data_mn1685 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Ni(dppe)Ni(PhPepS)].CH2Cl2 _chemical_melting_point ? _chemical_formula_moiety 'C46 H36 N2 Ni2 O2 P2 S2, C H2 Cl2' _chemical_formula_sum 'C47 H38 Cl2 N2 Ni2 O2 P2 S2' _chemical_formula_weight 977.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.0656(5) _cell_length_b 17.3249(6) _cell_length_c 17.5370(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.610(3) _cell_angle_gamma 90.00 _cell_volume 4273.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8180 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.51 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 1.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.867 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47099 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9784 _reflns_number_gt 7882 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex 2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL-97 _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^)+(0.0177P)^2^+4.1330P] 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 9784 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 0.555038(18) 0.338061(14) 0.116176(14) 0.01258(7) Uani 1 1 d . . . Ni2 Ni 0.594128(18) 0.494914(14) 0.147574(14) 0.01140(7) Uani 1 1 d . . . S1 S 0.45705(3) 0.42974(3) 0.14241(3) 0.01262(10) Uani 1 1 d . . . S2 S 0.60267(3) 0.42610(3) 0.03964(3) 0.01237(10) Uani 1 1 d . . . P1 P 0.56717(4) 0.56549(3) 0.24783(3) 0.01277(11) Uani 1 1 d . . . P2 P 0.73554(4) 0.54666(3) 0.14795(3) 0.01303(11) Uani 1 1 d . . . O1 O 0.49860(11) 0.23641(9) 0.31375(9) 0.0239(3) Uani 1 1 d . . . O2 O 0.79785(11) 0.21869(9) 0.08052(9) 0.0230(3) Uani 1 1 d . . . N1 N 0.50666(13) 0.26550(10) 0.18635(10) 0.0167(4) Uani 1 1 d . . . N2 N 0.64416(13) 0.26161(10) 0.08876(10) 0.0161(4) Uani 1 1 d . . . C1 C 0.39126(14) 0.40824(12) 0.22567(11) 0.0155(4) Uani 1 1 d . . . C2 C 0.31473(15) 0.45685(13) 0.24045(12) 0.0179(4) Uani 1 1 d . . . H2A H 0.3017 0.4988 0.2071 0.021 Uiso 1 1 calc R . . C3 C 0.25731(16) 0.44493(14) 0.30324(13) 0.0227(5) Uani 1 1 d . . . H3A H 0.2045 0.4778 0.3123 0.027 Uiso 1 1 calc R . . C4 C 0.27784(17) 0.38439(14) 0.35281(13) 0.0236(5) Uani 1 1 d . . . H4A H 0.2404 0.3765 0.3969 0.028 Uiso 1 1 calc R . . C5 C 0.35291(16) 0.33586(13) 0.33755(12) 0.0212(5) Uani 1 1 d . . . H5A H 0.3666 0.2951 0.3722 0.025 Uiso 1 1 calc R . . C6 C 0.40987(15) 0.34427(12) 0.27303(12) 0.0168(4) Uani 1 1 d . . . C7 C 0.47837(15) 0.27919(12) 0.25894(12) 0.0173(4) Uani 1 1 d . . . C8 C 0.54174(15) 0.19078(12) 0.16940(12) 0.0183(4) Uani 1 1 d . . . C9 C 0.50090(17) 0.12201(13) 0.19538(14) 0.0255(5) Uani 1 1 d . . . H9A H 0.4524 0.1236 0.2326 0.031 Uiso 1 1 calc R . . C10 C 0.53125(18) 0.05157(14) 0.16675(15) 0.0305(6) Uani 1 1 d . . . H10A H 0.5031 0.0050 0.1842 0.037 Uiso 1 1 calc R . . C11 C 0.60279(18) 0.04897(13) 0.11265(14) 0.0280(5) Uani 1 1 d . . . H11A H 0.6229 0.0007 0.0928 0.034 Uiso 1 1 calc R . . C12 C 0.64489(17) 0.11672(13) 0.08764(13) 0.0230(5) Uani 1 1 d . . . H12A H 0.6943 0.1148 0.0512 0.028 Uiso 1 1 calc R . . C13 C 0.61455(16) 0.18800(12) 0.11617(12) 0.0185(4) Uani 1 1 d . . . C14 C 0.73633(15) 0.26843(12) 0.06688(11) 0.0168(4) Uani 1 1 d . . . C15 C 0.76553(15) 0.33515(12) 0.01714(11) 0.0153(4) Uani 1 1 d . . . C16 C 0.85148(15) 0.32460(13) -0.02119(12) 0.0183(4) Uani 1 1 d . . . H16A H 0.8884 0.2800 -0.0101 0.022 Uiso 1 1 calc R . . C17 C 0.88471(15) 0.37656(13) -0.07442(12) 0.0199(5) Uani 1 1 d . . . H17A H 0.9433 0.3674 -0.0993 0.024 Uiso 1 1 calc R . . C18 C 0.83200(15) 0.44219(12) -0.09141(12) 0.0175(4) Uani 1 1 d . . . H18A H 0.8538 0.4779 -0.1285 0.021 Uiso 1 1 calc R . . C19 C 0.74749(15) 0.45523(12) -0.05396(11) 0.0154(4) Uani 1 1 d . . . H19A H 0.7114 0.5002 -0.0654 0.018 Uiso 1 1 calc R . . C20 C 0.71449(14) 0.40292(12) 0.00064(11) 0.0139(4) Uani 1 1 d . . . C21 C 0.58950(14) 0.51309(12) 0.33563(11) 0.0144(4) Uani 1 1 d . . . C22 C 0.59731(15) 0.43281(12) 0.33202(12) 0.0164(4) Uani 1 1 d . . . H22A H 0.5911 0.4072 0.2843 0.020 Uiso 1 1 calc R . . C23 C 0.61416(16) 0.39008(13) 0.39806(12) 0.0212(5) Uani 1 1 d . . . H23A H 0.6186 0.3354 0.3956 0.025 Uiso 1 1 calc R . . C24 C 0.62438(16) 0.42759(14) 0.46707(12) 0.0240(5) Uani 1 1 d . . . H24A H 0.6357 0.3985 0.5122 0.029 Uiso 1 1 calc R . . C25 C 0.61824(16) 0.50771(14) 0.47118(12) 0.0216(5) Uani 1 1 d . . . H25A H 0.6259 0.5330 0.5189 0.026 Uiso 1 1 calc R . . C26 C 0.60099(15) 0.55068(13) 0.40592(12) 0.0185(4) Uani 1 1 d . . . H26A H 0.5970 0.6053 0.4088 0.022 Uiso 1 1 calc R . . C27 C 0.45128(15) 0.61039(12) 0.25350(11) 0.0153(4) Uani 1 1 d . . . C28 C 0.39433(16) 0.60537(13) 0.31804(12) 0.0187(4) Uani 1 1 d . . . H28A H 0.4170 0.5791 0.3622 0.022 Uiso 1 1 calc R . . C29 C 0.30468(16) 0.63874(13) 0.31766(13) 0.0207(5) Uani 1 1 d . . . H29A H 0.2657 0.6348 0.3614 0.025 Uiso 1 1 calc R . . C30 C 0.27162(16) 0.67797(13) 0.25360(13) 0.0232(5) Uani 1 1 d . . . H30A H 0.2104 0.7011 0.2538 0.028 Uiso 1 1 calc R . . C31 C 0.32799(16) 0.68343(13) 0.18914(13) 0.0233(5) Uani 1 1 d . . . H31A H 0.3055 0.7105 0.1454 0.028 Uiso 1 1 calc R . . C32 C 0.41711(16) 0.64924(13) 0.18887(12) 0.0198(5) Uani 1 1 d . . . H32A H 0.4552 0.6522 0.1446 0.024 Uiso 1 1 calc R . . C33 C 0.65372(15) 0.64423(12) 0.24939(12) 0.0158(4) Uani 1 1 d . . . H33A H 0.6385 0.6828 0.2094 0.019 Uiso 1 1 calc R . . H33B H 0.6544 0.6703 0.2996 0.019 Uiso 1 1 calc R . . C34 C 0.74942(15) 0.60584(12) 0.23410(11) 0.0165(4) Uani 1 1 d . . . H34A H 0.7685 0.5731 0.2779 0.020 Uiso 1 1 calc R . . H34B H 0.7990 0.6455 0.2264 0.020 Uiso 1 1 calc R . . C35 C 0.76257(14) 0.61365(12) 0.07175(11) 0.0140(4) Uani 1 1 d . . . C36 C 0.69909(15) 0.62716(12) 0.01170(11) 0.0158(4) Uani 1 1 d . . . H36A H 0.6382 0.6034 0.0115 0.019 Uiso 1 1 calc R . . C37 C 0.72493(16) 0.67546(12) -0.04808(12) 0.0192(4) Uani 1 1 d . . . H37A H 0.6818 0.6844 -0.0892 0.023 Uiso 1 1 calc R . . C38 C 0.81314(16) 0.71037(12) -0.04775(12) 0.0197(5) Uani 1 1 d . . . H38A H 0.8316 0.7415 -0.0897 0.024 Uiso 1 1 calc R . . C39 C 0.87515(16) 0.70012(12) 0.01388(13) 0.0196(5) Uani 1 1 d . . . H39A H 0.9349 0.7257 0.0148 0.024 Uiso 1 1 calc R . . C40 C 0.84974(15) 0.65265(12) 0.07387(12) 0.0176(4) Uani 1 1 d . . . H40A H 0.8914 0.6466 0.1164 0.021 Uiso 1 1 calc R . . C41 C 0.83076(15) 0.47600(12) 0.15400(11) 0.0160(4) Uani 1 1 d . . . C42 C 0.90800(15) 0.47322(12) 0.10532(12) 0.0179(4) Uani 1 1 d . . . H42A H 0.9132 0.5097 0.0651 0.022 Uiso 1 1 calc R . . C43 C 0.97782(16) 0.41709(13) 0.11538(13) 0.0224(5) Uani 1 1 d . . . H43A H 1.0304 0.4153 0.0818 0.027 Uiso 1 1 calc R . . C44 C 0.97116(17) 0.36397(14) 0.17388(14) 0.0253(5) Uani 1 1 d . . . H44A H 1.0194 0.3261 0.1809 0.030 Uiso 1 1 calc R . . C45 C 0.89387(18) 0.36601(14) 0.22241(14) 0.0265(5) Uani 1 1 d . . . H45A H 0.8890 0.3293 0.2624 0.032 Uiso 1 1 calc R . . C46 C 0.82395(16) 0.42131(13) 0.21268(13) 0.0215(5) Uani 1 1 d . . . H46A H 0.7710 0.4223 0.2459 0.026 Uiso 1 1 calc R . . C47 C 0.54611(17) 0.82850(16) 0.02003(15) 0.0318(6) Uani 1 1 d . . . H47A H 0.5323 0.8712 -0.0159 0.038 Uiso 1 1 calc R . . H47B H 0.5416 0.7793 -0.0086 0.038 Uiso 1 1 calc R . . Cl1 Cl 0.66212(5) 0.83918(5) 0.05744(5) 0.0489(2) Uani 1 1 d . . . Cl2 Cl 0.46176(5) 0.82884(5) 0.09311(4) 0.04754(19) 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 0.01537(13) 0.00840(13) 0.01392(13) 0.00040(9) -0.00179(10) 0.00083(10) Ni2 0.01319(13) 0.00965(13) 0.01136(12) -0.00087(9) -0.00024(9) 0.00003(10) S1 0.0138(2) 0.0112(2) 0.0128(2) 0.00018(18) -0.00101(18) 0.00020(19) S2 0.0144(2) 0.0106(2) 0.0121(2) -0.00030(18) -0.00099(18) 0.00211(19) P1 0.0154(3) 0.0108(2) 0.0120(2) -0.00084(19) -0.00005(19) 0.0001(2) P2 0.0136(2) 0.0122(3) 0.0133(2) -0.00080(19) -0.00093(19) -0.0003(2) O1 0.0241(8) 0.0235(9) 0.0239(8) 0.0100(7) -0.0021(7) 0.0000(7) O2 0.0223(8) 0.0204(8) 0.0262(8) 0.0035(6) -0.0028(7) 0.0101(7) N1 0.0190(9) 0.0109(9) 0.0201(9) 0.0018(7) -0.0035(7) -0.0013(7) N2 0.0200(9) 0.0103(9) 0.0178(8) 0.0001(7) -0.0040(7) 0.0024(7) C1 0.0143(10) 0.0178(11) 0.0144(9) -0.0011(8) -0.0010(8) -0.0044(8) C2 0.0194(11) 0.0175(11) 0.0167(10) -0.0002(8) -0.0005(8) -0.0026(9) C3 0.0202(11) 0.0224(12) 0.0257(11) -0.0057(9) 0.0030(9) -0.0015(9) C4 0.0256(12) 0.0259(12) 0.0195(11) -0.0019(9) 0.0059(9) -0.0095(10) C5 0.0256(12) 0.0208(12) 0.0174(10) 0.0033(9) -0.0003(9) -0.0090(9) C6 0.0157(10) 0.0164(11) 0.0181(10) 0.0012(8) -0.0019(8) -0.0049(8) C7 0.0149(10) 0.0159(11) 0.0210(10) 0.0046(8) -0.0027(8) -0.0059(8) C8 0.0200(11) 0.0111(10) 0.0236(11) 0.0026(8) -0.0067(9) -0.0013(8) C9 0.0220(12) 0.0169(12) 0.0374(13) 0.0053(10) -0.0067(10) -0.0039(9) C10 0.0322(14) 0.0124(11) 0.0464(15) 0.0060(10) -0.0159(12) -0.0053(10) C11 0.0350(14) 0.0121(11) 0.0364(13) -0.0029(9) -0.0168(11) 0.0043(10) C12 0.0283(12) 0.0156(11) 0.0250(11) -0.0032(9) -0.0101(9) 0.0054(9) C13 0.0214(11) 0.0119(10) 0.0220(11) 0.0000(8) -0.0099(9) 0.0012(9) C14 0.0222(11) 0.0148(10) 0.0132(9) -0.0046(8) -0.0045(8) 0.0040(9) C15 0.0177(10) 0.0143(10) 0.0137(9) -0.0034(8) -0.0044(8) 0.0027(8) C16 0.0159(10) 0.0164(11) 0.0224(11) -0.0053(8) -0.0028(8) 0.0049(8) C17 0.0158(10) 0.0227(12) 0.0212(11) -0.0069(9) 0.0019(8) 0.0030(9) C18 0.0176(10) 0.0175(11) 0.0172(10) -0.0026(8) -0.0001(8) -0.0016(9) C19 0.0173(10) 0.0127(10) 0.0161(10) -0.0029(8) -0.0025(8) 0.0005(8) C20 0.0153(10) 0.0138(10) 0.0127(9) -0.0040(7) -0.0020(8) 0.0020(8) C21 0.0131(10) 0.0159(10) 0.0143(9) 0.0002(8) -0.0010(8) -0.0019(8) C22 0.0157(10) 0.0182(11) 0.0152(10) -0.0002(8) -0.0011(8) -0.0017(8) C23 0.0214(11) 0.0176(11) 0.0244(11) 0.0044(9) 0.0004(9) 0.0023(9) C24 0.0222(11) 0.0327(14) 0.0172(10) 0.0083(9) -0.0008(9) 0.0030(10) C25 0.0189(11) 0.0326(13) 0.0132(10) -0.0027(9) 0.0004(8) -0.0037(10) C26 0.0164(10) 0.0218(11) 0.0173(10) -0.0013(9) 0.0016(8) -0.0034(9) C27 0.0169(10) 0.0128(10) 0.0162(10) -0.0047(8) 0.0000(8) 0.0006(8) C28 0.0228(11) 0.0170(11) 0.0162(10) -0.0034(8) -0.0004(9) -0.0001(9) C29 0.0206(11) 0.0190(11) 0.0227(11) -0.0080(9) 0.0030(9) -0.0002(9) C30 0.0178(11) 0.0189(12) 0.0328(13) -0.0073(9) -0.0016(9) 0.0026(9) C31 0.0250(12) 0.0180(11) 0.0269(12) 0.0003(9) -0.0052(9) 0.0051(9) C32 0.0235(11) 0.0185(11) 0.0176(10) -0.0020(8) 0.0011(9) 0.0011(9) C33 0.0186(10) 0.0134(10) 0.0155(9) -0.0024(8) -0.0001(8) -0.0017(8) C34 0.0170(10) 0.0181(11) 0.0143(10) -0.0018(8) -0.0007(8) -0.0017(8) C35 0.0160(10) 0.0108(10) 0.0153(9) -0.0038(8) 0.0018(8) 0.0006(8) C36 0.0169(10) 0.0116(10) 0.0189(10) -0.0038(8) -0.0010(8) -0.0018(8) C37 0.0271(12) 0.0121(10) 0.0184(10) -0.0004(8) -0.0029(9) 0.0019(9) C38 0.0283(12) 0.0110(10) 0.0199(11) 0.0009(8) 0.0041(9) -0.0005(9) C39 0.0194(11) 0.0113(10) 0.0283(12) -0.0007(9) 0.0050(9) -0.0015(9) C40 0.0164(10) 0.0150(11) 0.0213(10) -0.0035(8) -0.0010(8) -0.0003(8) C41 0.0170(10) 0.0139(10) 0.0170(10) -0.0032(8) -0.0039(8) -0.0010(8) C42 0.0198(11) 0.0149(10) 0.0191(10) -0.0033(8) -0.0007(8) -0.0019(9) C43 0.0188(11) 0.0191(12) 0.0292(12) -0.0071(9) 0.0002(9) 0.0028(9) C44 0.0239(12) 0.0170(11) 0.0348(13) -0.0052(10) -0.0092(10) 0.0056(10) C45 0.0325(13) 0.0185(12) 0.0285(12) 0.0035(9) -0.0044(10) 0.0013(10) C46 0.0214(11) 0.0196(12) 0.0234(11) 0.0017(9) 0.0005(9) -0.0009(9) C47 0.0217(12) 0.0358(15) 0.0378(14) -0.0043(11) -0.0052(11) -0.0021(11) Cl1 0.0213(3) 0.0490(5) 0.0762(5) -0.0380(4) -0.0135(3) 0.0098(3) Cl2 0.0343(4) 0.0713(6) 0.0370(4) 0.0113(4) -0.0005(3) -0.0115(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.8895(17) . ? Ni1 N1 1.8909(17) . ? Ni1 S2 2.1438(5) . ? Ni1 S1 2.1558(5) . ? Ni1 Ni2 2.8255(4) . ? Ni2 P1 2.1781(6) . ? Ni2 P2 2.1816(6) . ? Ni2 S1 2.2354(6) . ? Ni2 S2 2.2413(5) . ? S1 C1 1.776(2) . ? S2 C20 1.768(2) . ? P1 C27 1.810(2) . ? P1 C21 1.812(2) . ? P1 C33 1.829(2) . ? P2 C35 1.813(2) . ? P2 C41 1.817(2) . ? P2 C34 1.835(2) . ? O1 C7 1.244(3) . ? O2 C14 1.243(3) . ? N1 C7 1.359(3) . ? N1 C8 1.418(3) . ? N2 C14 1.361(3) . ? N2 C13 1.426(3) . ? C1 C2 1.393(3) . ? C1 C6 1.408(3) . ? C2 C3 1.388(3) . ? C2 H2A 0.9500 . ? C3 C4 1.391(3) . ? C3 H3A 0.9500 . ? C4 C5 1.378(3) . ? C4 H4A 0.9500 . ? C5 C6 1.401(3) . ? C5 H5A 0.9500 . ? C6 C7 1.505(3) . ? C8 C13 1.394(3) . ? C8 C9 1.401(3) . ? C9 C10 1.388(3) . ? C9 H9A 0.9500 . ? C10 C11 1.391(4) . ? C10 H10A 0.9500 . ? C11 C12 1.388(3) . ? C11 H11A 0.9500 . ? C12 C13 1.401(3) . ? C12 H12A 0.9500 . ? C14 C15 1.508(3) . ? C15 C16 1.401(3) . ? C15 C20 1.405(3) . ? C16 C17 1.382(3) . ? C16 H16A 0.9500 . ? C17 C18 1.388(3) . ? C17 H17A 0.9500 . ? C18 C19 1.383(3) . ? C18 H18A 0.9500 . ? C19 C20 1.401(3) . ? C19 H19A 0.9500 . ? C21 C22 1.397(3) . ? C21 C26 1.402(3) . ? C22 C23 1.393(3) . ? C22 H22A 0.9500 . ? C23 C24 1.380(3) . ? C23 H23A 0.9500 . ? C24 C25 1.393(3) . ? C24 H24A 0.9500 . ? C25 C26 1.385(3) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.396(3) . ? C27 C32 1.399(3) . ? C28 C29 1.387(3) . ? C28 H28A 0.9500 . ? C29 C30 1.389(3) . ? C29 H29A 0.9500 . ? C30 C31 1.391(3) . ? C30 H30A 0.9500 . ? C31 C32 1.386(3) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.528(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.393(3) . ? C35 C40 1.400(3) . ? C36 C37 1.393(3) . ? C36 H36A 0.9500 . ? C37 C38 1.380(3) . ? C37 H37A 0.9500 . ? C38 C39 1.393(3) . ? C38 H38A 0.9500 . ? C39 C40 1.385(3) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.390(3) . ? C41 C46 1.403(3) . ? C42 C43 1.392(3) . ? C42 H42A 0.9500 . ? C43 C44 1.382(3) . ? C43 H43A 0.9500 . ? C44 C45 1.388(3) . ? C44 H44A 0.9500 . ? C45 C46 1.382(3) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 Cl2 1.756(3) . ? C47 Cl1 1.762(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? 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 86.79(8) . . ? N2 Ni1 S2 97.29(5) . . ? N1 Ni1 S2 175.92(6) . . ? N2 Ni1 S1 176.58(6) . . ? N1 Ni1 S1 96.64(6) . . ? S2 Ni1 S1 79.29(2) . . ? N2 Ni1 Ni2 126.55(6) . . ? N1 Ni1 Ni2 125.67(5) . . ? S2 Ni1 Ni2 51.412(15) . . ? S1 Ni1 Ni2 51.198(15) . . ? P1 Ni2 P2 86.18(2) . . ? P1 Ni2 S1 99.13(2) . . ? P2 Ni2 S1 173.53(2) . . ? P1 Ni2 S2 172.59(2) . . ? P2 Ni2 S2 99.44(2) . . ? S1 Ni2 S2 75.585(19) . . ? P1 Ni2 Ni1 131.452(18) . . ? P2 Ni2 Ni1 124.842(18) . . ? S1 Ni2 Ni1 48.725(14) . . ? S2 Ni2 Ni1 48.387(14) . . ? C1 S1 Ni1 111.15(7) . . ? C1 S1 Ni2 121.95(7) . . ? Ni1 S1 Ni2 80.077(19) . . ? C20 S2 Ni1 111.46(7) . . ? C20 S2 Ni2 120.23(7) . . ? Ni1 S2 Ni2 80.201(18) . . ? C27 P1 C21 108.46(9) . . ? C27 P1 C33 106.16(10) . . ? C21 P1 C33 104.58(10) . . ? C27 P1 Ni2 116.76(7) . . ? C21 P1 Ni2 112.00(7) . . ? C33 P1 Ni2 108.02(7) . . ? C35 P2 C41 108.30(9) . . ? C35 P2 C34 103.17(9) . . ? C41 P2 C34 104.87(10) . . ? C35 P2 Ni2 117.33(7) . . ? C41 P2 Ni2 113.25(7) . . ? C34 P2 Ni2 108.74(7) . . ? C7 N1 C8 117.51(17) . . ? C7 N1 Ni1 127.22(14) . . ? C8 N1 Ni1 110.00(13) . . ? C14 N2 C13 117.07(17) . . ? C14 N2 Ni1 130.34(14) . . ? C13 N2 Ni1 110.12(14) . . ? C2 C1 C6 120.35(19) . . ? C2 C1 S1 115.88(16) . . ? C6 C1 S1 123.69(16) . . ? C3 C2 C1 121.0(2) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C2 C3 C4 119.3(2) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 122.6(2) . . ? C4 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C5 C6 C1 117.0(2) . . ? C5 C6 C7 115.29(19) . . ? C1 C6 C7 127.46(18) . . ? O1 C7 N1 123.6(2) . . ? O1 C7 C6 117.44(19) . . ? N1 C7 C6 118.61(18) . . ? C13 C8 C9 119.7(2) . . ? C13 C8 N1 115.58(18) . . ? C9 C8 N1 124.3(2) . . ? C10 C9 C8 120.1(2) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C12 C11 C10 120.1(2) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 120.0(2) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C8 C13 C12 119.9(2) . . ? C8 C13 N2 114.46(18) . . ? C12 C13 N2 125.2(2) . . ? O2 C14 N2 123.3(2) . . ? O2 C14 C15 116.72(19) . . ? N2 C14 C15 119.73(18) . . ? C16 C15 C20 116.87(19) . . ? C16 C15 C14 114.78(18) . . ? C20 C15 C14 128.18(19) . . ? C17 C16 C15 122.6(2) . . ? C17 C16 H16A 118.7 . . ? C15 C16 H16A 118.7 . . ? C16 C17 C18 119.7(2) . . ? C16 C17 H17A 120.2 . . ? C18 C17 H17A 120.2 . . ? C19 C18 C17 119.5(2) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C18 C19 C20 120.8(2) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C19 C20 C15 120.60(19) . . ? C19 C20 S2 114.84(15) . . ? C15 C20 S2 124.40(16) . . ? C22 C21 C26 119.61(19) . . ? C22 C21 P1 118.25(15) . . ? C26 C21 P1 122.12(16) . . ? C23 C22 C21 120.3(2) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C22 119.6(2) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C23 C24 C25 120.6(2) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C26 C25 C24 120.2(2) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C25 C26 C21 119.6(2) . . ? C25 C26 H26A 120.2 . . ? C21 C26 H26A 120.2 . . ? C28 C27 C32 119.44(19) . . ? C28 C27 P1 122.86(16) . . ? C32 C27 P1 117.65(15) . . ? C29 C28 C27 120.0(2) . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 120.3(2) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C29 C30 C31 120.1(2) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? C32 C31 C30 119.8(2) . . ? C32 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? C31 C32 C27 120.4(2) . . ? C31 C32 H32A 119.8 . . ? C27 C32 H32A 119.8 . . ? C34 C33 P1 105.09(14) . . ? C34 C33 H33A 110.7 . . ? P1 C33 H33A 110.7 . . ? C34 C33 H33B 110.7 . . ? P1 C33 H33B 110.7 . . ? H33A C33 H33B 108.8 . . ? C33 C34 P2 107.55(14) . . ? C33 C34 H34A 110.2 . . ? P2 C34 H34A 110.2 . . ? C33 C34 H34B 110.2 . . ? P2 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? C36 C35 C40 119.54(19) . . ? C36 C35 P2 121.79(16) . . ? C40 C35 P2 118.67(16) . . ? C35 C36 C37 120.0(2) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C38 C37 C36 120.1(2) . . ? C38 C37 H37A 119.9 . . ? C36 C37 H37A 119.9 . . ? C37 C38 C39 120.2(2) . . ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 . . ? C40 C39 C38 120.0(2) . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C39 C40 C35 120.0(2) . . ? C39 C40 H40A 120.0 . . ? C35 C40 H40A 120.0 . . ? C42 C41 C46 119.2(2) . . ? C42 C41 P2 124.62(16) . . ? C46 C41 P2 116.22(16) . . ? C43 C42 C41 120.1(2) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 120.4(2) . . ? C42 C43 H43A 119.8 . . ? C44 C43 H43A 119.8 . . ? C43 C44 C45 119.9(2) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C46 C45 C44 120.2(2) . . ? C46 C45 H45A 119.9 . . ? C44 C45 H45A 119.9 . . ? C45 C46 C41 120.3(2) . . ? C45 C46 H46A 119.8 . . ? C41 C46 H46A 119.8 . . ? Cl2 C47 Cl1 110.99(15) . . ? Cl2 C47 H47A 109.4 . . ? Cl1 C47 H47A 109.4 . . ? Cl2 C47 H47B 109.4 . . ? Cl1 C47 H47B 109.4 . . ? H47A C47 H47B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.895 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.071