data_mgc_a _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety ? _chemical_formula_sum 'C35 H26 Cl2 N8 Ni O8 S2' _chemical_formula_weight 880.37 _chemical_melting_point ? 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' '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' 'Ni' 'Ni' 0.3393 1.1124 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _cell_length_a 9.134(2) _cell_length_b 9.293(2) _cell_length_c 12.052(3) _cell_angle_alpha 103.787(5) _cell_angle_beta 98.329(5) _cell_angle_gamma 112.385(5) _cell_volume 886.5(4) _cell_formula_units_Z 1 _cell_measurement_reflns_used 2497 _cell_measurement_temperature 100(1) _cell_measurement_theta_max 25.335 _cell_measurement_theta_min 2.499 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_T_max 0.9169 _exptl_absorpt_correction_T_min 0.7191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 450 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10289 _diffrn_reflns_theta_full 25.71 _diffrn_reflns_theta_max 25.71 _diffrn_reflns_theta_min 1.80 _diffrn_ambient_temperature 100(1) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _reflns_number_gt 2686 _reflns_number_total 3355 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_collection 'APEX2 v2009.3.0 (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.685 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.121 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 259 _refine_ls_number_reflns 3355 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0448 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+0.1490P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1216 _refine_ls_wR_factor_ref 0.1385 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 H00D H 0.6236 0.3476 0.5506 0.017 Uiso 1 1 calc R . . H00F H 0.4586 0.2809 1.0239 0.021 Uiso 1 1 calc R . . H00G H 0.6771 0.5254 1.0358 0.022 Uiso 1 1 calc R . . H00H H 0.1910 0.2404 0.7228 0.016 Uiso 1 1 calc R . . H00I H -0.0033 -0.0083 0.6147 0.019 Uiso 1 1 calc R . . H00J H 0.2263 -0.3763 0.6275 0.017 Uiso 1 1 calc R . . H00L H 0.5789 0.5651 0.6529 0.020 Uiso 1 1 calc R . . H00M H 0.4242 0.0307 0.8969 0.017 Uiso 1 1 calc R . . H00O H 0.3617 0.5126 0.7436 0.019 Uiso 1 1 calc R . . H00P H -0.0489 -0.4535 0.6268 0.023 Uiso 1 1 calc R . . H00Q H -0.1655 -0.2712 0.6150 0.024 Uiso 1 1 calc R . . H00R H 0.8646 0.5196 0.9237 0.021 Uiso 1 1 calc R . . C00B C 0.2776(4) -0.1459(4) 0.6221(3) 0.0112(7) Uani 1 1 d . . . C00C C 0.2093(4) -0.0336(4) 0.6192(3) 0.0118(7) Uani 1 1 d . . . C00D C 0.5351(4) 0.3257(4) 0.5866(3) 0.0139(7) Uani 1 1 d . . . C00E C 0.3124(4) 0.1362(4) 0.6262(3) 0.0111(7) Uani 1 1 d . . . C00F C 0.5332(4) 0.2785(4) 0.9770(3) 0.0177(8) Uani 1 1 d . . . C00G C 0.6636(4) 0.4237(4) 0.9844(3) 0.0180(8) Uani 1 1 d . . . C00H C 0.2812(4) 0.2641(4) 0.6884(3) 0.0133(7) Uani 1 1 d . . . C00I C 0.0439(4) -0.0831(4) 0.6170(3) 0.0157(7) Uani 1 1 d . . . C00J C 0.1802(4) -0.3008(4) 0.6249(3) 0.0140(7) Uani 1 1 d . . . C00K C 0.7484(4) 0.2713(4) 0.8406(3) 0.0148(7) Uani 1 1 d . . . C00L C 0.5094(4) 0.4558(4) 0.6474(3) 0.0164(7) Uani 1 1 d . . . C00M C 0.5123(4) 0.1299(4) 0.9009(3) 0.0144(7) Uani 1 1 d . . . C00N C 0.6189(4) 0.1252(4) 0.8307(3) 0.0119(7) Uani 1 1 d . . . C00O C 0.3810(4) 0.4249(4) 0.7001(3) 0.0155(7) Uani 1 1 d . . . C00P C 0.0160(4) -0.3475(4) 0.6237(3) 0.0190(8) Uani 1 1 d . . . C00Q C -0.0526(4) -0.2388(4) 0.6181(3) 0.0199(8) Uani 1 1 d . . . C00R C 0.7737(4) 0.4211(4) 0.9174(3) 0.0178(8) Uani 1 1 d . . . N007 N 0.4395(3) 0.1678(3) 0.5761(2) 0.0111(6) Uani 1 1 d . . . N008 N 0.4426(3) -0.1008(3) 0.6164(2) 0.0113(6) Uani 1 1 d . . . N009 N 0.8718(4) 0.2789(4) 0.7728(3) 0.0214(7) Uani 1 1 d . . . O00A O 1.0067(3) 0.3065(4) 0.8281(3) 0.0485(10) Uani 1 1 d . . . O004 O 0.7258(3) -0.0557(3) 0.6970(2) 0.0168(5) Uani 1 1 d . . . O005 O 0.5115(3) -0.1850(3) 0.7911(2) 0.0188(6) Uani 1 1 d . . . O006 O 0.8328(4) 0.2597(3) 0.6667(2) 0.0298(7) Uani 1 1 d . . . S002 S 0.57761(10) -0.06982(10) 0.73046(7) 0.0116(2) Uani 1 1 d . . . Ni01 Ni 0.5000 0.0000 0.5000 0.00876(19) Uani 1 2 d S . . H1SA H 0.1504 0.1455 0.1206 0.111 Uiso 0.50 1 calc PR A -1 H1SB H 0.0092 -0.0202 0.1226 0.111 Uiso 0.50 1 calc PR A -1 C1S C 0.042(2) 0.054(2) 0.0748(11) 0.092(6) Uani 0.50 1 d PD A -1 Cl1 Cl -0.0989(3) 0.1342(4) 0.0565(3) 0.0477(7) Uani 0.50 1 d PD A -1 Cl2 Cl 0.0658(6) -0.0527(8) -0.0537(4) 0.1114(19) Uani 0.50 1 d PD A -1 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 C00B 0.0101(16) 0.0123(17) 0.0087(16) 0.0015(13) 0.0021(13) 0.0035(14) C00C 0.0138(17) 0.0110(17) 0.0094(16) 0.0020(13) 0.0036(13) 0.0046(14) C00D 0.0124(17) 0.0119(17) 0.0153(17) 0.0043(13) 0.0046(13) 0.0026(14) C00E 0.0100(16) 0.0122(17) 0.0122(16) 0.0037(13) 0.0011(13) 0.0067(14) C00F 0.0213(19) 0.025(2) 0.0101(16) 0.0048(14) 0.0060(14) 0.0136(17) C00G 0.022(2) 0.0182(19) 0.0147(17) 0.0011(14) 0.0018(14) 0.0128(16) C00H 0.0140(17) 0.0160(18) 0.0141(17) 0.0055(14) 0.0065(14) 0.0095(15) C00I 0.0134(18) 0.0169(18) 0.0192(18) 0.0049(14) 0.0051(14) 0.0092(15) C00J 0.0147(18) 0.0087(17) 0.0170(17) 0.0045(14) 0.0042(14) 0.0031(14) C00K 0.0119(18) 0.0186(18) 0.0137(17) 0.0029(14) 0.0025(13) 0.0081(15) C00L 0.0210(19) 0.0109(17) 0.0168(17) 0.0033(14) 0.0059(15) 0.0066(15) C00M 0.0124(17) 0.0170(19) 0.0132(17) 0.0074(14) 0.0030(13) 0.0044(15) C00N 0.0124(17) 0.0126(17) 0.0112(16) 0.0031(13) -0.0003(13) 0.0076(14) C00O 0.0224(19) 0.0141(18) 0.0125(17) 0.0029(14) 0.0046(14) 0.0110(15) C00P 0.0162(19) 0.0114(18) 0.0237(19) 0.0058(15) 0.0080(15) -0.0011(15) C00Q 0.0115(18) 0.0186(19) 0.027(2) 0.0061(16) 0.0082(15) 0.0039(15) C00R 0.0163(19) 0.0141(18) 0.0185(18) 0.0023(14) 0.0005(14) 0.0052(15) N007 0.0105(14) 0.0098(14) 0.0130(14) 0.0045(11) 0.0032(11) 0.0039(12) N008 0.0104(14) 0.0107(14) 0.0120(14) 0.0031(11) 0.0016(11) 0.0046(12) N009 0.0142(17) 0.0148(16) 0.0254(18) -0.0036(13) 0.0067(13) 0.0017(13) O00A 0.0102(15) 0.074(2) 0.0310(17) -0.0200(16) -0.0016(13) 0.0117(15) O004 0.0129(13) 0.0180(13) 0.0204(13) 0.0024(10) 0.0027(10) 0.0105(11) O005 0.0225(14) 0.0140(13) 0.0181(13) 0.0069(10) 0.0010(11) 0.0064(11) O006 0.0399(17) 0.0336(16) 0.0280(16) 0.0179(13) 0.0220(13) 0.0189(14) S002 0.0119(4) 0.0094(4) 0.0134(4) 0.0031(3) 0.0020(3) 0.0054(3) Ni01 0.0089(3) 0.0069(3) 0.0112(3) 0.0034(2) 0.0044(2) 0.0033(2) C1S 0.088(11) 0.166(16) 0.053(8) 0.017(9) 0.003(7) 0.100(12) Cl1 0.0242(13) 0.069(2) 0.0547(17) 0.0372(16) 0.0072(11) 0.0160(13) Cl2 0.089(3) 0.200(6) 0.051(2) 0.008(3) 0.021(2) 0.087(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 C00B C00C 1.409(4) . ? C00B C00J 1.386(5) . ? C00C C00E 1.471(5) . ? C00C C00I 1.396(5) . ? C00D C00L 1.377(5) . ? C00E C00H 1.397(4) . ? C00F C00G 1.391(5) . ? C00F C00M 1.389(5) . ? C00G C00R 1.381(5) . ? C00H C00O 1.382(5) . ? C00I C00Q 1.383(5) . ? C00J C00P 1.390(5) . ? C00K C00N 1.385(5) . ? C00K C00R 1.388(5) . ? C00L C00O 1.381(5) . ? C00M C00N 1.384(5) . ? C00P C00Q 1.385(5) . ? N007 C00D 1.355(4) . ? N007 C00E 1.352(4) . ? N008 C00B 1.419(4) . ? N009 C00K 1.474(4) . ? N009 O00A 1.211(4) . ? O006 N009 1.227(4) . ? S002 C00N 1.786(3) . ? S002 N008 1.594(3) . ? S002 O004 1.435(2) . ? S002 O005 1.433(2) . ? Ni01 N007 1.923(3) . ? Ni01 N007 1.923(3) 2_656 ? Ni01 N008 1.894(3) . ? Ni01 N008 1.894(3) 2_656 ? C1S Cl2 1.718(10) . ? Cl1 C1S 1.732(10) . ? 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 C00C C00B N008 119.3(3) . . ? C00J C00B C00C 119.4(3) . . ? C00J C00B N008 121.3(3) . . ? C00B C00C C00E 120.8(3) . . ? C00I C00C C00B 118.8(3) . . ? C00I C00C C00E 120.3(3) . . ? N007 C00D C00L 122.8(3) . . ? C00H C00E C00C 119.5(3) . . ? N007 C00E C00C 119.9(3) . . ? N007 C00E C00H 120.6(3) . . ? C00M C00F C00G 119.9(3) . . ? C00R C00G C00F 120.4(3) . . ? C00O C00H C00E 120.2(3) . . ? C00Q C00I C00C 121.2(3) . . ? C00B C00J C00P 121.0(3) . . ? C00N C00K C00R 122.2(3) . . ? C00N C00K N009 122.6(3) . . ? C00R C00K N009 115.2(3) . . ? C00D C00L C00O 118.9(3) . . ? C00N C00M C00F 120.5(3) . . ? C00K C00N S002 124.0(3) . . ? C00M C00N C00K 118.4(3) . . ? C00M C00N S002 117.6(3) . . ? C00L C00O C00H 118.8(3) . . ? C00Q C00P C00J 119.8(3) . . ? C00I C00Q C00P 119.7(3) . . ? C00G C00R C00K 118.5(3) . . ? C00D N007 Ni01 118.4(2) . . ? C00E N007 C00D 118.7(3) . . ? C00E N007 Ni01 122.8(2) . . ? C00B N008 S002 119.2(2) . . ? C00B N008 Ni01 114.7(2) . . ? S002 N008 Ni01 121.41(16) . . ? O00A N009 C00K 116.5(3) . . ? O00A N009 O006 124.8(3) . . ? O006 N009 C00K 118.7(3) . . ? N008 S002 C00N 106.06(14) . . ? O004 S002 C00N 107.50(15) . . ? O004 S002 N008 108.62(14) . . ? O005 S002 C00N 104.83(15) . . ? O005 S002 N008 110.76(15) . . ? O005 S002 O004 118.30(14) . . ? N007 Ni01 N007 180.0 . 2_656 ? N008 Ni01 N007 88.50(11) . . ? N008 Ni01 N007 91.50(11) 2_656 . ? N008 Ni01 N007 88.50(11) 2_656 2_656 ? N008 Ni01 N007 91.50(11) . 2_656 ? N008 Ni01 N008 179.999(1) 2_656 . ? Cl2 C1S Cl1 115.5(8) . . ?