3) 0.0304(13) Uani 1 1 d . . . H18A H 0.4862 0.1220 0.3778 0.046 Uiso 1 1 calc R . . H18B H 0.4335 0.1220 0.3055 0.046 Uiso 1 1 calc R . . H18C H 0.3948 0.1269 0.3792 0.046 Uiso 1 1 calc R . . C19 C 0.0967(3) 0.08684(19) 0.7038(3) 0.0350(14) Uani 1 1 d . . . C20 C 0.0827(4) 0.1234(2) 0.7470(4) 0.0485(18) Uani 1 1 d . . . H20A H 0.0320 0.1338 0.7324 0.073 Uiso 1 1 calc R . . H20B H 0.1227 0.1420 0.7382 0.073 Uiso 1 1 calc R . . H20C H 0.0846 0.1173 0.7974 0.073 Uiso 1 1 calc R . . C21 C 0.0364(3) 0.0580(2) 0.7246(3) 0.0401(16) Uani 1 1 d . . . H21A H -0.0151 0.0666 0.7079 0.060 Uiso 1 1 calc R . . H21B H 0.0389 0.0553 0.7761 0.060 Uiso 1 1 calc R . . H21C H 0.0470 0.0335 0.7030 0.060 Uiso 1 1 calc R . . C22 C 0.0878(4) 0.0958(2) 0.6254(4) 0.054(2) Uani 1 1 d . . . H22A H 0.0351 0.1045 0.6132 0.081 Uiso 1 1 calc R . . H22B H 0.0981 0.0731 0.5982 0.081 Uiso 1 1 calc R . . H22C H 0.1244 0.1156 0.6143 0.081 Uiso 1 1 calc R . . C23 C 0.2143(4) 0.0210(2) 0.7012(4) 0.0417(16) Uani 1 1 d . . . C24 C 0.1788(4) -0.0086(2) 0.7482(4) 0.0505(19) Uani 1 1 d . . . H24A H 0.1889 -0.0339 0.7300 0.076 Uiso 1 1 calc R . . H24B H 0.1230 -0.0046 0.7480 0.076 Uiso 1 1 calc R . . H24C H 0.2016 -0.0063 0.7965 0.076 Uiso 1 1 calc R . . C25 C 0.1852(4) 0.0152(3) 0.6244(4) 0.059(2) Uani 1 1 d . . . H25A H 0.1968 -0.0106 0.6098 0.089 Uiso 1 1 calc R . . H25B H 0.2109 0.0332 0.5944 0.089 Uiso 1 1 calc R . . H25C H 0.1294 0.0194 0.6196 0.089 Uiso 1 1 calc R . . C26 C 0.3023(4) 0.0152(2) 0.7057(5) 0.064(3) Uani 1 1 d . . . H26A H 0.3142 -0.0100 0.6882 0.097 Uiso 1 1 calc R . . H26B H 0.3224 0.0176 0.7549 0.097 Uiso 1 1 calc R . . H26C H 0.3263 0.0343 0.6769 0.097 Uiso 1 1 calc R . . C27 C 0.2630(3) 0.1021(2) 0.6970(3) 0.0349(15) Uani 1 1 d . . . H27A H 0.2754 0.0923 0.6502 0.042 Uiso 1 1 calc R . . H27B H 0.2370 0.1268 0.6892 0.042 Uiso 1 1 calc R . . C28 C 0.3393(3) 0.10860(18) 0.7419(3) 0.0305(13) Uani 1 1 d . . . H28A H 0.3635 0.1321 0.7259 0.037 Uiso 1 1 calc R . . H28B H 0.3749 0.0875 0.7335 0.037 Uiso 1 1 calc R . . C29 C 0.4167(3) 0.09150(16) 0.8818(3) 0.0238(12) Uani 1 1 d . . . C30 C 0.4110(3) 0.04841(16) 0.8736(3) 0.0272(12) Uani 1 1 d . . . H30A H 0.4572 0.0366 0.8960 0.041 Uiso 1 1 calc R . . H30B H 0.4066 0.0419 0.8233 0.041 Uiso 1 1 calc R . . H30C H 0.3654 0.0393 0.8962 0.041 Uiso 1 1 calc R . . C31 C 0.4908(3) 0.10491(18) 0.8493(3) 0.0331(14) Uani 1 1 d . . . H31A H 0.5356 0.0932 0.8745 0.050 Uiso 1 1 calc R . . H31B H 0.4948 0.1324 0.8533 0.050 Uiso 1 1 calc R . . H31C H 0.4891 0.0977 0.7994 0.050 Uiso 1 1 calc R . . C32 C 0.4216(3) 0.10054(18) 0.9617(3) 0.0322(13) Uani 1 1 d . . . H32A H 0.4689 0.0896 0.9839 0.048 Uiso 1 1 calc R . . H32B H 0.3768 0.0898 0.9832 0.048 Uiso 1 1 calc R . . H32C H 0.4223 0.1280 0.9684 0.048 Uiso 1 1 calc R . . C33 C 0.3157(4) 0.16341(17) 0.8603(4) 0.0386(15) Uani 1 1 d . . . C34 C 0.3899(4) 0.18611(18) 0.8603(4) 0.0493(19) Uani 1 1 d . . . H34A H 0.3795 0.2124 0.8726 0.074 Uiso 1 1 calc R . . H34B H 0.4100 0.1851 0.8133 0.074 Uiso 1 1 calc R . . H34C H 0.4280 0.1754 0.8951 0.074 Uiso 1 1 calc R . . C35 C 0.2810(4) 0.1658(2) 0.9331(4) 0.0501(19) Uani 1 1 d . . . H35A H 0.2747 0.1923 0.9461 0.075 Uiso 1 1 calc R . . H35B H 0.3156 0.1533 0.9686 0.075 Uiso 1 1 calc R . . H35C H 0.2307 0.1532 0.9307 0.075 Uiso 1 1 calc R . . C36 C 0.2568(4) 0.18014(19) 0.8055(5) 0.058(2) Uani 1 1 d . . . H36A H 0.2494 0.2070 0.8155 0.088 Uiso 1 1 calc R . . H36B H 0.2076 0.1668 0.8076 0.088 Uiso 1 1 calc R . . H36C H 0.2758 0.1773 0.7583 0.088 Uiso 1 1 calc R . . C37 C 0.8865(3) 0.15152(15) 0.3322(3) 0.0201(11) Uani 1 1 d . . . C38 C 0.9202(3) 0.11613(15) 0.3399(3) 0.0210(11) Uani 1 1 d . . . H38A H 0.8941 0.0948 0.3197 0.025 Uiso 1 1 calc R . . C39 C 0.9921(3) 0.11127(15) 0.3771(3) 0.0215(11) Uani 1 1 d . . . C40 C 1.0315(3) 0.14182(16) 0.4065(3) 0.0225(11) Uani 1 1 d . . . H40A H 1.0801 0.1385 0.4315 0.027 Uiso 1 1 calc R . . C41 C 0.9991(3) 0.17749(15) 0.3990(3) 0.0206(11) Uani 1 1 d . . . C42 C 0.9282(3) 0.18215(15) 0.3616(3) 0.0218(11) Uani 1 1 d . . . H42A H 0.9076 0.2069 0.3558 0.026 Uiso 1 1 calc R . . C43 C 1.0282(3) 0.07295(16) 0.3846(3) 0.0278(12) Uani 1 1 d . . . C44 C 1.0421(3) 0.21048(16) 0.4311(3) 0.0250(12) Uani 1 1 d . . . C45 C 0.7891(3) 0.19605(15) 0.2488(2) 0.0183(11) Uani 1 1 d . . . C46 C 0.8481(3) 0.20806(16) 0.2066(3) 0.0240(12) Uani 1 1 d . . . H46A H 0.8977 0.1969 0.2136 0.029 Uiso 1 1 calc R . . C47 C 0.8367(3) 0.23552(16) 0.1552(3) 0.0271(12) Uani 1 1 d . . . C48 C 0.7652(3) 0.25360(16) 0.1446(3) 0.0283(13) Uani 1 1 d . . . H48A H 0.7575 0.2728 0.1100 0.034 Uiso 1 1 calc R . . C49 C 0.7061(3) 0.24270(16) 0.1859(3) 0.0231(11) Uani 1 1 d . . . C50 C 0.7179(3) 0.21426(15) 0.2361(3) 0.0214(11) Uani 1 1 d . . . H50A H 0.6760 0.2069 0.2628 0.026 Uiso 1 1 calc R . . C51 C 0.9000(4) 0.2449(2) 0.1082(3) 0.0399(16) Uani 1 1 d . . . C52 C 0.6290(3) 0.26152(17) 0.1763(3) 0.0335(14) Uani 1 1 d . . . C53 C 0.7460(3) 0.16005(15) 0.3678(3) 0.0196(11) Uani 1 1 d . . . C54 C 0.7278(3) 0.19427(15) 0.3999(3) 0.0214(11) Uani 1 1 d . . . H54A H 0.7432 0.2173 0.3792 0.026 Uiso 1 1 calc R . . C55 C 0.6877(3) 0.19564(16) 0.4610(3) 0.0251(12) Uani 1 1 d . . . C56 C 0.6654(3) 0.16268(16) 0.4937(3) 0.0262(12) Uani 1 1 d . . . H56A H 0.6383 0.1636 0.5356 0.031 Uiso 1 1 calc R . . C57 C 0.6834(3) 0.12851(15) 0.4638(3) 0.0220(11) Uani 1 1 d . . . C58 C 0.7234(3) 0.12735(15) 0.4025(3) 0.0223(11) Uani 1 1 d . . . H58A H 0.7357 0.1035 0.3835 0.027 Uiso 1 1 calc R . . C59 C 0.6685(4) 0.23343(18) 0.4911(3) 0.0364(15) Uani 1 1 d . . . C60 C 0.6563(3) 0.09269(16) 0.4952(3) 0.0280(13) Uani 1 1 d . . . C61 C 0.7677(3) 0.12546(15) 0.2420(3) 0.0203(11) Uani 1 1 d . . . C62 C 0.6906(3) 0.11356(15) 0.2352(3) 0.0232(12) Uani 1 1 d . . . H62A H 0.6564 0.1213 0.2696 0.028 Uiso 1 1 calc R . . C63 C 0.6627(3) 0.09075(16) 0.1796(3) 0.0270(12) Uani 1 1 d . . . C64 C 0.7098(3) 0.07920(16) 0.1277(3) 0.0271(12) Uani 1 1 d . . . H64A H 0.6901 0.0641 0.0893 0.033 Uiso 1 1 calc R . . C65 C 0.7860(3) 0.09016(15) 0.1332(3) 0.0225(11) Uani 1 1 d . . . C66 C 0.8135(3) 0.11254(15) 0.1895(3) 0.0235(12) Uani 1 1 d . . . H66A H 0.8665 0.1194 0.1922 0.028 Uiso 1 1 calc R . . C67 C 0.8369(3) 0.0795(2) 0.0763(3) 0.0419(17) Uani 1 1 d . . . C68 C 0.5793(4) 0.0799(2) 0.1729(3) 0.0431(17) Uani 1 1 d . . . C69 C 0.1507(3) 0.91620(15) 0.1651(3) 0.0198(11) Uani 1 1 d . . . C70 C 0.1036(3) 0.88822(15) 0.1337(3) 0.0187(11) Uani 1 1 d . . . H70A H 0.1171 0.8625 0.1411 0.022 Uiso 1 1 calc R . . C71 C 0.0373(3) 0.89695(15) 0.0920(3) 0.0227(11) Uani 1 1 d . . . C72 C 0.0154(3) 0.93413(16) 0.0806(3) 0.0247(12) Uani 1 1 d . . . H72A H -0.0286 0.9401 0.0504 0.030 Uiso 1 1 calc R . . C73 C 0.0589(3) 0.96251(15) 0.1142(3) 0.0234(12) Uani 1 1 d . . . C74 C 0.1258(3) 0.95341(15) 0.1545(3) 0.0201(11) Uani 1 1 d . . . H74A H 0.1558 0.9733 0.1757 0.024 Uiso 1 1 calc R . . C75 C -0.0092(3) 0.86590(17) 0.0572(3) 0.0313(13) Uani 1 1 d . . . C76 C 0.0346(3) 1.00292(17) 0.1078(3) 0.0311(13) Uani 1 1 d . . . C77 C 0.1953(3) 0.90161(15) 0.2958(3) 0.0197(11) Uani 1 1 d . . . C78 C 0.1759(3) 0.86596(15) 0.3210(3) 0.0212(11) Uani 1 1 d . . . H78A H 0.1858 0.8443 0.2936 0.025 Uiso 1 1 calc R . . C79 C 0.1422(3) 0.86136(16) 0.3857(3) 0.0254(12) Uani 1 1 d . . . C80 C 0.1276(3) 0.89208(17) 0.4277(3) 0.0265(12) Uani 1 1 d . . . H80A H 0.1059 0.8889 0.4720 0.032 Uiso 1 1 calc R . . C81 C 0.1458(3) 0.92783(16) 0.4030(3) 0.0251(12) Uani 1 1 d . . . C82 C 0.1791(3) 0.93241(15) 0.3389(3) 0.0225(11) Uani 1 1 d . . . H82A H 0.1912 0.9571 0.3238 0.027 Uiso 1 1 calc R . . C83 C 0.1188(4) 0.82262(17) 0.4082(3) 0.0334(14) Uani 1 1 d . . . C84 C 0.1269(3) 0.96154(18) 0.4464(3) 0.0323(14) Uani 1 1 d . . . C85 C 0.2767(3) 0.87022(14) 0.1908(3) 0.0192(11) Uani 1 1 d . . . C86 C 0.2773(3) 0.85956(15) 0.1200(3) 0.0213(11) Uani 1 1 d . . . H86A H 0.2423 0.8712 0.0862 0.026 Uiso 1 1 calc R . . C87 C 0.3286(3) 0.83189(15) 0.0977(3) 0.0248(12) Uani 1 1 d . . . C88 C 0.3783(3) 0.81366(15) 0.1462(3) 0.0281(13) Uani 1 1 d . . . H88A H 0.4117 0.7944 0.1314 0.034 Uiso 1 1 calc R . . C89 C 0.3788(3) 0.82382(16) 0.2164(3) 0.0263(12) Uani 1 1 d . . . C90 C 0.3283(3) 0.85166(15) 0.2385(3) 0.0213(11) Uani 1 1 d . . . H90A H 0.3293 0.8581 0.2871 0.026 Uiso 1 1 calc R . . C91 C 0.3299(4) 0.82261(18) 0.0214(3) 0.0350(14) Uani 1 1 d . . . C92 C 0.4326(4) 0.80531(19) 0.2704(3) 0.0377(15) Uani 1 1 d . . . C93 C 0.2919(3) 0.94076(14) 0.2121(3) 0.0176(10) Uani 1 1 d . . . C94 C 0.3075(3) 0.95484(14) 0.1451(3) 0.0194(11) Uani 1 1 d . . . H94A H 0.2758 0.9470 0.1052 0.023 Uiso 1 1 calc R . . C95 C 0.3677(3) 0.97984(14) 0.1354(3) 0.0192(11) Uani 1 1 d . . . C96 C 0.4136(3) 0.99226(14) 0.1932(3) 0.0223(11) Uani 1 1 d . . . H96A H 0.4546 1.0095 0.1871 0.027 Uiso 1 1 calc R . . C97 C 0.3992(3) 0.97931(15) 0.2599(3) 0.0212(11) Uani 1 1 d . . . C98 C 0.3390(3) 0.95364(14) 0.2689(3) 0.0199(11) Uani 1 1 d . . . H98A H 0.3303 0.9449 0.3150 0.024 Uiso 1 1 calc R . . C99 C 0.3821(3) 0.99172(15) 0.0619(3) 0.0231(12) Uani 1 1 d . . . C100 C 0.4482(3) 0.99247(18) 0.3219(3) 0.0326(14) Uani 1 1 d . . . C102 C 0.7976(3) 0.38099(18) 0.0172(3) 0.0319(14) Uani 1 1 d . . . C103 C 0.8705(3) 0.3762(2) 0.0492(3) 0.0372(15) Uani 1 1 d . . . H10C H 0.8848 0.3535 0.0732 0.045 Uiso 1 1 calc R . . C104 C 0.9221(4) 0.4061(2) 0.0451(4) 0.0450(17) Uani 1 1 d . . . H10D H 0.9728 0.4037 0.0664 0.054 Uiso 1 1 calc R . . C105 C 0.9011(4) 0.4385(2) 0.0110(4) 0.0487(18) Uani 1 1 d . . . H10E H 0.9372 0.4585 0.0087 0.058 Uiso 1 1 calc R . . C106 C 0.8273(4) 0.4428(2) -0.0206(4) 0.0433(16) Uani 1 1 d . . . H10F H 0.8126 0.4656 -0.0439 0.052 Uiso 1 1 calc R . . C107 C 0.7757(4) 0.41342(19) -0.0175(3) 0.0371(15) Uani 1 1 d . . . H10G H 0.7252 0.4157 -0.0393 0.045 Uiso 1 1 calc R . . Cl1 Cl 0.73081(9) 0.34395(5) 0.02292(8) 0.0397(4) Uani 1 1 d . . . F1 F 0.9844(2) 0.04534(10) 0.3579(2) 0.0441(9) Uani 1 1 d . . . F2 F 1.0476(2) 0.06413(10) 0.45171(19) 0.0464(10) Uani 1 1 d . . . F3 F 1.0949(2) 0.07101(11) 0.3521(2) 0.0499(10) Uani 1 1 d . . . F4 F 1.0677(2) 0.20425(11) 0.4973(2) 0.0493(10) Uani 1 1 d . . . F5 F 1.1052(2) 0.21877(11) 0.3972(2) 0.0515(11) Uani 1 1 d . . . F6 F 1.0005(2) 0.24189(10) 0.4316(2) 0.0497(11) Uani 1 1 d . . . F7 F 0.9686(2) 0.23568(13) 0.1332(2) 0.0518(11) Uani 1 1 d . . . F8 F 0.8911(3) 0.2274(3) 0.0479(3) 0.131(3) Uani 1 1 d . . . F9 F 0.9042(3) 0.28090(16) 0.0941(4) 0.130(3) Uani 1 1 d . . . F10 F 0.6308(2) 0.29342(11) 0.1391(2) 0.0516(11) Uani 1 1 d . . . F11 F 0.6016(2) 0.27094(10) 0.23871(18) 0.0390(9) Uani 1 1 d . . . F12 F 0.5761(2) 0.23905(12) 0.1445(2) 0.0564(12) Uani 1 1 d . . . F13 F 0.7309(2) 0.25136(11) 0.5192(2) 0.0574(12) Uani 1 1 d . . . F14 F 0.6392(2) 0.25720(11) 0.4417(2) 0.0508(10) Uani 1 1 d . . . F15 F 0.6159(3) 0.23180(11) 0.5390(2) 0.0666(14) Uani 1 1 d . . . F16 F 0.6490(3) 0.09531(11) 0.5649(2) 0.0510(10) Uani 1 1 d . . . F17 F 0.58693(19) 0.08210(11) 0.4672(2) 0.0451(10) Uani 1 1 d . . . F18 F 0.7029(2) 0.06317(10) 0.4863(2) 0.0402(9) Uani 1 1 d . . . F19 F 0.5466(2) 0.07843(17) 0.2328(2) 0.0819(18) Uani 1 1 d . . . F20 F 0.5384(3) 0.1033(3) 0.1363(5) 0.168(5) Uani 1 1 d . . . F21 F 0.5664(3) 0.0477(2) 0.1428(4) 0.140(4) Uani 1 1 d . . . F22 F 0.8235(3) 0.04510(19) 0.0527(4) 0.117(3) Uani 1 1 d . . . F23 F 0.8272(4) 0.1015(3) 0.0208(3) 0.142(4) Uani 1 1 d . . . F24 F 0.91132(19) 0.08095(11) 0.09537(19) 0.0397(9) Uani 1 1 d . . . F25 F -0.0078(3) 0.83430(13) 0.0939(3) 0.089(2) Uani 1 1 d . . . F26 F 0.0131(3) 0.85638(17) -0.0048(3) 0.091(2) Uani 1 1 d . . . F27 F -0.0835(2) 0.87427(12) 0.0473(3) 0.0706(15) Uani 1 1 d . . . F28 F -0.0300(2) 1.00753(11) 0.0677(3) 0.0582(12) Uani 1 1 d . . . F29 F 0.0876(2) 1.02477(10) 0.0800(2) 0.0431(9) Uani 1 1 d . . . F30 F 0.0247(2) 1.01812(10) 0.1711(2) 0.0479(10) Uani 1 1 d . . . F31 F 0.0493(2) 0.81310(12) 0.3810(3) 0.0648(13) Uani 1 1 d . . . F32 F 0.1662(3) 0.79552(10) 0.3874(2) 0.0538(11) Uani 1 1 d . . . F33 F 0.1182(3) 0.81903(11) 0.47772(19) 0.0503(10) Uani 1 1 d . . . F34 F 0.0577(2) 0.97646(12) 0.4245(2) 0.0561(12) Uani 1 1 d . . . F35 F 0.1782(2) 0.98958(10) 0.4417(2) 0.0459(10) Uani 1 1 d . . . F36 F 0.1228(2) 0.95381(11) 0.51472(19) 0.0478(10) Uani 1 1 d . . . F37 F 0.3481(5) 0.78869(18) 0.0087(3) 0.143(4) Uani 1 1 d . . . F38 F 0.2648(4) 0.8265(2) -0.0142(3) 0.132(3) Uani 1 1 d . . . F39 F 0.3737(6) 0.8433(3) -0.0109(3) 0.202(6) Uani 1 1 d . . . F40 F 0.4838(3) 0.82977(14) 0.2993(3) 0.0712(14) Uani 1 1 d . . . F41 F 0.4736(2) 0.77748(12) 0.2440(2) 0.0561(11) Uani 1 1 d . . . F42 F 0.3962(2) 0.79023(14) 0.3229(2) 0.0673(14) Uani 1 1 d . . . F43 F 0.4039(2) 0.96281(9) 0.02198(17) 0.0337(8) Uani 1 1 d . . . F44 F 0.31855(19) 1.00595(10) 0.02725(18) 0.0385(9) Uani 1 1 d . . . F45 F 0.43674(19) 1.01808(10) 0.05919(17) 0.0356(8) Uani 1 1 d . . . F46 F 0.4282(3) 0.98089(14) 0.38382(19) 0.0610(13) Uani 1 1 d . . . F47 F 0.5201(3) 0.9859(3) 0.3176(3) 0.145(4) Uani 1 1 d . . . F48 F 0.4451(4) 1.03007(15) 0.3299(3) 0.105(2) Uani 1 1 d . . . N1 N 0.3803(3) 0.19680(18) 0.1153(3) 0.0461(15) Uani 1 1 d . . . N2 N 0.1900(3) 0.05310(16) 0.9215(3) 0.0400(14) Uani 1 1 d . . . Ni1 Ni 0.33720(4) 0.18160(2) 0.18482(3) 0.02184(17) Uani 1 1 d . . . Ni2 Ni 0.22252(4) 0.07573(2) 0.85232(3) 0.02186(17) Uani 1 1 d . . . O1 O 0.4112(4) 0.2085(2) 0.0687(3) 0.100(3) Uani 1 1 d . . . O2 O 0.1772(3) 0.0339(2) 0.9649(3) 0.0757(18) Uani 1 1 d . . . P1 P 0.23928(8) 0.14170(4) 0.20721(7) 0.0206(3) Uani 1 1 d . . . P2 P 0.35985(8) 0.19520(4) 0.30045(7) 0.0199(3) Uani 1 1 d . . . P3 P 0.19521(8) 0.06945(4) 0.73567(7) 0.0250(3) Uani 1 1 d . . . P4 P 0.32693(8) 0.11213(4) 0.83796(7) 0.0214(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.013(3) 0.020(3) 0.030(3) 0.000(2) 0.007(2) -0.002(2) B2 0.016(3) 0.019(3) 0.026(3) 0.001(2) 0.003(2) -0.002(2) C1 0.026(3) 0.018(3) 0.058(4) -0.010(3) 0.004(3) -0.001(2) C2 0.028(3) 0.027(4) 0.081(5) -0.020(3) 0.006(3) 0.005(3) C3 0.036(4) 0.037(4) 0.055(4) -0.020(3) 0.010(3) 0.001(3) C4 0.039(4) 0.017(3) 0.084(5) -0.002(3) 0.002(4) -0.007(3) C5 0.017(3) 0.027(3) 0.033(3) 0.000(2) 0.002(2) 0.000(2) C6 0.037(3) 0.032(4) 0.037(3) 0.005(3) -0.001(3) -0.005(3) C7 0.015(3) 0.040(4) 0.055(4) 0.008(3) 0.003(3) -0.008(3) C8 0.022(3) 0.042(4) 0.040(4) -0.008(3) -0.003(3) 0.012(3) C9 0.018(3) 0.033(3) 0.026(3) 0.009(2) 0.002(2) 0.000(2) C10 0.022(3) 0.038(3) 0.023(3) 0.004(2) 0.010(2) 0.002(2) C11 0.028(3) 0.021(3) 0.043(4) -0.006(2) 0.004(3) 0.004(2) C12 0.031(3) 0.020(3) 0.054(4) 0.002(3) -0.003(3) 0.007(3) C13 0.055(4) 0.042(4) 0.044(4) -0.019(3) 0.000(3) 0.017(3) C14 0.035(4) 0.019(3) 0.064(5) -0.006(3) 0.002(3) -0.001(3) C15 0.017(3) 0.026(3) 0.034(3) 0.001(2) 0.001(2) 0.003(2) C16 0.032(3) 0.047(4) 0.027(3) 0.001(3) -0.006(3) 0.001(3) C17 0.020(3) 0.035(4) 0.040(3) 0.003(3) 0.008(2) 0.007(2) C18 0.021(3) 0.032(3) 0.038(3) 0.004(3) 0.000(2) 0.007(2) C19 0.019(3) 0.048(4) 0.038(3) 0.011(3) -0.001(2) -0.007(3) C20 0.021(3) 0.045(4) 0.079(5) 0.008(4) -0.001(3) 0.003(3) C21 0.024(3) 0.064(5) 0.032(3) 0.002(3) -0.003(3) -0.012(3) C22 0.028(3) 0.085(6) 0.047(4) 0.029(4) -0.007(3) -0.012(4) C23 0.032(3) 0.044(4) 0.048(4) -0.021(3) -0.006(3) -0.002(3) C24 0.050(4) 0.034(4) 0.066(5) -0.005(3) -0.011(4) -0.005(3) C25 0.042(4) 0.086(6) 0.051(5) -0.035(4) 0.013(3) -0.020(4) C26 0.037(4) 0.061(5) 0.093(6) -0.049(5) -0.012(4) 0.010(4) C27 0.026(3) 0.056(4) 0.023(3) 0.009(3) 0.002(2) -0.011(3) C28 0.024(3) 0.044(4) 0.024(3) 0.009(2) 0.002(2) -0.011(3) C29 0.016(3) 0.027(3) 0.028(3) 0.004(2) -0.001(2) -0.002(2) C30 0.018(3) 0.028(3) 0.035(3) 0.002(2) 0.000(2) 0.001(2) C31 0.020(3) 0.035(4) 0.045(4) 0.001(3) 0.003(3) -0.003(3) C32 0.024(3) 0.037(4) 0.035(3) 0.000(3) -0.004(2) 0.003(3) C33 0.033(3) 0.020(3) 0.062(4) -0.003(3) -0.004(3) -0.001(3) C34 0.041(4) 0.024(4) 0.082(6) 0.000(3) -0.006(4) -0.007(3) C35 0.041(4) 0.040(4) 0.069(5) -0.020(4) 0.004(4) 0.003(3) C36 0.053(5) 0.024(4) 0.095(6) 0.005(4) -0.023(4) 0.007(3) C37 0.018(3) 0.024(3) 0.019(3) -0.001(2) 0.003(2) -0.003(2) C38 0.021(3) 0.024(3) 0.019(3) -0.002(2) 0.004(2) -0.008(2) C39 0.020(3) 0.026(3) 0.020(3) 0.003(2) 0.006(2) -0.004(2) C40 0.015(3) 0.032(3) 0.021(3) 0.003(2) 0.002(2) -0.003(2) C41 0.018(3) 0.027(3) 0.017(3) -0.002(2) 0.007(2) -0.005(2) C42 0.026(3) 0.020(3) 0.021(3) 0.004(2) 0.005(2) -0.002(2) C43 0.022(3) 0.029(3) 0.031(3) 0.000(2) -0.005(2) -0.004(2) C44 0.020(3) 0.027(3) 0.028(3) -0.002(2) 0.002(2) -0.002(2) C45 0.015(2) 0.025(3) 0.015(2) -0.003(2) -0.0026(19) -0.005(2) C46 0.018(3) 0.031(3) 0.023(3) -0.001(2) 0.001(2) -0.002(2) C47 0.023(3) 0.030(3) 0.028(3) 0.000(2) 0.002(2) -0.007(2) C48 0.032(3) 0.028(3) 0.023(3) 0.005(2) -0.004(2) -0.006(3) C49 0.019(3) 0.028(3) 0.022(3) -0.003(2) -0.001(2) -0.002(2) C50 0.019(3) 0.021(3) 0.024(3) -0.001(2) -0.001(2) -0.004(2) C51 0.029(3) 0.060(5) 0.031(3) 0.017(3) -0.003(3) -0.014(3) C52 0.033(3) 0.033(3) 0.034(3) 0.008(3) -0.005(3) 0.003(3) C53 0.015(2) 0.021(3) 0.022(3) -0.002(2) -0.003(2) -0.003(2) C54 0.021(3) 0.023(3) 0.020(3) 0.000(2) 0.000(2) -0.004(2) C55 0.027(3) 0.024(3) 0.023(3) -0.001(2) -0.001(2) 0.000(2) C56 0.025(3) 0.030(3) 0.024(3) 0.006(2) 0.004(2) 0.001(2) C57 0.022(3) 0.024(3) 0.019(3) 0.006(2) -0.006(2) -0.001(2) C58 0.016(3) 0.022(3) 0.028(3) 0.000(2) 0.000(2) 0.002(2) C59 0.049(4) 0.034(4) 0.027(3) -0.003(3) 0.011(3) -0.003(3) C60 0.025(3) 0.027(3) 0.032(3) 0.005(2) 0.000(2) -0.003(2) C61 0.016(3) 0.024(3) 0.021(3) 0.005(2) 0.003(2) 0.001(2) C62 0.017(3) 0.026(3) 0.028(3) -0.001(2) 0.010(2) -0.004(2) C63 0.020(3) 0.031(3) 0.030(3) -0.001(2) 0.003(2) -0.006(2) C64 0.028(3) 0.023(3) 0.030(3) -0.008(2) -0.001(2) -0.002(2) C65 0.023(3) 0.026(3) 0.019(3) -0.003(2) 0.004(2) 0.003(2) C66 0.017(3) 0.028(3) 0.025(3) 0.001(2) 0.001(2) 0.001(2) C67 0.023(3) 0.068(5) 0.034(3) -0.020(3) -0.005(3) 0.014(3) C68 0.028(3) 0.065(5) 0.037(4) -0.009(3) -0.001(3) -0.021(3) C69 0.020(3) 0.023(3) 0.018(2) 0.001(2) 0.006(2) -0.002(2) C70 0.019(3) 0.018(3) 0.021(3) 0.001(2) 0.007(2) -0.001(2) C71 0.021(3) 0.026(3) 0.022(3) -0.001(2) 0.005(2) -0.004(2) C72 0.014(3) 0.034(3) 0.026(3) 0.001(2) 0.001(2) -0.004(2) C73 0.016(3) 0.025(3) 0.028(3) 0.001(2) 0.003(2) -0.001(2) C74 0.019(3) 0.023(3) 0.019(3) -0.001(2) 0.005(2) -0.005(2) C75 0.022(3) 0.033(4) 0.038(3) -0.003(3) -0.002(2) -0.005(2) C76 0.022(3) 0.028(3) 0.043(4) 0.008(3) -0.005(3) 0.002(2) C77 0.012(2) 0.022(3) 0.025(3) 0.003(2) -0.004(2) 0.001(2) C78 0.019(3) 0.021(3) 0.023(3) 0.001(2) -0.002(2) -0.001(2) C79 0.021(3) 0.029(3) 0.026(3) 0.002(2) 0.000(2) -0.004(2) C80 0.019(3) 0.038(4) 0.022(3) 0.004(2) 0.000(2) 0.000(2) C81 0.017(3) 0.031(3) 0.026(3) -0.006(2) -0.001(2) -0.002(2) C82 0.018(3) 0.019(3) 0.030(3) -0.001(2) -0.003(2) -0.002(2) C83 0.038(4) 0.032(3) 0.030(3) 0.011(3) 0.002(3) -0.001(3) C84 0.026(3) 0.038(4) 0.032(3) -0.012(3) -0.001(2) -0.008(3) C85 0.013(2) 0.015(3) 0.030(3) 0.002(2) 0.002(2) -0.005(2) C86 0.019(3) 0.018(3) 0.026(3) 0.001(2) 0.000(2) -0.002(2) C87 0.024(3) 0.016(3) 0.035(3) 0.002(2) 0.005(2) -0.003(2) C88 0.023(3) 0.018(3) 0.045(4) 0.005(2) 0.011(3) 0.003(2) C89 0.018(3) 0.022(3) 0.039(3) 0.010(2) 0.005(2) 0.000(2) C90 0.015(2) 0.023(3) 0.027(3) 0.006(2) 0.003(2) -0.004(2) C91 0.039(4) 0.036(4) 0.030(3) -0.001(3) 0.009(3) 0.006(3) C92 0.028(3) 0.043(4) 0.043(4) 0.013(3) 0.007(3) 0.010(3) C93 0.014(2) 0.016(3) 0.023(3) 0.001(2) 0.001(2) 0.004(2) C94 0.016(2) 0.017(3) 0.025(3) -0.001(2) -0.001(2) 0.002(2) C95 0.015(2) 0.011(3) 0.031(3) 0.001(2) 0.004(2) 0.004(2) C96 0.015(3) 0.013(3) 0.039(3) 0.002(2) 0.007(2) 0.000(2) C97 0.016(3) 0.020(3) 0.028(3) -0.001(2) 0.001(2) 0.000(2) C98 0.020(3) 0.021(3) 0.019(3) 0.005(2) 0.001(2) 0.002(2) C99 0.020(3) 0.024(3) 0.025(3) 0.000(2) 0.001(2) -0.002(2) C100 0.030(3) 0.042(4) 0.025(3) 0.004(3) -0.003(2) -0.016(3) C102 0.025(3) 0.040(4) 0.033(3) -0.011(3) 0.018(3) -0.001(3) C103 0.027(3) 0.052(4) 0.034(3) -0.005(3) 0.009(3) 0.009(3) C104 0.026(3) 0.072(5) 0.037(4) -0.010(3) 0.007(3) -0.001(3) C105 0.040(4) 0.051(5) 0.056(5) -0.008(4) 0.011(3) -0.007(3) C106 0.048(4) 0.043(4) 0.040(4) -0.005(3) 0.005(3) 0.000(3) C107 0.029(3) 0.050(4) 0.034(3) -0.009(3) 0.011(3) 0.003(3) Cl1 0.0379(8) 0.0489(10) 0.0338(8) -0.0073(7) 0.0132(7) -0.0066(7) F1 0.037(2) 0.0238(19) 0.069(3) -0.0065(17) -0.0162(18) 0.0021(15) F2 0.061(3) 0.037(2) 0.040(2) 0.0056(16) -0.0080(18) 0.0135(18) F3 0.034(2) 0.039(2) 0.080(3) 0.013(2) 0.026(2) 0.0110(17) F4 0.060(3) 0.045(2) 0.041(2) -0.0065(17) -0.0150(19) -0.0143(19) F5 0.037(2) 0.053(3) 0.067(3) -0.027(2) 0.0259(19) -0.0258(19) F6 0.0287(19) 0.028(2) 0.090(3) -0.0208(19) -0.0137(19) 0.0016(15) F7 0.029(2) 0.084(3) 0.043(2) 0.019(2) 0.0137(17) -0.002(2) F8 0.071(4) 0.290(10) 0.036(3) -0.031(4) 0.023(2) -0.099(5) F9 0.060(3) 0.083(4) 0.256(9) 0.110(5) 0.090(4) 0.031(3) F10 0.045(2) 0.052(3) 0.059(3) 0.028(2) 0.0116(19) 0.0191(19) F11 0.0338(19) 0.047(2) 0.037(2) 0.0043(16) 0.0098(15) 0.0121(16) F12 0.031(2) 0.060(3) 0.075(3) -0.014(2) -0.022(2) 0.0074(19) F13 0.064(3) 0.031(2) 0.074(3) -0.019(2) -0.016(2) 0.0040(19) F14 0.067(3) 0.036(2) 0.051(2) 0.0003(18) 0.011(2) 0.0195(19) F15 0.101(4) 0.037(2) 0.069(3) -0.010(2) 0.063(3) -0.003(2) F16 0.078(3) 0.042(2) 0.035(2) 0.0125(17) 0.0170(19) -0.005(2) F17 0.0252(18) 0.045(2) 0.064(3) 0.0220(19) -0.0072(17) -0.0117(16) F18 0.034(2) 0.028(2) 0.060(2) 0.0112(16) 0.0092(17) 0.0045(15) F19 0.038(2) 0.155(5) 0.054(3) -0.034(3) 0.022(2) -0.049(3) F20 0.026(3) 0.265(11) 0.207(8) 0.145(8) -0.039(4) -0.050(4) F21 0.073(4) 0.170(7) 0.187(7) -0.132(6) 0.073(4) -0.096(4) F22 0.039(3) 0.144(6) 0.171(6) -0.134(5) 0.036(3) -0.025(3) F23 0.100(4) 0.289(10) 0.042(3) 0.062(4) 0.044(3) 0.136(6) F24 0.0251(18) 0.052(2) 0.042(2) -0.0157(17) 0.0086(15) 0.0047(16) F25 0.105(4) 0.040(3) 0.112(4) 0.020(3) -0.066(3) -0.034(3) F26 0.080(4) 0.118(5) 0.081(4) -0.066(3) 0.039(3) -0.064(3) F27 0.023(2) 0.051(3) 0.135(5) -0.033(3) -0.019(2) -0.0006(18) F28 0.039(2) 0.030(2) 0.101(3) 0.003(2) -0.030(2) 0.0074(17) F29 0.040(2) 0.028(2) 0.062(3) 0.0153(17) 0.0022(18) -0.0062(16) F30 0.058(3) 0.033(2) 0.055(2) -0.0020(17) 0.014(2) 0.0109(18) F31 0.051(3) 0.056(3) 0.085(3) 0.026(2) -0.016(2) -0.029(2) F32 0.079(3) 0.031(2) 0.056(3) 0.0117(18) 0.036(2) 0.006(2) F33 0.071(3) 0.053(3) 0.028(2) 0.0127(17) 0.0132(18) -0.007(2) F34 0.041(2) 0.058(3) 0.068(3) -0.028(2) -0.011(2) 0.022(2) F35 0.050(2) 0.035(2) 0.054(2) -0.0167(17) 0.0157(19) -0.0103(18) F36 0.055(2) 0.058(3) 0.032(2) -0.0174(17) 0.0145(17) -0.007(2) F37 0.286(10) 0.091(4) 0.050(3) -0.017(3) -0.014(4) 0.125(6) F38 0.118(5) 0.227(8) 0.049(3) -0.062(4) -0.026(3) 0.089(5) F39 0.295(12) 0.266(11) 0.055(4) -0.068(5) 0.094(6) -0.211(10) F40 0.056(3) 0.069(3) 0.083(3) 0.004(3) -0.040(3) 0.003(2) F41 0.047(2) 0.059(3) 0.063(3) 0.018(2) 0.009(2) 0.034(2) F42 0.049(3) 0.095(4) 0.060(3) 0.048(3) 0.021(2) 0.035(2) F43 0.041(2) 0.032(2) 0.0293(18) -0.0037(14) 0.0123(15) 0.0023(15) F44 0.0242(17) 0.053(2) 0.039(2) 0.0204(17) 0.0063(15) 0.0103(16) F45 0.0374(19) 0.039(2) 0.0313(18) 0.0043(15) 0.0063(15) -0.0215(16) F46 0.064(3) 0.090(3) 0.027(2) 0.004(2) -0.0076(18) -0.044(2) F47 0.019(2) 0.348(11) 0.066(4) -0.086(5) -0.008(2) -0.003(4) F48 0.185(7) 0.058(3) 0.065(3) 0.007(3) -0.058(4) -0.052(4) N1 0.044(3) 0.068(4) 0.029(3) 0.004(3) 0.020(3) -0.010(3) N2 0.041(3) 0.046(3) 0.037(3) 0.028(3) 0.028(2) 0.018(3) Ni1 0.0210(4) 0.0244(4) 0.0207(3) -0.0012(3) 0.0061(3) -0.0041(3) Ni2 0.0168(3) 0.0290(4) 0.0201(3) 0.0019(3) 0.0035(3) -0.0044(3) O1 0.103(5) 0.155(7) 0.045(4) -0.007(4) 0.030(4) -0.062(5) O2 0.055(4) 0.102(5) 0.068(4) 0.018(4) -0.006(3) -0.013(3) P1 0.0166(6) 0.0206(7) 0.0250(7) 0.0006(5) 0.0050(5) -0.0005(5) P2 0.0188(7) 0.0202(7) 0.0209(7) -0.0007(5) 0.0026(5) 0.0027(5) P3 0.0189(7) 0.0342(9) 0.0220(7) 0.0020(6) 0.0024(5) -0.0079(6) P4 0.0156(6) 0.0232(7) 0.0256(7) 0.0025(5) 0.0014(5) -0.0025(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C61 1.632(8) . ? B1 C53 1.643(8) . ? B1 C45 1.644(8) . ? B1 C37 1.654(8) . ? B2 C93 1.638(8) . ? B2 C77 1.640(8) . ? B2 C69 1.642(8) . ? B2 C85 1.658(8) . ? C1 C3 1.514(10) . ? C1 C4 1.539(9) . ? C1 C2 1.543(8) . ? C1 P1 1.874(6) . ? C5 C7 1.531(8) . ? C5 C8 1.542(8) . ? C5 C6 1.545(8) . ? C5 P1 1.876(6) . ? C9 C10 1.544(8) . ? C9 P1 1.851(6) . ? C10 P2 1.851(6) . ? C11 C14 1.536(9) . ? C11 C13 1.533(9) . ? C11 C12 1.540(8) . ? C11 P2 1.879(6) . ? C15 C18 1.527(8) . ? C15 C16 1.534(8) . ? C15 C17 1.538(8) . ? C15 P2 1.876(6) . ? C19 C22 1.520(9) . ? C19 C21 1.534(9) . ? C19 C20 1.559(10) . ? C19 P3 1.884(6) . ? C23 C25 1.527(10) . ? C23 C24 1.531(10) . ? C23 C26 1.541(9) . ? C23 P3 1.875(7) . ? C27 C28 1.548(8) . ? C27 P3 1.838(6) . ? C28 P4 1.855(6) . ? C29 C30 1.537(8) . ? C29 C31 1.538(8) . ? C29 C32 1.546(8) . ? C29 P4 1.870(5) . ? C33 C34 1.520(9) . ? C33 C36 1.532(9) . ? C33 C35 1.545(10) . ? C33 P4 1.879(6) . ? C37 C38 1.387(8) . ? C37 C42 1.401(7) . ? C38 C39 1.406(7) . ? C39 C40 1.380(8) . ? C39 C43 1.499(8) . ? C40 C41 1.387(8) . ? C41 C42 1.392(8) . ? C41 C44 1.496(8) . ? C43 F1 1.321(6) . ? C43 F2 1.334(7) . ? C43 F3 1.349(7) . ? C44 F4 1.325(7) . ? C44 F6 1.328(7) . ? C44 F5 1.338(6) . ? C45 C50 1.403(7) . ? C45 C46 1.408(7) . ? C46 C47 1.382(8) . ? C47 C48 1.401(8) . ? C47 C51 1.499(8) . ? C48 C49 1.387(8) . ? C49 C50 1.392(8) . ? C49 C52 1.498(8) . ? C51 F7 1.298(7) . ? C51 F8 1.302(8) . ? C51 F9 1.305(8) . ? C52 F12 1.331(7) . ? C52 F10 1.334(7) . ? C52 F11 1.348(7) . ? C53 C54 1.402(7) . ? C53 C58 1.402(7) . ? C54 C55 1.392(8) . ? C55 C56 1.389(8) . ? C55 C59 1.501(8) . ? C56 C57 1.382(8) . ? C57 C58 1.393(8) . ? C57 C60 1.491(8) . ? C59 F15 1.332(7) . ? C59 F14 1.336(7) . ? C59 F13 1.338(8) . ? C60 F17 1.339(7) . ? C60 F16 1.341(7) . ? C60 F18 1.341(7) . ? C61 C66 1.392(8) . ? C61 C62 1.404(7) . ? C62 C63 1.392(8) . ? C63 C64 1.383(8) . ? C63 C68 1.497(8) . ? C64 C65 1.378(8) . ? C65 C66 1.391(8) . ? C65 C67 1.490(8) . ? C67 F23 1.312(9) . ? C67 F22 1.314(9) . ? C67 F24 1.321(7) . ? C68 F20 1.270(10) . ? C68 F21 1.292(9) . ? C68 F19 1.303(8) . ? C69 C70 1.395(7) . ? C69 C74 1.398(8) . ? C70 C71 1.391(7) . ? C71 C72 1.384(8) . ? C71 C75 1.494(8) . ? C72 C73 1.389(8) . ? C73 C74 1.387(7) . ? C73 C76 1.496(8) . ? C75 F26 1.307(8) . ? C75 F25 1.317(8) . ? C75 F27 1.328(7) . ? C76 F28 1.326(7) . ? C76 F29 1.337(7) . ? C76 F30 1.338(7) . ? C77 C78 1.400(7) . ? C77 C82 1.403(7) . ? C78 C79 1.403(8) . ? C79 C80 1.383(8) . ? C79 C83 1.501(8) . ? C80 C81 1.394(8) . ? C81 C82 1.390(8) . ? C81 C84 1.498(8) . ? C83 F33 1.326(7) . ? C83 F31 1.327(7) . ? C83 F32 1.341(7) . ? C84 F36 1.333(7) . ? C84 F35 1.342(7) . ? C84 F34 1.355(7) . ? C85 C90 1.397(7) . ? C85 C86 1.398(8) . ? C86 C87 1.409(8) . ? C87 C88 1.382(8) . ? C87 C91 1.487(8) . ? C88 C89 1.381(9) . ? C89 C90 1.401(8) . ? C89 C92 1.494(8) . ? C91 F39 1.247(9) . ? C91 F37 1.270(8) . ? C91 F38 1.287(8) . ? C92 F42 1.326(7) . ? C92 F41 1.333(8) . ? C92 F40 1.336(8) . ? C93 C98 1.390(7) . ? C93 C94 1.407(7) . ? C94 C95 1.392(7) . ? C95 C96 1.387(8) . ? C95 C99 1.495(8) . ? C96 C97 1.384(8) . ? C97 C98 1.405(7) . ? C97 C100 1.483(8) . ? C99 F45 1.336(6) . ? C99 F43 1.343(6) . ? C99 F44 1.347(6) . ? C100 F47 1.278(8) . ? C100 F46 1.313(7) . ? C100 F48 1.342(8) . ? C102 C107 1.366(9) . ? C102 C103 1.380(9) . ? C102 Cl1 1.761(6) . ? C103 C104 1.391(10) . ? C104 C105 1.358(11) . ? C105 C106 1.389(10) . ? C106 C107 1.377(10) . ? N1 O1 1.141(8) . ? N1 Ni1 1.649(5) . ? N2 O2 1.101(7) . ? N2 Ni2 1.668(5) . ? Ni1 P2 2.258(2) . ? Ni1 P1 2.273(2) . ? Ni2 P3 2.246(3) . ? Ni2 P4 2.257(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C61 B1 C53 113.0(4) . . ? C61 B1 C45 101.1(4) . . ? C53 B1 C45 112.9(4) . . ? C61 B1 C37 114.0(4) . . ? C53 B1 C37 103.7(4) . . ? C45 B1 C37 112.5(4) . . ? C93 B2 C77 114.5(4) . . ? C93 B2 C69 110.9(4) . . ? C77 B2 C69 105.0(4) . . ? C93 B2 C85 100.9(4) . . ? C77 B2 C85 113.0(4) . . ? C69 B2 C85 112.8(4) . . ? C3 C1 C4 110.6(5) . . ? C3 C1 C2 107.7(6) . . ? C4 C1 C2 108.7(6) . . ? C3 C1 P1 110.1(4) . . ? C4 C1 P1 113.7(5) . . ? C2 C1 P1 105.7(4) . . ? C7 C5 C8 108.0(5) . . ? C7 C5 C6 111.3(5) . . ? C8 C5 C6 107.8(5) . . ? C7 C5 P1 113.8(4) . . ? C8 C5 P1 107.8(4) . . ? C6 C5 P1 108.0(4) . . ? C10 C9 P1 114.0(4) . . ? C9 C10 P2 112.7(4) . . ? C14 C11 C13 110.4(5) . . ? C14 C11 C12 108.5(5) . . ? C13 C11 C12 108.2(5) . . ? C14 C11 P2 109.5(4) . . ? C13 C11 P2 114.5(5) . . ? C12 C11 P2 105.6(4) . . ? C18 C15 C16 108.5(5) . . ? C18 C15 C17 108.4(5) . . ? C16 C15 C17 109.7(5) . . ? C18 C15 P2 108.3(4) . . ? C16 C15 P2 112.7(4) . . ? C17 C15 P2 109.2(4) . . ? C22 C19 C21 111.3(5) . . ? C22 C19 C20 109.4(6) . . ? C21 C19 C20 106.7(5) . . ? C22 C19 P3 114.6(5) . . ? C21 C19 P3 108.7(4) . . ? C20 C19 P3 105.8(4) . . ? C25 C23 C24 110.1(6) . . ? C25 C23 C26 107.6(6) . . ? C24 C23 C26 108.2(7) . . ? C25 C23 P3 113.6(5) . . ? C24 C23 P3 109.7(5) . . ? C26 C23 P3 107.5(4) . . ? C28 C27 P3 114.9(4) . . ? C27 C28 P4 113.7(4) . . ? C30 C29 C31 108.5(5) . . ? C30 C29 C32 107.7(5) . . ? C31 C29 C32 109.5(5) . . ? C30 C29 P4 107.2(4) . . ? C31 C29 P4 113.4(4) . . ? C32 C29 P4 110.4(4) . . ? C34 C33 C36 109.0(6) . . ? C34 C33 C35 110.6(6) . . ? C36 C33 C35 107.8(6) . . ? C34 C33 P4 114.3(5) . . ? C36 C33 P4 107.2(5) . . ? C35 C33 P4 107.8(5) . . ? C38 C37 C42 117.0(5) . . ? C38 C37 B1 122.9(5) . . ? C42 C37 B1 119.7(5) . . ? C37 C38 C39 121.3(5) . . ? C40 C39 C38 120.7(5) . . ? C40 C39 C43 118.5(5) . . ? C38 C39 C43 120.8(5) . . ? C39 C40 C41 119.0(5) . . ? C40 C41 C42 120.1(5) . . ? C40 C41 C44 118.7(5) . . ? C42 C41 C44 121.2(5) . . ? C41 C42 C37 122.0(5) . . ? F1 C43 F2 107.3(5) . . ? F1 C43 F3 106.2(5) . . ? F2 C43 F3 104.7(4) . . ? F1 C43 C39 113.9(4) . . ? F2 C43 C39 112.5(5) . . ? F3 C43 C39 111.6(5) . . ? F4 C44 F6 106.4(5) . . ? F4 C44 F5 104.9(5) . . ? F6 C44 F5 106.4(5) . . ? F4 C44 C41 112.7(5) . . ? F6 C44 C41 113.5(4) . . ? F5 C44 C41 112.3(4) . . ? C50 C45 C46 115.4(5) . . ? C50 C45 B1 121.4(4) . . ? C46 C45 B1 122.1(5) . . ? C47 C46 C45 122.5(5) . . ? C46 C47 C48 120.6(5) . . ? C46 C47 C51 119.9(5) . . ? C48 C47 C51 119.4(5) . . ? C49 C48 C47 118.3(5) . . ? C48 C49 C50 120.4(5) . . ? C48 C49 C52 119.8(5) . . ? C50 C49 C52 119.8(5) . . ? C49 C50 C45 122.7(5) . . ? F7 C51 F8 104.9(6) . . ? F7 C51 F9 105.0(6) . . ? F8 C51 F9 106.8(7) . . ? F7 C51 C47 114.7(5) . . ? F8 C51 C47 111.6(5) . . ? F9 C51 C47 113.0(6) . . ? F12 C52 F10 107.8(5) . . ? F12 C52 F11 105.9(5) . . ? F10 C52 F11 106.1(5) . . ? F12 C52 C49 112.1(5) . . ? F10 C52 C49 113.0(5) . . ? F11 C52 C49 111.5(5) . . ? C54 C53 C58 115.6(5) . . ? C54 C53 B1 122.5(5) . . ? C58 C53 B1 121.7(5) . . ? C55 C54 C53 122.1(5) . . ? C56 C55 C54 120.8(5) . . ? C56 C55 C59 120.3(5) . . ? C54 C55 C59 118.9(5) . . ? C57 C56 C55 118.3(5) . . ? C56 C57 C58 120.5(5) . . ? C56 C57 C60 119.7(5) . . ? C58 C57 C60 119.7(5) . . ? C57 C58 C53 122.6(5) . . ? F15 C59 F14 105.0(5) . . ? F15 C59 F13 108.8(5) . . ? F14 C59 F13 104.1(5) . . ? F15 C59 C55 113.6(5) . . ? F14 C59 C55 112.3(5) . . ? F13 C59 C55 112.4(5) . . ? F17 C60 F16 105.8(5) . . ? F17 C60 F18 105.5(5) . . ? F16 C60 F18 105.9(5) . . ? F17 C60 C57 112.3(4) . . ? F16 C60 C57 112.8(5) . . ? F18 C60 C57 113.8(5) . . ? C66 C61 C62 115.0(5) . . ? C66 C61 B1 121.9(5) . . ? C62 C61 B1 122.2(5) . . ? C63 C62 C61 121.9(5) . . ? C64 C63 C62 121.3(5) . . ? C64 C63 C68 118.6(5) . . ? C62 C63 C68 120.1(5) . . ? C65 C64 C63 118.2(5) . . ? C64 C65 C66 120.1(5) . . ? C64 C65 C67 119.1(5) . . ? C66 C65 C67 120.7(5) . . ? C65 C66 C61 123.6(5) . . ? F23 C67 F22 105.4(7) . . ? F23 C67 F24 105.8(6) . . ? F22 C67 F24 106.2(5) . . ? F23 C67 C65 112.3(5) . . ? F22 C67 C65 112.4(6) . . ? F24 C67 C65 114.1(5) . . ? F20 C68 F21 105.0(8) . . ? F20 C68 F19 104.2(7) . . ? F21 C68 F19 106.1(6) . . ? F20 C68 C63 112.7(6) . . ? F21 C68 C63 113.8(6) . . ? F19 C68 C63 114.2(5) . . ? C70 C69 C74 116.1(5) . . ? C70 C69 B2 123.5(5) . . ? C74 C69 B2 120.2(5) . . ? C71 C70 C69 121.9(5) . . ? C72 C71 C70 120.7(5) . . ? C72 C71 C75 119.7(5) . . ? C70 C71 C75 119.6(5) . . ? C71 C72 C73 118.7(5) . . ? C74 C73 C72 119.8(5) . . ? C74 C73 C76 119.3(5) . . ? C72 C73 C76 120.8(5) . . ? C73 C74 C69 122.7(5) . . ? F26 C75 F25 105.0(6) . . ? F26 C75 F27 105.7(5) . . ? F25 C75 F27 104.5(5) . . ? F26 C75 C71 113.8(5) . . ? F25 C75 C71 113.7(5) . . ? F27 C75 C71 113.2(5) . . ? F28 C76 F29 106.4(5) . . ? F28 C76 F30 108.3(5) . . ? F29 C76 F30 104.7(5) . . ? F28 C76 C73 112.9(5) . . ? F29 C76 C73 112.8(5) . . ? F30 C76 C73 111.3(5) . . ? C78 C77 C82 116.1(5) . . ? C78 C77 B2 121.7(5) . . ? C82 C77 B2 122.0(5) . . ? C79 C78 C77 121.9(5) . . ? C80 C79 C78 121.1(5) . . ? C80 C79 C83 119.4(5) . . ? C78 C79 C83 119.5(5) . . ? C79 C80 C81 117.8(5) . . ? C82 C81 C80 121.1(5) . . ? C82 C81 C84 120.4(5) . . ? C80 C81 C84 118.5(5) . . ? C81 C82 C77 122.1(5) . . ? F33 C83 F31 107.3(5) . . ? F33 C83 F32 105.6(5) . . ? F31 C83 F32 105.4(5) . . ? F33 C83 C79 113.0(5) . . ? F31 C83 C79 112.2(5) . . ? F32 C83 C79 112.8(5) . . ? F36 C84 F35 107.0(5) . . ? F36 C84 F34 106.1(5) . . ? F35 C84 F34 105.8(5) . . ? F36 C84 C81 113.5(5) . . ? F35 C84 C81 112.6(5) . . ? F34 C84 C81 111.4(5) . . ? C90 C85 C86 116.9(5) . . ? C90 C85 B2 119.9(5) . . ? C86 C85 B2 122.6(5) . . ? C85 C86 C87 121.3(5) . . ? C88 C87 C86 120.4(5) . . ? C88 C87 C91 119.9(5) . . ? C86 C87 C91 119.7(5) . . ? C89 C88 C87 119.1(5) . . ? C88 C89 C90 120.4(5) . . ? C88 C89 C92 120.9(5) . . ? C90 C89 C92 118.7(5) . . ? C85 C90 C89 121.8(5) . . ? F39 C91 F37 107.2(8) . . ? F39 C91 F38 102.9(8) . . ? F37 C91 F38 102.8(7) . . ? F39 C91 C87 113.4(6) . . ? F37 C91 C87 114.5(6) . . ? F38 C91 C87 114.9(5) . . ? F42 C92 F41 106.1(5) . . ? F42 C92 F40 106.9(6) . . ? F41 C92 F40 106.0(5) . . ? F42 C92 C89 112.6(5) . . ? F41 C92 C89 113.1(6) . . ? F40 C92 C89 111.7(5) . . ? C98 C93 C94 116.6(5) . . ? C98 C93 B2 124.3(5) . . ? C94 C93 B2 118.8(4) . . ? C95 C94 C93 122.3(5) . . ? C96 C95 C94 119.8(5) . . ? C96 C95 C99 121.8(5) . . ? C94 C95 C99 118.3(5) . . ? C97 C96 C95 119.3(5) . . ? C96 C97 C98 120.4(5) . . ? C96 C97 C100 119.5(5) . . ? C98 C97 C100 120.1(5) . . ? C93 C98 C97 121.6(5) . . ? F45 C99 F43 106.5(4) . . ? F45 C99 F44 106.4(4) . . ? F43 C99 F44 105.2(4) . . ? F45 C99 C95 113.3(4) . . ? F43 C99 C95 112.5(4) . . ? F44 C99 C95 112.4(4) . . ? F47 C100 F46 108.4(6) . . ? F47 C100 F48 103.5(7) . . ? F46 C100 F48 101.1(6) . . ? F47 C100 C97 114.1(5) . . ? F46 C100 C97 116.2(5) . . ? F48 C100 C97 112.2(5) . . ? C107 C102 C103 122.3(6) . . ? C107 C102 Cl1 119.4(5) . . ? C103 C102 Cl1 118.2(5) . . ? C102 C103 C104 117.3(7) . . ? C105 C104 C103 121.0(7) . . ? C104 C105 C106 120.7(7) . . ? C107 C106 C105 119.0(7) . . ? C102 C107 C106 119.6(6) . . ? O1 N1 Ni1 177.4(7) . . ? O2 N2 Ni2 168.5(6) . . ? N1 Ni1 P2 130.5(2) . . ? N1 Ni1 P1 137.4(2) . . ? P2 Ni1 P1 92.13(6) . . ? N2 Ni2 P3 131.9(2) . . ? N2 Ni2 P4 133.2(2) . . ? P3 Ni2 P4 93.37(6) . . ? C9 P1 C1 105.9(3) . . ? C9 P1 C5 108.1(3) . . ? C1 P1 C5 111.7(3) . . ? C9 P1 Ni1 102.97(18) . . ? C1 P1 Ni1 109.5(2) . . ? C5 P1 Ni1 117.66(19) . . ? C10 P2 C15 105.6(3) . . ? C10 P2 C11 105.0(3) . . ? C15 P2 C11 112.5(3) . . ? C10 P2 Ni1 104.13(19) . . ? C15 P2 Ni1 118.40(19) . . ? C11 P2 Ni1 109.8(2) . . ? C27 P3 C23 107.8(3) . . ? C27 P3 C19 105.0(3) . . ? C23 P3 C19 111.4(3) . . ? C27 P3 Ni2 103.4(2) . . ? C23 P3 Ni2 113.8(2) . . ? C19 P3 Ni2 114.5(2) . . ? C28 P4 C29 105.4(3) . . ? C28 P4 C33 107.9(3) . . ? C29 P4 C33 111.9(3) . . ? C28 P4 Ni2 103.00(18) . . ? C29 P4 Ni2 112.20(19) . . ? C33 P4 Ni2 115.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C9 C10 P2 -43.5(5) . . . . ? P3 C27 C28 P4 -39.7(6) . . . . ? C61 B1 C37 C38 -28.1(7) . . . . ? C53 B1 C37 C38 95.2(6) . . . . ? C45 B1 C37 C38 -142.5(5) . . . . ? C61 B1 C37 C42 158.8(5) . . . . ? C53 B1 C37 C42 -77.8(6) . . . . ? C45 B1 C37 C42 44.4(7) . . . . ? C42 C37 C38 C39 1.5(7) . . . . ? B1 C37 C38 C39 -171.8(5) . . . . ? C37 C38 C39 C40 -0.5(8) . . . . ? C37 C38 C39 C43 -179.6(5) . . . . ? C38 C39 C40 C41 0.1(8) . . . . ? C43 C39 C40 C41 179.2(5) . . . . ? C39 C40 C41 C42 -0.7(8) . . . . ? C39 C40 C41 C44 180.0(5) . . . . ? C40 C41 C42 C37 1.8(8) . . . . ? C44 C41 C42 C37 -178.9(5) . . . . ? C38 C37 C42 C41 -2.1(8) . . . . ? B1 C37 C42 C41 171.4(5) . . . . ? C40 C39 C43 F1 176.7(5) . . . . ? C38 C39 C43 F1 -4.3(7) . . . . ? C40 C39 C43 F2 54.2(7) . . . . ? C38 C39 C43 F2 -126.7(5) . . . . ? C40 C39 C43 F3 -63.1(6) . . . . ? C38 C39 C43 F3 116.0(5) . . . . ? C40 C41 C44 F4 -47.8(7) . . . . ? C42 C41 C44 F4 132.9(5) . . . . ? C40 C41 C44 F6 -168.9(5) . . . . ? C42 C41 C44 F6 11.8(7) . . . . ? C40 C41 C44 F5 70.3(6) . . . . ? C42 C41 C44 F5 -109.0(6) . . . . ? C61 B1 C45 C50 81.2(6) . . . . ? C53 B1 C45 C50 -39.8(7) . . . . ? C37 B1 C45 C50 -156.8(5) . . . . ? C61 B1 C45 C46 -86.5(5) . . . . ? C53 B1 C45 C46 152.4(5) . . . . ? C37 B1 C45 C46 35.5(7) . . . . ? C50 C45 C46 C47 -0.9(8) . . . . ? B1 C45 C46 C47 167.5(5) . . . . ? C45 C46 C47 C48 2.0(9) . . . . ? C45 C46 C47 C51 -175.2(5) . . . . ? C46 C47 C48 C49 -1.2(8) . . . . ? C51 C47 C48 C49 176.0(5) . . . . ? C47 C48 C49 C50 -0.5(8) . . . . ? C47 C48 C49 C52 179.8(5) . . . . ? C48 C49 C50 C45 1.7(8) . . . . ? C52 C49 C50 C45 -178.6(5) . . . . ? C46 C45 C50 C49 -0.9(8) . . . . ? B1 C45 C50 C49 -169.5(5) . . . . ? C46 C47 C51 F7 -21.7(9) . . . . ? C48 C47 C51 F7 161.1(6) . . . . ? C46 C47 C51 F8 97.5(8) . . . . ? C48 C47 C51 F8 -79.7(8) . . . . ? C46 C47 C51 F9 -142.0(7) . . . . ? C48 C47 C51 F9 40.7(9) . . . . ? C48 C49 C52 F12 107.3(6) . . . . ? C50 C49 C52 F12 -72.4(7) . . . . ? C48 C49 C52 F10 -14.8(8) . . . . ? C50 C49 C52 F10 165.5(5) . . . . ? C48 C49 C52 F11 -134.2(5) . . . . ? C50 C49 C52 F11 46.1(7) . . . . ? C61 B1 C53 C54 -142.2(5) . . . . ? C45 B1 C53 C54 -28.2(7) . . . . ? C37 B1 C53 C54 93.8(6) . . . . ? C61 B1 C53 C58 43.6(7) . . . . ? C45 B1 C53 C58 157.6(5) . . . . ? C37 B1 C53 C58 -80.4(6) . . . . ? C58 C53 C54 C55 -1.8(7) . . . . ? B1 C53 C54 C55 -176.4(5) . . . . ? C53 C54 C55 C56 1.2(8) . . . . ? C53 C54 C55 C59 -178.4(5) . . . . ? C54 C55 C56 C57 -0.4(8) . . . . ? C59 C55 C56 C57 179.2(5) . . . . ? C55 C56 C57 C58 0.3(8) . . . . ? C55 C56 C57 C60 -176.5(5) . . . . ? C56 C57 C58 C53 -1.0(8) . . . . ? C60 C57 C58 C53 175.7(5) . . . . ? C54 C53 C58 C57 1.7(7) . . . . ? B1 C53 C58 C57 176.4(5) . . . . ? C56 C55 C59 F15 -14.2(8) . . . . ? C54 C55 C59 F15 165.4(5) . . . . ? C56 C55 C59 F14 -133.1(6) . . . . ? C54 C55 C59 F14 46.5(7) . . . . ? C56 C55 C59 F13 109.9(6) . . . . ? C54 C55 C59 F13 -70.5(7) . . . . ? C56 C57 C60 F17 89.9(6) . . . . ? C58 C57 C60 F17 -86.9(6) . . . . ? C56 C57 C60 F16 -29.6(7) . . . . ? C58 C57 C60 F16 153.7(5) . . . . ? C56 C57 C60 F18 -150.3(5) . . . . ? C58 C57 C60 F18 33.0(7) . . . . ? C53 B1 C61 C66 -163.5(5) . . . . ? C45 B1 C61 C66 75.6(6) . . . . ? C37 B1 C61 C66 -45.3(7) . . . . ? C53 B1 C61 C62 28.0(7) . . . . ? C45 B1 C61 C62 -92.9(6) . . . . ? C37 B1 C61 C62 146.2(5) . . . . ? C66 C61 C62 C63 -0.4(8) . . . . ? B1 C61 C62 C63 168.9(5) . . . . ? C61 C62 C63 C64 -1.0(9) . . . . ? C61 C62 C63 C68 -177.7(6) . . . . ? C62 C63 C64 C65 1.5(9) . . . . ? C68 C63 C64 C65 178.2(6) . . . . ? C63 C64 C65 C66 -0.6(8) . . . . ? C63 C64 C65 C67 -177.3(6) . . . . ? C64 C65 C66 C61 -0.8(9) . . . . ? C67 C65 C66 C61 175.8(6) . . . . ? C62 C61 C66 C65 1.3(8) . . . . ? B1 C61 C66 C65 -168.0(5) . . . . ? C64 C65 C67 F23 79.0(9) . . . . ? C66 C65 C67 F23 -97.6(8) . . . . ? C64 C65 C67 F22 -39.6(8) . . . . ? C66 C65 C67 F22 143.8(6) . . . . ? C64 C65 C67 F24 -160.6(6) . . . . ? C66 C65 C67 F24 22.8(9) . . . . ? C64 C63 C68 F20 -86.8(9) . . . . ? C62 C63 C68 F20 90.0(9) . . . . ? C64 C63 C68 F21 32.6(10) . . . . ? C62 C63 C68 F21 -150.6(7) . . . . ? C64 C63 C68 F19 154.6(7) . . . . ? C62 C63 C68 F19 -28.6(10) . . . . ? C93 B2 C69 C70 150.5(5) . . . . ? C77 B2 C69 C70 -85.3(6) . . . . ? C85 B2 C69 C70 38.1(7) . . . . ? C93 B2 C69 C74 -34.5(7) . . . . ? C77 B2 C69 C74 89.6(5) . . . . ? C85 B2 C69 C74 -146.9(5) . . . . ? C74 C69 C70 C71 2.5(7) . . . . ? B2 C69 C70 C71 177.7(5) . . . . ? C69 C70 C71 C72 -0.6(8) . . . . ? C69 C70 C71 C75 177.5(5) . . . . ? C70 C71 C72 C73 -2.8(8) . . . . ? C75 C71 C72 C73 179.2(5) . . . . ? C71 C72 C73 C74 4.1(8) . . . . ? C71 C72 C73 C76 -175.6(5) . . . . ? C72 C73 C74 C69 -2.2(8) . . . . ? C76 C73 C74 C69 177.5(5) . . . . ? C70 C69 C74 C73 -1.1(8) . . . . ? B2 C69 C74 C73 -176.4(5) . . . . ? C72 C71 C75 F26 89.9(7) . . . . ? C70 C71 C75 F26 -88.1(7) . . . . ? C72 C71 C75 F25 -149.8(6) . . . . ? C70 C71 C75 F25 32.1(8) . . . . ? C72 C71 C75 F27 -30.8(8) . . . . ? C70 C71 C75 F27 151.1(5) . . . . ? C74 C73 C76 F28 179.8(5) . . . . ? C72 C73 C76 F28 -0.4(8) . . . . ? C74 C73 C76 F29 59.2(7) . . . . ? C72 C73 C76 F29 -121.1(6) . . . . ? C74 C73 C76 F30 -58.1(7) . . . . ? C72 C73 C76 F30 121.6(6) . . . . ? C93 B2 C77 C78 -145.4(5) . . . . ? C69 B2 C77 C78 92.8(5) . . . . ? C85 B2 C77 C78 -30.5(7) . . . . ? C93 B2 C77 C82 40.5(7) . . . . ? C69 B2 C77 C82 -81.3(6) . . . . ? C85 B2 C77 C82 155.4(5) . . . . ? C82 C77 C78 C79 0.0(7) . . . . ? B2 C77 C78 C79 -174.5(5) . . . . ? C77 C78 C79 C80 -0.9(8) . . . . ? C77 C78 C79 C83 176.8(5) . . . . ? C78 C79 C80 C81 1.5(8) . . . . ? C83 C79 C80 C81 -176.2(5) . . . . ? C79 C80 C81 C82 -1.4(8) . . . . ? C79 C80 C81 C84 177.1(5) . . . . ? C80 C81 C82 C77 0.6(8) . . . . ? C84 C81 C82 C77 -177.9(5) . . . . ? C78 C77 C82 C81 0.2(7) . . . . ? B2 C77 C82 C81 174.6(5) . . . . ? C80 C79 C83 F33 -28.4(8) . . . . ? C78 C79 C83 F33 153.8(5) . . . . ? C80 C79 C83 F31 93.1(7) . . . . ? C78 C79 C83 F31 -84.6(7) . . . . ? C80 C79 C83 F32 -148.1(5) . . . . ? C78 C79 C83 F32 34.2(7) . . . . ? C82 C81 C84 F36 -156.6(5) . . . . ? C80 C81 C84 F36 25.0(7) . . . . ? C82 C81 C84 F35 -34.9(7) . . . . ? C80 C81 C84 F35 146.7(5) . . . . ? C82 C81 C84 F34 83.8(7) . . . . ? C80 C81 C84 F34 -94.7(6) . . . . ? C93 B2 C85 C90 81.4(5) . . . . ? C77 B2 C85 C90 -41.4(6) . . . . ? C69 B2 C85 C90 -160.3(5) . . . . ? C93 B2 C85 C86 -89.4(5) . . . . ? C77 B2 C85 C86 147.8(5) . . . . ? C69 B2 C85 C86 29.0(7) . . . . ? C90 C85 C86 C87 -1.2(7) . . . . ? B2 C85 C86 C87 169.8(5) . . . . ? C85 C86 C87 C88 2.1(8) . . . . ? C85 C86 C87 C91 -177.2(5) . . . . ? C86 C87 C88 C89 -2.2(8) . . . . ? C91 C87 C88 C89 177.1(5) . . . . ? C87 C88 C89 C90 1.4(8) . . . . ? C87 C88 C89 C92 -178.9(5) . . . . ? C86 C85 C90 C89 0.4(7) . . . . ? B2 C85 C90 C89 -170.8(5) . . . . ? C88 C89 C90 C85 -0.5(8) . . . . ? C92 C89 C90 C85 179.8(5) . . . . ? C88 C87 C91 F39 -92.2(10) . . . . ? C86 C87 C91 F39 87.2(10) . . . . ? C88 C87 C91 F37 31.3(9) . . . . ? C86 C87 C91 F37 -149.4(7) . . . . ? C88 C87 C91 F38 149.9(7) . . . . ? C86 C87 C91 F38 -30.7(9) . . . . ? C88 C89 C92 F42 -124.6(6) . . . . ? C90 C89 C92 F42 55.1(8) . . . . ? C88 C89 C92 F41 -4.3(8) . . . . ? C90 C89 C92 F41 175.4(5) . . . . ? C88 C89 C92 F40 115.1(7) . . . . ? C90 C89 C92 F40 -65.2(7) . . . . ? C77 B2 C93 C98 24.9(7) . . . . ? C69 B2 C93 C98 143.4(5) . . . . ? C85 B2 C93 C98 -96.9(6) . . . . ? C77 B2 C93 C94 -162.8(4) . . . . ? C69 B2 C93 C94 -44.2(6) . . . . ? C85 B2 C93 C94 75.5(5) . . . . ? C98 C93 C94 C95 1.2(7) . . . . ? B2 C93 C94 C95 -171.8(5) . . . . ? C93 C94 C95 C96 -1.3(8) . . . . ? C93 C94 C95 C99 177.0(5) . . . . ? C94 C95 C96 C97 0.5(8) . . . . ? C99 C95 C96 C97 -177.8(5) . . . . ? C95 C96 C97 C98 0.5(8) . . . . ? C95 C96 C97 C100 179.9(5) . . . . ? C94 C93 C98 C97 -0.2(8) . . . . ? B2 C93 C98 C97 172.3(5) . . . . ? C96 C97 C98 C93 -0.6(8) . . . . ? C100 C97 C98 C93 179.9(5) . . . . ? C96 C95 C99 F45 -7.0(7) . . . . ? C94 C95 C99 F45 174.7(4) . . . . ? C96 C95 C99 F43 113.8(5) . . . . ? C94 C95 C99 F43 -64.5(6) . . . . ? C96 C95 C99 F44 -127.7(5) . . . . ? C94 C95 C99 F44 54.0(6) . . . . ? C96 C97 C100 F47 -57.0(9) . . . . ? C98 C97 C100 F47 122.5(7) . . . . ? C96 C97 C100 F46 175.9(5) . . . . ? C98 C97 C100 F46 -4.6(9) . . . . ? C96 C97 C100 F48 60.2(8) . . . . ? C98 C97 C100 F48 -120.3(6) . . . . ? C107 C102 C103 C104 -0.1(9) . . . . ? Cl1 C102 C103 C104 -179.0(5) . . . . ? C102 C103 C104 C105 0.3(10) . . . . ? C103 C104 C105 C106 0.1(11) . . . . ? C104 C105 C106 C107 -0.7(11) . . . . ? C103 C102 C107 C106 -0.4(9) . . . . ? Cl1 C102 C107 C106 178.4(5) . . . . ? C105 C106 C107 C102 0.8(10) . . . . ? O1 N1 Ni1 P2 -18(17) . . . . ? O1 N1 Ni1 P1 162(17) . . . . ? O2 N2 Ni2 P3 82(3) . . . . ? O2 N2 Ni2 P4 -80(3) . . . . ? C10 C9 P1 C1 147.5(4) . . . . ? C10 C9 P1 C5 -92.7(4) . . . . ? C10 C9 P1 Ni1 32.5(4) . . . . ? C3 C1 P1 C9 168.7(4) . . . . ? C4 C1 P1 C9 44.0(5) . . . . ? C2 C1 P1 C9 -75.2(5) . . . . ? C3 C1 P1 C5 51.2(5) . . . . ? C4 C1 P1 C5 -73.5(5) . . . . ? C2 C1 P1 C5 167.3(4) . . . . ? C3 C1 P1 Ni1 -80.9(4) . . . . ? C4 C1 P1 Ni1 154.4(4) . . . . ? C2 C1 P1 Ni1 35.2(5) . . . . ? C7 C5 P1 C9 -77.4(5) . . . . ? C8 C5 P1 C9 42.3(5) . . . . ? C6 C5 P1 C9 158.4(4) . . . . ? C7 C5 P1 C1 38.7(5) . . . . ? C8 C5 P1 C1 158.4(4) . . . . ? C6 C5 P1 C1 -85.5(5) . . . . ? C7 C5 P1 Ni1 166.6(4) . . . . ? C8 C5 P1 Ni1 -73.7(4) . . . . ? C6 C5 P1 Ni1 42.4(4) . . . . ? N1 Ni1 P1 C9 169.9(4) . . . . ? P2 Ni1 P1 C9 -9.91(19) . . . . ? N1 Ni1 P1 C1 57.5(4) . . . . ? P2 Ni1 P1 C1 -122.2(2) . . . . ? N1 Ni1 P1 C5 -71.4(4) . . . . ? P2 Ni1 P1 C5 108.8(2) . . . . ? C9 C10 P2 C15 -94.0(4) . . . . ? C9 C10 P2 C11 146.9(4) . . . . ? C9 C10 P2 Ni1 31.5(4) . . . . ? C18 C15 P2 C10 47.9(5) . . . . ? C16 C15 P2 C10 -72.1(5) . . . . ? C17 C15 P2 C10 165.8(4) . . . . ? C18 C15 P2 C11 162.0(4) . . . . ? C16 C15 P2 C11 41.9(5) . . . . ? C17 C15 P2 C11 -80.2(5) . . . . ? C18 C15 P2 Ni1 -68.1(4) . . . . ? C16 C15 P2 Ni1 171.8(3) . . . . ? C17 C15 P2 Ni1 49.7(4) . . . . ? C14 C11 P2 C10 171.1(4) . . . . ? C13 C11 P2 C10 46.5(5) . . . . ? C12 C11 P2 C10 -72.4(5) . . . . ? C14 C11 P2 C15 56.7(5) . . . . ? C13 C11 P2 C15 -67.9(5) . . . . ? C12 C11 P2 C15 173.3(4) . . . . ? C14 C11 P2 Ni1 -77.5(4) . . . . ? C13 C11 P2 Ni1 158.0(4) . . . . ? C12 C11 P2 Ni1 39.1(4) . . . . ? N1 Ni1 P2 C10 171.1(3) . . . . ? P1 Ni1 P2 C10 -9.1(2) . . . . ? N1 Ni1 P2 C15 -72.1(4) . . . . ? P1 Ni1 P2 C15 107.7(2) . . . . ? N1 Ni1 P2 C11 59.0(4) . . . . ? P1 Ni1 P2 C11 -121.2(2) . . . . ? C28 C27 P3 C23 -92.3(5) . . . . ? C28 C27 P3 C19 148.8(5) . . . . ? C28 C27 P3 Ni2 28.5(5) . . . . ? C25 C23 P3 C27 -74.1(5) . . . . ? C24 C23 P3 C27 162.2(4) . . . . ? C26 C23 P3 C27 44.8(6) . . . . ? C25 C23 P3 C19 40.5(6) . . . . ? C24 C23 P3 C19 -83.1(5) . . . . ? C26 C23 P3 C19 159.4(5) . . . . ? C25 C23 P3 Ni2 171.9(4) . . . . ? C24 C23 P3 Ni2 48.2(5) . . . . ? C26 C23 P3 Ni2 -69.2(6) . . . . ? C22 C19 P3 C27 46.6(6) . . . . ? C21 C19 P3 C27 171.9(5) . . . . ? C20 C19 P3 C27 -73.9(5) . . . . ? C22 C19 P3 C23 -69.8(6) . . . . ? C21 C19 P3 C23 55.5(5) . . . . ? C20 C19 P3 C23 169.7(4) . . . . ? C22 C19 P3 Ni2 159.3(5) . . . . ? C21 C19 P3 Ni2 -75.5(5) . . . . ? C20 C19 P3 Ni2 38.7(5) . . . . ? N2 Ni2 P3 C27 -174.8(3) . . . . ? P4 Ni2 P3 C27 -7.7(2) . . . . ? N2 Ni2 P3 C23 -58.2(3) . . . . ? P4 Ni2 P3 C23 108.9(2) . . . . ? N2 Ni2 P3 C19 71.6(3) . . . . ? P4 Ni2 P3 C19 -121.3(2) . . . . ? C27 C28 P4 C29 147.3(5) . . . . ? C27 C28 P4 C33 -93.0(5) . . . . ? C27 C28 P4 Ni2 29.5(5) . . . . ? C30 C29 P4 C28 -75.2(4) . . . . ? C31 C29 P4 C28 44.4(5) . . . . ? C32 C29 P4 C28 167.7(4) . . . . ? C30 C29 P4 C33 167.7(4) . . . . ? C31 C29 P4 C33 -72.6(5) . . . . ? C32 C29 P4 C33 50.7(5) . . . . ? C30 C29 P4 Ni2 36.1(4) . . . . ? C31 C29 P4 Ni2 155.8(4) . . . . ? C32 C29 P4 Ni2 -80.9(4) . . . . ? C34 C33 P4 C28 -73.8(6) . . . . ? C36 C33 P4 C28 47.1(6) . . . . ? C35 C33 P4 C28 162.9(4) . . . . ? C34 C33 P4 C29 41.8(6) . . . . ? C36 C33 P4 C29 162.6(5) . . . . ? C35 C33 P4 C29 -81.6(5) . . . . ? C34 C33 P4 Ni2 171.7(5) . . . . ? C36 C33 P4 Ni2 -67.4(6) . . . . ? C35 C33 P4 Ni2 48.3(5) . . . . ? N2 Ni2 P4 C28 157.2(3) . . . . ? P3 Ni2 P4 C28 -9.6(2) . . . . ? N2 Ni2 P4 C29 44.3(3) . . . . ? P3 Ni2 P4 C29 -122.5(2) . . . . ? N2 Ni2 P4 C33 -85.4(4) . . . . ? P3 Ni2 P4 C33 107.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.726 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.119