Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author ;Dr Maria Carla Aragoni Dipartimento di Chimica Inorganica ed Analitica Universita degli Studi di Cagliari Cittadella Universitaria di Monserr Cagliari 09042 ITALY ; _publ_contact_author_email ARAGONI@UNICA.IT _publ_contact_author_name 'Dr Maria Carla Aragoni' loop_ _publ_author_name M.C.Aragoni 'Massimiliano Arca ' 'Miriam Crespo ' 'Francesco A Devillanova ' 'M. Hursthouse ' ; S.L.Huth ; 'Francesco Isaia ' 'Vito Lippolis ' data_04slh0878 _database_code_depnum_ccdc_archive 'CCDC 644007' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H28 N2 Ni O4 P2 S6' _chemical_formula_weight 745.51 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3232(8) _cell_length_b 18.5768(12) _cell_length_c 12.4832(8) _cell_angle_alpha 90.00 _cell_angle_beta 111.061(4) _cell_angle_gamma 90.00 _cell_volume 3099.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7369 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7997 _exptl_absorpt_correction_T_max 0.8349 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\F & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69288 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7109 _reflns_number_gt 6481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0286P)^2^+3.4611P] 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 7109 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 C1 C 0.79707(13) 0.21326(10) 0.17592(16) 0.0203(4) Uani 1 1 d . . . C2 C 0.83825(14) 0.26790(10) 0.25508(17) 0.0236(4) Uani 1 1 d . . . H2 H 0.7991 0.2896 0.2936 0.028 Uiso 1 1 calc R . . C3 C 0.93522(14) 0.29098(10) 0.27845(18) 0.0260(4) Uani 1 1 d . . . H3 H 0.9619 0.3289 0.3317 0.031 Uiso 1 1 calc R . . C4 C 0.99357(13) 0.25872(10) 0.22426(17) 0.0221(4) Uani 1 1 d . . . C5 C 0.95438(16) 0.20368(13) 0.1464(2) 0.0329(5) Uani 1 1 d . . . H5 H 0.9942 0.1811 0.1095 0.039 Uiso 1 1 calc R . . C6 C 0.85654(16) 0.18172(13) 0.1227(2) 0.0336(5) Uani 1 1 d . . . H6 H 0.8297 0.1442 0.0688 0.040 Uiso 1 1 calc R . . C7 C 1.15370(15) 0.24837(12) 0.20908(19) 0.0296(4) Uani 1 1 d . . . H7A H 1.1619 0.1983 0.2357 0.044 Uiso 1 1 calc R . . H7B H 1.2190 0.2724 0.2357 0.044 Uiso 1 1 calc R . . H7C H 1.1253 0.2493 0.1250 0.044 Uiso 1 1 calc R . . C8 C 0.59001(15) 0.05977(11) 0.07222(18) 0.0278(4) Uani 1 1 d . . . H8A H 0.5525 0.0639 0.1240 0.042 Uiso 1 1 calc R . . H8B H 0.6087 0.0094 0.0681 0.042 Uiso 1 1 calc R . . H8C H 0.5482 0.0765 -0.0045 0.042 Uiso 1 1 calc R . . C10 C 0.65675(13) 0.38375(10) 0.30147(15) 0.0186(3) Uani 1 1 d . . . H10 H 0.6297 0.3607 0.3518 0.022 Uiso 1 1 calc R . . C11 C 0.73414(13) 0.43208(10) 0.34728(16) 0.0209(4) Uani 1 1 d . . . H11 H 0.7588 0.4428 0.4270 0.025 Uiso 1 1 calc R . . C12 C 0.77511(13) 0.46471(10) 0.27452(16) 0.0199(4) Uani 1 1 d . . . C13 C 0.73621(14) 0.44869(10) 0.15838(17) 0.0216(4) Uani 1 1 d . . . H13 H 0.7627 0.4705 0.1066 0.026 Uiso 1 1 calc R . . C14 C 0.65769(13) 0.40007(10) 0.11940(16) 0.0194(3) Uani 1 1 d . . . H14 H 0.6309 0.3892 0.0397 0.023 Uiso 1 1 calc R . . C15 C 0.76438(13) 0.61565(10) 0.44005(16) 0.0210(4) Uani 1 1 d . . . C16 C 0.74383(14) 0.64580(10) 0.53106(16) 0.0234(4) Uani 1 1 d . . . H16 H 0.7836 0.6344 0.6082 0.028 Uiso 1 1 calc R . . C17 C 0.66414(14) 0.69280(10) 0.50667(16) 0.0209(4) Uani 1 1 d . . . H17 H 0.6500 0.7132 0.5690 0.025 Uiso 1 1 calc R . . C18 C 0.62391(13) 0.67852(10) 0.31343(15) 0.0178(3) Uani 1 1 d . . . H18 H 0.5814 0.6894 0.2371 0.021 Uiso 1 1 calc R . . C19 C 0.70075(14) 0.63006(10) 0.32901(16) 0.0208(4) Uani 1 1 d . . . H19 H 0.7097 0.6072 0.2653 0.025 Uiso 1 1 calc R . . C20 C 0.21702(13) 0.41367(10) 0.08364(15) 0.0188(3) Uani 1 1 d . . . C21 C 0.14810(14) 0.37788(11) -0.00810(17) 0.0232(4) Uani 1 1 d . . . H21 H 0.1703 0.3533 -0.0613 0.028 Uiso 1 1 calc R . . C22 C 0.04651(14) 0.37725(11) -0.02382(17) 0.0250(4) Uani 1 1 d . . . H22 H 0.0000 0.3524 -0.0871 0.030 Uiso 1 1 calc R . . C23 C 0.01407(13) 0.41319(10) 0.05383(17) 0.0223(4) Uani 1 1 d . . . C24 C 0.08274(14) 0.45030(11) 0.14591(17) 0.0239(4) Uani 1 1 d . . . H24 H 0.0603 0.4755 0.1984 0.029 Uiso 1 1 calc R . . C25 C 0.18278(14) 0.45045(10) 0.16087(16) 0.0220(4) Uani 1 1 d . . . H25 H 0.2291 0.4756 0.2239 0.026 Uiso 1 1 calc R . . C26 C -0.15455(15) 0.37455(13) -0.0398(2) 0.0342(5) Uani 1 1 d . . . H26A H -0.1558 0.3910 -0.1149 0.051 Uiso 1 1 calc R . . H26B H -0.2208 0.3812 -0.0350 0.051 Uiso 1 1 calc R . . H26C H -0.1365 0.3234 -0.0301 0.051 Uiso 1 1 calc R . . C27 C 0.47288(14) 0.52063(10) 0.16598(18) 0.0238(4) Uani 1 1 d . . . H27A H 0.5143 0.4969 0.2373 0.036 Uiso 1 1 calc R . . H27B H 0.4740 0.5728 0.1782 0.036 Uiso 1 1 calc R . . H27C H 0.4993 0.5098 0.1054 0.036 Uiso 1 1 calc R . . N1 N 0.61773(11) 0.36765(8) 0.18892(12) 0.0164(3) Uani 1 1 d . . . N2 N 0.60585(11) 0.71113(8) 0.39984(13) 0.0164(3) Uani 1 1 d . . . O1 O 1.08837(10) 0.28474(8) 0.25387(14) 0.0296(3) Uani 1 1 d . . . O2 O 0.67925(9) 0.10337(7) 0.11518(12) 0.0232(3) Uani 1 1 d . . . O3 O -0.08219(10) 0.41550(8) 0.04880(13) 0.0292(3) Uani 1 1 d . . . O4 O 0.37163(9) 0.49483(7) 0.13223(11) 0.0196(3) Uani 1 1 d . . . P1 P 0.66859(3) 0.18711(2) 0.14162(4) 0.01636(9) Uani 1 1 d . . . P2 P 0.34913(3) 0.41009(2) 0.11361(4) 0.01570(9) Uani 1 1 d . . . S1 S 0.62448(3) 0.20430(2) 0.27320(4) 0.01731(9) Uani 1 1 d . . . S2 S 0.57545(3) 0.23698(3) 0.00298(4) 0.01910(9) Uani 1 1 d . . . S3 S 0.42036(3) 0.35440(2) 0.25645(4) 0.01682(9) Uani 1 1 d . . . S4 S 0.38677(3) 0.37148(2) -0.01417(4) 0.01829(9) Uani 1 1 d . . . S5 S 0.87517(3) 0.52772(3) 0.32126(5) 0.02522(11) Uani 1 1 d . . . S6 S 0.87373(4) 0.56115(3) 0.47613(4) 0.02609(11) Uani 1 1 d . . . Ni1 Ni 0.503522(16) 0.290593(12) 0.135205(18) 0.01392(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 C1 0.0157(8) 0.0218(9) 0.0236(9) -0.0018(7) 0.0074(7) -0.0013(7) C2 0.0181(9) 0.0221(9) 0.0306(10) -0.0073(8) 0.0087(8) 0.0016(7) C3 0.0197(9) 0.0219(9) 0.0347(11) -0.0094(8) 0.0077(8) -0.0020(7) C4 0.0152(8) 0.0211(9) 0.0282(10) 0.0006(7) 0.0057(7) -0.0019(7) C5 0.0225(10) 0.0424(13) 0.0393(12) -0.0172(10) 0.0177(9) -0.0066(9) C6 0.0247(10) 0.0419(13) 0.0384(12) -0.0228(10) 0.0164(9) -0.0120(9) C7 0.0196(9) 0.0348(11) 0.0378(11) -0.0011(9) 0.0144(9) -0.0014(8) C8 0.0262(10) 0.0229(10) 0.0317(11) -0.0050(8) 0.0073(8) -0.0096(8) C10 0.0169(8) 0.0186(8) 0.0198(8) 0.0008(7) 0.0061(7) 0.0015(7) C11 0.0184(8) 0.0199(9) 0.0222(9) -0.0001(7) 0.0044(7) 0.0022(7) C12 0.0140(8) 0.0162(8) 0.0286(9) -0.0004(7) 0.0065(7) 0.0015(6) C13 0.0199(9) 0.0198(9) 0.0285(10) 0.0037(7) 0.0129(8) 0.0010(7) C14 0.0192(8) 0.0189(8) 0.0223(9) 0.0024(7) 0.0100(7) 0.0015(7) C15 0.0152(8) 0.0174(9) 0.0282(9) -0.0001(7) 0.0052(7) 0.0002(7) C16 0.0225(9) 0.0230(9) 0.0193(9) 0.0012(7) 0.0010(7) 0.0018(7) C17 0.0218(9) 0.0218(9) 0.0184(8) 0.0001(7) 0.0063(7) 0.0007(7) C18 0.0158(8) 0.0187(8) 0.0192(8) -0.0015(7) 0.0067(7) -0.0012(7) C19 0.0192(9) 0.0197(9) 0.0243(9) -0.0025(7) 0.0086(7) 0.0001(7) C20 0.0169(8) 0.0178(8) 0.0217(9) 0.0021(7) 0.0068(7) 0.0020(7) C21 0.0192(9) 0.0261(10) 0.0245(9) -0.0046(8) 0.0079(7) 0.0006(7) C22 0.0177(9) 0.0287(10) 0.0260(9) -0.0078(8) 0.0048(7) -0.0021(7) C23 0.0148(8) 0.0246(9) 0.0262(9) -0.0007(8) 0.0058(7) 0.0013(7) C24 0.0192(9) 0.0284(10) 0.0244(9) -0.0057(8) 0.0083(7) 0.0011(7) C25 0.0180(9) 0.0250(9) 0.0220(9) -0.0032(7) 0.0060(7) -0.0011(7) C26 0.0165(9) 0.0420(13) 0.0417(12) -0.0160(10) 0.0075(9) -0.0068(9) C27 0.0181(9) 0.0190(9) 0.0343(10) -0.0012(8) 0.0095(8) -0.0022(7) N1 0.0145(7) 0.0165(7) 0.0185(7) 0.0011(6) 0.0066(6) 0.0005(5) N2 0.0144(7) 0.0166(7) 0.0187(7) 0.0000(6) 0.0064(6) -0.0004(5) O1 0.0151(6) 0.0294(8) 0.0442(9) -0.0074(6) 0.0105(6) -0.0040(5) O2 0.0178(6) 0.0193(6) 0.0306(7) -0.0070(5) 0.0065(5) -0.0024(5) O3 0.0147(6) 0.0391(8) 0.0332(8) -0.0119(6) 0.0080(6) -0.0036(6) O4 0.0159(6) 0.0163(6) 0.0254(6) 0.0007(5) 0.0062(5) -0.0002(5) P1 0.0134(2) 0.0174(2) 0.0187(2) -0.00296(17) 0.00623(17) -0.00085(16) P2 0.0140(2) 0.0156(2) 0.0175(2) 0.00108(16) 0.00573(17) 0.00099(16) S1 0.0153(2) 0.0205(2) 0.0166(2) 0.00169(16) 0.00632(16) 0.00118(16) S2 0.0185(2) 0.0244(2) 0.0158(2) -0.00105(17) 0.00777(16) 0.00025(17) S3 0.0161(2) 0.0191(2) 0.01579(19) 0.00151(16) 0.00634(16) 0.00114(16) S4 0.0187(2) 0.0207(2) 0.01620(19) 0.00224(16) 0.00712(16) 0.00240(16) S5 0.0171(2) 0.0215(2) 0.0379(3) -0.0051(2) 0.0110(2) -0.00222(17) S6 0.0175(2) 0.0231(2) 0.0317(3) -0.00375(19) 0.00151(19) 0.00306(17) Ni1 0.01241(11) 0.01538(11) 0.01458(11) 0.00045(8) 0.00560(8) -0.00043(8) _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 C1 C6 1.384(3) . ? C1 C2 1.391(3) . ? C1 P1 1.7998(18) . ? C2 C3 1.381(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 O1 1.361(2) . ? C4 C5 1.383(3) . ? C5 C6 1.386(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O1 1.422(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O2 1.444(2) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 N1 1.346(2) . ? C10 C11 1.381(3) . ? C10 H10 0.9500 . ? C11 C12 1.386(3) . ? C11 H11 0.9500 . ? C12 C13 1.386(3) . ? C12 S5 1.7787(18) . ? C13 C14 1.387(3) . ? C13 H13 0.9500 . ? C14 N1 1.342(2) . ? C14 H14 0.9500 . ? C15 C19 1.384(3) . ? C15 C16 1.390(3) . ? C15 S6 1.7815(18) . ? C16 C17 1.381(3) . ? C16 H16 0.9500 . ? C17 N2 1.338(2) . ? C17 H17 0.9500 . ? C18 N2 1.341(2) . ? C18 C19 1.380(2) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.384(3) . ? C20 C25 1.406(3) . ? C20 P2 1.7933(18) . ? C21 C22 1.397(3) . ? C21 H21 0.9500 . ? C22 C23 1.387(3) . ? C22 H22 0.9500 . ? C23 O3 1.358(2) . ? C23 C24 1.397(3) . ? C24 C25 1.377(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 O3 1.433(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O4 1.439(2) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? N1 Ni1 2.0943(15) . ? N2 Ni1 2.0814(15) 2_655 ? O2 P1 1.6088(14) . ? O4 P2 1.6070(13) . ? P1 S1 1.9862(6) . ? P1 S2 1.9935(6) . ? P2 S4 1.9919(6) . ? P2 S3 1.9958(6) . ? S1 Ni1 2.5287(5) . ? S2 Ni1 2.4494(5) . ? S3 Ni1 2.5318(5) . ? S4 Ni1 2.5080(5) . ? S5 S6 2.0378(7) . ? Ni1 N2 2.0814(15) 2_645 ? 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 C6 C1 C2 118.21(17) . . ? C6 C1 P1 121.63(15) . . ? C2 C1 P1 120.14(14) . . ? C3 C2 C1 120.93(18) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.99(18) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? O1 C4 C5 124.51(18) . . ? O1 C4 C3 115.57(17) . . ? C5 C4 C3 119.92(17) . . ? C4 C5 C6 119.44(19) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 121.50(19) . . ? C1 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C10 C11 123.19(17) . . ? N1 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C10 C11 C12 118.62(17) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C11 C12 C13 119.08(17) . . ? C11 C12 S5 123.64(15) . . ? C13 C12 S5 117.28(14) . . ? C12 C13 C14 118.52(17) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? N1 C14 C13 123.09(17) . . ? N1 C14 H14 118.5 . . ? C13 C14 H14 118.5 . . ? C19 C15 C16 118.95(17) . . ? C19 C15 S6 124.46(15) . . ? C16 C15 S6 116.58(14) . . ? C17 C16 C15 118.39(17) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? N2 C17 C16 123.41(17) . . ? N2 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? N2 C18 C19 123.77(17) . . ? N2 C18 H18 118.1 . . ? C19 C18 H18 118.1 . . ? C18 C19 C15 118.16(17) . . ? C18 C19 H19 120.9 . . ? C15 C19 H19 120.9 . . ? C21 C20 C25 118.68(17) . . ? C21 C20 P2 122.70(14) . . ? C25 C20 P2 118.48(14) . . ? C20 C21 C22 121.17(17) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 119.43(18) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? O3 C23 C22 124.91(17) . . ? O3 C23 C24 115.17(17) . . ? C22 C23 C24 119.92(17) . . ? C25 C24 C23 120.22(18) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C20 120.56(17) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? O3 C26 H26A 109.5 . . ? O3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O4 C27 H27A 109.5 . . ? O4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C14 N1 C10 117.50(16) . . ? C14 N1 Ni1 124.43(12) . . ? C10 N1 Ni1 118.02(12) . . ? C17 N2 C18 117.07(16) . . ? C17 N2 Ni1 122.87(12) . 2_655 ? C18 N2 Ni1 119.97(12) . 2_655 ? C4 O1 C7 117.25(16) . . ? C8 O2 P1 118.81(12) . . ? C23 O3 C26 117.35(16) . . ? C27 O4 P2 119.81(11) . . ? O2 P1 C1 98.37(8) . . ? O2 P1 S1 114.02(6) . . ? C1 P1 S1 111.21(6) . . ? O2 P1 S2 110.76(6) . . ? C1 P1 S2 112.90(7) . . ? S1 P1 S2 109.31(3) . . ? O4 P2 C20 97.79(8) . . ? O4 P2 S4 111.76(5) . . ? C20 P2 S4 114.54(6) . . ? O4 P2 S3 111.53(5) . . ? C20 P2 S3 111.59(6) . . ? S4 P2 S3 109.28(3) . . ? P1 S1 Ni1 83.24(2) . . ? P1 S2 Ni1 85.20(2) . . ? P2 S3 Ni1 84.71(2) . . ? P2 S4 Ni1 85.44(2) . . ? C12 S5 S6 103.31(7) . . ? C15 S6 S5 103.95(7) . . ? N2 Ni1 N1 173.90(6) 2_645 . ? N2 Ni1 S2 92.13(4) 2_645 . ? N1 Ni1 S2 91.40(4) . . ? N2 Ni1 S4 91.05(4) 2_645 . ? N1 Ni1 S4 93.67(4) . . ? S2 Ni1 S4 94.136(17) . . ? N2 Ni1 S1 88.46(4) 2_645 . ? N1 Ni1 S1 87.14(4) . . ? S2 Ni1 S1 81.384(16) . . ? S4 Ni1 S1 175.470(17) . . ? N2 Ni1 S3 88.71(4) 2_645 . ? N1 Ni1 S3 88.27(4) . . ? S2 Ni1 S3 174.462(17) . . ? S4 Ni1 S3 80.372(16) . . ? S1 Ni1 S3 104.116(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.673 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.063 # Attachment '2dpts.cif' data_04slh0877 _database_code_depnum_ccdc_archive 'CCDC 644008' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H32 N2 Ni O4 P2 S7' _chemical_formula_weight 805.63 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.618(3) _cell_length_b 8.0323(16) _cell_length_c 25.068(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.63(3) _cell_angle_gamma 90.00 _cell_volume 3486.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4227 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'cut shard' _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8431 _exptl_absorpt_correction_T_max 0.9783 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\F & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21889 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3979 _reflns_number_gt 3782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick ,1997)' _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^)+(0.1131P)^2^+2.3627P] 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 3979 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.1941 _refine_ls_wR_factor_gt 0.1914 _refine_ls_goodness_of_fit_ref 1.485 _refine_ls_restrained_S_all 1.485 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.12872(16) 0.7288(3) 0.15076(11) 0.0147(5) Uani 1 1 d . . . C2 C 0.18693(16) 0.8307(4) 0.17847(11) 0.0173(5) Uani 1 1 d . . . H2 H 0.2118 0.9084 0.1588 0.021 Uiso 1 1 calc R . . C3 C 0.20916(16) 0.8197(4) 0.23469(11) 0.0190(6) Uani 1 1 d . . . H3 H 0.2490 0.8893 0.2533 0.023 Uiso 1 1 calc R . . C4 C 0.17256(17) 0.7064(4) 0.26327(11) 0.0179(6) Uani 1 1 d . . . C5 C 0.11322(17) 0.6054(4) 0.23596(11) 0.0207(6) Uani 1 1 d . . . H5 H 0.0876 0.5292 0.2556 0.025 Uiso 1 1 calc R . . C6 C 0.09195(17) 0.6171(4) 0.18004(11) 0.0199(6) Uani 1 1 d . . . H6 H 0.0518 0.5480 0.1615 0.024 Uiso 1 1 calc R . . C7 C 0.2501(2) 0.7861(5) 0.34778(13) 0.0324(8) Uani 1 1 d . . . H7A H 0.2976 0.7720 0.3331 0.049 Uiso 1 1 calc R . . H7B H 0.2597 0.7536 0.3861 0.049 Uiso 1 1 calc R . . H7C H 0.2340 0.9030 0.3445 0.049 Uiso 1 1 calc R . . C8 C 0.15282(17) 0.9227(4) 0.00751(11) 0.0186(6) Uani 1 1 d . . . H8A H 0.0992 0.9310 -0.0128 0.022 Uiso 1 1 calc R . . H8B H 0.1797 0.8339 -0.0092 0.022 Uiso 1 1 calc R . . C9 C 0.19390(16) 1.0859(4) 0.00578(12) 0.0193(6) Uani 1 1 d . . . H9A H 0.1659 1.1733 0.0214 0.029 Uiso 1 1 calc R . . H9B H 0.1961 1.1139 -0.0320 0.029 Uiso 1 1 calc R . . H9C H 0.2465 1.0769 0.0268 0.029 Uiso 1 1 calc R . . C10 C 0.01429(16) 0.2361(3) 0.08897(11) 0.0147(5) Uani 1 1 d . . . H10 H 0.0560 0.1989 0.0729 0.018 Uiso 1 1 calc R . . C11 C 0.00000(17) 0.1536(3) 0.13446(11) 0.0179(5) Uani 1 1 d . . . H11 H 0.0310 0.0620 0.1492 0.021 Uiso 1 1 calc R . . C12 C -0.06101(17) 0.2083(4) 0.15808(11) 0.0178(6) Uani 1 1 d . . . C13 C -0.10594(17) 0.3412(4) 0.13462(11) 0.0196(6) Uani 1 1 d . . . H13 H -0.1484 0.3800 0.1496 0.024 Uiso 1 1 calc R . . C14 C -0.08727(16) 0.4153(4) 0.08910(11) 0.0167(5) Uani 1 1 d . . . H14 H -0.1182 0.5056 0.0731 0.020 Uiso 1 1 calc R . . N1 N -0.02771(13) 0.3665(3) 0.06614(9) 0.0134(4) Uani 1 1 d . . . O1 O 0.19028(13) 0.6832(3) 0.31801(8) 0.0256(5) Uani 1 1 d . . . O2 O 0.15292(12) 0.8841(2) 0.06464(8) 0.0174(4) Uani 1 1 d . . . P1 P 0.10298(4) 0.72840(8) 0.07790(3) 0.0128(2) Uani 1 1 d . . . S1 S 0.13607(4) 0.51727(8) 0.04721(3) 0.0140(2) Uani 1 1 d . . . S2 S -0.00944(4) 0.76254(8) 0.05112(3) 0.0147(2) Uani 1 1 d . . . S3 S -0.08837(5) 0.12316(10) 0.21694(3) 0.0236(2) Uani 1 1 d . . . S4 S 0.0000 -0.03112(13) 0.2500 0.0226(3) Uani 1 2 d S . . Ni1 Ni 0.0000 0.5000 0.0000 0.01086(19) Uani 1 2 d S . . 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 C1 0.0179(13) 0.0125(12) 0.0123(12) -0.0023(9) -0.0004(10) 0.0009(9) C2 0.0186(12) 0.0165(13) 0.0160(12) -0.0016(10) 0.0011(10) -0.0033(10) C3 0.0188(13) 0.0197(13) 0.0166(13) -0.0035(11) -0.0017(10) -0.0040(11) C4 0.0215(13) 0.0179(13) 0.0124(12) -0.0009(10) -0.0017(10) 0.0027(11) C5 0.0259(14) 0.0195(14) 0.0152(13) 0.0018(10) -0.0003(11) -0.0053(11) C6 0.0246(14) 0.0188(13) 0.0137(13) -0.0008(10) -0.0030(10) -0.0061(11) C7 0.043(2) 0.0348(19) 0.0132(13) -0.0005(12) -0.0104(13) -0.0102(15) C8 0.0247(14) 0.0167(13) 0.0143(12) 0.0005(10) 0.0030(10) -0.0030(11) C9 0.0198(13) 0.0174(13) 0.0216(13) 0.0006(11) 0.0064(10) -0.0034(10) C10 0.0198(13) 0.0123(12) 0.0120(12) -0.0003(9) 0.0031(10) 0.0012(9) C11 0.0249(14) 0.0151(13) 0.0136(12) 0.0013(10) 0.0033(10) 0.0009(10) C12 0.0233(14) 0.0183(14) 0.0122(12) -0.0002(10) 0.0046(10) -0.0052(11) C13 0.0205(13) 0.0223(14) 0.0172(13) -0.0038(11) 0.0065(10) -0.0002(11) C14 0.0159(12) 0.0195(14) 0.0142(12) -0.0020(10) 0.0015(9) 0.0011(10) N1 0.0165(10) 0.0125(11) 0.0104(9) -0.0019(8) 0.0005(8) 0.0001(8) O1 0.0355(12) 0.0263(12) 0.0112(10) 0.0007(8) -0.0054(8) -0.0065(10) O2 0.0234(10) 0.0148(9) 0.0129(9) -0.0002(7) 0.0007(7) -0.0045(8) P1 0.0159(4) 0.0109(4) 0.0105(4) -0.0012(2) -0.0006(3) -0.0004(2) S1 0.0153(4) 0.0128(4) 0.0129(4) -0.0015(2) 0.0001(3) 0.0023(2) S2 0.0164(4) 0.0130(4) 0.0133(4) -0.0023(2) -0.0009(3) 0.0034(2) S3 0.0291(4) 0.0270(4) 0.0163(4) 0.0041(3) 0.0084(3) -0.0014(3) S4 0.0368(6) 0.0164(5) 0.0142(5) 0.000 0.0040(4) 0.000 Ni1 0.0132(3) 0.0101(3) 0.0086(3) -0.00092(14) 0.0001(2) 0.00084(15) _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 C1 C6 1.393(4) . ? C1 C2 1.393(4) . ? C1 P1 1.799(3) . ? C2 C3 1.394(4) . ? C2 H2 0.9500 . ? C3 C4 1.389(4) . ? C3 H3 0.9500 . ? C4 O1 1.363(3) . ? C4 C5 1.398(4) . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O1 1.436(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O2 1.465(3) . ? C8 C9 1.502(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N1 1.348(4) . ? C10 C11 1.382(4) . ? C10 H10 0.9500 . ? C11 C12 1.391(4) . ? C11 H11 0.9500 . ? C12 C13 1.393(4) . ? C12 S3 1.772(3) . ? C13 C14 1.379(4) . ? C13 H13 0.9500 . ? C14 N1 1.345(3) . ? C14 H14 0.9500 . ? N1 Ni1 2.106(2) . ? O2 P1 1.599(2) . ? P1 S2 1.9897(11) . ? P1 S1 1.9932(10) . ? S1 Ni1 2.4738(10) . ? S2 Ni1 2.4891(7) . ? S3 S4 2.0422(11) . ? S4 S3 2.0422(11) 2 ? Ni1 N1 2.106(2) 5_565 ? Ni1 S1 2.4738(10) 5_565 ? Ni1 S2 2.4891(7) 5_565 ? 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 C6 C1 C2 119.1(3) . . ? C6 C1 P1 118.6(2) . . ? C2 C1 P1 122.1(2) . . ? C1 C2 C3 120.7(3) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 119.5(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? O1 C4 C3 124.5(3) . . ? O1 C4 C5 115.2(3) . . ? C3 C4 C5 120.3(3) . . ? C6 C5 C4 119.6(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C1 120.8(3) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 C8 C9 107.4(2) . . ? O2 C8 H8A 110.2 . . ? C9 C8 H8A 110.2 . . ? O2 C8 H8B 110.2 . . ? C9 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 123.6(3) . . ? N1 C10 H10 118.2 . . ? C11 C10 H10 118.2 . . ? C10 C11 C12 118.2(3) . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? C11 C12 C13 119.1(3) . . ? C11 C12 S3 125.7(2) . . ? C13 C12 S3 115.3(2) . . ? C14 C13 C12 118.4(3) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? N1 C14 C13 123.6(3) . . ? N1 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? C14 N1 C10 117.1(2) . . ? C14 N1 Ni1 120.09(19) . . ? C10 N1 Ni1 122.76(18) . . ? C4 O1 C7 117.1(2) . . ? C8 O2 P1 117.87(17) . . ? O2 P1 C1 99.45(12) . . ? O2 P1 S2 111.95(8) . . ? C1 P1 S2 113.02(10) . . ? O2 P1 S1 111.95(9) . . ? C1 P1 S1 110.90(9) . . ? S2 P1 S1 109.32(4) . . ? P1 S1 Ni1 84.59(3) . . ? P1 S2 Ni1 84.26(3) . . ? C12 S3 S4 105.54(10) . . ? S3 S4 S3 105.28(7) 2 . ? N1 Ni1 N1 180.00(13) . 5_565 ? N1 Ni1 S1 89.82(7) . . ? N1 Ni1 S1 90.18(7) 5_565 . ? N1 Ni1 S1 90.18(7) . 5_565 ? N1 Ni1 S1 89.82(7) 5_565 5_565 ? S1 Ni1 S1 180.00(4) . 5_565 ? N1 Ni1 S2 91.22(6) . 5_565 ? N1 Ni1 S2 88.78(6) 5_565 5_565 ? S1 Ni1 S2 98.22(3) . 5_565 ? S1 Ni1 S2 81.78(3) 5_565 5_565 ? N1 Ni1 S2 88.78(6) . . ? N1 Ni1 S2 91.22(6) 5_565 . ? S1 Ni1 S2 81.78(3) . . ? S1 Ni1 S2 98.22(3) 5_565 . ? S2 Ni1 S2 180.00(4) 5_565 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.940 _refine_diff_density_min -3.941 _refine_diff_density_rms 0.583 # Attachment '3dps.cif' data_04slh0874 _database_code_depnum_ccdc_archive 'CCDC 644009' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 N2 Ni O4 P2 S5' _chemical_formula_weight 617.37 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1601(4) _cell_length_b 9.4126(11) _cell_length_c 17.9991(9) _cell_angle_alpha 99.453(7) _cell_angle_beta 99.986(5) _cell_angle_gamma 94.511(9) _cell_volume 1334.85(18) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6130 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'cut block' _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 1.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8839 _exptl_absorpt_correction_T_max 0.9280 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\F & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49804 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6113 _reflns_number_gt 5918 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick ,1997)' _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^)+(0.0680P)^2^+1.8065P] 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 6113 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1264 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.212 _refine_ls_restrained_S_all 1.212 _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 C1 C 0.4916(3) 0.6770(3) 0.64256(16) 0.0217(5) Uani 1 1 d . . . H1A H 0.4941 0.5790 0.6130 0.026 Uiso 1 1 calc R . . H1B H 0.4077 0.6711 0.6759 0.026 Uiso 1 1 calc R . . C2 C 0.6621(4) 0.7332(3) 0.69048(18) 0.0278(6) Uani 1 1 d . . . H2A H 0.6950 0.6676 0.7261 0.042 Uiso 1 1 calc R . . H2B H 0.6580 0.8300 0.7196 0.042 Uiso 1 1 calc R . . H2C H 0.7441 0.7384 0.6569 0.042 Uiso 1 1 calc R . . C3 C 0.1596(3) 0.9285(3) 0.44527(15) 0.0180(5) Uani 1 1 d . . . H3A H 0.1258 1.0261 0.4607 0.022 Uiso 1 1 calc R . . H3B H 0.0605 0.8566 0.4384 0.022 Uiso 1 1 calc R . . C4 C 0.2221(4) 0.9207(3) 0.37116(16) 0.0248(6) Uani 1 1 d . . . H4A H 0.1333 0.9406 0.3313 0.037 Uiso 1 1 calc R . . H4B H 0.2544 0.8236 0.3558 0.037 Uiso 1 1 calc R . . H4C H 0.3195 0.9928 0.3780 0.037 Uiso 1 1 calc R . . C5 C -0.1323(4) 1.3297(4) -0.14551(19) 0.0313(7) Uani 1 1 d . . . H5A H -0.1380 1.2278 -0.1717 0.038 Uiso 1 1 calc R . . H5B H -0.0143 1.3640 -0.1213 0.038 Uiso 1 1 calc R . . C6 C -0.1958(4) 1.4226(3) -0.20205(17) 0.0294(6) Uani 1 1 d . . . H6A H -0.1273 1.4178 -0.2419 0.044 Uiso 1 1 calc R . . H6B H -0.1890 1.5231 -0.1755 0.044 Uiso 1 1 calc R . . H6C H -0.3125 1.3876 -0.2257 0.044 Uiso 1 1 calc R . . C7 C -0.3767(6) 1.2624(6) 0.0876(3) 0.0551(10) Uani 1 1 d . . . H7A H -0.2652 1.2651 0.1203 0.066 Uiso 1 1 calc R . . H7B H -0.4358 1.1640 0.0812 0.066 Uiso 1 1 calc R . . C8 C -0.4735(7) 1.3700(6) 0.1253(2) 0.0572(11) Uani 1 1 d . . . H8A H -0.4861 1.3476 0.1754 0.086 Uiso 1 1 calc R . . H8B H -0.5843 1.3663 0.0932 0.086 Uiso 1 1 calc R . . H8C H -0.4141 1.4673 0.1322 0.086 Uiso 1 1 calc R . . C10 C -0.1260(3) 0.6017(3) 0.35155(14) 0.0162(5) Uani 1 1 d . . . H10 H -0.0513 0.5381 0.3331 0.019 Uiso 1 1 calc R . . C11 C -0.2028(3) 0.6866(3) 0.30292(14) 0.0183(5) Uani 1 1 d . . . H11 H -0.1802 0.6820 0.2526 0.022 Uiso 1 1 calc R . . C12 C -0.3142(3) 0.7790(3) 0.32920(14) 0.0166(5) Uani 1 1 d . . . C13 C -0.3482(3) 0.7769(3) 0.40244(14) 0.0151(4) Uani 1 1 d . . . H13 H -0.4277 0.8346 0.4213 0.018 Uiso 1 1 calc R . . C14 C -0.2640(3) 0.6894(3) 0.44689(14) 0.0138(4) Uani 1 1 d . . . H14 H -0.2871 0.6893 0.4968 0.017 Uiso 1 1 calc R . . C15 C -0.0751(3) 1.0344(3) 0.16124(15) 0.0203(5) Uani 1 1 d . . . H15 H 0.0209 1.1037 0.1722 0.024 Uiso 1 1 calc R . . C16 C -0.1594(4) 1.0154(3) 0.22019(15) 0.0224(5) Uani 1 1 d . . . H16 H -0.1236 1.0721 0.2701 0.027 Uiso 1 1 calc R . . C17 C -0.2970(3) 0.9117(3) 0.20451(15) 0.0199(5) Uani 1 1 d . . . C18 C -0.3447(3) 0.8314(3) 0.13150(15) 0.0201(5) Uani 1 1 d . . . H18 H -0.4369 0.7580 0.1196 0.024 Uiso 1 1 calc R . . C19 C -0.2554(3) 0.8597(3) 0.07594(15) 0.0189(5) Uani 1 1 d . . . H19 H -0.2899 0.8055 0.0254 0.023 Uiso 1 1 calc R . . N1 N -0.1514(3) 0.6044(2) 0.42345(12) 0.0131(4) Uani 1 1 d . . . N2 N -0.1230(3) 0.9597(2) 0.08975(12) 0.0166(4) Uani 1 1 d . . . O1 O 0.4487(2) 0.77725(19) 0.59090(10) 0.0177(4) Uani 1 1 d . . . O2 O 0.2912(2) 0.89902(19) 0.50476(11) 0.0175(4) Uani 1 1 d . . . O3 O -0.2362(3) 1.3396(2) -0.08832(11) 0.0226(4) Uani 1 1 d . . . O4 O -0.3575(3) 1.2924(3) 0.01637(13) 0.0376(6) Uani 1 1 d . . . P1 P 0.27178(7) 0.75076(6) 0.53491(4) 0.01319(14) Uani 1 1 d . . . P2 P -0.21660(8) 1.23433(7) -0.02731(4) 0.01853(15) Uani 1 1 d . . . S1 S 0.25159(7) 0.57997(6) 0.45178(3) 0.01435(14) Uani 1 1 d . . . S2 S 0.08119(7) 0.73379(6) 0.58956(3) 0.01465(14) Uani 1 1 d . . . S3 S 0.00607(8) 1.26581(7) 0.04073(4) 0.01990(15) Uani 1 1 d . . . S4 S -0.27102(8) 1.02856(7) -0.07772(4) 0.01962(15) Uani 1 1 d . . . S5 S -0.42103(9) 0.89441(8) 0.27532(4) 0.02429(16) Uani 1 1 d . . . Ni1 Ni 0.0000 0.5000 0.5000 0.01090(11) Uani 1 2 d S . . Ni2 Ni 0.0000 1.0000 0.0000 0.01417(12) Uani 1 2 d S . . 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 C1 0.0203(12) 0.0199(12) 0.0263(13) 0.0112(10) 0.0007(10) 0.0035(10) C2 0.0240(14) 0.0283(14) 0.0300(15) 0.0115(12) -0.0042(11) 0.0030(11) C3 0.0165(11) 0.0154(11) 0.0235(12) 0.0081(9) 0.0026(9) 0.0034(9) C4 0.0254(13) 0.0283(14) 0.0240(13) 0.0122(11) 0.0059(11) 0.0039(11) C5 0.0347(16) 0.0345(16) 0.0358(16) 0.0211(13) 0.0181(13) 0.0152(13) C6 0.0401(17) 0.0258(14) 0.0250(14) 0.0099(11) 0.0073(12) 0.0057(12) C7 0.054(2) 0.066(3) 0.051(2) 0.015(2) 0.019(2) 0.010(2) C8 0.071(3) 0.067(3) 0.036(2) -0.0039(19) 0.023(2) 0.022(2) C10 0.0172(11) 0.0161(11) 0.0167(11) 0.0031(9) 0.0051(9) 0.0046(9) C11 0.0207(12) 0.0222(12) 0.0145(11) 0.0060(9) 0.0063(9) 0.0059(10) C12 0.0157(11) 0.0179(11) 0.0175(11) 0.0070(9) 0.0024(9) 0.0035(9) C13 0.0141(11) 0.0146(11) 0.0179(11) 0.0039(9) 0.0045(9) 0.0035(8) C14 0.0144(11) 0.0136(10) 0.0142(10) 0.0036(8) 0.0043(8) 0.0012(8) C15 0.0215(12) 0.0215(12) 0.0168(12) 0.0023(10) 0.0021(10) 0.0018(10) C16 0.0286(14) 0.0247(13) 0.0145(11) 0.0033(10) 0.0044(10) 0.0062(11) C17 0.0211(12) 0.0250(13) 0.0186(12) 0.0119(10) 0.0065(10) 0.0108(10) C18 0.0167(11) 0.0242(13) 0.0213(12) 0.0094(10) 0.0024(9) 0.0048(9) C19 0.0192(12) 0.0216(12) 0.0158(11) 0.0050(9) 0.0013(9) 0.0025(9) N1 0.0151(9) 0.0113(9) 0.0138(9) 0.0041(7) 0.0031(7) 0.0016(7) N2 0.0178(10) 0.0196(10) 0.0127(9) 0.0046(8) 0.0014(8) 0.0033(8) O1 0.0145(8) 0.0174(8) 0.0210(9) 0.0068(7) 0.0003(7) 0.0003(6) O2 0.0180(8) 0.0125(8) 0.0219(9) 0.0071(7) 0.0008(7) -0.0007(6) O3 0.0274(10) 0.0226(9) 0.0218(9) 0.0085(7) 0.0077(8) 0.0107(8) O4 0.0284(11) 0.0660(17) 0.0217(10) 0.0062(10) 0.0084(9) 0.0218(11) P1 0.0131(3) 0.0110(3) 0.0160(3) 0.0041(2) 0.0029(2) 0.0007(2) P2 0.0192(3) 0.0214(3) 0.0167(3) 0.0051(2) 0.0045(2) 0.0066(2) S1 0.0161(3) 0.0124(3) 0.0167(3) 0.0040(2) 0.0071(2) 0.0022(2) S2 0.0156(3) 0.0133(3) 0.0152(3) 0.0011(2) 0.0046(2) 0.0021(2) S3 0.0205(3) 0.0177(3) 0.0195(3) 0.0006(2) 0.0016(2) 0.0010(2) S4 0.0172(3) 0.0206(3) 0.0199(3) 0.0060(2) -0.0015(2) 0.0013(2) S5 0.0243(3) 0.0348(4) 0.0234(3) 0.0185(3) 0.0122(3) 0.0167(3) Ni1 0.0123(2) 0.0097(2) 0.0119(2) 0.00360(15) 0.00378(15) 0.00180(15) Ni2 0.0150(2) 0.0156(2) 0.0114(2) 0.00250(16) 0.00108(16) 0.00181(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 C1 O1 1.451(3) . ? C1 C2 1.509(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 O2 1.457(3) . ? C3 C4 1.501(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 O3 1.439(3) . ? C5 C6 1.500(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O4 1.389(5) . ? C7 C8 1.482(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 N1 1.342(3) . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.394(3) . ? C11 H11 0.9500 . ? C12 C13 1.396(3) . ? C12 S5 1.756(2) . ? C13 C14 1.380(3) . ? C13 H13 0.9500 . ? C14 N1 1.342(3) . ? C14 H14 0.9500 . ? C15 N2 1.337(3) . ? C15 C16 1.388(4) . ? C15 H15 0.9500 . ? C16 C17 1.386(4) . ? C16 H16 0.9500 . ? C17 C18 1.378(4) . ? C17 S5 1.779(3) . ? C18 C19 1.383(4) . ? C18 H18 0.9500 . ? C19 N2 1.336(3) . ? C19 H19 0.9500 . ? N1 Ni1 2.106(2) . ? N2 Ni2 2.113(2) . ? O1 P1 1.5866(18) . ? O2 P1 1.5847(18) . ? O3 P2 1.592(2) . ? O4 P2 1.584(2) . ? P1 S1 1.9832(9) . ? P1 S2 1.9887(9) . ? P2 S3 1.9782(10) . ? P2 S4 1.9798(10) . ? S1 Ni1 2.4747(6) . ? S2 Ni1 2.4729(6) . ? S3 Ni2 2.4830(7) . ? S4 Ni2 2.4626(6) . ? Ni1 N1 2.106(2) 2_566 ? Ni1 S2 2.4729(6) 2_566 ? Ni1 S1 2.4747(6) 2_566 ? Ni2 N2 2.113(2) 2_575 ? Ni2 S4 2.4626(6) 2_575 ? Ni2 S3 2.4830(7) 2_575 ? 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 O1 C1 C2 107.4(2) . . ? O1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? O1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 C3 C4 109.7(2) . . ? O2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? O2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 107.6(2) . . ? O3 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? O3 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 C8 110.3(4) . . ? O4 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? O4 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? 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 . . ? N1 C10 C11 123.5(2) . . ? N1 C10 H10 118.3 . . ? C11 C10 H10 118.3 . . ? C10 C11 C12 118.7(2) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C11 C12 C13 118.2(2) . . ? C11 C12 S5 124.54(19) . . ? C13 C12 S5 117.21(19) . . ? C14 C13 C12 118.7(2) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? N1 C14 C13 123.6(2) . . ? N1 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? N2 C15 C16 123.0(3) . . ? N2 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C17 C16 C15 118.4(2) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C18 C17 C16 119.1(2) . . ? C18 C17 S5 120.5(2) . . ? C16 C17 S5 120.2(2) . . ? C17 C18 C19 118.6(3) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? N2 C19 C18 123.3(2) . . ? N2 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? C10 N1 C14 117.1(2) . . ? C10 N1 Ni1 121.06(16) . . ? C14 N1 Ni1 121.39(16) . . ? C19 N2 C15 117.7(2) . . ? C19 N2 Ni2 120.36(17) . . ? C15 N2 Ni2 121.96(18) . . ? C1 O1 P1 119.44(16) . . ? C3 O2 P1 118.78(15) . . ? C5 O3 P2 119.19(17) . . ? C7 O4 P2 123.4(3) . . ? O2 P1 O1 95.30(10) . . ? O2 P1 S1 112.33(8) . . ? O1 P1 S1 113.01(8) . . ? O2 P1 S2 113.25(8) . . ? O1 P1 S2 113.00(8) . . ? S1 P1 S2 109.44(4) . . ? O4 P2 O3 96.07(12) . . ? O4 P2 S3 111.87(9) . . ? O3 P2 S3 113.30(9) . . ? O4 P2 S4 112.62(11) . . ? O3 P2 S4 111.46(8) . . ? S3 P2 S4 110.80(4) . . ? P1 S1 Ni1 84.35(3) . . ? P1 S2 Ni1 84.28(3) . . ? P2 S3 Ni2 83.10(3) . . ? P2 S4 Ni2 83.61(3) . . ? C12 S5 C17 102.70(12) . . ? N1 Ni1 N1 180.00(9) . 2_566 ? N1 Ni1 S2 89.70(6) . . ? N1 Ni1 S2 90.30(6) 2_566 . ? N1 Ni1 S2 90.30(6) . 2_566 ? N1 Ni1 S2 89.70(6) 2_566 2_566 ? S2 Ni1 S2 180.0 . 2_566 ? N1 Ni1 S1 90.78(6) . . ? N1 Ni1 S1 89.22(6) 2_566 . ? S2 Ni1 S1 81.89(2) . . ? S2 Ni1 S1 98.11(2) 2_566 . ? N1 Ni1 S1 89.22(6) . 2_566 ? N1 Ni1 S1 90.78(6) 2_566 2_566 ? S2 Ni1 S1 98.11(2) . 2_566 ? S2 Ni1 S1 81.89(2) 2_566 2_566 ? S1 Ni1 S1 180.000(1) . 2_566 ? N2 Ni2 N2 180.00(12) . 2_575 ? N2 Ni2 S4 90.34(6) . 2_575 ? N2 Ni2 S4 89.66(6) 2_575 2_575 ? N2 Ni2 S4 89.66(6) . . ? N2 Ni2 S4 90.34(6) 2_575 . ? S4 Ni2 S4 180.0 2_575 . ? N2 Ni2 S3 88.69(6) . 2_575 ? N2 Ni2 S3 91.31(6) 2_575 2_575 ? S4 Ni2 S3 82.41(2) 2_575 2_575 ? S4 Ni2 S3 97.59(2) . 2_575 ? N2 Ni2 S3 91.31(6) . . ? N2 Ni2 S3 88.69(6) 2_575 . ? S4 Ni2 S3 97.59(2) 2_575 . ? S4 Ni2 S3 82.41(2) . . ? S3 Ni2 S3 180.00(3) 2_575 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.766 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.257