# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jarl Ivar van der Vlugt' _publ_contact_author_email J.I.V.D.VLUGT@TUE.NL _publ_section_title ; Cationic and Neutral NiII Complexes Containing a Non-Innocent PNP Ligand: Formation of Alkyl and Thiolate Species ; loop_ _publ_author_name 'J.I.van der Vlugt' 'Martin Lutz' 'Evgeny Pidko' 'A. Spek' 'Dieter Vogt' # Attachment 'JIvdV_DT_25082008_xtal_deposit.cif' data_s4049a _database_code_depnum_ccdc_archive 'CCDC 699865' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H46 N2 Ni P2, 2(B F4), C2 H3 N' _chemical_formula_sum 'C27 H49 B2 F8 N3 Ni P2' _chemical_formula_weight 709.96 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.8057(1) _cell_length_b 15.4958(2) _cell_length_c 20.2129(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.5118(8) _cell_angle_gamma 90.00 _cell_volume 3415.96(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 47572 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37081 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7806 _reflns_number_gt 5653 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, Sortav' _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^)+(0.0485P)^2^+0.3038P] 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 7806 _refine_ls_number_parameters 439 _refine_ls_number_restraints 285 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.334 _refine_ls_shift/su_max 0.009 _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 0.29119(3) 0.29646(2) 0.469266(15) 0.02276(10) Uani 1 1 d . . . P1 P 0.15677(6) 0.37100(4) 0.37892(3) 0.02510(15) Uani 1 1 d . . . P2 P 0.42876(5) 0.23475(4) 0.56650(3) 0.02277(15) Uani 1 1 d . . . N1 N 0.29256(16) 0.39157(12) 0.52992(10) 0.0216(4) Uani 1 1 d . . . N2 N 0.29334(18) 0.20719(14) 0.40960(11) 0.0283(5) Uani 1 1 d . . . C1 C 0.2388(2) 0.46839(15) 0.50228(12) 0.0234(5) Uani 1 1 d . . . C2 C 0.2555(2) 0.54162(16) 0.54384(13) 0.0267(5) Uani 1 1 d . . . H2 H 0.2183 0.5945 0.5227 0.032 Uiso 1 1 calc R . . C3 C 0.3262(2) 0.53781(17) 0.61586(13) 0.0302(6) Uani 1 1 d . . . H3 H 0.3404 0.5882 0.6447 0.036 Uiso 1 1 calc R . . C4 C 0.3762(2) 0.45967(17) 0.64554(13) 0.0294(6) Uani 1 1 d . . . H4 H 0.4235 0.4555 0.6955 0.035 Uiso 1 1 calc R . . C5 C 0.3573(2) 0.38759(16) 0.60250(12) 0.0235(5) Uani 1 1 d . . . C6 C 0.1593(2) 0.47237(17) 0.42479(13) 0.0343(6) Uani 1 1 d . . . H6A H 0.1894 0.5187 0.4019 0.041 Uiso 1 1 calc R . . H6B H 0.0747 0.4873 0.4195 0.041 Uiso 1 1 calc R . . C7 C -0.0019(2) 0.32850(18) 0.35130(13) 0.0318(6) Uani 1 1 d . . . C8 C -0.0256(3) 0.3239(2) 0.42088(15) 0.0519(8) Uani 1 1 d . . . H8A H -0.0251 0.3823 0.4396 0.078 Uiso 1 1 calc R . . H8B H 0.0387 0.2893 0.4563 0.078 Uiso 1 1 calc R . . H8C H -0.1056 0.2971 0.4111 0.078 Uiso 1 1 calc R . . C9 C -0.0130(2) 0.23749(19) 0.31976(16) 0.0425(7) Uani 1 1 d . . . H9A H -0.0961 0.2156 0.3085 0.064 Uiso 1 1 calc R . . H9B H 0.0463 0.1993 0.3547 0.064 Uiso 1 1 calc R . . H9C H 0.0040 0.2394 0.2759 0.064 Uiso 1 1 calc R . . C10 C -0.0966(2) 0.3881(2) 0.29848(14) 0.0404(7) Uani 1 1 d . . . H10A H -0.0858 0.3879 0.2528 0.061 Uiso 1 1 calc R . . H10B H -0.0856 0.4469 0.3178 0.061 Uiso 1 1 calc R . . H10C H -0.1793 0.3678 0.2909 0.061 Uiso 1 1 calc R . . C11 C 0.2057(2) 0.40210(18) 0.30433(13) 0.0324(6) Uani 1 1 d . . . C12 C 0.1788(3) 0.3311(2) 0.24834(15) 0.0466(8) Uani 1 1 d . . . H12A H 0.0899 0.3232 0.2246 0.070 Uiso 1 1 calc R . . H12B H 0.2165 0.2771 0.2716 0.070 Uiso 1 1 calc R . . H12C H 0.2125 0.3473 0.2127 0.070 Uiso 1 1 calc R . . C13 C 0.1440(3) 0.4856(2) 0.26618(15) 0.0458(7) Uani 1 1 d . . . H13A H 0.1744 0.4997 0.2287 0.069 Uiso 1 1 calc R . . H13B H 0.1634 0.5328 0.3010 0.069 Uiso 1 1 calc R . . H13C H 0.0550 0.4772 0.2446 0.069 Uiso 1 1 calc R . . C14 C 0.3444(3) 0.4161(2) 0.33981(16) 0.0469(8) Uani 1 1 d . . . H14A H 0.3854 0.3604 0.3554 0.070 Uiso 1 1 calc R . . H14B H 0.3629 0.4542 0.3814 0.070 Uiso 1 1 calc R . . H14C H 0.3739 0.4427 0.3053 0.070 Uiso 1 1 calc R . . C15 C 0.4042(2) 0.30140(15) 0.63340(12) 0.0259(5) Uani 1 1 d . . . H15A H 0.3443 0.2732 0.6498 0.031 Uiso 1 1 calc R . . H15B H 0.4823 0.3083 0.6753 0.031 Uiso 1 1 calc R . . C16 C 0.4011(2) 0.12267(16) 0.58997(13) 0.0277(5) Uani 1 1 d . . . C17 C 0.2616(2) 0.11317(18) 0.56563(15) 0.0355(6) Uani 1 1 d . . . H17A H 0.2233 0.1188 0.5134 0.053 Uiso 1 1 calc R . . H17B H 0.2301 0.1583 0.5880 0.053 Uiso 1 1 calc R . . H17C H 0.2423 0.0564 0.5799 0.053 Uiso 1 1 calc R . . C18 C 0.4470(3) 0.05577(17) 0.55047(14) 0.0345(6) Uani 1 1 d . . . H18A H 0.4256 -0.0022 0.5612 0.052 Uiso 1 1 calc R . . H18B H 0.5363 0.0605 0.5661 0.052 Uiso 1 1 calc R . . H18C H 0.4086 0.0662 0.4988 0.052 Uiso 1 1 calc R . . C19 C 0.4609(3) 0.10606(18) 0.67094(13) 0.0369(6) Uani 1 1 d . . . H19A H 0.4399 0.0479 0.6814 0.055 Uiso 1 1 calc R . . H19B H 0.4310 0.1486 0.6963 0.055 Uiso 1 1 calc R . . H19C H 0.5502 0.1111 0.6868 0.055 Uiso 1 1 calc R . . C20 C 0.5881(2) 0.25578(17) 0.57286(13) 0.0289(6) Uani 1 1 d . . . C21 C 0.6037(2) 0.2222(2) 0.50548(15) 0.0393(7) Uani 1 1 d . . . H21A H 0.5425 0.2494 0.4630 0.059 Uiso 1 1 calc R . . H21B H 0.5923 0.1595 0.5024 0.059 Uiso 1 1 calc R . . H21C H 0.6861 0.2363 0.5080 0.059 Uiso 1 1 calc R . . C22 C 0.6052(2) 0.35355(18) 0.57574(16) 0.0397(7) Uani 1 1 d . . . H22A H 0.6852 0.3675 0.5742 0.060 Uiso 1 1 calc R . . H22B H 0.6015 0.3759 0.6202 0.060 Uiso 1 1 calc R . . H22C H 0.5401 0.3800 0.5346 0.060 Uiso 1 1 calc R . . C23 C 0.6860(2) 0.2169(2) 0.64005(15) 0.0397(7) Uani 1 1 d . . . H23A H 0.7674 0.2354 0.6434 0.060 Uiso 1 1 calc R . . H23B H 0.6809 0.1538 0.6373 0.060 Uiso 1 1 calc R . . H23C H 0.6725 0.2366 0.6825 0.060 Uiso 1 1 calc R . . C24 C 0.2927(2) 0.15405(18) 0.37092(13) 0.0312(6) Uani 1 1 d . . . C25 C 0.2910(3) 0.08665(19) 0.32052(15) 0.0476(8) Uani 1 1 d . . . H25A H 0.2349 0.1031 0.2723 0.071 Uiso 1 1 calc R . . H25B H 0.2630 0.0325 0.3342 0.071 Uiso 1 1 calc R . . H25C H 0.3737 0.0789 0.3211 0.071 Uiso 1 1 calc R . . F1A F 0.6289(9) 0.1143(3) 0.3765(4) 0.073(2) Uani 0.529(14) 1 d PDU A 1 F2A F 0.6428(8) 0.1473(8) 0.2697(4) 0.094(3) Uani 0.529(14) 1 d PDU A 1 F3A F 0.6957(6) 0.2422(4) 0.3616(6) 0.089(2) Uani 0.529(14) 1 d PDU A 1 F4A F 0.5033(5) 0.2141(6) 0.3064(3) 0.066(2) Uani 0.529(14) 1 d PDU A 1 F1B F 0.7017(12) 0.1326(7) 0.3882(3) 0.117(4) Uani 0.471(14) 1 d PDU A 2 F2B F 0.6326(11) 0.1208(7) 0.2725(4) 0.092(4) Uani 0.471(14) 1 d PDU A 2 F3B F 0.6594(10) 0.2506(4) 0.3182(8) 0.103(3) Uani 0.471(14) 1 d PDU A 2 F4B F 0.5052(6) 0.1617(11) 0.3173(5) 0.121(4) Uani 0.471(14) 1 d PDU A 2 B1 B 0.6219(3) 0.1740(2) 0.32688(15) 0.0479(9) Uani 1 1 d D . . F12 F 0.06364(14) 0.08234(10) 0.07895(9) 0.0468(4) Uani 1 1 d D . . F22 F 0.11916(14) 0.21989(10) 0.11193(9) 0.0477(4) Uani 1 1 d D . . F32 F -0.07880(14) 0.17992(11) 0.07804(9) 0.0487(4) Uani 1 1 d D . . F42 F 0.05902(18) 0.13214(13) 0.18239(9) 0.0647(5) Uani 1 1 d D . . B2 B 0.0418(2) 0.15387(18) 0.11351(14) 0.0302(6) Uani 1 1 d D . . N3 N 0.8468(4) 0.4732(3) 0.09444(19) 0.0938(12) Uani 1 1 d U . . C26 C 0.8823(3) 0.4329(3) 0.0606(2) 0.0605(9) Uani 1 1 d U . . C27 C 0.9254(3) 0.3802(2) 0.0162(2) 0.0723(11) Uani 1 1 d U . . H27A H 0.8570 0.3673 -0.0290 0.109 Uiso 1 1 calc R . . H27B H 0.9591 0.3262 0.0412 0.109 Uiso 1 1 calc R . . H27C H 0.9894 0.4113 0.0062 0.109 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 0.02290(17) 0.02274(18) 0.02109(17) -0.00365(12) 0.00669(13) 0.00248(12) P1 0.0256(3) 0.0259(3) 0.0214(3) -0.0017(3) 0.0063(3) 0.0017(3) P2 0.0226(3) 0.0227(3) 0.0226(3) -0.0013(2) 0.0083(3) 0.0026(2) N1 0.0203(9) 0.0217(10) 0.0223(10) -0.0032(8) 0.0077(8) 0.0003(8) N2 0.0290(11) 0.0287(12) 0.0246(11) -0.0024(9) 0.0075(9) 0.0039(9) C1 0.0235(12) 0.0231(13) 0.0252(12) -0.0009(10) 0.0110(10) 0.0006(10) C2 0.0285(12) 0.0230(13) 0.0305(13) -0.0006(10) 0.0133(11) 0.0028(10) C3 0.0362(14) 0.0249(14) 0.0313(14) -0.0082(11) 0.0150(12) -0.0022(11) C4 0.0325(13) 0.0303(14) 0.0245(12) -0.0056(11) 0.0100(11) -0.0005(11) C5 0.0217(11) 0.0264(13) 0.0231(12) -0.0010(10) 0.0096(10) 0.0006(10) C6 0.0394(15) 0.0273(14) 0.0289(13) -0.0040(11) 0.0050(11) 0.0068(12) C7 0.0257(13) 0.0375(15) 0.0305(13) 0.0000(12) 0.0088(11) 0.0003(11) C8 0.0359(16) 0.083(3) 0.0399(17) 0.0104(17) 0.0185(14) 0.0037(16) C9 0.0311(15) 0.0366(17) 0.0585(19) -0.0030(14) 0.0158(14) -0.0059(12) C10 0.0277(14) 0.0480(18) 0.0361(15) -0.0029(13) 0.0019(12) 0.0047(13) C11 0.0369(14) 0.0313(15) 0.0319(14) -0.0001(11) 0.0163(12) -0.0046(12) C12 0.068(2) 0.0446(18) 0.0363(15) -0.0045(14) 0.0299(15) -0.0084(16) C13 0.0540(18) 0.0440(18) 0.0376(16) 0.0103(14) 0.0155(14) 0.0013(15) C14 0.0393(16) 0.051(2) 0.0528(18) 0.0078(15) 0.0201(14) -0.0054(14) C15 0.0283(13) 0.0267(13) 0.0217(12) -0.0022(10) 0.0083(10) 0.0032(10) C16 0.0332(13) 0.0227(13) 0.0292(13) -0.0004(10) 0.0141(11) 0.0034(11) C17 0.0373(15) 0.0286(15) 0.0443(16) -0.0043(12) 0.0197(13) -0.0050(12) C18 0.0440(15) 0.0260(14) 0.0342(14) 0.0002(11) 0.0157(12) 0.0087(12) C19 0.0505(17) 0.0284(15) 0.0348(14) 0.0056(12) 0.0196(13) 0.0070(13) C20 0.0225(12) 0.0323(15) 0.0317(13) -0.0003(11) 0.0101(11) 0.0016(11) C21 0.0307(14) 0.0504(19) 0.0421(16) -0.0038(14) 0.0198(13) -0.0005(13) C22 0.0332(14) 0.0371(17) 0.0519(17) -0.0045(13) 0.0196(13) -0.0062(12) C23 0.0246(13) 0.0517(19) 0.0379(16) 0.0005(13) 0.0065(12) 0.0041(12) C24 0.0326(14) 0.0319(15) 0.0260(13) -0.0007(12) 0.0077(11) 0.0045(11) C25 0.067(2) 0.0376(17) 0.0360(16) -0.0107(13) 0.0169(15) 0.0105(15) F1A 0.122(6) 0.042(3) 0.063(3) 0.010(2) 0.043(4) -0.014(3) F2A 0.059(4) 0.184(10) 0.045(4) 0.033(4) 0.029(3) 0.041(5) F3A 0.063(3) 0.055(3) 0.130(6) 0.017(4) 0.014(4) -0.024(3) F4A 0.042(3) 0.102(5) 0.061(3) 0.010(3) 0.026(2) 0.004(3) F1B 0.131(8) 0.150(8) 0.040(3) 0.022(4) -0.001(4) 0.006(6) F2B 0.120(7) 0.081(5) 0.039(4) -0.007(3) -0.008(4) 0.026(4) F3B 0.105(6) 0.045(4) 0.146(8) 0.009(4) 0.035(6) -0.009(3) F4B 0.070(4) 0.211(11) 0.091(5) -0.008(7) 0.041(4) -0.072(6) B1 0.042(2) 0.070(3) 0.0233(16) 0.0032(17) 0.0041(15) -0.0185(19) F12 0.0476(9) 0.0342(9) 0.0688(11) -0.0126(8) 0.0338(9) -0.0074(8) F22 0.0406(9) 0.0368(10) 0.0670(11) -0.0081(8) 0.0219(8) -0.0161(7) F32 0.0320(9) 0.0442(10) 0.0651(11) 0.0000(9) 0.0133(8) 0.0020(7) F42 0.0864(14) 0.0699(14) 0.0339(9) 0.0063(9) 0.0187(9) -0.0084(11) B2 0.0290(15) 0.0287(16) 0.0316(16) -0.0014(13) 0.0103(13) -0.0040(12) N3 0.119(3) 0.087(3) 0.069(2) 0.002(2) 0.028(2) 0.017(2) C26 0.051(2) 0.053(2) 0.066(2) 0.0183(19) 0.0093(18) 0.0048(17) C27 0.059(2) 0.057(2) 0.109(3) 0.018(2) 0.041(2) 0.0158(19) _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 N2 1.842(2) . ? Ni1 N1 1.9132(19) . ? Ni1 P1 2.2289(7) . ? Ni1 P2 2.2295(7) . ? P1 C6 1.818(3) . ? P1 C7 1.859(3) . ? P1 C11 1.872(3) . ? P2 C15 1.811(2) . ? P2 C16 1.862(3) . ? P2 C20 1.864(2) . ? N1 C1 1.364(3) . ? N1 C5 1.372(3) . ? N2 C24 1.133(3) . ? C1 C2 1.380(3) . ? C1 C6 1.487(3) . ? C2 C3 1.374(3) . ? C2 H2 0.9500 . ? C3 C4 1.380(4) . ? C3 H3 0.9500 . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C15 1.488(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C10 1.526(4) . ? C7 C9 1.533(4) . ? C7 C8 1.537(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.522(4) . ? C11 C14 1.532(4) . ? C11 C13 1.539(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.529(3) . ? C16 C17 1.534(3) . ? C16 C19 1.536(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.527(4) . ? C20 C23 1.530(4) . ? C20 C21 1.533(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.454(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? F1A B1 1.344(5) . ? F2A B1 1.335(6) . ? F3A B1 1.378(5) . ? F4A B1 1.440(5) . ? F1B B1 1.394(6) . ? F2B B1 1.419(6) . ? F3B B1 1.301(6) . ? F4B B1 1.330(6) . ? F12 B2 1.386(3) . ? F22 B2 1.380(3) . ? F32 B2 1.387(3) . ? F42 B2 1.370(3) . ? N3 C26 1.120(5) . ? C26 C27 1.442(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 177.93(9) . . ? N2 Ni1 P1 92.10(6) . . ? N1 Ni1 P1 87.40(6) . . ? N2 Ni1 P2 93.85(6) . . ? N1 Ni1 P2 86.61(6) . . ? P1 Ni1 P2 173.90(3) . . ? C6 P1 C7 106.10(13) . . ? C6 P1 C11 103.78(13) . . ? C7 P1 C11 115.81(11) . . ? C6 P1 Ni1 99.34(8) . . ? C7 P1 Ni1 112.47(9) . . ? C11 P1 Ni1 116.80(9) . . ? C15 P2 C16 104.35(11) . . ? C15 P2 C20 107.12(12) . . ? C16 P2 C20 114.60(11) . . ? C15 P2 Ni1 98.21(8) . . ? C16 P2 Ni1 119.02(8) . . ? C20 P2 Ni1 111.16(8) . . ? C1 N1 C5 117.30(19) . . ? C1 N1 Ni1 121.43(15) . . ? C5 N1 Ni1 121.01(16) . . ? C24 N2 Ni1 177.6(2) . . ? N1 C1 C2 122.2(2) . . ? N1 C1 C6 118.3(2) . . ? C2 C1 C6 119.5(2) . . ? C3 C2 C1 119.8(2) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 118.9(2) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 119.8(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 121.8(2) . . ? N1 C5 C15 117.0(2) . . ? C4 C5 C15 121.1(2) . . ? C1 C6 P1 112.45(18) . . ? C1 C6 H6A 109.1 . . ? P1 C6 H6A 109.1 . . ? C1 C6 H6B 109.1 . . ? P1 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C10 C7 C9 110.1(2) . . ? C10 C7 C8 109.1(2) . . ? C9 C7 C8 108.8(3) . . ? C10 C7 P1 112.33(19) . . ? C9 C7 P1 111.48(17) . . ? C8 C7 P1 104.91(18) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C14 109.4(2) . . ? C12 C11 C13 108.1(2) . . ? C14 C11 C13 109.4(2) . . ? C12 C11 P1 111.82(18) . . ? C14 C11 P1 105.29(18) . . ? C13 C11 P1 112.79(18) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C15 P2 109.79(16) . . ? C5 C15 H15A 109.7 . . ? P2 C15 H15A 109.7 . . ? C5 C15 H15B 109.7 . . ? P2 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C18 C16 C17 108.6(2) . . ? C18 C16 C19 109.4(2) . . ? C17 C16 C19 109.0(2) . . ? C18 C16 P2 111.56(17) . . ? C17 C16 P2 106.22(17) . . ? C19 C16 P2 111.95(18) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C23 108.2(2) . . ? C22 C20 C21 108.1(2) . . ? C23 C20 C21 110.4(2) . . ? C22 C20 P2 106.96(17) . . ? C23 C20 P2 113.07(18) . . ? C21 C20 P2 109.90(17) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 C25 179.2(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? F3B B1 F4B 119.9(7) . . ? F2A B1 F1A 117.0(6) . . ? F2A B1 F3A 112.8(6) . . ? F1A B1 F3A 107.6(4) . . ? F3B B1 F1B 113.0(5) . . ? F4B B1 F1B 111.9(5) . . ? F3B B1 F2B 106.8(6) . . ? F4B B1 F2B 101.5(7) . . ? F1B B1 F2B 101.0(6) . . ? F2A B1 F4A 111.5(5) . . ? F1A B1 F4A 106.7(4) . . ? F3A B1 F4A 99.9(4) . . ? F42 B2 F22 111.3(2) . . ? F42 B2 F12 109.4(2) . . ? F22 B2 F12 109.2(2) . . ? F42 B2 F32 108.7(2) . . ? F22 B2 F32 109.3(2) . . ? F12 B2 F32 108.9(2) . . ? N3 C26 C27 178.8(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? 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 N2 Ni1 P1 C6 -171.41(11) . . . . ? N1 Ni1 P1 C6 6.58(11) . . . . ? N2 Ni1 P1 C7 76.75(11) . . . . ? N1 Ni1 P1 C7 -105.26(11) . . . . ? N2 Ni1 P1 C11 -60.71(12) . . . . ? N1 Ni1 P1 C11 117.28(11) . . . . ? N2 Ni1 P2 C15 -165.04(10) . . . . ? N1 Ni1 P2 C15 16.98(10) . . . . ? N2 Ni1 P2 C16 -53.54(11) . . . . ? N1 Ni1 P2 C16 128.48(10) . . . . ? N2 Ni1 P2 C20 82.95(11) . . . . ? N1 Ni1 P2 C20 -95.04(10) . . . . ? P1 Ni1 N1 C1 -10.62(16) . . . . ? P2 Ni1 N1 C1 168.23(17) . . . . ? P1 Ni1 N1 C5 175.39(16) . . . . ? P2 Ni1 N1 C5 -5.76(16) . . . . ? C5 N1 C1 C2 4.9(3) . . . . ? Ni1 N1 C1 C2 -169.33(17) . . . . ? C5 N1 C1 C6 -174.9(2) . . . . ? Ni1 N1 C1 C6 10.9(3) . . . . ? N1 C1 C2 C3 -1.5(3) . . . . ? C6 C1 C2 C3 178.3(2) . . . . ? C1 C2 C3 C4 -1.9(4) . . . . ? C2 C3 C4 C5 1.7(4) . . . . ? C1 N1 C5 C4 -5.1(3) . . . . ? Ni1 N1 C5 C4 169.14(17) . . . . ? C1 N1 C5 C15 173.5(2) . . . . ? Ni1 N1 C5 C15 -12.3(3) . . . . ? C3 C4 C5 N1 1.9(4) . . . . ? C3 C4 C5 C15 -176.6(2) . . . . ? N1 C1 C6 P1 -3.6(3) . . . . ? C2 C1 C6 P1 176.63(18) . . . . ? C7 P1 C6 C1 113.38(19) . . . . ? C11 P1 C6 C1 -124.11(19) . . . . ? Ni1 P1 C6 C1 -3.4(2) . . . . ? C6 P1 C7 C10 62.8(2) . . . . ? C11 P1 C7 C10 -51.7(2) . . . . ? Ni1 P1 C7 C10 170.36(15) . . . . ? C6 P1 C7 C9 -173.16(19) . . . . ? C11 P1 C7 C9 72.3(2) . . . . ? Ni1 P1 C7 C9 -65.6(2) . . . . ? C6 P1 C7 C8 -55.6(2) . . . . ? C11 P1 C7 C8 -170.1(2) . . . . ? Ni1 P1 C7 C8 52.0(2) . . . . ? C6 P1 C11 C12 -165.5(2) . . . . ? C7 P1 C11 C12 -49.7(2) . . . . ? Ni1 P1 C11 C12 86.4(2) . . . . ? C6 P1 C11 C14 75.8(2) . . . . ? C7 P1 C11 C14 -168.37(19) . . . . ? Ni1 P1 C11 C14 -32.3(2) . . . . ? C6 P1 C11 C13 -43.4(2) . . . . ? C7 P1 C11 C13 72.4(2) . . . . ? Ni1 P1 C11 C13 -151.53(16) . . . . ? N1 C5 C15 P2 27.4(3) . . . . ? C4 C5 C15 P2 -153.97(19) . . . . ? C16 P2 C15 C5 -149.64(17) . . . . ? C20 P2 C15 C5 88.45(18) . . . . ? Ni1 P2 C15 C5 -26.77(17) . . . . ? C15 P2 C16 C18 -166.38(17) . . . . ? C20 P2 C16 C18 -49.5(2) . . . . ? Ni1 P2 C16 C18 85.52(18) . . . . ? C15 P2 C16 C17 75.44(18) . . . . ? C20 P2 C16 C17 -167.72(16) . . . . ? Ni1 P2 C16 C17 -32.65(18) . . . . ? C15 P2 C16 C19 -43.4(2) . . . . ? C20 P2 C16 C19 73.4(2) . . . . ? Ni1 P2 C16 C19 -151.48(14) . . . . ? C15 P2 C20 C22 -47.0(2) . . . . ? C16 P2 C20 C22 -162.23(17) . . . . ? Ni1 P2 C20 C22 59.25(18) . . . . ? C15 P2 C20 C23 72.1(2) . . . . ? C16 P2 C20 C23 -43.2(2) . . . . ? Ni1 P2 C20 C23 178.29(17) . . . . ? C15 P2 C20 C21 -164.15(18) . . . . ? C16 P2 C20 C21 80.6(2) . . . . ? Ni1 P2 C20 C21 -57.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.448 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.061 #===END data_s4096a _database_code_depnum_ccdc_archive 'CCDC 699866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H43 N4 Ni P2, B F4' _chemical_formula_sum 'C23 H43 B F4 N4 Ni P2' _chemical_formula_weight 583.07 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 14.9094(2) _cell_length_b 12.4818(2) _cell_length_c 15.5634(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.6351(6) _cell_angle_gamma 90.00 _cell_volume 2789.12(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37535 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'triangular prism' _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.826 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33661 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6389 _reflns_number_gt 4837 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, Sortav' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+1.3744P] 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 6389 _refine_ls_number_parameters 400 _refine_ls_number_restraints 291 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.271 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.74248(2) 0.35188(2) 0.21689(2) 0.02150(11) Uani 1 1 d . . . P1 P 0.75330(4) 0.52797(5) 0.22377(4) 0.02370(16) Uani 1 1 d . . . P2 P 0.73213(4) 0.17844(5) 0.18951(4) 0.02367(15) Uani 1 1 d . . . N1 N 0.84626(13) 0.35337(16) 0.16614(13) 0.0240(4) Uani 1 1 d . . . N2 N 0.65133(19) 0.34905(18) 0.28024(16) 0.0360(6) Uani 1 1 d . . . N3 N 0.5765(2) 0.35116(18) 0.26700(17) 0.0391(6) Uani 1 1 d . . . N4 N 0.4933(2) 0.3506(3) 0.2606(2) 0.0682(9) Uani 1 1 d . . . C1 C 0.88913(17) 0.4465(2) 0.15617(17) 0.0282(6) Uani 1 1 d . . . C2 C 0.95443(18) 0.4511(3) 0.10726(19) 0.0370(7) Uani 1 1 d . . . H2 H 0.9832 0.5173 0.1006 0.044 Uiso 1 1 calc R . . C3 C 0.97728(19) 0.3600(3) 0.06868(18) 0.0406(8) Uani 1 1 d . . . H3 H 1.0200 0.3631 0.0332 0.049 Uiso 1 1 calc R . . C4 C 0.93764(18) 0.2644(3) 0.08199(18) 0.0364(7) Uani 1 1 d . . . H4 H 0.9534 0.2004 0.0564 0.044 Uiso 1 1 calc R . . C5 C 0.87450(17) 0.2617(2) 0.13288(17) 0.0290(6) Uani 1 1 d . . . C6 C 0.86824(18) 0.5421(2) 0.20451(19) 0.0327(6) Uani 1 1 d . . . H6A H 0.8699 0.6074 0.1689 0.039 Uiso 1 1 calc R . . H6B H 0.9160 0.5495 0.2623 0.039 Uiso 1 1 calc R . . C7 C 0.66958(19) 0.5956(2) 0.12848(17) 0.0309(6) Uani 1 1 d . . . C8 C 0.6928(2) 0.5588(2) 0.04251(18) 0.0396(7) Uani 1 1 d . . . H8A H 0.6447 0.5846 -0.0095 0.059 Uiso 1 1 calc R . . H8B H 0.6951 0.4803 0.0412 0.059 Uiso 1 1 calc R . . H8C H 0.7534 0.5879 0.0411 0.059 Uiso 1 1 calc R . . C9 C 0.5707(2) 0.5582(3) 0.1246(2) 0.0419(7) Uani 1 1 d . . . H9A H 0.5565 0.5758 0.1808 0.063 Uiso 1 1 calc R . . H9B H 0.5663 0.4805 0.1152 0.063 Uiso 1 1 calc R . . H9C H 0.5261 0.5942 0.0751 0.063 Uiso 1 1 calc R . . C10 C 0.6747(2) 0.7175(2) 0.1329(2) 0.0428(7) Uani 1 1 d . . . H10A H 0.6353 0.7477 0.0773 0.064 Uiso 1 1 calc R . . H10B H 0.7392 0.7405 0.1408 0.064 Uiso 1 1 calc R . . H10C H 0.6528 0.7427 0.1833 0.064 Uiso 1 1 calc R . . C11 C 0.76378(19) 0.5920(2) 0.33421(17) 0.0312(6) Uani 1 1 d . . . C12 C 0.8165(2) 0.6986(2) 0.3426(2) 0.0442(8) Uani 1 1 d . . . H12A H 0.7800 0.7501 0.2997 0.066 Uiso 1 1 calc R . . H12B H 0.8769 0.6871 0.3303 0.066 Uiso 1 1 calc R . . H12C H 0.8264 0.7267 0.4032 0.066 Uiso 1 1 calc R . . C13 C 0.6690(2) 0.6100(2) 0.3514(2) 0.0407(7) Uani 1 1 d . . . H13A H 0.6777 0.6351 0.4128 0.061 Uiso 1 1 calc R . . H13B H 0.6340 0.5426 0.3428 0.061 Uiso 1 1 calc R . . H13C H 0.6343 0.6640 0.3098 0.061 Uiso 1 1 calc R . . C14 C 0.8206(2) 0.5130(2) 0.40396(18) 0.0392(7) Uani 1 1 d . . . H14A H 0.8306 0.5436 0.4638 0.059 Uiso 1 1 calc R . . H14B H 0.8809 0.4997 0.3921 0.059 Uiso 1 1 calc R . . H14C H 0.7864 0.4453 0.4004 0.059 Uiso 1 1 calc R . . C15 C 0.84170(18) 0.1583(2) 0.1606(2) 0.0336(6) Uani 1 1 d . . . H15A H 0.8891 0.1293 0.2127 0.040 Uiso 1 1 calc R . . H15B H 0.8326 0.1058 0.1113 0.040 Uiso 1 1 calc R . . C16 C 0.63892(18) 0.1432(2) 0.08675(17) 0.0294(6) Uani 1 1 d . . . C17 C 0.6619(2) 0.2035(3) 0.00953(18) 0.0413(7) Uani 1 1 d . . . H17A H 0.6103 0.1956 -0.0445 0.062 Uiso 1 1 calc R . . H17B H 0.7188 0.1738 -0.0011 0.062 Uiso 1 1 calc R . . H17C H 0.6713 0.2796 0.0248 0.062 Uiso 1 1 calc R . . C18 C 0.6346(2) 0.0230(2) 0.0667(2) 0.0439(8) Uani 1 1 d . . . H18A H 0.5932 0.0103 0.0071 0.066 Uiso 1 1 calc R . . H18B H 0.6107 -0.0149 0.1111 0.066 Uiso 1 1 calc R . . H18C H 0.6972 -0.0033 0.0692 0.066 Uiso 1 1 calc R . . C19 C 0.54519(19) 0.1834(3) 0.0952(2) 0.0393(7) Uani 1 1 d . . . H19A H 0.5478 0.2613 0.1037 0.059 Uiso 1 1 calc R . . H19B H 0.5309 0.1492 0.1467 0.059 Uiso 1 1 calc R . . H19C H 0.4965 0.1657 0.0409 0.059 Uiso 1 1 calc R . . C20 C 0.7376(2) 0.0889(2) 0.28671(17) 0.0339(6) Uani 1 1 d . . . C21 C 0.6427(2) 0.0788(2) 0.3049(2) 0.0435(8) Uani 1 1 d . . . H21A H 0.5999 0.0411 0.2552 0.065 Uiso 1 1 calc R . . H21B H 0.6181 0.1503 0.3110 0.065 Uiso 1 1 calc R . . H21C H 0.6489 0.0383 0.3602 0.065 Uiso 1 1 calc R . . C22 C 0.7757(3) -0.0223(2) 0.2751(2) 0.0503(8) Uani 1 1 d . . . H22A H 0.7871 -0.0619 0.3313 0.075 Uiso 1 1 calc R . . H22B H 0.8342 -0.0150 0.2583 0.075 Uiso 1 1 calc R . . H22C H 0.7303 -0.0612 0.2282 0.075 Uiso 1 1 calc R . . C23 C 0.8046(2) 0.1447(2) 0.36655(19) 0.0442(8) Uani 1 1 d . . . H23A H 0.7788 0.2143 0.3766 0.066 Uiso 1 1 calc R . . H23B H 0.8650 0.1553 0.3541 0.066 Uiso 1 1 calc R . . H23C H 0.8128 0.1000 0.4199 0.066 Uiso 1 1 calc R . . F1A F 0.0245(9) 0.2739(10) 0.2914(5) 0.058(3) Uani 0.42 1 d PDU A 1 F2A F 0.0933(6) 0.2346(6) 0.4327(6) 0.061(3) Uani 0.42 1 d PDU A 1 F3A F -0.0115(6) 0.3610(7) 0.4048(6) 0.094(3) Uani 0.42 1 d PDU A 1 F4A F 0.1269(5) 0.3877(6) 0.3763(5) 0.0800(18) Uani 0.42 1 d PDU A 1 F1B F 0.1497(5) 0.3076(11) 0.4120(7) 0.071(3) Uani 0.28 1 d PDU A 2 F2B F 0.0087(8) 0.3263(12) 0.4362(7) 0.089(4) Uani 0.28 1 d PDU A 2 F3B F 0.0152(13) 0.2489(11) 0.3096(8) 0.076(6) Uani 0.28 1 d PDU A 2 F4B F 0.0477(11) 0.4242(6) 0.3384(8) 0.091(5) Uani 0.28 1 d PDU A 2 F1C F 0.1208(8) 0.2642(10) 0.4350(7) 0.054(4) Uani 0.30 1 d PDU A 3 F2C F -0.0305(6) 0.2905(12) 0.3774(9) 0.138(5) Uani 0.30 1 d PDU A 3 F3C F 0.0632(7) 0.2941(10) 0.2886(5) 0.059(3) Uani 0.30 1 d PDU A 3 F4C F 0.0577(10) 0.4298(5) 0.3751(7) 0.069(3) Uani 0.30 1 d PDU A 3 B1 B 0.0563(2) 0.3198(2) 0.37318(19) 0.0393(8) Uani 1 1 d 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 0.02140(17) 0.01930(18) 0.02541(18) -0.00294(12) 0.00910(13) -0.00239(12) P1 0.0252(3) 0.0188(3) 0.0270(3) -0.0014(2) 0.0069(3) -0.0031(3) P2 0.0255(3) 0.0199(3) 0.0249(3) -0.0040(2) 0.0056(3) -0.0006(3) N1 0.0187(10) 0.0296(12) 0.0233(11) -0.0007(8) 0.0052(8) 0.0005(9) N2 0.0517(16) 0.0286(13) 0.0399(14) -0.0091(10) 0.0333(13) -0.0128(12) N3 0.0513(17) 0.0212(13) 0.0420(15) -0.0014(10) 0.0080(13) 0.0068(12) N4 0.0387(16) 0.076(2) 0.097(3) 0.0142(18) 0.0311(17) 0.0090(15) C1 0.0204(12) 0.0360(16) 0.0272(13) 0.0056(11) 0.0044(10) -0.0033(11) C2 0.0235(13) 0.0522(19) 0.0360(16) 0.0129(13) 0.0095(12) -0.0043(13) C3 0.0230(14) 0.073(2) 0.0275(15) 0.0079(14) 0.0097(12) 0.0083(14) C4 0.0263(14) 0.054(2) 0.0298(15) -0.0037(13) 0.0081(12) 0.0083(13) C5 0.0198(12) 0.0377(16) 0.0282(14) -0.0067(11) 0.0042(10) 0.0030(11) C6 0.0264(14) 0.0304(15) 0.0408(16) 0.0019(12) 0.0081(12) -0.0078(12) C7 0.0334(14) 0.0296(15) 0.0273(14) -0.0010(11) 0.0040(11) 0.0026(12) C8 0.0504(18) 0.0398(18) 0.0274(15) 0.0016(12) 0.0082(13) 0.0053(14) C9 0.0322(15) 0.0495(19) 0.0391(17) -0.0008(14) 0.0012(13) 0.0001(14) C10 0.0536(19) 0.0297(16) 0.0396(17) 0.0064(13) 0.0034(14) 0.0056(14) C11 0.0397(16) 0.0257(14) 0.0262(14) -0.0050(10) 0.0055(12) -0.0035(12) C12 0.060(2) 0.0272(16) 0.0388(17) -0.0068(12) 0.0022(15) -0.0099(15) C13 0.0509(18) 0.0357(16) 0.0383(16) -0.0094(13) 0.0166(14) 0.0033(14) C14 0.0522(18) 0.0333(16) 0.0275(14) -0.0016(12) 0.0028(13) -0.0041(14) C15 0.0274(14) 0.0313(16) 0.0422(16) -0.0118(12) 0.0097(12) 0.0041(12) C16 0.0308(14) 0.0317(15) 0.0231(13) -0.0063(10) 0.0030(11) -0.0050(11) C17 0.0489(18) 0.0487(19) 0.0242(14) -0.0028(13) 0.0061(13) -0.0077(15) C18 0.0482(18) 0.0369(17) 0.0419(17) -0.0172(14) 0.0040(14) -0.0072(14) C19 0.0297(15) 0.0466(18) 0.0375(16) -0.0044(13) 0.0017(12) -0.0032(13) C20 0.0430(16) 0.0252(15) 0.0283(14) 0.0010(11) 0.0006(12) 0.0005(12) C21 0.059(2) 0.0364(17) 0.0376(16) 0.0081(13) 0.0178(15) -0.0098(15) C22 0.070(2) 0.0260(16) 0.0475(19) 0.0028(13) 0.0027(17) 0.0078(16) C23 0.056(2) 0.0383(18) 0.0284(15) 0.0012(12) -0.0055(14) 0.0032(15) F1A 0.069(7) 0.049(5) 0.034(4) -0.014(4) -0.025(4) 0.020(5) F2A 0.086(6) 0.059(4) 0.039(4) 0.002(3) 0.019(4) -0.009(4) F3A 0.087(5) 0.098(6) 0.116(6) -0.007(5) 0.058(5) 0.054(5) F4A 0.096(5) 0.064(4) 0.098(5) -0.008(3) 0.057(4) -0.039(4) F1B 0.042(5) 0.105(8) 0.061(6) -0.016(5) 0.006(4) 0.024(5) F2B 0.086(7) 0.131(9) 0.064(6) 0.017(6) 0.048(5) -0.022(7) F3B 0.070(8) 0.059(8) 0.075(9) -0.022(6) -0.021(6) 0.025(6) F4B 0.109(8) 0.075(7) 0.084(8) 0.020(5) 0.016(7) -0.029(6) F1C 0.044(6) 0.078(8) 0.030(5) -0.009(5) -0.008(4) 0.021(6) F2C 0.115(8) 0.173(10) 0.142(9) 0.024(8) 0.063(7) -0.062(7) F3C 0.068(7) 0.069(6) 0.036(4) -0.006(4) 0.008(4) 0.018(5) F4C 0.111(8) 0.040(5) 0.052(6) -0.019(3) 0.017(5) -0.008(5) B1 0.0403(19) 0.043(2) 0.0354(18) -0.0049(15) 0.0109(15) 0.0035(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 N2 1.882(2) . ? Ni1 N1 1.918(2) . ? Ni1 P2 2.2037(7) . ? Ni1 P1 2.2043(7) . ? P1 C6 1.826(3) . ? P1 C7 1.863(3) . ? P1 C11 1.864(3) . ? P2 C15 1.825(3) . ? P2 C20 1.865(3) . ? P2 C16 1.867(3) . ? N1 C1 1.356(3) . ? N1 C5 1.368(3) . ? N2 N3 1.078(3) . ? N3 N4 1.218(4) . ? C1 C2 1.389(4) . ? C1 C6 1.488(4) . ? C2 C3 1.371(4) . ? C2 H2 0.9500 . ? C3 C4 1.372(4) . ? C3 H3 0.9500 . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 C15 1.485(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C10 1.524(4) . ? C7 C9 1.532(4) . ? C7 C8 1.540(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.525(4) . ? C11 C12 1.533(4) . ? C11 C14 1.541(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C19 1.524(4) . ? C16 C18 1.530(4) . ? C16 C17 1.533(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.521(4) . ? C20 C22 1.529(4) . ? C20 C23 1.536(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? F1A B1 1.359(6) . ? F2A B1 1.421(6) . ? F3A B1 1.340(6) . ? F4A B1 1.341(5) . ? F1B B1 1.369(6) . ? F2B B1 1.359(7) . ? F3B B1 1.346(7) . ? F4B B1 1.403(7) . ? F1C B1 1.354(6) . ? F2C B1 1.364(7) . ? F3C B1 1.385(7) . ? F4C B1 1.372(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 N2 Ni1 N1 173.05(10) . . ? N2 Ni1 P2 93.45(7) . . ? N1 Ni1 P2 87.25(6) . . ? N2 Ni1 P1 92.69(7) . . ? N1 Ni1 P1 87.35(6) . . ? P2 Ni1 P1 171.60(3) . . ? C6 P1 C7 106.41(13) . . ? C6 P1 C11 105.11(13) . . ? C7 P1 C11 114.28(12) . . ? C6 P1 Ni1 98.51(9) . . ? C7 P1 Ni1 112.87(9) . . ? C11 P1 Ni1 117.35(9) . . ? C15 P2 C20 105.75(13) . . ? C15 P2 C16 105.40(13) . . ? C20 P2 C16 114.43(12) . . ? C15 P2 Ni1 99.34(9) . . ? C20 P2 Ni1 116.51(9) . . ? C16 P2 Ni1 113.21(9) . . ? C1 N1 C5 118.1(2) . . ? C1 N1 Ni1 120.87(17) . . ? C5 N1 Ni1 120.85(17) . . ? N3 N2 Ni1 139.0(3) . . ? N2 N3 N4 173.6(3) . . ? N1 C1 C2 121.3(3) . . ? N1 C1 C6 117.4(2) . . ? C2 C1 C6 121.1(2) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C15 117.2(2) . . ? C4 C5 C15 121.0(2) . . ? C1 C6 P1 109.83(18) . . ? C1 C6 H6A 109.7 . . ? P1 C6 H6A 109.7 . . ? C1 C6 H6B 109.7 . . ? P1 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C10 C7 C9 110.0(2) . . ? C10 C7 C8 108.5(2) . . ? C9 C7 C8 108.3(2) . . ? C10 C7 P1 113.71(19) . . ? C9 C7 P1 108.92(19) . . ? C8 C7 P1 107.26(19) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 109.6(2) . . ? C13 C11 C14 109.3(2) . . ? C12 C11 C14 108.9(2) . . ? C13 C11 P1 111.97(18) . . ? C12 C11 P1 111.39(19) . . ? C14 C11 P1 105.58(18) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C15 P2 109.80(18) . . ? C5 C15 H15A 109.7 . . ? P2 C15 H15A 109.7 . . ? C5 C15 H15B 109.7 . . ? P2 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C19 C16 C18 110.6(2) . . ? C19 C16 C17 108.1(2) . . ? C18 C16 C17 109.1(2) . . ? C19 C16 P2 109.67(18) . . ? C18 C16 P2 112.71(19) . . ? C17 C16 P2 106.50(18) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 109.9(3) . . ? C21 C20 C23 108.8(2) . . ? C22 C20 C23 109.0(2) . . ? C21 C20 P2 111.20(19) . . ? C22 C20 P2 112.6(2) . . ? C23 C20 P2 105.1(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? F3A B1 F4A 113.9(6) . . ? F3A B1 F1A 113.5(7) . . ? F4A B1 F1A 111.9(7) . . ? F3B B1 F2B 110.3(9) . . ? F1C B1 F2C 109.2(8) . . ? F3B B1 F1B 117.3(9) . . ? F2B B1 F1B 110.8(7) . . ? F1C B1 F4C 119.6(7) . . ? F2C B1 F4C 106.0(8) . . ? F1C B1 F3C 109.6(7) . . ? F2C B1 F3C 107.4(7) . . ? F4C B1 F3C 104.3(7) . . ? F3B B1 F4B 110.5(8) . . ? F2B B1 F4B 102.3(8) . . ? F1B B1 F4B 104.5(7) . . ? F3A B1 F2A 104.2(6) . . ? F4A B1 F2A 106.7(5) . . ? F1A B1 F2A 105.7(6) . . ? 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 N2 Ni1 P1 C6 159.10(13) . . . . ? N1 Ni1 P1 C6 -13.95(11) . . . . ? N2 Ni1 P1 C7 -88.99(13) . . . . ? N1 Ni1 P1 C7 97.97(11) . . . . ? N2 Ni1 P1 C11 47.12(13) . . . . ? N1 Ni1 P1 C11 -125.92(12) . . . . ? N2 Ni1 P2 C15 -162.15(13) . . . . ? N1 Ni1 P2 C15 10.93(11) . . . . ? N2 Ni1 P2 C20 -49.23(14) . . . . ? N1 Ni1 P2 C20 123.84(12) . . . . ? N2 Ni1 P2 C16 86.54(13) . . . . ? N1 Ni1 P2 C16 -100.38(11) . . . . ? P2 Ni1 N1 C1 176.29(18) . . . . ? P1 Ni1 N1 C1 2.73(18) . . . . ? P2 Ni1 N1 C5 1.29(18) . . . . ? P1 Ni1 N1 C5 -172.27(19) . . . . ? P2 Ni1 N2 N3 -83.6(3) . . . . ? P1 Ni1 N2 N3 90.7(3) . . . . ? C5 N1 C1 C2 5.3(4) . . . . ? Ni1 N1 C1 C2 -169.86(19) . . . . ? C5 N1 C1 C6 -170.8(2) . . . . ? Ni1 N1 C1 C6 14.1(3) . . . . ? N1 C1 C2 C3 -0.6(4) . . . . ? C6 C1 C2 C3 175.3(3) . . . . ? C1 C2 C3 C4 -2.5(4) . . . . ? C2 C3 C4 C5 0.9(4) . . . . ? C1 N1 C5 C4 -6.9(4) . . . . ? Ni1 N1 C5 C4 168.20(19) . . . . ? C1 N1 C5 C15 167.4(2) . . . . ? Ni1 N1 C5 C15 -17.4(3) . . . . ? C3 C4 C5 N1 3.9(4) . . . . ? C3 C4 C5 C15 -170.2(3) . . . . ? N1 C1 C6 P1 -26.1(3) . . . . ? C2 C1 C6 P1 157.9(2) . . . . ? C7 P1 C6 C1 -93.3(2) . . . . ? C11 P1 C6 C1 145.14(19) . . . . ? Ni1 P1 C6 C1 23.70(19) . . . . ? C6 P1 C7 C10 -74.1(2) . . . . ? C11 P1 C7 C10 41.4(2) . . . . ? Ni1 P1 C7 C10 178.91(18) . . . . ? C6 P1 C7 C9 162.80(19) . . . . ? C11 P1 C7 C9 -81.7(2) . . . . ? Ni1 P1 C7 C9 55.8(2) . . . . ? C6 P1 C7 C8 45.8(2) . . . . ? C11 P1 C7 C8 161.36(19) . . . . ? Ni1 P1 C7 C8 -61.1(2) . . . . ? C6 P1 C11 C13 167.1(2) . . . . ? C7 P1 C11 C13 50.8(2) . . . . ? Ni1 P1 C11 C13 -84.7(2) . . . . ? C6 P1 C11 C12 43.9(2) . . . . ? C7 P1 C11 C12 -72.4(2) . . . . ? Ni1 P1 C11 C12 152.13(18) . . . . ? C6 P1 C11 C14 -74.1(2) . . . . ? C7 P1 C11 C14 169.60(18) . . . . ? Ni1 P1 C11 C14 34.1(2) . . . . ? N1 C5 C15 P2 26.2(3) . . . . ? C4 C5 C15 P2 -159.5(2) . . . . ? C20 P2 C15 C5 -142.54(19) . . . . ? C16 P2 C15 C5 95.9(2) . . . . ? Ni1 P2 C15 C5 -21.5(2) . . . . ? C15 P2 C16 C19 -165.8(2) . . . . ? C20 P2 C16 C19 78.4(2) . . . . ? Ni1 P2 C16 C19 -58.3(2) . . . . ? C15 P2 C16 C18 70.5(2) . . . . ? C20 P2 C16 C18 -45.2(2) . . . . ? Ni1 P2 C16 C18 178.07(17) . . . . ? C15 P2 C16 C17 -49.1(2) . . . . ? C20 P2 C16 C17 -164.83(19) . . . . ? Ni1 P2 C16 C17 58.4(2) . . . . ? C15 P2 C20 C21 -167.4(2) . . . . ? C16 P2 C20 C21 -51.8(2) . . . . ? Ni1 P2 C20 C21 83.4(2) . . . . ? C15 P2 C20 C22 -43.5(2) . . . . ? C16 P2 C20 C22 72.0(2) . . . . ? Ni1 P2 C20 C22 -152.70(19) . . . . ? C15 P2 C20 C23 75.0(2) . . . . ? C16 P2 C20 C23 -169.42(19) . . . . ? Ni1 P2 C20 C23 -34.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.687 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.063 #===END data_s4098a _database_code_depnum_ccdc_archive 'CCDC 699867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H50 N Ni P2 S, B F4' _chemical_formula_sum 'C30 H50 B F4 N Ni P2 S' _chemical_formula_weight 664.23 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7077(2) _cell_length_b 11.0192(3) _cell_length_c 17.2498(4) _cell_angle_alpha 94.763(1) _cell_angle_beta 90.893(2) _cell_angle_gamma 101.983(1) _cell_volume 1612.58(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21908 _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.810 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26222 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0078 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.45 _reflns_number_total 7366 _reflns_number_gt 6765 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement Peakref _computing_data_reduction 'Pixel15, Twinabs' _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^)+(0.0641P)^2^+1.7924P] 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 7366 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.005 _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 0.27776(3) 0.85839(2) 0.264176(15) 0.01382(9) Uani 1 1 d . . . S1 S 0.31429(8) 0.76625(6) 0.14915(4) 0.02754(15) Uani 1 1 d . . . P1 P 0.22027(7) 1.01307(5) 0.20369(3) 0.01573(13) Uani 1 1 d . . . P2 P 0.30112(6) 0.70763(5) 0.34043(3) 0.01386(12) Uani 1 1 d . . . N1 N 0.2761(2) 0.96437(17) 0.36147(11) 0.0159(4) Uani 1 1 d . . . C1 C 0.2382(3) 1.0778(2) 0.36047(13) 0.0193(4) Uani 1 1 d . . . C2 C 0.1969(3) 1.1404(2) 0.42736(15) 0.0256(5) Uani 1 1 d . . . H2 H 0.1652 1.2174 0.4247 0.031 Uiso 1 1 calc R . . C3 C 0.2021(3) 1.0901(2) 0.49776(14) 0.0256(5) Uani 1 1 d . . . H3 H 0.1696 1.1301 0.5437 0.031 Uiso 1 1 calc R . . C4 C 0.2551(3) 0.9810(2) 0.50040(14) 0.0225(5) Uani 1 1 d . . . H4 H 0.2662 0.9475 0.5487 0.027 Uiso 1 1 calc R . . C5 C 0.2923(3) 0.9206(2) 0.43157(13) 0.0174(4) Uani 1 1 d . . . C6 C 0.2529(3) 1.1350(2) 0.28486(13) 0.0209(5) Uani 1 1 d . . . H6A H 0.3590 1.1882 0.2822 0.025 Uiso 1 1 calc R . . H6B H 0.1748 1.1882 0.2810 0.025 Uiso 1 1 calc R . . C7 C 0.3472(3) 1.0867(2) 0.12619(13) 0.0207(4) Uani 1 1 d . . . C8 C 0.2959(3) 1.0256(3) 0.04433(14) 0.0293(5) Uani 1 1 d . . . H8A H 0.1933 1.0423 0.0301 0.044 Uiso 1 1 calc R . . H8B H 0.2882 0.9355 0.0434 0.044 Uiso 1 1 calc R . . H8C H 0.3734 1.0600 0.0070 0.044 Uiso 1 1 calc R . . C9 C 0.3510(3) 1.2270(2) 0.12711(17) 0.0307(6) Uani 1 1 d . . . H9A H 0.4175 1.2617 0.0856 0.046 Uiso 1 1 calc R . . H9B H 0.3938 1.2688 0.1776 0.046 Uiso 1 1 calc R . . H9C H 0.2442 1.2399 0.1188 0.046 Uiso 1 1 calc R . . C10 C 0.5142(3) 1.0706(2) 0.14534(15) 0.0245(5) Uani 1 1 d . . . H10A H 0.5182 0.9822 0.1376 0.037 Uiso 1 1 calc R . . H10B H 0.5430 1.1015 0.1997 0.037 Uiso 1 1 calc R . . H10C H 0.5881 1.1179 0.1110 0.037 Uiso 1 1 calc R . . C11 C 0.0052(3) 0.9891(2) 0.17960(16) 0.0255(5) Uani 1 1 d . . . C12 C -0.0802(3) 0.9649(3) 0.25585(19) 0.0357(6) Uani 1 1 d . . . H12A H -0.0526 1.0395 0.2925 0.053 Uiso 1 1 calc R . . H12B H -0.0484 0.8948 0.2785 0.053 Uiso 1 1 calc R . . H12C H -0.1939 0.9450 0.2452 0.053 Uiso 1 1 calc R . . C13 C -0.0490(4) 0.8737(3) 0.1219(2) 0.0397(7) Uani 1 1 d . . . H13A H -0.1622 0.8617 0.1110 0.060 Uiso 1 1 calc R . . H13B H -0.0266 0.8003 0.1446 0.060 Uiso 1 1 calc R . . H13C H 0.0073 0.8855 0.0735 0.060 Uiso 1 1 calc R . . C14 C -0.0394(3) 1.1026(3) 0.14733(18) 0.0330(6) Uani 1 1 d . . . H14A H -0.1539 1.0885 0.1407 0.050 Uiso 1 1 calc R . . H14B H 0.0088 1.1156 0.0969 0.050 Uiso 1 1 calc R . . H14C H -0.0018 1.1763 0.1837 0.050 Uiso 1 1 calc R . . C15 C 0.3583(3) 0.8059(2) 0.43167(13) 0.0184(4) Uani 1 1 d . . . H15A H 0.3184 0.7590 0.4763 0.022 Uiso 1 1 calc R . . H15B H 0.4742 0.8292 0.4373 0.022 Uiso 1 1 calc R . . C16 C 0.1121(3) 0.6022(2) 0.36282(13) 0.0185(4) Uani 1 1 d . . . C17 C 0.0109(3) 0.6841(2) 0.40524(16) 0.0261(5) Uani 1 1 d . . . H17A H -0.0942 0.6341 0.4121 0.039 Uiso 1 1 calc R . . H17B H 0.0024 0.7533 0.3743 0.039 Uiso 1 1 calc R . . H17C H 0.0599 0.7172 0.4563 0.039 Uiso 1 1 calc R . . C18 C 0.1317(3) 0.5004(2) 0.41501(14) 0.0237(5) Uani 1 1 d . . . H18A H 0.1877 0.5387 0.4636 0.036 Uiso 1 1 calc R . . H18B H 0.1919 0.4447 0.3881 0.036 Uiso 1 1 calc R . . H18C H 0.0280 0.4525 0.4268 0.036 Uiso 1 1 calc R . . C19 C 0.0234(3) 0.5434(3) 0.28688(15) 0.0291(6) Uani 1 1 d . . . H19A H -0.0792 0.4939 0.2989 0.044 Uiso 1 1 calc R . . H19B H 0.0843 0.4895 0.2588 0.044 Uiso 1 1 calc R . . H19C H 0.0085 0.6093 0.2545 0.044 Uiso 1 1 calc R . . C20 C 0.4667(3) 0.6240(2) 0.32815(14) 0.0202(4) Uani 1 1 d . . . C21 C 0.5204(3) 0.5820(3) 0.40497(16) 0.0284(5) Uani 1 1 d . . . H21A H 0.6088 0.5410 0.3956 0.043 Uiso 1 1 calc R . . H21B H 0.4332 0.5236 0.4256 0.043 Uiso 1 1 calc R . . H21C H 0.5532 0.6548 0.4427 0.043 Uiso 1 1 calc R . . C22 C 0.4230(3) 0.5116(2) 0.26739(16) 0.0291(5) Uani 1 1 d . . . H22A H 0.5098 0.4675 0.2637 0.044 Uiso 1 1 calc R . . H22B H 0.4030 0.5403 0.2167 0.044 Uiso 1 1 calc R . . H22C H 0.3284 0.4552 0.2830 0.044 Uiso 1 1 calc R . . C23 C 0.6036(3) 0.7181(3) 0.29817(16) 0.0262(5) Uani 1 1 d . . . H23A H 0.6281 0.7929 0.3349 0.039 Uiso 1 1 calc R . . H23B H 0.5740 0.7409 0.2471 0.039 Uiso 1 1 calc R . . H23C H 0.6962 0.6807 0.2934 0.039 Uiso 1 1 calc R . . C24 C 0.1765(4) 0.6222(3) 0.11561(15) 0.0309(6) Uani 1 1 d . . . H24A H 0.1901 0.5547 0.1479 0.037 Uiso 1 1 calc R . . H24B H 0.0672 0.6340 0.1202 0.037 Uiso 1 1 calc R . . C25 C 0.2083(3) 0.5883(2) 0.03205(14) 0.0222(5) Uani 1 1 d . . . C26 C 0.2858(4) 0.4919(3) 0.01427(18) 0.0378(7) Uani 1 1 d . . . H26 H 0.3206 0.4497 0.0548 0.045 Uiso 1 1 calc R . . C27 C 0.3126(4) 0.4568(3) -0.0641(2) 0.0463(8) Uani 1 1 d . . . H27 H 0.3652 0.3907 -0.0765 0.056 Uiso 1 1 calc R . . C28 C 0.2630(4) 0.5178(4) -0.12146(17) 0.0427(8) Uani 1 1 d . . . H28 H 0.2813 0.4942 -0.1742 0.051 Uiso 1 1 calc R . . C29 C 0.1874(4) 0.6126(3) -0.10442(16) 0.0384(7) Uani 1 1 d . . . H29 H 0.1527 0.6545 -0.1451 0.046 Uiso 1 1 calc R . . C30 C 0.1612(4) 0.6475(3) -0.02828(16) 0.0330(6) Uani 1 1 d . . . H30 H 0.1092 0.7143 -0.0171 0.040 Uiso 1 1 calc R . . F1 F 0.6194(3) 0.1431(2) 0.35259(14) 0.0654(7) Uani 1 1 d . . . F2 F 0.8705(3) 0.2352(3) 0.3424(3) 0.1210(16) Uani 1 1 d . . . F3 F 0.6840(3) 0.3064(2) 0.28175(12) 0.0639(7) Uani 1 1 d . . . F4 F 0.7251(4) 0.3413(3) 0.40899(13) 0.0741(8) Uani 1 1 d . . . B1 B 0.7219(4) 0.2556(3) 0.34655(19) 0.0348(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01682(15) 0.01181(14) 0.01311(14) 0.00093(10) -0.00135(10) 0.00382(10) S1 0.0277(3) 0.0297(3) 0.0215(3) -0.0080(2) 0.0015(2) 0.0015(3) P1 0.0177(3) 0.0139(3) 0.0162(3) 0.0034(2) -0.0022(2) 0.0043(2) P2 0.0160(3) 0.0122(2) 0.0138(2) 0.00227(19) -0.00019(19) 0.0033(2) N1 0.0190(9) 0.0136(8) 0.0147(8) -0.0006(7) -0.0012(7) 0.0037(7) C1 0.0237(11) 0.0146(10) 0.0200(11) 0.0020(8) -0.0008(9) 0.0049(8) C2 0.0364(14) 0.0176(11) 0.0246(12) -0.0013(9) 0.0017(10) 0.0113(10) C3 0.0334(13) 0.0246(12) 0.0193(11) -0.0040(9) 0.0017(10) 0.0091(10) C4 0.0292(12) 0.0218(11) 0.0162(10) -0.0006(9) -0.0004(9) 0.0056(9) C5 0.0184(10) 0.0161(10) 0.0169(10) -0.0002(8) -0.0023(8) 0.0026(8) C6 0.0288(12) 0.0148(10) 0.0201(11) 0.0021(8) 0.0001(9) 0.0067(9) C7 0.0241(11) 0.0201(11) 0.0184(10) 0.0063(8) 0.0020(9) 0.0044(9) C8 0.0327(14) 0.0379(15) 0.0183(11) 0.0052(10) -0.0012(10) 0.0085(11) C9 0.0366(14) 0.0223(12) 0.0350(14) 0.0129(11) 0.0071(11) 0.0058(11) C10 0.0201(11) 0.0270(12) 0.0260(12) 0.0032(10) 0.0003(9) 0.0038(9) C11 0.0187(11) 0.0246(12) 0.0345(13) 0.0111(10) -0.0040(10) 0.0042(9) C12 0.0207(12) 0.0423(16) 0.0469(17) 0.0206(14) 0.0049(11) 0.0065(11) C13 0.0301(14) 0.0353(16) 0.0497(18) 0.0030(13) -0.0181(13) -0.0009(12) C14 0.0242(13) 0.0346(14) 0.0452(16) 0.0171(12) -0.0029(11) 0.0122(11) C15 0.0213(11) 0.0171(10) 0.0172(10) 0.0006(8) -0.0040(8) 0.0054(8) C16 0.0181(10) 0.0187(10) 0.0174(10) 0.0036(8) -0.0002(8) 0.0002(8) C17 0.0195(11) 0.0301(13) 0.0304(13) 0.0072(10) 0.0057(9) 0.0070(10) C18 0.0268(12) 0.0206(11) 0.0230(11) 0.0075(9) 0.0028(9) 0.0006(9) C19 0.0280(13) 0.0332(14) 0.0201(11) 0.0049(10) -0.0039(10) -0.0082(11) C20 0.0206(11) 0.0181(11) 0.0241(11) 0.0037(9) 0.0029(9) 0.0084(9) C21 0.0265(12) 0.0303(13) 0.0337(14) 0.0125(11) 0.0003(10) 0.0142(10) C22 0.0332(14) 0.0218(12) 0.0338(14) -0.0020(10) 0.0075(11) 0.0105(10) C23 0.0180(11) 0.0311(13) 0.0306(13) 0.0068(10) 0.0028(9) 0.0058(10) C24 0.0380(15) 0.0265(13) 0.0244(12) -0.0021(10) 0.0026(11) -0.0004(11) C25 0.0237(11) 0.0210(11) 0.0183(11) -0.0018(9) -0.0009(9) -0.0020(9) C26 0.0486(18) 0.0280(14) 0.0372(15) -0.0017(12) -0.0142(13) 0.0119(13) C27 0.0397(17) 0.0400(17) 0.059(2) -0.0164(15) -0.0006(15) 0.0161(14) C28 0.0298(14) 0.066(2) 0.0240(13) -0.0111(14) 0.0027(11) -0.0041(14) C29 0.0499(18) 0.0390(16) 0.0210(12) 0.0053(11) -0.0059(12) -0.0031(13) C30 0.0446(16) 0.0248(13) 0.0286(13) -0.0003(10) -0.0118(12) 0.0067(11) F1 0.0587(13) 0.0601(14) 0.0662(14) 0.0379(12) -0.0307(11) -0.0236(11) F2 0.0486(15) 0.0496(15) 0.261(5) -0.021(2) -0.025(2) 0.0171(12) F3 0.0992(19) 0.0472(12) 0.0340(10) 0.0161(9) -0.0196(11) -0.0137(12) F4 0.105(2) 0.0741(17) 0.0343(11) -0.0039(11) 0.0064(12) 0.0010(15) B1 0.0448(18) 0.0280(15) 0.0302(15) 0.0043(12) -0.0116(13) 0.0043(13) _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 N1 1.9655(18) . ? Ni1 P1 2.2085(6) . ? Ni1 S1 2.2110(6) . ? Ni1 P2 2.2419(6) . ? S1 C24 1.825(3) . ? P1 C6 1.834(2) . ? P1 C11 1.871(3) . ? P1 C7 1.877(2) . ? P2 C15 1.834(2) . ? P2 C20 1.871(2) . ? P2 C16 1.873(2) . ? N1 C5 1.355(3) . ? N1 C1 1.358(3) . ? C1 C2 1.386(3) . ? C1 C6 1.491(3) . ? C2 C3 1.380(4) . ? C2 H2 0.9500 . ? C3 C4 1.379(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(3) . ? C4 H4 0.9500 . ? C5 C15 1.493(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.531(3) . ? C7 C10 1.535(3) . ? C7 C9 1.538(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.528(3) . ? C11 C13 1.534(4) . ? C11 C12 1.536(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.530(3) . ? C16 C19 1.534(3) . ? C16 C17 1.540(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.534(3) . ? C20 C23 1.536(3) . ? C20 C21 1.536(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.503(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.374(4) . ? C25 C26 1.388(4) . ? C26 C27 1.411(5) . ? C26 H26 0.9500 . ? C27 C28 1.355(5) . ? C27 H27 0.9500 . ? C28 C29 1.361(5) . ? C28 H28 0.9500 . ? C29 C30 1.373(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? F1 B1 1.382(4) . ? F2 B1 1.361(5) . ? F3 B1 1.357(4) . ? F4 B1 1.368(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 N1 Ni1 P1 86.70(6) . . ? N1 Ni1 S1 169.70(6) . . ? P1 Ni1 S1 88.30(3) . . ? N1 Ni1 P2 85.98(6) . . ? P1 Ni1 P2 169.40(2) . . ? S1 Ni1 P2 100.10(3) . . ? C24 S1 Ni1 117.86(9) . . ? C6 P1 C11 103.68(12) . . ? C6 P1 C7 103.22(11) . . ? C11 P1 C7 113.25(11) . . ? C6 P1 Ni1 99.38(8) . . ? C11 P1 Ni1 112.15(8) . . ? C7 P1 Ni1 121.81(8) . . ? C15 P2 C20 102.38(11) . . ? C15 P2 C16 103.88(11) . . ? C20 P2 C16 112.77(11) . . ? C15 P2 Ni1 98.15(7) . . ? C20 P2 Ni1 120.41(8) . . ? C16 P2 Ni1 115.35(7) . . ? C5 N1 C1 117.88(19) . . ? C5 N1 Ni1 121.08(15) . . ? C1 N1 Ni1 120.50(15) . . ? N1 C1 C2 121.7(2) . . ? N1 C1 C6 116.6(2) . . ? C2 C1 C6 121.6(2) . . ? C3 C2 C1 119.6(2) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 119.0(2) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 122.2(2) . . ? N1 C5 C15 116.55(19) . . ? C4 C5 C15 121.3(2) . . ? C1 C6 P1 110.11(16) . . ? C1 C6 H6A 109.6 . . ? P1 C6 H6A 109.6 . . ? C1 C6 H6B 109.6 . . ? P1 C6 H6B 109.6 . . ? H6A C6 H6B 108.2 . . ? C8 C7 C10 109.3(2) . . ? C8 C7 C9 108.5(2) . . ? C10 C7 C9 108.0(2) . . ? C8 C7 P1 112.78(17) . . ? C10 C7 P1 106.13(16) . . ? C9 C7 P1 111.98(17) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C13 109.9(2) . . ? C14 C11 C12 108.7(2) . . ? C13 C11 C12 107.9(2) . . ? C14 C11 P1 112.74(18) . . ? C13 C11 P1 110.70(19) . . ? C12 C11 P1 106.67(18) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C15 P2 109.79(15) . . ? C5 C15 H15A 109.7 . . ? P2 C15 H15A 109.7 . . ? C5 C15 H15B 109.7 . . ? P2 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C18 C16 C19 109.9(2) . . ? C18 C16 C17 108.07(19) . . ? C19 C16 C17 107.4(2) . . ? C18 C16 P2 114.19(16) . . ? C19 C16 P2 109.86(16) . . ? C17 C16 P2 107.07(16) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C23 108.7(2) . . ? C22 C20 C21 109.8(2) . . ? C23 C20 C21 108.5(2) . . ? C22 C20 P2 111.09(17) . . ? C23 C20 P2 105.85(16) . . ? C21 C20 P2 112.75(17) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 S1 108.27(18) . . ? C25 C24 H24A 110.0 . . ? S1 C24 H24A 110.0 . . ? C25 C24 H24B 110.0 . . ? S1 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? C30 C25 C26 118.1(2) . . ? C30 C25 C24 122.7(3) . . ? C26 C25 C24 119.2(2) . . ? C25 C26 C27 119.9(3) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 119.7(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.7(3) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C30 119.9(3) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C25 121.7(3) . . ? C29 C30 H30 119.1 . . ? C25 C30 H30 119.1 . . ? F3 B1 F2 110.1(4) . . ? F3 B1 F4 108.2(3) . . ? F2 B1 F4 105.7(3) . . ? F3 B1 F1 109.7(3) . . ? F2 B1 F1 108.6(3) . . ? F4 B1 F1 114.5(3) . . ? 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 N1 Ni1 S1 C24 -173.7(3) . . . . ? P1 Ni1 S1 C24 -112.75(12) . . . . ? P2 Ni1 S1 C24 60.74(12) . . . . ? N1 Ni1 P1 C6 10.93(10) . . . . ? S1 Ni1 P1 C6 -160.07(9) . . . . ? P2 Ni1 P1 C6 57.29(16) . . . . ? N1 Ni1 P1 C11 -98.10(11) . . . . ? S1 Ni1 P1 C11 90.91(10) . . . . ? P2 Ni1 P1 C11 -51.73(17) . . . . ? N1 Ni1 P1 C7 122.96(11) . . . . ? S1 Ni1 P1 C7 -48.04(9) . . . . ? P2 Ni1 P1 C7 169.32(14) . . . . ? N1 Ni1 P2 C15 -15.63(9) . . . . ? P1 Ni1 P2 C15 -62.04(15) . . . . ? S1 Ni1 P2 C15 155.99(8) . . . . ? N1 Ni1 P2 C20 -125.22(11) . . . . ? P1 Ni1 P2 C20 -171.63(14) . . . . ? S1 Ni1 P2 C20 46.40(9) . . . . ? N1 Ni1 P2 C16 94.01(10) . . . . ? P1 Ni1 P2 C16 47.60(16) . . . . ? S1 Ni1 P2 C16 -94.37(8) . . . . ? P1 Ni1 N1 C5 174.29(17) . . . . ? S1 Ni1 N1 C5 -124.6(3) . . . . ? P2 Ni1 N1 C5 1.96(17) . . . . ? P1 Ni1 N1 C1 2.92(17) . . . . ? S1 Ni1 N1 C1 64.0(4) . . . . ? P2 Ni1 N1 C1 -169.41(17) . . . . ? C5 N1 C1 C2 -8.4(3) . . . . ? Ni1 N1 C1 C2 163.24(19) . . . . ? C5 N1 C1 C6 167.9(2) . . . . ? Ni1 N1 C1 C6 -20.4(3) . . . . ? N1 C1 C2 C3 3.5(4) . . . . ? C6 C1 C2 C3 -172.6(2) . . . . ? C1 C2 C3 C4 2.8(4) . . . . ? C2 C3 C4 C5 -4.1(4) . . . . ? C1 N1 C5 C4 7.1(3) . . . . ? Ni1 N1 C5 C4 -164.47(18) . . . . ? C1 N1 C5 C15 -170.6(2) . . . . ? Ni1 N1 C5 C15 17.8(3) . . . . ? C3 C4 C5 N1 -0.9(4) . . . . ? C3 C4 C5 C15 176.7(2) . . . . ? N1 C1 C6 P1 29.1(3) . . . . ? C2 C1 C6 P1 -154.6(2) . . . . ? C11 P1 C6 C1 92.64(18) . . . . ? C7 P1 C6 C1 -149.03(17) . . . . ? Ni1 P1 C6 C1 -23.05(18) . . . . ? C6 P1 C7 C8 -158.43(18) . . . . ? C11 P1 C7 C8 -47.0(2) . . . . ? Ni1 P1 C7 C8 91.53(18) . . . . ? C6 P1 C7 C10 81.88(18) . . . . ? C11 P1 C7 C10 -166.70(16) . . . . ? Ni1 P1 C7 C10 -28.16(19) . . . . ? C6 P1 C7 C9 -35.7(2) . . . . ? C11 P1 C7 C9 75.7(2) . . . . ? Ni1 P1 C7 C9 -145.75(16) . . . . ? C6 P1 C11 C14 66.3(2) . . . . ? C7 P1 C11 C14 -44.8(2) . . . . ? Ni1 P1 C11 C14 172.58(18) . . . . ? C6 P1 C11 C13 -170.11(19) . . . . ? C7 P1 C11 C13 78.7(2) . . . . ? Ni1 P1 C11 C13 -63.8(2) . . . . ? C6 P1 C11 C12 -52.9(2) . . . . ? C7 P1 C11 C12 -164.06(18) . . . . ? Ni1 P1 C11 C12 53.3(2) . . . . ? N1 C5 C15 P2 -31.3(2) . . . . ? C4 C5 C15 P2 150.9(2) . . . . ? C20 P2 C15 C5 151.55(16) . . . . ? C16 P2 C15 C5 -90.91(17) . . . . ? Ni1 P2 C15 C5 27.83(16) . . . . ? C15 P2 C16 C18 -73.75(19) . . . . ? C20 P2 C16 C18 36.3(2) . . . . ? Ni1 P2 C16 C18 -179.93(14) . . . . ? C15 P2 C16 C19 162.20(18) . . . . ? C20 P2 C16 C19 -87.72(19) . . . . ? Ni1 P2 C16 C19 56.02(19) . . . . ? C15 P2 C16 C17 45.83(18) . . . . ? C20 P2 C16 C17 155.91(16) . . . . ? Ni1 P2 C16 C17 -60.35(17) . . . . ? C15 P2 C20 C22 164.81(17) . . . . ? C16 P2 C20 C22 53.8(2) . . . . ? Ni1 P2 C20 C22 -87.90(17) . . . . ? C15 P2 C20 C23 -77.40(18) . . . . ? C16 P2 C20 C23 171.59(15) . . . . ? Ni1 P2 C20 C23 29.89(19) . . . . ? C15 P2 C20 C21 41.1(2) . . . . ? C16 P2 C20 C21 -69.9(2) . . . . ? Ni1 P2 C20 C21 148.37(15) . . . . ? Ni1 S1 C24 C25 171.03(15) . . . . ? S1 C24 C25 C30 -76.5(3) . . . . ? S1 C24 C25 C26 104.7(3) . . . . ? C30 C25 C26 C27 -0.6(4) . . . . ? C24 C25 C26 C27 178.3(3) . . . . ? C25 C26 C27 C28 0.2(5) . . . . ? C26 C27 C28 C29 -0.1(5) . . . . ? C27 C28 C29 C30 0.3(5) . . . . ? C28 C29 C30 C25 -0.6(5) . . . . ? C26 C25 C30 C29 0.8(4) . . . . ? C24 C25 C30 C29 -178.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.971 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.093 #===END data_s4128a _database_code_depnum_ccdc_archive 'CCDC 699868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H48 N Ni P2 S, B F4' _chemical_formula_sum 'C29 H48 B F4 N Ni P2 S' _chemical_formula_weight 650.20 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 14.2312(1) _cell_length_b 13.7370(1) _cell_length_c 18.1600(1) _cell_angle_alpha 90.00 _cell_angle_beta 117.1778(3) _cell_angle_gamma 90.00 _cell_volume 3158.21(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 68186 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.52 _exptl_absorpt_correction_T_max 0.72 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77735 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7246 _reflns_number_gt 6262 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, denzox, Sadabs' _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^)+(0.0474P)^2^+1.9825P] 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 7246 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.742199(16) 0.178622(15) 0.178925(13) 0.01731(7) Uani 1 1 d . . . S1 S 0.69341(3) 0.20680(3) 0.27431(3) 0.02404(10) Uani 1 1 d . . . P1 P 0.60714(3) 0.23320(3) 0.06007(3) 0.02065(10) Uani 1 1 d . . . P2 P 0.89502(3) 0.12606(3) 0.27995(3) 0.01862(10) Uani 1 1 d . . . N1 N 0.79171(11) 0.12153(10) 0.10438(9) 0.0203(3) Uani 1 1 d . . . C1 C 0.72350(14) 0.10100(13) 0.02431(11) 0.0237(4) Uani 1 1 d . . . C2 C 0.75535(16) 0.05334(14) -0.02720(12) 0.0304(4) Uani 1 1 d . . . H2 H 0.7053 0.0378 -0.0823 0.037 Uiso 1 1 calc R . . C3 C 0.85938(17) 0.02826(16) 0.00106(13) 0.0346(4) Uani 1 1 d . . . H3 H 0.8822 -0.0046 -0.0339 0.042 Uiso 1 1 calc R . . C4 C 0.93004(15) 0.05167(15) 0.08116(12) 0.0306(4) Uani 1 1 d . . . H4 H 1.0029 0.0370 0.1015 0.037 Uiso 1 1 calc R . . C5 C 0.89441(14) 0.09672(13) 0.13184(11) 0.0229(3) Uani 1 1 d . . . C6 C 0.61238(14) 0.13431(14) -0.00535(11) 0.0268(4) Uani 1 1 d . . . H6A H 0.5684 0.0793 -0.0039 0.032 Uiso 1 1 calc R . . H6B H 0.5837 0.1571 -0.0633 0.032 Uiso 1 1 calc R . . C7 C 0.46296(14) 0.23029(14) 0.03381(12) 0.0283(4) Uani 1 1 d . . . C8 C 0.45147(15) 0.14702(15) 0.08543(13) 0.0337(4) Uani 1 1 d . . . H8A H 0.4971 0.1595 0.1443 0.051 Uiso 1 1 calc R . . H8B H 0.4721 0.0855 0.0696 0.051 Uiso 1 1 calc R . . H8C H 0.3778 0.1428 0.0754 0.051 Uiso 1 1 calc R . . C9 C 0.39113(16) 0.20817(19) -0.05823(13) 0.0418(5) Uani 1 1 d . . . H9A H 0.3172 0.2082 -0.0688 0.063 Uiso 1 1 calc R . . H9B H 0.4091 0.1442 -0.0720 0.063 Uiso 1 1 calc R . . H9C H 0.4014 0.2581 -0.0925 0.063 Uiso 1 1 calc R . . C10 C 0.42640(16) 0.32612(15) 0.05551(13) 0.0329(4) Uani 1 1 d . . . H10A H 0.3571 0.3168 0.0536 0.049 Uiso 1 1 calc R . . H10B H 0.4212 0.3763 0.0155 0.049 Uiso 1 1 calc R . . H10C H 0.4775 0.3466 0.1113 0.049 Uiso 1 1 calc R . . C11 C 0.64537(15) 0.34615(14) 0.02131(12) 0.0277(4) Uani 1 1 d . . . C12 C 0.74574(17) 0.32554(15) 0.01248(14) 0.0359(5) Uani 1 1 d . . . H12A H 0.7687 0.3854 -0.0039 0.054 Uiso 1 1 calc R . . H12B H 0.7309 0.2754 -0.0298 0.054 Uiso 1 1 calc R . . H12C H 0.8017 0.3027 0.0655 0.054 Uiso 1 1 calc R . . C13 C 0.55986(19) 0.38066(17) -0.06325(13) 0.0414(5) Uani 1 1 d . . . H13A H 0.4965 0.3994 -0.0584 0.062 Uiso 1 1 calc R . . H13B H 0.5424 0.3278 -0.1036 0.062 Uiso 1 1 calc R . . H13C H 0.5861 0.4368 -0.0817 0.062 Uiso 1 1 calc R . . C14 C 0.67112(17) 0.42593(14) 0.08610(13) 0.0338(4) Uani 1 1 d . . . H14A H 0.7283 0.4039 0.1389 0.051 Uiso 1 1 calc R . . H14B H 0.6083 0.4403 0.0932 0.051 Uiso 1 1 calc R . . H14C H 0.6934 0.4848 0.0679 0.051 Uiso 1 1 calc R . . C15 C 0.96763(14) 0.12195(15) 0.21910(11) 0.0258(4) Uani 1 1 d . . . H15A H 1.0005 0.1861 0.2212 0.031 Uiso 1 1 calc R . . H15B H 1.0245 0.0727 0.2426 0.031 Uiso 1 1 calc R . . C16 C 0.89044(14) -0.00302(13) 0.31211(11) 0.0238(4) Uani 1 1 d . . . C17 C 0.83141(16) -0.06181(14) 0.23199(12) 0.0316(4) Uani 1 1 d . . . H17A H 0.8236 -0.1293 0.2457 0.047 Uiso 1 1 calc R . . H17B H 0.8716 -0.0604 0.2002 0.047 Uiso 1 1 calc R . . H17C H 0.7614 -0.0332 0.1989 0.047 Uiso 1 1 calc R . . C18 C 0.82795(15) -0.01101(15) 0.36201(13) 0.0310(4) Uani 1 1 d . . . H18A H 0.8203 -0.0797 0.3728 0.046 Uiso 1 1 calc R . . H18B H 0.7579 0.0180 0.3304 0.046 Uiso 1 1 calc R . . H18C H 0.8658 0.0236 0.4147 0.046 Uiso 1 1 calc R . . C19 C 1.00015(15) -0.04701(16) 0.36258(13) 0.0343(4) Uani 1 1 d . . . H19A H 1.0354 -0.0141 0.4163 0.051 Uiso 1 1 calc R . . H19B H 1.0420 -0.0385 0.3326 0.051 Uiso 1 1 calc R . . H19C H 0.9934 -0.1166 0.3712 0.051 Uiso 1 1 calc R . . C20 C 0.98049(14) 0.20893(14) 0.36760(12) 0.0276(4) Uani 1 1 d . . . C21 C 1.09854(15) 0.19017(18) 0.39634(14) 0.0395(5) Uani 1 1 d . . . H21A H 1.1152 0.2027 0.3504 0.059 Uiso 1 1 calc R . . H21B H 1.1152 0.1223 0.4143 0.059 Uiso 1 1 calc R . . H21C H 1.1406 0.2336 0.4426 0.059 Uiso 1 1 calc R . . C22 C 0.95875(17) 0.19966(18) 0.44251(12) 0.0379(5) Uani 1 1 d . . . H22A H 0.9969 0.2509 0.4827 0.057 Uiso 1 1 calc R . . H22B H 0.9826 0.1358 0.4684 0.057 Uiso 1 1 calc R . . H22C H 0.8828 0.2064 0.4244 0.057 Uiso 1 1 calc R . . C23 C 0.95373(18) 0.31266(15) 0.33340(15) 0.0408(5) Uani 1 1 d . . . H23A H 1.0016 0.3587 0.3747 0.061 Uiso 1 1 calc R . . H23B H 0.8807 0.3279 0.3209 0.061 Uiso 1 1 calc R . . H23C H 0.9618 0.3178 0.2827 0.061 Uiso 1 1 calc R . . C24 C 0.60852(14) 0.30683(13) 0.26129(10) 0.0233(4) Uani 1 1 d . . . C25 C 0.63977(15) 0.40228(14) 0.25929(11) 0.0273(4) Uani 1 1 d . . . H25 H 0.7065 0.4148 0.2613 0.033 Uiso 1 1 calc R . . C26 C 0.57421(16) 0.47934(15) 0.25439(12) 0.0332(4) Uani 1 1 d . . . H26 H 0.5955 0.5442 0.2516 0.040 Uiso 1 1 calc R . . C27 C 0.47778(17) 0.46212(16) 0.25352(12) 0.0369(5) Uani 1 1 d . . . H27 H 0.4331 0.5151 0.2503 0.044 Uiso 1 1 calc R . . C28 C 0.44669(16) 0.36770(16) 0.25733(12) 0.0334(4) Uani 1 1 d . . . H28 H 0.3810 0.3558 0.2574 0.040 Uiso 1 1 calc R . . C29 C 0.51164(15) 0.28998(15) 0.26103(11) 0.0281(4) Uani 1 1 d . . . H29 H 0.4899 0.2252 0.2634 0.034 Uiso 1 1 calc R . . F1 F 0.11652(12) 0.22254(10) 0.16064(11) 0.0591(4) Uani 1 1 d . . . F2 F 0.28593(17) 0.19454(15) 0.24970(14) 0.1047(8) Uani 1 1 d . . . F3 F 0.2288(2) 0.17062(19) 0.11616(18) 0.1151(9) Uani 1 1 d . . . F4 F 0.17846(11) 0.06856(11) 0.18614(12) 0.0670(5) Uani 1 1 d . . . B1 B 0.2030(2) 0.1649(2) 0.1798(2) 0.0444(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01677(11) 0.01785(12) 0.01708(11) 0.00093(8) 0.00752(9) 0.00148(8) S1 0.0242(2) 0.0288(2) 0.0208(2) 0.00300(17) 0.01174(17) 0.00687(17) P1 0.0204(2) 0.0202(2) 0.0186(2) 0.00085(16) 0.00649(17) 0.00196(16) P2 0.0158(2) 0.0217(2) 0.0176(2) 0.00117(16) 0.00692(16) -0.00034(15) N1 0.0218(7) 0.0207(7) 0.0195(7) 0.0015(5) 0.0105(6) 0.0015(5) C1 0.0275(9) 0.0210(8) 0.0207(8) 0.0009(7) 0.0094(7) -0.0001(7) C2 0.0384(11) 0.0314(10) 0.0226(9) -0.0048(8) 0.0149(8) -0.0016(8) C3 0.0415(11) 0.0374(11) 0.0340(10) -0.0072(9) 0.0252(9) 0.0005(9) C4 0.0295(10) 0.0357(10) 0.0340(10) -0.0003(8) 0.0210(8) 0.0022(8) C5 0.0232(8) 0.0238(9) 0.0252(9) 0.0043(7) 0.0140(7) 0.0018(7) C6 0.0256(9) 0.0275(9) 0.0215(8) -0.0031(7) 0.0057(7) 0.0021(7) C7 0.0207(8) 0.0338(10) 0.0250(9) -0.0025(8) 0.0058(7) 0.0024(7) C8 0.0272(10) 0.0333(10) 0.0411(11) -0.0058(9) 0.0160(9) -0.0073(8) C9 0.0256(10) 0.0576(14) 0.0291(11) -0.0097(10) 0.0011(8) 0.0041(9) C10 0.0280(10) 0.0395(11) 0.0280(10) 0.0013(8) 0.0100(8) 0.0108(8) C11 0.0340(10) 0.0251(9) 0.0254(9) 0.0069(7) 0.0148(8) 0.0042(7) C12 0.0431(12) 0.0303(10) 0.0437(12) 0.0079(9) 0.0279(10) 0.0001(9) C13 0.0534(14) 0.0384(12) 0.0277(10) 0.0120(9) 0.0144(10) 0.0113(10) C14 0.0465(12) 0.0222(9) 0.0363(11) 0.0023(8) 0.0220(9) -0.0012(8) C15 0.0196(8) 0.0359(10) 0.0241(9) 0.0027(7) 0.0119(7) 0.0012(7) C16 0.0226(8) 0.0224(8) 0.0240(9) 0.0051(7) 0.0086(7) 0.0017(7) C17 0.0366(10) 0.0225(9) 0.0314(10) -0.0005(8) 0.0117(8) -0.0026(8) C18 0.0298(10) 0.0322(10) 0.0342(10) 0.0101(8) 0.0174(8) 0.0016(8) C19 0.0289(10) 0.0361(11) 0.0360(11) 0.0125(9) 0.0132(8) 0.0105(8) C20 0.0215(9) 0.0327(10) 0.0256(9) -0.0053(8) 0.0081(7) -0.0063(7) C21 0.0201(9) 0.0556(14) 0.0354(11) -0.0079(10) 0.0062(8) -0.0086(9) C22 0.0338(11) 0.0526(13) 0.0232(9) -0.0112(9) 0.0096(8) -0.0087(9) C23 0.0399(12) 0.0293(11) 0.0480(13) -0.0065(9) 0.0156(10) -0.0126(9) C24 0.0255(9) 0.0273(9) 0.0171(8) -0.0004(7) 0.0097(7) 0.0043(7) C25 0.0281(9) 0.0295(9) 0.0204(8) -0.0024(7) 0.0077(7) 0.0012(7) C26 0.0382(11) 0.0263(10) 0.0258(9) -0.0030(8) 0.0065(8) 0.0048(8) C27 0.0389(11) 0.0372(11) 0.0280(10) -0.0035(8) 0.0096(9) 0.0152(9) C28 0.0273(9) 0.0468(12) 0.0259(9) 0.0000(9) 0.0119(8) 0.0098(9) C29 0.0291(9) 0.0325(10) 0.0241(9) 0.0016(8) 0.0134(8) 0.0034(8) F1 0.0563(9) 0.0355(7) 0.1018(13) 0.0040(8) 0.0504(9) 0.0024(6) F2 0.0854(15) 0.0785(13) 0.0916(15) -0.0314(11) -0.0104(12) -0.0210(11) F3 0.136(2) 0.133(2) 0.136(2) -0.0224(16) 0.1137(19) -0.0040(16) F4 0.0383(8) 0.0387(8) 0.1058(13) -0.0068(8) 0.0171(8) 0.0026(6) B1 0.0340(13) 0.0411(14) 0.0633(18) -0.0194(13) 0.0266(12) -0.0099(11) _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 N1 1.9534(14) . ? Ni1 S1 2.1751(5) . ? Ni1 P2 2.2299(5) . ? Ni1 P1 2.2639(5) . ? S1 C24 1.7727(18) . ? P1 C6 1.8284(19) . ? P1 C7 1.8830(19) . ? P1 C11 1.8837(19) . ? P2 C15 1.8262(18) . ? P2 C16 1.8773(18) . ? P2 C20 1.8816(19) . ? N1 C5 1.355(2) . ? N1 C1 1.359(2) . ? C1 C2 1.377(3) . ? C1 C6 1.491(2) . ? C2 C3 1.371(3) . ? C2 H2 0.9500 . ? C3 C4 1.376(3) . ? C3 H3 0.9500 . ? C4 C5 1.383(3) . ? C4 H4 0.9500 . ? C5 C15 1.486(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C10 1.532(3) . ? C7 C8 1.534(3) . ? C7 C9 1.540(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.525(3) . ? C11 C12 1.535(3) . ? C11 C13 1.535(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C19 1.528(2) . ? C16 C17 1.536(3) . ? C16 C18 1.536(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C23 1.531(3) . ? C20 C22 1.532(3) . ? C20 C21 1.536(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.390(3) . ? C24 C29 1.396(3) . ? C25 C26 1.387(3) . ? C25 H25 0.9500 . ? C26 C27 1.385(3) . ? C26 H26 0.9500 . ? C27 C28 1.382(3) . ? C27 H27 0.9500 . ? C28 C29 1.394(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? F1 B1 1.369(3) . ? F2 B1 1.342(3) . ? F3 B1 1.365(4) . ? F4 B1 1.387(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 N1 Ni1 S1 166.11(4) . . ? N1 Ni1 P2 85.14(4) . . ? S1 Ni1 P2 87.051(17) . . ? N1 Ni1 P1 83.69(4) . . ? S1 Ni1 P1 105.043(18) . . ? P2 Ni1 P1 167.399(19) . . ? C24 S1 Ni1 118.54(6) . . ? C6 P1 C7 100.53(8) . . ? C6 P1 C11 105.35(9) . . ? C7 P1 C11 112.97(9) . . ? C6 P1 Ni1 96.00(6) . . ? C7 P1 Ni1 125.93(6) . . ? C11 P1 Ni1 111.39(6) . . ? C15 P2 C16 105.58(9) . . ? C15 P2 C20 101.82(9) . . ? C16 P2 C20 114.15(8) . . ? C15 P2 Ni1 96.95(6) . . ? C16 P2 Ni1 113.73(6) . . ? C20 P2 Ni1 120.72(6) . . ? C5 N1 C1 117.71(15) . . ? C5 N1 Ni1 121.06(12) . . ? C1 N1 Ni1 121.16(12) . . ? N1 C1 C2 121.98(17) . . ? N1 C1 C6 116.38(15) . . ? C2 C1 C6 121.64(16) . . ? C3 C2 C1 119.95(18) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 118.67(18) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 119.65(18) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.96(17) . . ? N1 C5 C15 116.55(15) . . ? C4 C5 C15 121.48(16) . . ? C1 C6 P1 110.16(12) . . ? C1 C6 H6A 109.6 . . ? P1 C6 H6A 109.6 . . ? C1 C6 H6B 109.6 . . ? P1 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C10 C7 C8 109.88(17) . . ? C10 C7 C9 108.29(16) . . ? C8 C7 C9 108.24(17) . . ? C10 C7 P1 112.06(13) . . ? C8 C7 P1 105.61(12) . . ? C9 C7 P1 112.67(14) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 107.82(17) . . ? C14 C11 C13 110.56(16) . . ? C12 C11 C13 107.63(17) . . ? C14 C11 P1 108.19(13) . . ? C12 C11 P1 109.18(13) . . ? C13 C11 P1 113.32(15) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C15 P2 109.73(12) . . ? C5 C15 H15A 109.7 . . ? P2 C15 H15A 109.7 . . ? C5 C15 H15B 109.7 . . ? P2 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C19 C16 C17 109.09(16) . . ? C19 C16 C18 109.03(15) . . ? C17 C16 C18 107.93(15) . . ? C19 C16 P2 112.89(13) . . ? C17 C16 P2 106.48(12) . . ? C18 C16 P2 111.27(13) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C23 C20 C22 108.90(18) . . ? C23 C20 C21 108.95(17) . . ? C22 C20 C21 108.51(17) . . ? C23 C20 P2 105.96(13) . . ? C22 C20 P2 112.72(13) . . ? C21 C20 P2 111.71(14) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 118.91(17) . . ? C25 C24 S1 121.86(14) . . ? C29 C24 S1 118.93(14) . . ? C26 C25 C24 120.51(18) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 120.28(19) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 119.85(18) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 120.1(2) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C24 120.36(19) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? F2 B1 F3 108.9(2) . . ? F2 B1 F1 111.4(2) . . ? F3 B1 F1 108.0(3) . . ? F2 B1 F4 110.9(3) . . ? F3 B1 F4 107.5(2) . . ? F1 B1 F4 109.97(19) . . ? 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 N1 Ni1 S1 C24 -157.37(19) . . . . ? P2 Ni1 S1 C24 146.84(7) . . . . ? P1 Ni1 S1 C24 -29.57(7) . . . . ? N1 Ni1 P1 C6 28.13(8) . . . . ? S1 Ni1 P1 C6 -140.87(7) . . . . ? P2 Ni1 P1 C6 55.79(11) . . . . ? N1 Ni1 P1 C7 135.78(9) . . . . ? S1 Ni1 P1 C7 -33.22(8) . . . . ? P2 Ni1 P1 C7 163.44(10) . . . . ? N1 Ni1 P1 C11 -80.97(8) . . . . ? S1 Ni1 P1 C11 110.03(7) . . . . ? P2 Ni1 P1 C11 -53.30(11) . . . . ? N1 Ni1 P2 C15 23.88(8) . . . . ? S1 Ni1 P2 C15 -167.61(7) . . . . ? P1 Ni1 P2 C15 -3.71(11) . . . . ? N1 Ni1 P2 C16 -86.56(8) . . . . ? S1 Ni1 P2 C16 81.95(7) . . . . ? P1 Ni1 P2 C16 -114.15(10) . . . . ? N1 Ni1 P2 C20 132.08(8) . . . . ? S1 Ni1 P2 C20 -59.41(7) . . . . ? P1 Ni1 P2 C20 104.49(11) . . . . ? S1 Ni1 N1 C5 -71.3(2) . . . . ? P2 Ni1 N1 C5 -15.27(13) . . . . ? P1 Ni1 N1 C5 158.90(13) . . . . ? S1 Ni1 N1 C1 105.5(2) . . . . ? P2 Ni1 N1 C1 161.51(13) . . . . ? P1 Ni1 N1 C1 -24.33(13) . . . . ? C5 N1 C1 C2 2.5(3) . . . . ? Ni1 N1 C1 C2 -174.43(14) . . . . ? C5 N1 C1 C6 -176.60(16) . . . . ? Ni1 N1 C1 C6 6.5(2) . . . . ? N1 C1 C2 C3 -2.4(3) . . . . ? C6 C1 C2 C3 176.63(18) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C2 C3 C4 C5 2.1(3) . . . . ? C1 N1 C5 C4 -0.3(3) . . . . ? Ni1 N1 C5 C4 176.63(14) . . . . ? C1 N1 C5 C15 178.72(15) . . . . ? Ni1 N1 C5 C15 -4.4(2) . . . . ? C3 C4 C5 N1 -2.0(3) . . . . ? C3 C4 C5 C15 179.06(18) . . . . ? N1 C1 C6 P1 21.7(2) . . . . ? C2 C1 C6 P1 -157.34(15) . . . . ? C7 P1 C6 C1 -161.55(13) . . . . ? C11 P1 C6 C1 80.89(14) . . . . ? Ni1 P1 C6 C1 -33.26(13) . . . . ? C6 P1 C7 C10 -160.04(14) . . . . ? C11 P1 C7 C10 -48.25(16) . . . . ? Ni1 P1 C7 C10 94.52(14) . . . . ? C6 P1 C7 C8 80.34(14) . . . . ? C11 P1 C7 C8 -167.86(13) . . . . ? Ni1 P1 C7 C8 -25.09(16) . . . . ? C6 P1 C7 C9 -37.62(17) . . . . ? C11 P1 C7 C9 74.18(17) . . . . ? Ni1 P1 C7 C9 -143.05(13) . . . . ? C6 P1 C11 C14 -165.21(13) . . . . ? C7 P1 C11 C14 85.99(15) . . . . ? Ni1 P1 C11 C14 -62.27(14) . . . . ? C6 P1 C11 C12 -48.12(16) . . . . ? C7 P1 C11 C12 -156.92(14) . . . . ? Ni1 P1 C11 C12 54.82(15) . . . . ? C6 P1 C11 C13 71.82(16) . . . . ? C7 P1 C11 C13 -36.98(17) . . . . ? Ni1 P1 C11 C13 174.77(13) . . . . ? N1 C5 C15 P2 27.1(2) . . . . ? C4 C5 C15 P2 -153.89(15) . . . . ? C16 P2 C15 C5 84.54(14) . . . . ? C20 P2 C15 C5 -155.96(13) . . . . ? Ni1 P2 C15 C5 -32.51(13) . . . . ? C15 P2 C16 C19 58.83(15) . . . . ? C20 P2 C16 C19 -52.15(16) . . . . ? Ni1 P2 C16 C19 163.89(12) . . . . ? C15 P2 C16 C17 -60.85(14) . . . . ? C20 P2 C16 C17 -171.83(12) . . . . ? Ni1 P2 C16 C17 44.21(14) . . . . ? C15 P2 C16 C18 -178.20(13) . . . . ? C20 P2 C16 C18 70.81(15) . . . . ? Ni1 P2 C16 C18 -73.15(13) . . . . ? C15 P2 C20 C23 79.70(15) . . . . ? C16 P2 C20 C23 -167.06(13) . . . . ? Ni1 P2 C20 C23 -25.85(16) . . . . ? C15 P2 C20 C22 -161.30(15) . . . . ? C16 P2 C20 C22 -48.06(17) . . . . ? Ni1 P2 C20 C22 93.15(15) . . . . ? C15 P2 C20 C21 -38.81(16) . . . . ? C16 P2 C20 C21 74.43(16) . . . . ? Ni1 P2 C20 C21 -144.36(13) . . . . ? Ni1 S1 C24 C25 -63.97(16) . . . . ? Ni1 S1 C24 C29 122.29(13) . . . . ? C29 C24 C25 C26 -2.1(3) . . . . ? S1 C24 C25 C26 -175.81(14) . . . . ? C24 C25 C26 C27 1.6(3) . . . . ? C25 C26 C27 C28 -0.2(3) . . . . ? C26 C27 C28 C29 -0.8(3) . . . . ? C27 C28 C29 C24 0.3(3) . . . . ? C25 C24 C29 C28 1.1(3) . . . . ? S1 C24 C29 C28 175.05(14) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.710 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.058 #===END data_s3897a _database_code_depnum_ccdc_archive 'CCDC 699869' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H43 Cl N Ni P2, B F4' _chemical_formula_sum 'C23 H43 B Cl F4 N Ni P2' _chemical_formula_weight 576.49 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3356(1) _cell_length_b 12.2538(1) _cell_length_c 14.6565(2) _cell_angle_alpha 73.5826(5) _cell_angle_beta 75.8775(6) _cell_angle_gamma 87.7751(8) _cell_volume 1391.89(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29114 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34132 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6356 _reflns_number_gt 5719 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement HKL2000 _computing_data_reduction 'HKL2000, denzox, Sadabs' _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^)+(0.0282P)^2^+0.6447P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6356 _refine_ls_number_parameters 338 _refine_ls_number_restraints 123 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.215 _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 0.26844(2) 0.218320(16) 0.260460(14) 0.01712(6) Uani 1 1 d . . . Cl1 Cl 0.04373(5) 0.16225(4) 0.37353(3) 0.03255(11) Uani 1 1 d . . . P1 P 0.31349(5) 0.04583(3) 0.24151(3) 0.01775(9) Uani 1 1 d . . . P2 P 0.26083(5) 0.39083(3) 0.28102(3) 0.01652(9) Uani 1 1 d . . . N1 N 0.46711(16) 0.26871(11) 0.15849(9) 0.0170(3) Uani 1 1 d . . . C1 C 0.55925(19) 0.19352(14) 0.11591(11) 0.0192(3) Uani 1 1 d . . . C2 C 0.7210(2) 0.22045(15) 0.06121(12) 0.0240(3) Uani 1 1 d . . . H2 H 0.7848 0.1654 0.0352 0.029 Uiso 1 1 calc R . . C3 C 0.7892(2) 0.32738(16) 0.04464(12) 0.0262(4) Uani 1 1 d . . . H3 H 0.9014 0.3455 0.0100 0.031 Uiso 1 1 calc R . . C4 C 0.6906(2) 0.40767(15) 0.07953(12) 0.0243(3) Uani 1 1 d . . . H4 H 0.7322 0.4833 0.0651 0.029 Uiso 1 1 calc R . . C5 C 0.53058(19) 0.37674(14) 0.13571(11) 0.0192(3) Uani 1 1 d . . . C6 C 0.4748(2) 0.08302(14) 0.12677(12) 0.0212(3) Uani 1 1 d . . . H6A H 0.5566 0.0222 0.1273 0.025 Uiso 1 1 calc R . . H6B H 0.4250 0.0903 0.0706 0.025 Uiso 1 1 calc R . . C7 C 0.4174(2) -0.04708(15) 0.33446(12) 0.0253(4) Uani 1 1 d . . . C8 C 0.5796(2) 0.01545(18) 0.32507(15) 0.0348(4) Uani 1 1 d . . . H8A H 0.6326 -0.0268 0.3767 0.052 Uiso 1 1 calc R . . H8B H 0.5556 0.0921 0.3318 0.052 Uiso 1 1 calc R . . H8C H 0.6540 0.0208 0.2608 0.052 Uiso 1 1 calc R . . C9 C 0.3088(3) -0.06229(19) 0.43842(13) 0.0383(5) Uani 1 1 d . . . H9A H 0.2045 -0.1018 0.4456 0.057 Uiso 1 1 calc R . . H9B H 0.2857 0.0125 0.4496 0.057 Uiso 1 1 calc R . . H9C H 0.3670 -0.1074 0.4864 0.057 Uiso 1 1 calc R . . C10 C 0.4585(3) -0.16363(17) 0.31684(16) 0.0395(5) Uani 1 1 d . . . H10A H 0.5261 -0.1531 0.2499 0.059 Uiso 1 1 calc R . . H10B H 0.3556 -0.2057 0.3255 0.059 Uiso 1 1 calc R . . H10C H 0.5200 -0.2066 0.3638 0.059 Uiso 1 1 calc R . . C11 C 0.1459(2) -0.02920(14) 0.21528(13) 0.0233(3) Uani 1 1 d . . . C12 C 0.2181(2) -0.10298(16) 0.14645(15) 0.0323(4) Uani 1 1 d . . . H12A H 0.2911 -0.1589 0.1764 0.049 Uiso 1 1 calc R . . H12B H 0.2814 -0.0543 0.0836 0.049 Uiso 1 1 calc R . . H12C H 0.1277 -0.1427 0.1356 0.049 Uiso 1 1 calc R . . C13 C 0.0301(2) -0.10267(16) 0.30937(14) 0.0314(4) Uani 1 1 d . . . H13A H -0.0627 -0.1331 0.2928 0.047 Uiso 1 1 calc R . . H13B H -0.0123 -0.0560 0.3539 0.047 Uiso 1 1 calc R . . H13C H 0.0913 -0.1658 0.3414 0.047 Uiso 1 1 calc R . . C14 C 0.0452(2) 0.06476(16) 0.16190(15) 0.0318(4) Uani 1 1 d . . . H14A H -0.0365 0.0300 0.1398 0.048 Uiso 1 1 calc R . . H14B H 0.1200 0.1163 0.1051 0.048 Uiso 1 1 calc R . . H14C H -0.0117 0.1077 0.2069 0.048 Uiso 1 1 calc R . . C15 C 0.4181(2) 0.46290(14) 0.17094(12) 0.0218(3) Uani 1 1 d . . . H15A H 0.3639 0.5050 0.1189 0.026 Uiso 1 1 calc R . . H15B H 0.4835 0.5183 0.1861 0.026 Uiso 1 1 calc R . . C16 C 0.3459(2) 0.39829(14) 0.38648(12) 0.0225(3) Uani 1 1 d . . . C17 C 0.5222(2) 0.35221(18) 0.36774(15) 0.0329(4) Uani 1 1 d . . . H17A H 0.5919 0.4030 0.3082 0.049 Uiso 1 1 calc R . . H17B H 0.5176 0.2759 0.3594 0.049 Uiso 1 1 calc R . . H17C H 0.5690 0.3485 0.4237 0.049 Uiso 1 1 calc R . . C18 C 0.3562(2) 0.52039(16) 0.39339(14) 0.0299(4) Uani 1 1 d . . . H18A H 0.4125 0.5211 0.4447 0.045 Uiso 1 1 calc R . . H18B H 0.2443 0.5487 0.4096 0.045 Uiso 1 1 calc R . . H18C H 0.4185 0.5694 0.3303 0.045 Uiso 1 1 calc R . . C19 C 0.2429(2) 0.32090(17) 0.48358(13) 0.0316(4) Uani 1 1 d . . . H19A H 0.2902 0.3251 0.5376 0.047 Uiso 1 1 calc R . . H19B H 0.2444 0.2422 0.4800 0.047 Uiso 1 1 calc R . . H19C H 0.1286 0.3461 0.4951 0.047 Uiso 1 1 calc R . . C20 C 0.0715(2) 0.47612(14) 0.27076(13) 0.0224(3) Uani 1 1 d . . . C21 C -0.0004(2) 0.43804(16) 0.19661(15) 0.0302(4) Uani 1 1 d . . . H21A H -0.0947 0.4847 0.1833 0.045 Uiso 1 1 calc R . . H21B H -0.0371 0.3579 0.2240 0.045 Uiso 1 1 calc R . . H21C H 0.0850 0.4473 0.1355 0.045 Uiso 1 1 calc R . . C22 C 0.1120(2) 0.60495(15) 0.23193(14) 0.0293(4) Uani 1 1 d . . . H22A H 0.0111 0.6458 0.2227 0.044 Uiso 1 1 calc R . . H22B H 0.1947 0.6213 0.1691 0.044 Uiso 1 1 calc R . . H22C H 0.1559 0.6298 0.2793 0.044 Uiso 1 1 calc R . . C23 C -0.0583(2) 0.45214(16) 0.36886(14) 0.0300(4) Uani 1 1 d . . . H23A H -0.0158 0.4802 0.4151 0.045 Uiso 1 1 calc R . . H23B H -0.0818 0.3700 0.3955 0.045 Uiso 1 1 calc R . . H23C H -0.1602 0.4910 0.3587 0.045 Uiso 1 1 calc R . . F1 F 0.68324(18) 0.65574(12) 0.19198(10) 0.0540(4) Uani 1 1 d D A . F2A F 0.7437(11) 0.6881(5) 0.0217(4) 0.096(3) Uani 0.483(7) 1 d PDU A 1 F3A F 0.8887(4) 0.7754(4) 0.0874(3) 0.0696(18) Uani 0.483(7) 1 d PDU A 1 F4A F 0.6347(6) 0.8277(4) 0.0804(2) 0.0627(17) Uani 0.483(7) 1 d PDU A 1 F2B F 0.8092(6) 0.6812(5) 0.0366(4) 0.0730(19) Uani 0.517(7) 1 d PDU A 2 F3B F 0.7826(10) 0.8293(4) 0.1036(3) 0.120(3) Uani 0.517(7) 1 d PDU A 2 F4B F 0.5641(5) 0.7495(6) 0.0862(3) 0.086(2) Uani 0.517(7) 1 d PDU A 2 B1 B 0.7245(3) 0.73309(18) 0.10017(17) 0.0365(5) Uani 1 1 d 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 0.01718(11) 0.01434(10) 0.01715(11) -0.00419(8) 0.00076(7) -0.00117(7) Cl1 0.0288(2) 0.0243(2) 0.0350(2) -0.01057(18) 0.01364(17) -0.00691(16) P1 0.0198(2) 0.01458(19) 0.01653(19) -0.00389(15) -0.00084(15) 0.00092(14) P2 0.01756(19) 0.01471(19) 0.01710(19) -0.00443(14) -0.00380(14) -0.00044(14) N1 0.0165(6) 0.0189(6) 0.0139(6) -0.0029(5) -0.0027(5) -0.0009(5) C1 0.0196(7) 0.0227(8) 0.0141(7) -0.0040(6) -0.0031(6) 0.0007(6) C2 0.0207(8) 0.0328(9) 0.0173(8) -0.0076(7) -0.0018(6) 0.0015(7) C3 0.0178(8) 0.0392(10) 0.0192(8) -0.0066(7) -0.0008(6) -0.0057(7) C4 0.0238(8) 0.0285(9) 0.0185(8) -0.0033(6) -0.0036(6) -0.0094(7) C5 0.0209(8) 0.0212(8) 0.0149(7) -0.0032(6) -0.0045(6) -0.0035(6) C6 0.0224(8) 0.0219(8) 0.0176(7) -0.0068(6) -0.0004(6) 0.0009(6) C7 0.0302(9) 0.0235(8) 0.0192(8) -0.0030(6) -0.0047(7) 0.0061(7) C8 0.0316(10) 0.0404(11) 0.0324(10) -0.0057(8) -0.0141(8) 0.0059(8) C9 0.0429(11) 0.0459(12) 0.0187(9) -0.0015(8) -0.0032(8) 0.0062(9) C10 0.0530(13) 0.0263(10) 0.0402(11) -0.0078(8) -0.0176(10) 0.0166(9) C11 0.0240(8) 0.0193(8) 0.0260(9) -0.0070(6) -0.0034(7) -0.0030(6) C12 0.0362(10) 0.0289(9) 0.0352(10) -0.0183(8) -0.0029(8) -0.0053(8) C13 0.0299(9) 0.0235(9) 0.0353(10) -0.0067(7) 0.0013(8) -0.0072(7) C14 0.0274(9) 0.0304(10) 0.0374(10) -0.0060(8) -0.0113(8) -0.0013(7) C15 0.0250(8) 0.0183(8) 0.0195(8) -0.0024(6) -0.0030(6) -0.0039(6) C16 0.0244(8) 0.0238(8) 0.0206(8) -0.0058(6) -0.0082(6) 0.0007(6) C17 0.0280(9) 0.0426(11) 0.0341(10) -0.0138(8) -0.0161(8) 0.0070(8) C18 0.0372(10) 0.0297(9) 0.0287(9) -0.0124(7) -0.0141(8) -0.0017(8) C19 0.0393(10) 0.0324(10) 0.0211(9) -0.0029(7) -0.0087(7) -0.0005(8) C20 0.0225(8) 0.0203(8) 0.0283(9) -0.0098(7) -0.0104(7) 0.0040(6) C21 0.0310(9) 0.0304(9) 0.0372(10) -0.0133(8) -0.0192(8) 0.0041(7) C22 0.0357(10) 0.0197(8) 0.0364(10) -0.0088(7) -0.0159(8) 0.0061(7) C23 0.0223(8) 0.0313(10) 0.0392(10) -0.0172(8) -0.0045(7) 0.0042(7) F1 0.0567(8) 0.0465(8) 0.0458(8) 0.0008(6) -0.0029(6) -0.0087(6) F2A 0.199(8) 0.039(3) 0.046(2) -0.0194(18) -0.012(4) -0.024(4) F3A 0.0364(19) 0.098(3) 0.057(2) 0.015(2) -0.0191(16) -0.0224(19) F4A 0.073(3) 0.063(3) 0.0369(16) -0.0032(16) -0.0042(17) 0.045(2) F2B 0.062(2) 0.047(2) 0.070(3) -0.007(2) 0.045(2) 0.0142(19) F3B 0.179(8) 0.067(3) 0.090(3) -0.036(2) 0.044(4) -0.082(4) F4B 0.061(2) 0.118(5) 0.061(2) 0.003(2) -0.0212(18) 0.046(3) B1 0.0381(12) 0.0287(11) 0.0404(13) -0.0071(9) -0.0091(10) 0.0063(9) _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 N1 1.9254(13) . ? Ni1 Cl1 2.1606(4) . ? Ni1 P2 2.2144(4) . ? Ni1 P1 2.2147(4) . ? P1 C6 1.8318(16) . ? P1 C11 1.8722(17) . ? P1 C7 1.8772(17) . ? P2 C15 1.8315(17) . ? P2 C20 1.8723(16) . ? P2 C16 1.8763(17) . ? N1 C5 1.365(2) . ? N1 C1 1.365(2) . ? C1 C2 1.388(2) . ? C1 C6 1.500(2) . ? C2 C3 1.382(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(2) . ? C4 H4 0.9500 . ? C5 C15 1.502(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C10 1.533(3) . ? C7 C9 1.535(2) . ? C7 C8 1.538(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.537(2) . ? C11 C12 1.541(2) . ? C11 C14 1.542(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.535(2) . ? C16 C19 1.538(2) . ? C16 C17 1.543(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C23 1.533(2) . ? C20 C22 1.539(2) . ? C20 C21 1.544(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? F1 B1 1.381(3) . ? F2A B1 1.383(5) . ? F3A B1 1.432(3) . ? F4A B1 1.356(3) . ? F2B B1 1.323(4) . ? F3B B1 1.311(4) . ? F4B B1 1.400(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 N1 Ni1 Cl1 179.29(4) . . ? N1 Ni1 P2 87.46(4) . . ? Cl1 Ni1 P2 92.611(17) . . ? N1 Ni1 P1 87.31(4) . . ? Cl1 Ni1 P1 92.694(17) . . ? P2 Ni1 P1 171.750(17) . . ? C6 P1 C11 105.03(8) . . ? C6 P1 C7 104.84(8) . . ? C11 P1 C7 114.03(8) . . ? C6 P1 Ni1 98.91(5) . . ? C11 P1 Ni1 118.65(5) . . ? C7 P1 Ni1 112.74(6) . . ? C15 P2 C20 104.28(8) . . ? C15 P2 C16 105.09(8) . . ? C20 P2 C16 113.52(7) . . ? C15 P2 Ni1 99.02(6) . . ? C20 P2 Ni1 119.12(5) . . ? C16 P2 Ni1 113.12(5) . . ? C5 N1 C1 117.97(13) . . ? C5 N1 Ni1 120.79(11) . . ? C1 N1 Ni1 120.72(11) . . ? N1 C1 C2 121.44(15) . . ? N1 C1 C6 116.90(14) . . ? C2 C1 C6 121.59(15) . . ? C3 C2 C1 119.98(16) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 118.67(15) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 119.53(16) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.85(15) . . ? N1 C5 C15 117.29(14) . . ? C4 C5 C15 120.83(15) . . ? C1 C6 P1 109.32(11) . . ? C1 C6 H6A 109.8 . . ? P1 C6 H6A 109.8 . . ? C1 C6 H6B 109.8 . . ? P1 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C10 C7 C9 110.05(16) . . ? C10 C7 C8 108.73(16) . . ? C9 C7 C8 108.34(16) . . ? C10 C7 P1 112.47(13) . . ? C9 C7 P1 110.25(12) . . ? C8 C7 P1 106.85(12) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 109.77(15) . . ? C13 C11 C14 108.93(15) . . ? C12 C11 C14 108.07(15) . . ? C13 C11 P1 112.26(12) . . ? C12 C11 P1 111.43(12) . . ? C14 C11 P1 106.20(12) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C15 P2 109.69(11) . . ? C5 C15 H15A 109.7 . . ? P2 C15 H15A 109.7 . . ? C5 C15 H15B 109.7 . . ? P2 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? C18 C16 C19 110.28(15) . . ? C18 C16 C17 108.84(15) . . ? C19 C16 C17 108.11(14) . . ? C18 C16 P2 112.50(11) . . ? C19 C16 P2 110.70(12) . . ? C17 C16 P2 106.22(12) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C23 C20 C22 108.78(14) . . ? C23 C20 C21 109.10(15) . . ? C22 C20 C21 109.15(14) . . ? C23 C20 P2 112.12(12) . . ? C22 C20 P2 112.25(12) . . ? C21 C20 P2 105.34(11) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? F3B B1 F2B 119.6(4) . . ? F3B B1 F1 111.4(3) . . ? F2B B1 F1 109.0(3) . . ? F4A B1 F1 119.5(2) . . ? F4A B1 F2A 106.6(4) . . ? F1 B1 F2A 115.8(3) . . ? F3B B1 F4B 108.5(4) . . ? F2B B1 F4B 108.5(3) . . ? F1 B1 F4B 97.5(2) . . ? F4A B1 F3A 104.6(3) . . ? F1 B1 F3A 106.4(2) . . ? F2A B1 F3A 101.9(4) . . ? 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 N1 Ni1 P1 C6 -12.19(6) . . . . ? Cl1 Ni1 P1 C6 167.10(6) . . . . ? N1 Ni1 P1 C11 -124.82(7) . . . . ? Cl1 Ni1 P1 C11 54.47(6) . . . . ? N1 Ni1 P1 C7 98.11(7) . . . . ? Cl1 Ni1 P1 C7 -82.60(6) . . . . ? N1 Ni1 P2 C15 11.71(6) . . . . ? Cl1 Ni1 P2 C15 -167.59(6) . . . . ? N1 Ni1 P2 C20 123.69(7) . . . . ? Cl1 Ni1 P2 C20 -55.61(7) . . . . ? N1 Ni1 P2 C16 -99.05(7) . . . . ? Cl1 Ni1 P2 C16 81.66(6) . . . . ? P2 Ni1 N1 C5 0.56(11) . . . . ? P1 Ni1 N1 C5 -173.05(11) . . . . ? P2 Ni1 N1 C1 172.17(11) . . . . ? P1 Ni1 N1 C1 -1.45(11) . . . . ? C5 N1 C1 C2 8.2(2) . . . . ? Ni1 N1 C1 C2 -163.65(12) . . . . ? C5 N1 C1 C6 -168.84(13) . . . . ? Ni1 N1 C1 C6 19.33(18) . . . . ? N1 C1 C2 C3 -3.4(2) . . . . ? C6 C1 C2 C3 173.52(15) . . . . ? C1 C2 C3 C4 -3.1(2) . . . . ? C2 C3 C4 C5 4.4(2) . . . . ? C1 N1 C5 C4 -6.8(2) . . . . ? Ni1 N1 C5 C4 165.06(12) . . . . ? C1 N1 C5 C15 171.14(13) . . . . ? Ni1 N1 C5 C15 -17.03(18) . . . . ? C3 C4 C5 N1 0.5(2) . . . . ? C3 C4 C5 C15 -177.34(15) . . . . ? N1 C1 C6 P1 -29.06(17) . . . . ? C2 C1 C6 P1 153.93(13) . . . . ? C11 P1 C6 C1 146.76(11) . . . . ? C7 P1 C6 C1 -92.75(12) . . . . ? Ni1 P1 C6 C1 23.76(11) . . . . ? C6 P1 C7 C10 -69.69(15) . . . . ? C11 P1 C7 C10 44.64(16) . . . . ? Ni1 P1 C7 C10 -176.24(12) . . . . ? C6 P1 C7 C9 167.08(14) . . . . ? C11 P1 C7 C9 -78.60(15) . . . . ? Ni1 P1 C7 C9 60.52(15) . . . . ? C6 P1 C7 C8 49.55(14) . . . . ? C11 P1 C7 C8 163.87(12) . . . . ? Ni1 P1 C7 C8 -57.00(13) . . . . ? C6 P1 C11 C13 159.85(12) . . . . ? C7 P1 C11 C13 45.64(15) . . . . ? Ni1 P1 C11 C13 -90.91(12) . . . . ? C6 P1 C11 C12 36.25(14) . . . . ? C7 P1 C11 C12 -77.96(14) . . . . ? Ni1 P1 C11 C12 145.49(11) . . . . ? C6 P1 C11 C14 -81.20(13) . . . . ? C7 P1 C11 C14 164.59(12) . . . . ? Ni1 P1 C11 C14 28.04(14) . . . . ? N1 C5 C15 P2 26.54(17) . . . . ? C4 C5 C15 P2 -155.53(13) . . . . ? C20 P2 C15 C5 -145.42(11) . . . . ? C16 P2 C15 C5 94.90(12) . . . . ? Ni1 P2 C15 C5 -22.13(12) . . . . ? C15 P2 C16 C18 67.21(14) . . . . ? C20 P2 C16 C18 -46.12(15) . . . . ? Ni1 P2 C16 C18 174.16(11) . . . . ? C15 P2 C16 C19 -168.90(12) . . . . ? C20 P2 C16 C19 77.77(14) . . . . ? Ni1 P2 C16 C19 -61.95(13) . . . . ? C15 P2 C16 C17 -51.77(14) . . . . ? C20 P2 C16 C17 -165.10(12) . . . . ? Ni1 P2 C16 C17 55.19(13) . . . . ? C15 P2 C20 C23 -162.94(12) . . . . ? C16 P2 C20 C23 -49.13(14) . . . . ? Ni1 P2 C20 C23 87.98(12) . . . . ? C15 P2 C20 C22 -40.14(14) . . . . ? C16 P2 C20 C22 73.67(14) . . . . ? Ni1 P2 C20 C22 -149.22(10) . . . . ? C15 P2 C20 C21 78.52(13) . . . . ? C16 P2 C20 C21 -167.66(12) . . . . ? Ni1 P2 C20 C21 -30.56(14) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.496 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.048 #===END