# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1823 #========================================================================== data_global #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Dr. Duan Chun-ying' _publ_contact_author_address ; Coordination Chemistry Institute The State Key Laboratory of Coordination Chemistry Nanjing University , Nanjing 210093 P. R. China ; _publ_contact_author_email duancy@hotmail.com _publ_contact_author_fax '00 86 25 331 7761' _publ_contact_author_phone '00 86 25 359 3763' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; Self-assembled macrocyclic tetranuclear molecular square [Ni(HL)]4 and molecular rectangle [Cu2Cl2L]2 [ H2L = Bis(2-benzoylpyridine) thiocarbazone ] ; loop_ _publ_author_name _publ_author_address 'He Cheng' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; 'Duan Chun-ying' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; 'Fang Chen-jie' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; 'Liu Yong-jiang' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; 'Meng Qing-jin' ; Coordination Chemistry Institute and State Key Laboratory of Coordination Chemistry, Nanjing University,Nanjing,210093, People's Republic of China ; #============================================================================== data_compound_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(2-benzoyl pyridine) thiocarbazone ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H20 N6 S' _chemical_formula_weight 436.53 _chemical_melting_point ? _chemical_compound_source synthesized 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' '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 '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 8.677(3) _cell_length_b 21.385(9) _cell_length_c 12.229(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.06(3) _cell_angle_gamma 90.00 _cell_volume 2157.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 5.13 _cell_measurement_theta_max 9.96 _exptl_crystal_description 'block ' _exptl_crystal_colour 'yellow ' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method ? _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.176 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 8.26 _diffrn_reflns_number 4870 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0967 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3804 _reflns_number_observed 2016 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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_details 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.3064P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3804 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1372 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1221 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.03799(12) 0.59173(5) -0.00192(8) 0.0551(3) Uani 1 1 d . . . N1 N -0.2715(4) 0.45176(19) 0.1759(3) 0.0711(11) Uani 1 1 d . . . N2 N -0.0763(3) 0.56780(14) 0.2783(2) 0.0477(8) Uani 1 1 d . . . N3 N -0.0752(4) 0.56305(16) 0.1675(3) 0.0497(9) Uani 1 1 d . . . H3N H -0.140(4) 0.5407(17) 0.122(3) 0.047(12) Uiso 1 1 d . . . N4 N 0.1493(4) 0.62376(16) 0.2207(3) 0.0506(9) Uani 1 1 d . . . H4N H 0.134(4) 0.6260(16) 0.290(3) 0.048(11) Uiso 1 1 d . . . N5 N 0.2856(4) 0.64981(14) 0.2059(3) 0.0487(8) Uani 1 1 d . . . N6 N 0.2415(5) 0.7228(2) 0.4155(4) 0.0920(13) Uani 1 1 d . . . C1 C -0.3876(5) 0.4147(2) 0.1056(4) 0.0697(13) Uani 1 1 d . . . H2A H -0.347(6) 0.380(2) 0.065(4) 0.12(2) Uiso 1 1 d . . . C2 C -0.5497(5) 0.4264(2) 0.0862(4) 0.0615(12) Uani 1 1 d . . . H2A H -0.629(4) 0.3985(16) 0.044(3) 0.045(10) Uiso 1 1 d . . . C3 C -0.5951(5) 0.4772(2) 0.1365(4) 0.0588(12) Uani 1 1 d . . . H3A H -0.713(5) 0.4856(19) 0.121(3) 0.085(14) Uiso 1 1 d . . . C4 C -0.4794(5) 0.5139(2) 0.2098(4) 0.0504(11) Uani 1 1 d . . . H4A H -0.505(6) 0.545(2) 0.245(4) 0.092(18) Uiso 1 1 d . . . C5 C -0.3174(4) 0.50048(18) 0.2292(3) 0.0432(9) Uani 1 1 d . . . C6 C -0.1899(4) 0.54034(17) 0.3084(3) 0.0435(9) Uani 1 1 d . . . C7 C -0.1869(4) 0.54931(18) 0.4278(3) 0.0458(9) Uani 1 1 d . . . C8 C -0.2675(6) 0.5110(2) 0.4786(4) 0.0533(12) Uani 1 1 d . . . H8A H -0.301(5) 0.4858(17) 0.450(3) 0.043(15) Uiso 1 1 d . . . C9 C -0.2612(6) 0.5185(3) 0.5897(4) 0.0675(13) Uani 1 1 d . . . H9A H -0.323(6) 0.490(2) 0.614(4) 0.097(18) Uiso 1 1 d . . . C10 C -0.1725(6) 0.5659(3) 0.6549(4) 0.0759(15) Uani 1 1 d . . . H10A H -0.171(6) 0.568(2) 0.736(4) 0.115(18) Uiso 1 1 d . . . C11 C -0.0912(7) 0.6053(3) 0.6055(5) 0.0886(17) Uani 1 1 d . . . H11A H -0.023(6) 0.642(2) 0.651(4) 0.12(2) Uiso 1 1 d . . . C12 C -0.0995(6) 0.5986(3) 0.4917(4) 0.0739(14) Uani 1 1 d . . . H12A H -0.047(5) 0.627(2) 0.454(4) 0.094(16) Uiso 1 1 d . . . C13 C 0.0412(4) 0.59348(17) 0.1336(3) 0.0414(9) Uani 1 1 d . . . C14 C 0.2139(7) 0.7277(4) 0.5185(6) 0.103(2) Uani 1 1 d . . . H14A H 0.134(8) 0.750(3) 0.537(5) 0.15(3) Uiso 1 1 d . . . C15 C 0.2920(8) 0.6931(3) 0.6110(6) 0.0862(19) Uani 1 1 d . . . H15A H 0.286(5) 0.6961(19) 0.683(4) 0.077(15) Uiso 1 1 d . . . C16 C 0.4130(9) 0.6530(3) 0.6036(5) 0.0905(18) Uani 1 1 d . . . H16A H 0.474(6) 0.628(2) 0.670(5) 0.12(2) Uiso 1 1 d . . . C17 C 0.4437(7) 0.6483(2) 0.5006(4) 0.0722(14) Uani 1 1 d . . . H17A H 0.517(5) 0.624(2) 0.486(4) 0.085(16) Uiso 1 1 d . . . C18 C 0.3577(4) 0.68214(18) 0.4076(3) 0.0481(10) Uani 1 1 d . . . C19 C 0.3847(4) 0.67617(17) 0.2946(3) 0.0459(9) Uani 1 1 d . . . C20 C 0.5369(4) 0.70148(18) 0.2809(3) 0.0464(10) Uani 1 1 d . . . C21 C 0.6272(6) 0.7423(3) 0.3594(6) 0.0661(15) Uani 1 1 d . . . H21A H 0.609(7) 0.748(3) 0.404(4) 0.09(2) Uiso 1 1 d . . . C22 C 0.7678(6) 0.7661(3) 0.3479(5) 0.0904(17) Uani 1 1 d . . . H22A H 0.831(6) 0.801(2) 0.409(4) 0.116(18) Uiso 1 1 d . . . C23 C 0.8206(6) 0.7487(3) 0.2579(6) 0.0841(17) Uani 1 1 d . . . H23A H 0.919(7) 0.767(3) 0.251(4) 0.14(2) Uiso 1 1 d . . . C24 C 0.7297(6) 0.7082(3) 0.1784(5) 0.0771(15) Uani 1 1 d . . . H24A H 0.763(5) 0.698(2) 0.119(4) 0.081(17) Uiso 1 1 d . . . C25 C 0.5874(5) 0.6847(2) 0.1887(4) 0.0600(12) Uani 1 1 d . . . H25A H 0.527(5) 0.657(2) 0.141(3) 0.072(15) Uiso 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 S1 0.0494(6) 0.0690(7) 0.0471(6) -0.0013(6) 0.0151(5) -0.0141(6) N1 0.052(2) 0.091(3) 0.073(2) -0.028(2) 0.0241(19) -0.011(2) N2 0.0395(18) 0.055(2) 0.0488(19) 0.0005(16) 0.0145(15) -0.0031(16) N3 0.0416(19) 0.062(2) 0.046(2) -0.0052(18) 0.0146(17) -0.0160(18) N4 0.0416(19) 0.061(2) 0.051(2) -0.0051(18) 0.0169(17) -0.0158(17) N5 0.0430(18) 0.0466(19) 0.056(2) 0.0004(17) 0.0142(16) -0.0114(16) N6 0.072(3) 0.102(3) 0.088(3) -0.026(3) 0.004(2) 0.013(3) C1 0.054(3) 0.085(4) 0.068(3) -0.026(3) 0.015(2) -0.009(3) C2 0.056(3) 0.070(3) 0.054(3) -0.005(2) 0.009(2) -0.023(3) C3 0.040(3) 0.075(3) 0.061(3) 0.008(3) 0.015(2) -0.007(3) C4 0.043(2) 0.055(3) 0.056(3) 0.001(2) 0.019(2) 0.002(2) C5 0.040(2) 0.050(2) 0.045(2) 0.0045(19) 0.0201(18) -0.0026(18) C6 0.032(2) 0.047(2) 0.053(2) -0.0005(19) 0.0149(18) 0.0001(18) C7 0.040(2) 0.051(2) 0.047(2) -0.002(2) 0.0143(18) 0.001(2) C8 0.063(3) 0.051(3) 0.049(3) -0.002(2) 0.022(2) -0.007(3) C9 0.075(3) 0.077(4) 0.058(3) 0.007(3) 0.031(3) 0.003(3) C10 0.064(3) 0.113(5) 0.049(3) -0.016(3) 0.016(3) 0.006(3) C11 0.086(4) 0.111(5) 0.078(4) -0.038(3) 0.038(3) -0.034(4) C12 0.069(3) 0.089(4) 0.075(3) -0.030(3) 0.037(3) -0.024(3) C13 0.0325(19) 0.042(2) 0.048(2) -0.0020(19) 0.0093(17) -0.0031(18) C14 0.070(4) 0.142(6) 0.092(5) -0.056(5) 0.019(4) 0.007(4) C15 0.101(5) 0.096(5) 0.074(4) -0.038(4) 0.046(4) -0.050(4) C16 0.137(6) 0.067(4) 0.075(4) 0.006(3) 0.044(4) -0.007(4) C17 0.094(4) 0.062(3) 0.066(3) 0.002(3) 0.033(3) 0.009(3) C18 0.040(2) 0.039(2) 0.061(3) -0.004(2) 0.010(2) -0.005(2) C19 0.042(2) 0.041(2) 0.051(2) 0.0021(19) 0.0089(19) -0.0021(19) C20 0.035(2) 0.044(2) 0.054(2) 0.006(2) 0.0050(19) -0.0044(19) C21 0.054(3) 0.068(4) 0.071(4) -0.007(3) 0.011(3) -0.026(3) C22 0.072(4) 0.087(4) 0.100(4) -0.005(3) 0.010(3) -0.036(3) C23 0.048(3) 0.086(4) 0.115(5) 0.021(4) 0.020(3) -0.017(3) C24 0.060(3) 0.091(4) 0.084(4) 0.016(3) 0.029(3) -0.009(3) C25 0.050(3) 0.060(3) 0.067(3) -0.002(3) 0.015(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C13 1.649(4) . yes N1 C5 1.353(5) . ? N1 C1 1.358(5) . ? N2 C6 1.295(4) . ? N2 N3 1.362(4) . yes N3 C13 1.370(4) . yes N4 C13 1.347(4) . yes N4 N5 1.369(4) . yes N5 C19 1.286(4) . ? N6 C14 1.357(7) . ? N6 C18 1.358(5) . ? C1 C2 1.375(6) . ? C2 C3 1.366(6) . ? C3 C4 1.366(6) . ? C4 C5 1.381(5) . ? C5 C6 1.491(5) . ? C6 C7 1.465(5) . ? C7 C8 1.347(6) . ? C7 C12 1.389(6) . ? C8 C9 1.353(6) . ? C9 C10 1.369(7) . ? C10 C11 1.355(7) . ? C11 C12 1.378(6) . ? C14 C15 1.346(8) . ? C15 C16 1.380(8) . ? C16 C17 1.369(7) . ? C17 C18 1.359(6) . ? C18 C19 1.477(5) . ? C19 C20 1.483(5) . ? C20 C21 1.354(6) . ? C20 C25 1.379(6) . ? C21 C22 1.369(7) . ? C22 C23 1.369(7) . ? C23 C24 1.356(7) . ? C24 C25 1.375(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 C5 N1 C1 118.9(4) . . ? C6 N2 N3 119.3(3) . . ? N2 N3 C13 120.0(3) . . ? C13 N4 N5 120.6(3) . . ? C19 N5 N4 116.5(3) . . ? C14 N6 C18 117.6(5) . . ? N1 C1 C2 121.5(5) . . ? C3 C2 C1 119.2(4) . . ? C4 C3 C2 119.8(4) . . ? C3 C4 C5 119.7(4) . . ? N1 C5 C4 120.8(4) . . ? N1 C5 C6 118.9(3) . . ? C4 C5 C6 120.3(4) . . ? N2 C6 C7 116.3(3) . . ? N2 C6 C5 123.5(3) . . ? C7 C6 C5 120.1(3) . . ? C8 C7 C12 118.2(4) . . ? C8 C7 C6 121.9(4) . . ? C12 C7 C6 119.9(4) . . ? C7 C8 C9 121.8(5) . . ? C8 C9 C10 120.8(5) . . ? C11 C10 C9 118.5(5) . . ? C10 C11 C12 120.9(5) . . ? C11 C12 C7 119.8(5) . . ? N4 C13 N3 112.7(3) . . ? N4 C13 S1 126.6(3) . . ? N3 C13 S1 120.6(3) . . ? C15 C14 N6 123.4(6) . . ? C14 C15 C16 118.7(6) . . ? C17 C16 C15 118.3(6) . . ? C18 C17 C16 121.2(6) . . ? N6 C18 C17 120.6(4) . . ? N6 C18 C19 117.3(4) . . ? C17 C18 C19 122.1(4) . . ? N5 C19 C18 124.6(3) . . ? N5 C19 C20 116.8(3) . . ? C18 C19 C20 118.6(3) . . ? C21 C20 C25 119.2(5) . . ? C21 C20 C19 119.7(4) . . ? C25 C20 C19 121.1(4) . . ? C20 C21 C22 120.4(6) . . ? C23 C22 C21 120.8(6) . . ? C24 C23 C22 119.1(5) . . ? C23 C24 C25 120.5(6) . . ? C24 C25 C20 120.1(5) . . ? _refine_diff_density_max 0.191 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.045 ##END ############### data_compound_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H25.50 F6 N6 Ni O1.25 P S' _chemical_formula_weight 689.77 _chemical_melting_point ? _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'O' 'O' 0.0106 0.0060 '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 27.045(9) _cell_length_b 16.385(7) _cell_length_c 29.595(9) _cell_angle_alpha 90.00 _cell_angle_beta 109.38(2) _cell_angle_gamma 90.00 _cell_volume 12371.6(75) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _exptl_crystal_description 'prism ' _exptl_crystal_colour 'black ' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method ? _exptl_crystal_F_000 5640 _exptl_absorpt_coefficient_mu 0.815 _exptl_crystal_density_meas ? _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.4914 _exptl_absorpt_correction_T_max 0.5871 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% 14.35 _diffrn_reflns_number 8968 _diffrn_reflns_av_R_equivalents 0.1168 _diffrn_reflns_av_sigmaI/netI 0.3284 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8081 _reflns_number_observed 2499 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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 'riding mdoel' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8081 _refine_ls_number_parameters 897 _refine_ls_number_restraints 304 _refine_ls_R_factor_all 0.2630 _refine_ls_R_factor_obs 0.0787 _refine_ls_wR_factor_all 0.2556 _refine_ls_wR_factor_obs 0.1623 _refine_ls_goodness_of_fit_all 0.819 _refine_ls_goodness_of_fit_obs 1.068 _refine_ls_restrained_S_all 0.822 _refine_ls_restrained_S_obs 1.041 _refine_ls_shift/esd_max -0.047 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.12873(4) 0.41461(7) 0.26245(4) 0.0432(3) Uani 1 d . . Ni2 Ni 0.03443(4) 0.45484(7) 0.36963(4) 0.0460(3) Uani 1 d . . S1 S 0.09306(8) 0.41971(15) 0.32618(8) 0.0574(7) Uani 1 d . . S2 S 0.04441(9) 0.4465(2) 0.20137(8) 0.0618(8) Uani 1 d . . N1 N -0.0082(2) 0.4421(4) 0.4156(2) 0.045(2) Uani 1 d . . N2 N 0.0428(2) 0.3344(4) 0.3850(2) 0.059(2) Uani 1 d . . N3 N 0.0648(2) 0.2827(4) 0.3606(2) 0.061(2) Uani 1 d . . H3A H 0.0651(2) 0.2308(4) 0.3650(2) 0.073 Uiso 1 calc R . N4 N 0.1003(2) 0.2597(4) 0.3019(2) 0.050(2) Uani 1 d . . N5 N 0.1188(2) 0.2946(4) 0.2685(2) 0.050(2) Uani 1 d . . N6 N 0.1537(2) 0.3693(4) 0.2086(2) 0.046(2) Uani 1 d . . N7 N 0.2036(3) 0.4294(4) 0.3097(2) 0.056(2) Uani 1 d . . N8 N 0.1374(2) 0.5373(4) 0.2592(2) 0.050(2) Uani 1 d . . N9 N 0.0993(2) 0.5852(4) 0.2339(2) 0.053(2) Uani 1 d . . H9A H 0.1026(2) 0.6374(4) 0.2356(2) 0.063 Uiso 1 calc R . N10 N 0.0189(2) 0.6064(4) 0.1810(2) 0.055(2) Uani 1 d . . N11 N -0.0242(2) 0.5737(4) 0.1473(2) 0.053(2) Uani 1 d . . N12 N -0.0997(2) 0.5086(4) 0.0786(2) 0.051(2) Uani 1 d . . C1 C -0.0358(3) 0.4981(6) 0.4281(3) 0.064(3) Uani 1 d . . H1A H -0.0357(3) 0.5509(6) 0.4166(3) 0.077 Uiso 1 calc R . C2 C -0.0657(3) 0.4819(6) 0.4585(3) 0.071(3) Uani 1 d . . H2A H -0.0863(3) 0.5218(6) 0.4659(3) 0.086 Uiso 1 calc R . C3 C -0.0627(3) 0.4059(6) 0.4757(3) 0.076(4) Uani 1 d . . H3B H -0.0813(3) 0.3935(6) 0.4963(3) 0.091 Uiso 1 calc R . C4 C -0.0332(3) 0.3444(6) 0.4644(3) 0.073(3) Uani 1 d . . H4A H -0.0313(3) 0.2921(6) 0.4770(3) 0.087 Uiso 1 calc R . C5 C -0.0066(3) 0.3659(6) 0.4329(3) 0.053(3) Uani 1 d . . C6 C 0.0217(3) 0.3048(6) 0.4148(3) 0.062(3) Uani 1 d . . C7 C 0.0251(3) 0.2199(6) 0.4287(3) 0.082(3) Uani 1 d . . C8 C 0.0699(5) 0.1861(7) 0.4571(4) 0.130(5) Uani 1 d . . H8A H 0.0991(5) 0.2200(7) 0.4674(4) 0.156 Uiso 1 calc R . C9 C 0.0770(5) 0.1058(8) 0.4725(5) 0.163(6) Uani 1 d . . H9B H 0.1099(5) 0.0863(8) 0.4904(5) 0.195 Uiso 1 calc R . C10 C 0.0351(4) 0.0576(7) 0.4606(4) 0.142(5) Uani 1 d . . H10A H 0.0377(4) 0.0032(7) 0.4701(4) 0.170 Uiso 1 calc R . C11 C -0.0122(5) 0.0910(7) 0.4340(5) 0.143(6) Uani 1 d . . H11A H -0.0424(5) 0.0593(7) 0.4265(5) 0.171 Uiso 1 calc R . C12 C -0.0156(5) 0.1704(7) 0.4181(4) 0.130(5) Uani 1 d . . H12A H -0.0481(5) 0.1901(7) 0.3990(4) 0.156 Uiso 1 calc R . C13 C 0.0866(3) 0.3160(5) 0.3289(3) 0.051(3) Uani 1 d . . C14 C 0.1671(3) 0.4156(5) 0.1781(3) 0.058(3) Uani 1 d . . H14A H 0.1725(3) 0.4713(5) 0.1838(3) 0.070 Uiso 1 calc R . C15 C 0.1731(3) 0.3801(6) 0.1369(3) 0.079(4) Uani 1 d . . H15A H 0.1819(3) 0.4121(6) 0.1147(3) 0.095 Uiso 1 calc R . C16 C 0.1658(3) 0.2970(6) 0.1298(3) 0.077(3) Uani 1 d . . H16A H 0.1697(3) 0.2721(6) 0.1030(3) 0.093 Uiso 1 calc R . C17 C 0.1529(3) 0.2525(5) 0.1630(3) 0.056(3) Uani 1 d . . H17A H 0.1482(3) 0.1965(5) 0.1586(3) 0.068 Uiso 1 calc R . C18 C 0.1466(3) 0.2882(5) 0.2026(3) 0.047(3) Uani 1 d . . C19 C 0.1273(3) 0.2474(5) 0.2361(3) 0.054(3) Uani 1 d . . C20 C 0.1156(3) 0.1595(5) 0.2327(3) 0.072(3) Uani 1 d . . C21 C 0.1542(5) 0.1074(6) 0.2410(4) 0.123(5) Uani 1 d . . H21A H 0.1885(5) 0.1265(6) 0.2523(4) 0.147 Uiso 1 calc R . C22 C 0.1453(6) 0.0229(8) 0.2333(5) 0.179(6) Uani 1 d . . H22A H 0.1726(6) -0.0120(8) 0.2341(5) 0.215 Uiso 1 calc R . C23 C 0.0987(6) -0.0049(7) 0.2251(5) 0.200(7) Uani 1 d . . H23A H 0.0942(6) -0.0605(7) 0.2288(5) 0.240 Uiso 1 calc R . C24 C 0.0556(5) 0.0445(8) 0.2114(4) 0.150(6) Uani 1 d . . H24A H 0.0219(5) 0.0231(8) 0.1986(4) 0.180 Uiso 1 calc R . C25 C 0.0648(4) 0.1343(7) 0.2177(4) 0.111(4) Uani 1 d . . H25A H 0.0372(4) 0.1711(7) 0.2117(4) 0.133 Uiso 1 calc R . C26 C 0.2356(3) 0.3719(6) 0.3330(3) 0.076(4) Uani 1 d . . H26A H 0.2254(3) 0.3176(6) 0.3270(3) 0.091 Uiso 1 calc R . C27 C 0.2853(4) 0.3896(6) 0.3669(4) 0.090(4) Uani 1 d . . H27A H 0.3065(4) 0.3484(6) 0.3848(4) 0.108 Uiso 1 calc R . C28 C 0.3011(4) 0.4691(7) 0.3724(4) 0.096(4) Uani 1 d . . H28A H 0.3346(4) 0.4829(7) 0.3925(4) 0.115 Uiso 1 calc R . C29 C 0.2667(3) 0.5286(6) 0.3476(3) 0.069(3) Uani 1 d . . H29A H 0.2765(3) 0.5832(6) 0.3515(3) 0.082 Uiso 1 calc R . C30 C 0.2181(3) 0.5072(6) 0.3174(3) 0.057(3) Uani 1 d . . C31 C 0.1811(3) 0.5695(5) 0.2895(3) 0.048(3) Uani 1 d . . C32 C 0.1897(3) 0.6588(5) 0.2977(3) 0.050(3) Uani 1 d . . C33 C 0.1935(3) 0.6939(5) 0.3406(3) 0.064(3) Uani 1 d . . H33A H 0.1916(3) 0.6613(5) 0.3657(3) 0.076 Uiso 1 calc R . C34 C 0.2003(4) 0.7803(6) 0.3474(4) 0.098(4) Uani 1 d . . H34A H 0.2054(4) 0.8032(6) 0.3774(4) 0.117 Uiso 1 calc R . C35 C 0.1993(4) 0.8290(7) 0.3095(4) 0.100(5) Uani 1 d . . H35A H 0.2012(4) 0.8855(7) 0.3128(4) 0.119 Uiso 1 calc R . C36 C 0.1956(4) 0.7936(6) 0.2674(4) 0.102(5) Uani 1 d . . H36A H 0.1968(4) 0.8264(6) 0.2422(4) 0.122 Uiso 1 calc R . C37 C 0.1901(3) 0.7102(6) 0.2603(4) 0.077(4) Uani 1 d . . H37A H 0.1866(3) 0.6883(6) 0.2305(4) 0.092 Uiso 1 calc R . C38 C 0.0552(3) 0.5503(5) 0.2053(3) 0.046(3) Uani 1 d . . C39 C -0.1365(3) 0.4725(6) 0.0440(3) 0.063(3) Uani 1 d . . H39A H -0.1326(3) 0.4174(6) 0.0386(3) 0.075 Uiso 1 calc R . C40 C -0.1809(3) 0.5122(6) 0.0151(3) 0.084(4) Uani 1 d . . H40A H -0.2065(3) 0.4841(6) -0.0088(3) 0.101 Uiso 1 calc R . C41 C -0.1865(4) 0.5946(7) 0.0225(3) 0.081(4) Uani 1 d . . H41A H -0.2150(4) 0.6235(7) 0.0027(3) 0.098 Uiso 1 calc R . C42 C -0.1501(3) 0.6322(6) 0.0586(3) 0.058(3) Uani 1 d . . H42A H -0.1553(3) 0.6862(6) 0.0656(3) 0.070 Uiso 1 calc R . C43 C -0.1039(3) 0.5913(5) 0.0864(3) 0.045(3) Uani 1 d . . C44 C -0.0607(3) 0.6275(5) 0.1258(3) 0.051(3) Uani 1 d . . C45 C -0.0625(3) 0.7111(6) 0.1425(3) 0.059(3) Uani 1 d . . C46 C -0.0655(4) 0.7758(6) 0.1119(4) 0.089(4) Uani 1 d . . H46A H -0.0680(4) 0.7664(6) 0.0803(4) 0.107 Uiso 1 calc R . C47 C -0.0650(4) 0.8573(6) 0.1291(4) 0.116(5) Uani 1 d . . H47A H -0.0662(4) 0.9014(6) 0.1090(4) 0.139 Uiso 1 calc R . C48 C -0.0625(4) 0.8701(6) 0.1754(4) 0.105(5) Uani 1 d . . H48A H -0.0621(4) 0.9234(6) 0.1864(4) 0.126 Uiso 1 calc R . C49 C -0.0608(4) 0.8067(6) 0.2062(4) 0.086(4) Uani 1 d . . H49A H -0.0595(4) 0.8160(6) 0.2376(4) 0.103 Uiso 1 calc R . C50 C -0.0611(3) 0.7274(6) 0.1883(3) 0.081(4) Uani 1 d . . H50A H -0.0602(3) 0.6837(6) 0.2086(3) 0.097 Uiso 1 calc R . P1 P 0.34243(9) 0.64360(15) 0.48087(9) 0.0817(11) Uani 1 d D . F1 F 0.3577(2) 0.6306(4) 0.4343(2) 0.127(3) Uani 1 d D . F2 F 0.3922(3) 0.5954(6) 0.5124(4) 0.136(5) Uani 0.584(6) d PDU 1 F3 F 0.3078(3) 0.5643(4) 0.4718(4) 0.115(4) Uani 0.584(6) d PDU 1 F4 F 0.2941(3) 0.6964(5) 0.4515(3) 0.111(4) Uani 0.584(6) d PDU 1 F5 F 0.3751(3) 0.7246(4) 0.4871(3) 0.085(4) Uani 0.584(6) d PDU 1 F2' F 0.3375(7) 0.5482(4) 0.4822(7) 0.139(7) Uani 0.416(6) d PDU 2 F3' F 0.2852(3) 0.6494(10) 0.4445(4) 0.102(6) Uani 0.416(6) d PDU 2 F4' F 0.3537(6) 0.7379(4) 0.4844(6) 0.109(6) Uani 0.416(6) d PDU 2 F5' F 0.4016(3) 0.6338(11) 0.5127(6) 0.141(8) Uani 0.416(6) d PDU 2 F6 F 0.3264(2) 0.6587(4) 0.5266(2) 0.122(3) Uani 1 d D . P2 P 0.19012(15) 0.6392(2) 0.11811(13) 0.157(2) Uani 0.799(4) d PDU 1 F7 F 0.1533(5) 0.6816(7) 0.0721(3) 0.247(6) Uani 0.799(4) d PDU 1 F8 F 0.1836(4) 0.7155(4) 0.1473(3) 0.199(4) Uani 0.799(4) d PDU 1 F9 F 0.1427(2) 0.6004(5) 0.1299(3) 0.166(4) Uani 0.799(4) d PDU 1 F10 F 0.1960(4) 0.5625(4) 0.0889(3) 0.192(4) Uani 0.799(4) d PDU 1 F12 F 0.2257(4) 0.5932(6) 0.1642(3) 0.227(5) Uani 0.799(4) d PDU 1 F11 F 0.2383(3) 0.6824(6) 0.1101(4) 0.215(5) Uani 0.799(4) d PDU 1 P2' P 0.2237(2) 0.6238(3) 0.1274(2) 0.199(5) Uiso 0.201(4) d PDU 2 F7' F 0.1943(4) 0.7023(4) 0.1023(4) 0.211(7) Uiso 0.201(4) d PDU 2 F8' F 0.1710(3) 0.5750(6) 0.1092(5) 0.190(8) Uiso 0.201(4) d PDU 2 F9' F 0.2356(4) 0.6017(8) 0.0808(2) 0.226(9) Uiso 0.201(4) d PDU 2 F10' F 0.2764(3) 0.6721(6) 0.1466(5) 0.213(11) Uiso 0.201(4) d PDU 2 F11' F 0.2122(4) 0.6466(8) 0.1743(3) 0.211(8) Uiso 0.201(4) d PDU 2 F12' F 0.2528(4) 0.5447(5) 0.1518(4) 0.207(11) Uiso 0.201(4) d PDU 2 O1 O 0.0895(3) 0.1106(6) 0.3444(3) 0.155(5) Uani 0.685(9) d PDU 1 H1B H 0.0864(3) 0.1621(6) 0.3453(3) 0.233 Uiso 0.685(9) d PR 1 C51 C 0.1424(4) 0.0783(8) 0.3855(5) 0.220(6) Uani 0.685(9) d PDU 1 H51A H 0.1350(4) 0.1015(8) 0.4124(5) 0.265 Uiso 0.685(9) d PR 1 H51B H 0.1701(4) 0.1113(8) 0.3817(5) 0.265 Uiso 0.685(9) d PR 1 C52 C 0.1692(8) 0.0143(9) 0.4092(8) 0.232(10) Uani 0.685(9) d PDU 1 H52A H 0.1983(8) 0.0270(9) 0.4373(8) 0.349 Uiso 0.685(9) d PR 1 H52B H 0.1456(8) -0.0218(9) 0.4176(8) 0.349 Uiso 0.685(9) d PR 1 H52C H 0.1817(8) -0.0117(9) 0.3860(8) 0.349 Uiso 0.685(9) d PR 1 O1' O 0.1734(4) 0.0335(9) 0.3696(10) 0.223(11) Uani 0.315(9) d PDU 2 H1'A H 0.1965(4) 0.0446(9) 0.3583(10) 0.335 Uiso 0.315(9) calc PR 2 C51' C 0.1212(4) 0.0867(13) 0.3424(7) 0.208(8) Uani 0.315(9) d PDU 2 H51C H 0.1330(4) 0.1417(13) 0.3396(7) 0.250 Uiso 0.315(9) calc PR 2 H51D H 0.1073(4) 0.0652(13) 0.3101(7) 0.250 Uiso 0.315(9) calc PR 2 C52' C 0.0806(7) 0.0936(32) 0.3582(10) 0.195(10) Uani 0.315(9) d PDU 2 H52D H 0.0563(7) 0.1328(32) 0.3390(10) 0.293 Uiso 0.315(9) calc PR 2 H52E H 0.0929(7) 0.1114(32) 0.3910(10) 0.293 Uiso 0.315(9) calc PR 2 H52F H 0.0636(7) 0.0417(32) 0.3560(10) 0.293 Uiso 0.315(9) calc PR 2 O2 O 0.0702(4) 0.7586(4) 0.1782(3) 0.266(8) Uani 1 d D . H2B H 0.0700(4) 0.7505(4) 0.2066(3) 0.320 Uiso 1 d R . C54 C 0.0608(10) 0.8369(17) 0.0909(4) 0.241(9) Uani 0.581(9) d PDU 1 H54A H 0.0813(10) 0.8753(17) 0.0801(4) 0.361 Uiso 0.581(9) d PR 1 H54B H 0.0530(10) 0.7904(17) 0.0700(4) 0.361 Uiso 0.581(9) d PR 1 H54C H 0.0287(10) 0.8623(17) 0.0907(4) 0.361 Uiso 0.581(9) d PR 1 C53 C 0.0713(8) 0.8243(8) 0.1375(4) 0.237(10) Uani 0.581(9) d PDU 1 H53A H 0.1035(8) 0.8053(8) 0.1343(4) 0.284 Uiso 0.581(9) d PR 1 H53D H 0.0800(8) 0.8751(8) 0.1544(4) 0.284 Uiso 0.581(9) d PR 1 C53' C 0.0668(11) 0.7112(10) 0.1291(4) 0.249(13) Uani 0.419(9) d PDU 2 H53B H 0.0428(11) 0.6661(10) 0.1224(4) 0.299 Uiso 0.419(9) d PR 2 H53C H 0.0999(11) 0.6911(10) 0.1285(4) 0.299 Uiso 0.419(9) d PR 2 C54' C 0.0494(15) 0.7536(16) 0.0885(7) 0.242(10) Uani 0.419(9) d PDU 2 H54D H 0.0460(15) 0.7294(16) 0.0580(7) 0.363 Uiso 0.419(9) d PR 2 H54E H 0.0158(15) 0.7731(16) 0.0882(7) 0.363 Uiso 0.419(9) d PR 2 H54F H 0.0736(15) 0.7983(16) 0.0944(7) 0.363 Uiso 0.419(9) d PR 2 O1W O 0.2351(11) 1.2818(11) 0.4836(8) 0.297(14) Uani 0.50 d P . H1WA H 0.2009(11) 1.2812(11) 0.4408(8) 0.356 Uiso 0.50 d PR . H1WB H 0.2697(11) 1.3203(11) 0.4922(8) 0.356 Uiso 0.50 d PR . 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 0.0463(5) 0.0389(6) 0.0504(6) -0.0003(6) 0.0239(4) 0.0023(6) Ni2 0.0497(6) 0.0486(7) 0.0464(5) 0.0004(6) 0.0251(4) 0.0020(6) S1 0.0714(13) 0.048(2) 0.0704(13) -0.0037(12) 0.0470(10) -0.0048(13) S2 0.0517(13) 0.061(2) 0.0682(15) -0.0022(14) 0.0142(12) 0.0032(14) N1 0.045(4) 0.046(5) 0.041(3) -0.003(3) 0.013(3) 0.003(4) N2 0.053(4) 0.084(6) 0.052(4) 0.014(4) 0.035(3) 0.012(4) N3 0.079(4) 0.045(5) 0.073(4) 0.017(4) 0.044(4) 0.015(4) N4 0.062(4) 0.046(5) 0.055(4) -0.002(4) 0.034(3) 0.007(4) N5 0.054(4) 0.057(5) 0.049(4) 0.011(4) 0.033(3) 0.007(4) N6 0.057(4) 0.038(4) 0.053(4) 0.005(3) 0.031(3) -0.003(4) N7 0.075(4) 0.021(4) 0.079(4) 0.000(4) 0.036(4) 0.003(4) N8 0.053(4) 0.056(5) 0.049(4) 0.021(4) 0.029(3) 0.015(4) N9 0.057(4) 0.048(5) 0.047(4) -0.002(4) 0.009(3) 0.014(4) N10 0.042(4) 0.062(5) 0.054(4) 0.001(4) 0.008(3) 0.007(4) N11 0.050(4) 0.055(5) 0.046(4) -0.008(4) 0.005(3) -0.009(4) N12 0.054(4) 0.065(5) 0.037(4) -0.004(4) 0.017(3) -0.019(4) C1 0.056(5) 0.087(7) 0.054(5) -0.011(5) 0.023(4) 0.003(6) C2 0.068(5) 0.090(8) 0.069(5) -0.017(5) 0.040(4) 0.018(6) C3 0.068(6) 0.099(8) 0.065(6) 0.012(6) 0.029(5) 0.010(7) C4 0.066(5) 0.086(8) 0.083(6) -0.011(6) 0.049(4) -0.010(6) C5 0.065(5) 0.069(6) 0.032(4) 0.000(5) 0.027(4) 0.009(5) C6 0.060(5) 0.056(6) 0.078(6) -0.009(5) 0.035(5) -0.017(5) C7 0.086(6) 0.075(7) 0.110(7) 0.035(6) 0.064(5) 0.023(6) C8 0.108(8) 0.119(10) 0.168(11) 0.061(9) 0.053(8) 0.004(9) C9 0.137(10) 0.116(10) 0.232(14) 0.101(10) 0.058(10) 0.054(9) C10 0.208(9) 0.074(9) 0.209(9) 0.065(7) 0.157(7) 0.050(8) C11 0.152(10) 0.088(10) 0.218(12) 0.030(9) 0.102(9) 0.011(9) C12 0.157(10) 0.074(8) 0.166(10) 0.065(8) 0.062(9) -0.006(8) C13 0.044(5) 0.058(6) 0.050(5) 0.009(5) 0.014(4) -0.004(5) C14 0.058(5) 0.050(6) 0.074(5) -0.024(5) 0.032(4) -0.005(5) C15 0.047(5) 0.120(9) 0.082(6) 0.018(6) 0.035(4) 0.006(6) C16 0.094(6) 0.070(7) 0.083(6) 0.010(6) 0.050(5) 0.035(6) C17 0.067(5) 0.050(6) 0.059(5) -0.009(5) 0.031(4) 0.008(5) C18 0.045(5) 0.040(6) 0.061(5) -0.004(5) 0.024(4) 0.016(5) C19 0.069(5) 0.040(6) 0.068(5) 0.004(5) 0.041(4) 0.017(5) C20 0.108(6) 0.046(6) 0.089(6) 0.009(5) 0.070(5) 0.036(5) C21 0.185(12) 0.046(7) 0.133(10) 0.006(7) 0.047(9) 0.017(8) C22 0.286(13) 0.111(12) 0.213(11) 0.040(9) 0.179(9) 0.048(11) C23 0.431(17) 0.034(8) 0.238(11) -0.009(8) 0.247(11) -0.020(11) C24 0.239(12) 0.098(10) 0.147(9) -0.022(9) 0.110(9) -0.070(10) C25 0.111(7) 0.115(10) 0.135(8) -0.032(8) 0.078(6) -0.025(8) C26 0.080(7) 0.068(7) 0.072(6) -0.004(6) 0.015(6) 0.018(6) C27 0.081(7) 0.049(7) 0.108(8) -0.009(6) -0.012(7) 0.017(6) C28 0.056(6) 0.095(9) 0.123(9) 0.005(8) 0.012(6) 0.029(7) C29 0.062(6) 0.049(6) 0.086(7) -0.017(6) 0.014(5) 0.013(5) C30 0.054(5) 0.064(7) 0.056(5) 0.006(5) 0.022(4) 0.018(5) C31 0.059(5) 0.051(6) 0.036(4) -0.001(4) 0.017(4) -0.006(5) C32 0.039(4) 0.055(6) 0.063(5) -0.003(5) 0.027(4) -0.001(5) C33 0.054(5) 0.067(7) 0.084(6) 0.008(5) 0.041(4) 0.011(5) C34 0.079(7) 0.083(8) 0.098(8) -0.061(7) -0.015(7) 0.005(7) C35 0.073(7) 0.086(9) 0.107(9) 0.026(7) -0.014(7) 0.005(7) C36 0.131(9) 0.064(8) 0.092(8) 0.020(7) 0.011(8) -0.018(7) C37 0.074(6) 0.071(7) 0.084(7) -0.004(6) 0.025(5) -0.014(6) C38 0.038(4) 0.055(6) 0.044(5) -0.006(5) 0.010(4) -0.005(5) C39 0.040(5) 0.081(7) 0.073(6) -0.020(5) 0.028(4) -0.006(5) C40 0.066(6) 0.105(9) 0.086(7) -0.021(7) 0.030(5) -0.010(7) C41 0.073(6) 0.111(9) 0.055(6) -0.019(6) 0.014(5) 0.009(7) C42 0.064(6) 0.061(6) 0.047(5) 0.006(5) 0.016(4) 0.018(5) C43 0.051(5) 0.050(6) 0.034(4) -0.006(4) 0.015(4) -0.017(5) C44 0.071(5) 0.060(6) 0.025(4) 0.000(4) 0.020(4) 0.001(5) C45 0.037(5) 0.059(7) 0.064(6) 0.008(5) -0.007(5) -0.006(5) C46 0.119(8) 0.059(7) 0.088(7) 0.002(6) 0.033(6) -0.007(7) C47 0.182(10) 0.049(7) 0.132(9) -0.014(7) 0.072(8) 0.014(8) C48 0.136(9) 0.041(7) 0.131(9) -0.022(7) 0.037(8) 0.002(7) C49 0.093(7) 0.068(7) 0.100(7) -0.047(6) 0.036(6) -0.009(6) C50 0.063(6) 0.089(8) 0.093(7) -0.023(7) 0.027(5) -0.006(6) P1 0.088(2) 0.083(2) 0.074(2) 0.010(2) 0.028(2) -0.010(2) F1 0.162(5) 0.129(6) 0.108(4) -0.023(4) 0.070(4) -0.033(5) F2 0.116(8) 0.110(8) 0.159(9) 0.051(7) 0.015(7) 0.038(7) F3 0.090(7) 0.084(7) 0.165(8) -0.003(7) 0.035(6) -0.032(6) F4 0.094(7) 0.117(9) 0.115(8) 0.021(7) 0.026(6) 0.010(7) F5 0.072(5) 0.076(7) 0.117(7) 0.000(6) 0.046(5) -0.023(5) F2' 0.125(12) 0.072(9) 0.169(12) 0.052(10) -0.019(11) 0.020(10) F3' 0.047(8) 0.127(12) 0.107(10) -0.001(10) -0.008(7) -0.002(9) F4' 0.127(11) 0.103(11) 0.112(10) -0.044(9) 0.061(8) -0.015(10) F5' 0.112(12) 0.128(14) 0.141(13) -0.023(12) -0.015(11) 0.026(11) F6 0.130(4) 0.169(7) 0.084(4) 0.000(4) 0.056(3) -0.015(5) P2 0.218(4) 0.130(4) 0.156(3) -0.006(3) 0.104(3) -0.039(4) F7 0.288(11) 0.245(11) 0.173(9) 0.055(9) 0.031(9) 0.034(10) F8 0.290(9) 0.139(8) 0.206(8) 0.009(7) 0.134(7) -0.044(7) F9 0.192(7) 0.133(7) 0.189(7) 0.005(6) 0.085(6) -0.039(7) F10 0.254(8) 0.169(8) 0.190(6) -0.075(6) 0.125(6) -0.033(7) F12 0.220(9) 0.211(9) 0.228(9) 0.014(8) 0.047(8) -0.013(8) F11 0.224(8) 0.193(8) 0.246(8) 0.008(7) 0.101(7) -0.045(7) O1 0.221(10) 0.087(8) 0.195(9) 0.044(7) 0.120(8) -0.001(8) C51 0.248(10) 0.193(10) 0.251(10) 0.010(10) 0.124(9) 0.040(10) C52 0.257(15) 0.200(16) 0.269(16) 0.037(15) 0.125(14) 0.020(15) O1' 0.269(17) 0.196(17) 0.239(17) -0.031(16) 0.131(16) 0.050(16) C51' 0.244(12) 0.175(11) 0.235(12) 0.014(11) 0.119(11) 0.030(11) C52' 0.234(15) 0.154(15) 0.225(15) 0.007(15) 0.111(15) 0.019(15) O2 0.152(9) 0.174(11) 0.443(19) 0.030(12) 0.058(11) -0.029(9) C54 0.283(15) 0.210(17) 0.323(16) -0.016(15) 0.226(13) -0.055(15) C53 0.293(15) 0.187(17) 0.321(16) -0.045(16) 0.224(14) -0.049(15) C53' 0.293(21) 0.201(23) 0.353(23) -0.034(22) 0.241(18) -0.054(21) C54' 0.292(15) 0.203(16) 0.325(16) -0.040(16) 0.229(14) -0.049(15) O1W 0.551(33) 0.135(19) 0.247(22) 0.022(17) 0.191(22) 0.167(22) _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 N5 2.001(7) . ? Ni1 N8 2.029(7) . ? Ni1 N7 2.057(6) . ? Ni1 N6 2.063(6) . ? Ni1 S1 2.388(3) . ? Ni1 S2 2.450(2) . ? Ni2 N11 2.008(7) 2 ? Ni2 N2 2.020(7) . ? Ni2 N1 2.066(7) . ? Ni2 N12 2.108(6) 2 ? Ni2 S1 2.419(3) . ? Ni2 S2 2.451(2) 2 ? S1 C13 1.713(9) . ? S2 C38 1.723(9) . ? S2 Ni2 2.451(2) 2 ? N1 C1 1.312(10) . ? N1 C5 1.343(10) . ? N2 C6 1.292(11) . ? N2 N3 1.373(9) . ? N3 C13 1.374(10) . ? N4 C13 1.349(10) . ? N4 N5 1.373(9) . ? N5 C19 1.310(10) . ? N6 C14 1.321(10) . ? N6 C18 1.345(10) . ? N7 C26 1.312(10) . ? N7 C30 1.332(10) . ? N8 N9 1.314(8) . ? N8 C31 1.332(9) . ? N9 C38 1.341(9) . ? N10 C38 1.362(10) . ? N10 N11 1.369(8) . ? N11 C44 1.318(10) . ? N11 Ni2 2.008(7) 2 ? N12 C39 1.308(9) . ? N12 C43 1.385(10) . ? N12 Ni2 2.108(6) 2 ? C1 C2 1.419(12) . ? C2 C3 1.339(13) . ? C3 C4 1.394(13) . ? C4 C5 1.398(12) . ? C5 C6 1.467(12) . ? C6 C7 1.446(13) . ? C7 C12 1.319(14) . ? C7 C8 1.342(13) . ? C8 C9 1.38(2) . ? C9 C10 1.33(2) . ? C10 C11 1.373(15) . ? C11 C12 1.377(15) . ? C14 C15 1.409(12) . ? C15 C16 1.382(13) . ? C16 C17 1.357(12) . ? C17 C18 1.372(11) . ? C18 C19 1.431(12) . ? C19 C20 1.470(12) . ? C20 C21 1.309(14) . ? C20 C25 1.359(13) . ? C21 C22 1.41(2) . ? C22 C23 1.29(2) . ? C23 C24 1.37(2) . ? C24 C25 1.49(2) . ? C26 C27 1.415(12) . ? C27 C28 1.363(13) . ? C28 C29 1.380(12) . ? C29 C30 1.367(11) . ? C30 C31 1.476(11) . ? C31 C32 1.490(11) . ? C32 C33 1.367(11) . ? C32 C37 1.392(12) . ? C33 C34 1.433(13) . ? C34 C35 1.371(15) . ? C35 C36 1.348(15) . ? C36 C37 1.384(13) . ? C39 C40 1.385(11) . ? C40 C41 1.384(14) . ? C41 C42 1.338(11) . ? C42 C43 1.417(10) . ? C43 C44 1.474(10) . ? C44 C45 1.462(12) . ? C45 C50 1.369(13) . ? C45 C46 1.378(13) . ? C46 C47 1.428(14) . ? C47 C48 1.367(15) . ? C48 C49 1.372(14) . ? C49 C50 1.403(13) . ? P1 F3' 1.567(7) . ? P1 F4 1.569(7) . ? P1 F2' 1.570(7) . ? P1 F5 1.572(6) . ? P1 F4' 1.572(7) . ? P1 F6 1.571(5) . ? P1 F5' 1.572(7) . ? P1 F3 1.572(6) . ? P1 F2 1.573(7) . ? P1 F1 1.580(5) . ? P2 F7 1.559(7) . ? P2 F8 1.561(7) . ? P2 F10 1.564(7) . ? P2 F11 1.567(7) . ? P2 F9 1.569(7) . ? P2 F12 1.577(7) . ? P2' F11' 1.562(8) . ? P2' F9' 1.562(8) . ? P2' F12' 1.563(7) . ? P2' F10' 1.563(7) . ? P2' F7' 1.564(7) . ? P2' F8' 1.565(7) . ? O1 C51 1.628(10) . ? C51 C52 1.33(2) . ? O1' C51' 1.627(11) . ? C51' C52' 1.33(2) . ? O2 C53 1.624(11) . ? O2 C53' 1.625(11) . ? C54 C53 1.328(14) . ? C53' C54' 1.33(2) . ? O1W O1W 1.47(4) 7_576 ? 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 N5 Ni1 N8 177.0(3) . . ? N5 Ni1 N7 100.7(2) . . ? N8 Ni1 N7 79.2(2) . . ? N5 Ni1 N6 78.6(3) . . ? N8 Ni1 N6 104.4(3) . . ? N7 Ni1 N6 93.9(3) . . ? N5 Ni1 S1 82.1(2) . . ? N8 Ni1 S1 94.9(2) . . ? N7 Ni1 S1 91.3(2) . . ? N6 Ni1 S1 160.7(2) . . ? N5 Ni1 S2 99.0(2) . . ? N8 Ni1 S2 81.3(2) . . ? N7 Ni1 S2 160.2(2) . . ? N6 Ni1 S2 88.3(2) . . ? S1 Ni1 S2 93.11(9) . . ? N11 Ni2 N2 178.3(2) 2 . ? N11 Ni2 N1 101.7(3) 2 . ? N2 Ni2 N1 78.3(3) . . ? N11 Ni2 N12 77.8(2) 2 2 ? N2 Ni2 N12 103.9(2) . 2 ? N1 Ni2 N12 94.6(2) . 2 ? N11 Ni2 S1 99.1(2) 2 . ? N2 Ni2 S1 81.0(2) . . ? N1 Ni2 S1 159.0(2) . . ? N12 Ni2 S1 87.0(2) 2 . ? N11 Ni2 S2 80.3(2) 2 2 ? N2 Ni2 S2 98.0(2) . 2 ? N1 Ni2 S2 92.4(2) . 2 ? N12 Ni2 S2 157.9(2) 2 2 ? S1 Ni2 S2 93.90(9) . 2 ? C13 S1 Ni1 94.4(3) . . ? C13 S1 Ni2 96.7(3) . . ? Ni1 S1 Ni2 159.39(11) . . ? C38 S2 Ni1 93.8(3) . . ? C38 S2 Ni2 94.7(2) . 2 ? Ni1 S2 Ni2 167.50(13) . 2 ? C1 N1 C5 119.4(8) . . ? C1 N1 Ni2 127.5(6) . . ? C5 N1 Ni2 113.0(5) . . ? C6 N2 N3 119.6(8) . . ? C6 N2 Ni2 118.6(6) . . ? N3 N2 Ni2 121.3(5) . . ? N2 N3 C13 118.3(7) . . ? C13 N4 N5 112.2(7) . . ? C19 N5 N4 118.4(7) . . ? C19 N5 Ni1 117.0(6) . . ? N4 N5 Ni1 124.5(5) . . ? C14 N6 C18 122.5(7) . . ? C14 N6 Ni1 123.8(6) . . ? C18 N6 Ni1 112.9(5) . . ? C26 N7 C30 119.5(7) . . ? C26 N7 Ni1 127.0(6) . . ? C30 N7 Ni1 113.4(5) . . ? N9 N8 C31 120.0(7) . . ? N9 N8 Ni1 122.5(5) . . ? C31 N8 Ni1 116.8(5) . . ? N8 N9 C38 118.1(7) . . ? C38 N10 N11 114.2(7) . . ? C44 N11 N10 114.3(7) . . ? C44 N11 Ni2 120.6(5) . 2 ? N10 N11 Ni2 125.1(5) . 2 ? C39 N12 C43 119.3(7) . . ? C39 N12 Ni2 128.0(6) . 2 ? C43 N12 Ni2 112.5(4) . 2 ? N1 C1 C2 123.0(9) . . ? C3 C2 C1 116.2(9) . . ? C2 C3 C4 123.2(9) . . ? C5 C4 C3 116.1(9) . . ? N1 C5 C4 122.0(8) . . ? N1 C5 C6 116.7(7) . . ? C4 C5 C6 121.2(8) . . ? N2 C6 C7 123.8(9) . . ? N2 C6 C5 113.3(8) . . ? C7 C6 C5 123.0(9) . . ? C12 C7 C8 113.9(10) . . ? C12 C7 C6 123.6(9) . . ? C8 C7 C6 122.3(9) . . ? C7 C8 C9 126.5(11) . . ? C10 C9 C8 117.7(12) . . ? C9 C10 C11 117.7(11) . . ? C10 C11 C12 121.1(12) . . ? C7 C12 C11 122.9(11) . . ? N4 C13 N3 113.3(8) . . ? N4 C13 S1 126.8(7) . . ? N3 C13 S1 119.9(7) . . ? N6 C14 C15 119.4(8) . . ? C16 C15 C14 119.1(9) . . ? C17 C16 C15 118.6(9) . . ? C16 C17 C18 121.6(9) . . ? N6 C18 C17 118.8(8) . . ? N6 C18 C19 116.0(7) . . ? C17 C18 C19 124.8(8) . . ? N5 C19 C18 115.1(7) . . ? N5 C19 C20 122.9(8) . . ? C18 C19 C20 122.0(8) . . ? C21 C20 C25 121.3(10) . . ? C21 C20 C19 119.1(9) . . ? C25 C20 C19 119.5(9) . . ? C20 C21 C22 121.9(12) . . ? C23 C22 C21 118.8(14) . . ? C22 C23 C24 122.2(13) . . ? C23 C24 C25 117.0(12) . . ? C20 C25 C24 116.7(10) . . ? N7 C26 C27 122.1(9) . . ? C28 C27 C26 117.9(9) . . ? C27 C28 C29 118.8(9) . . ? C30 C29 C28 120.0(9) . . ? N7 C30 C29 121.5(8) . . ? N7 C30 C31 117.3(7) . . ? C29 C30 C31 121.1(8) . . ? N8 C31 C30 112.9(7) . . ? N8 C31 C32 123.7(7) . . ? C30 C31 C32 123.1(7) . . ? C33 C32 C37 117.7(9) . . ? C33 C32 C31 121.7(8) . . ? C37 C32 C31 120.4(8) . . ? C32 C33 C34 120.9(9) . . ? C35 C34 C33 119.6(10) . . ? C36 C35 C34 118.8(11) . . ? C35 C36 C37 122.4(11) . . ? C36 C37 C32 120.4(10) . . ? N9 C38 N10 112.3(7) . . ? N9 C38 S2 123.9(6) . . ? N10 C38 S2 123.8(6) . . ? N12 C39 C40 123.4(9) . . ? C41 C40 C39 118.5(8) . . ? C42 C41 C40 119.1(9) . . ? C41 C42 C43 121.2(9) . . ? N12 C43 C42 118.1(7) . . ? N12 C43 C44 116.0(7) . . ? C42 C43 C44 125.7(8) . . ? N11 C44 C45 124.5(7) . . ? N11 C44 C43 112.4(7) . . ? C45 C44 C43 122.6(7) . . ? C50 C45 C46 118.4(9) . . ? C50 C45 C44 121.7(9) . . ? C46 C45 C44 120.0(9) . . ? C45 C46 C47 119.6(10) . . ? C48 C47 C46 119.5(10) . . ? C47 C48 C49 122.0(10) . . ? C48 C49 C50 117.1(10) . . ? C45 C50 C49 123.4(10) . . ? F3' P1 F2' 90.2(8) . . ? F4 P1 F5 86.1(4) . . ? F3' P1 F4' 96.5(8) . . ? F2' P1 F4' 173.3(8) . . ? F3' P1 F6 95.2(6) . . ? F4 P1 F6 88.5(5) . . ? F2' P1 F6 94.9(8) . . ? F5 P1 F6 94.1(5) . . ? F4' P1 F6 83.7(7) . . ? F3' P1 F5' 173.7(9) . . ? F2' P1 F5' 87.8(9) . . ? F4' P1 F5' 85.6(9) . . ? F6 P1 F5' 90.9(7) . . ? F4 P1 F3 91.2(5) . . ? F5 P1 F3 176.8(5) . . ? F6 P1 F3 87.6(5) . . ? F4 P1 F2 176.4(6) . . ? F5 P1 F2 91.0(5) . . ? F6 P1 F2 89.7(5) . . ? F3 P1 F2 91.8(5) . . ? F3' P1 F1 83.9(6) . . ? F4 P1 F1 90.1(5) . . ? F2' P1 F1 86.3(8) . . ? F5 P1 F1 85.2(5) . . ? F4' P1 F1 95.1(7) . . ? F6 P1 F1 178.4(4) . . ? F5' P1 F1 90.0(7) . . ? F3 P1 F1 93.1(5) . . ? F2 P1 F1 91.7(5) . . ? F7 P2 F8 88.3(6) . . ? F7 P2 F10 91.5(6) . . ? F8 P2 F10 179.3(6) . . ? F7 P2 F11 89.3(6) . . ? F8 P2 F11 88.5(6) . . ? F10 P2 F11 92.1(6) . . ? F7 P2 F9 92.5(6) . . ? F8 P2 F9 87.2(5) . . ? F10 P2 F9 92.1(5) . . ? F11 P2 F9 175.3(6) . . ? F7 P2 F12 177.6(7) . . ? F8 P2 F12 93.0(5) . . ? F10 P2 F12 87.1(5) . . ? F11 P2 F12 92.7(6) . . ? F9 P2 F12 85.6(6) . . ? F11' P2' F9' 179.3(7) . . ? F11' P2' F12' 90.4(6) . . ? F9' P2' F12' 89.7(6) . . ? F11' P2' F10' 89.0(6) . . ? F9' P2' F10' 90.3(6) . . ? F12' P2' F10' 89.6(6) . . ? F11' P2' F7' 90.5(6) . . ? F9' P2' F7' 89.4(6) . . ? F12' P2' F7' 179.1(7) . . ? F10' P2' F7' 90.8(6) . . ? F11' P2' F8' 90.1(6) . . ? F9' P2' F8' 90.5(6) . . ? F12' P2' F8' 89.9(6) . . ? F10' P2' F8' 179.0(7) . . ? F7' P2' F8' 89.8(6) . . ? C52 C51 O1 146.9(14) . . ? C52' C51' O1' 123.5(22) . . ? C54 C53 O2 145.5(16) . . ? C54' C53' O2 117.2(17) . . ? _refine_diff_density_max 0.380 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.079 ##END## #################### data_compound_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H18 Cl2 Cu2 N6 S' _chemical_formula_weight 632.49 _chemical_melting_point ? _chemical_compound_source ? 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' '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' 'Cu' 'Cu' 0.3201 1.2651 '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)/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 12.142(3) _cell_length_b 10.625(2) _cell_length_c 19.535(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.43(2) _cell_angle_gamma 90.00 _cell_volume 2520.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 5.13 _cell_measurement_theta_max 10.47 _exptl_crystal_description block _exptl_crystal_colour dark-blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method ? _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 2.010 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_decay_% ? _diffrn_reflns_number 3559 _diffrn_reflns_av_R_equivalents 0.0995 _diffrn_reflns_av_sigmaI/netI 0.1836 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 23.00 _reflns_number_total 3365 _reflns_number_observed 1600 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 631 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+0.0000P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2734 _refine_ls_number_parameters 371 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.1850 _refine_ls_R_factor_obs 0.0728 _refine_ls_wR_factor_all 0.1519 _refine_ls_wR_factor_obs 0.1129 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.222 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.173 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.12928(8) -0.18678(10) 0.43144(5) 0.0392(3) Uani 1 d . . Cu2 Cu -0.18660(8) 0.03563(10) 0.41830(5) 0.0400(3) Uani 1 d . . Cl1 Cl 0.0893(2) -0.2518(2) 0.53630(11) 0.0524(7) Uani 1 d . . Cl2 Cl -0.2380(2) -0.0225(2) 0.52414(10) 0.0435(6) Uani 1 d . . S1 S -0.0323(2) -0.0866(2) 0.40962(10) 0.0447(7) Uani 1 d . . N1 N 0.2615(5) -0.2980(5) 0.4201(3) 0.034(2) Uani 1 d . . C1 C 0.3016(7) -0.3842(8) 0.4589(5) 0.051(3) Uani 1 d . . H1A H 0.2676(7) -0.3970(8) 0.5008(5) 0.062 Uiso 1 calc R . C2 C 0.3913(7) -0.4600(8) 0.4437(5) 0.061(3) Uani 1 d . . H2A H 0.4179(7) -0.5205(8) 0.4739(5) 0.073 Uiso 1 calc R . C3 C 0.4380(7) -0.4392(7) 0.3808(5) 0.057(3) Uani 1 d . . H3A H 0.4973(7) -0.4883(7) 0.3671(5) 0.069 Uiso 1 calc R . C4 C 0.3987(7) -0.3478(7) 0.3381(4) 0.047(3) Uani 1 d . . H4A H 0.4338(7) -0.3325(7) 0.2967(4) 0.056 Uiso 1 calc R . C5 C 0.3087(6) -0.2786(7) 0.3554(4) 0.038(2) Uani 1 d . . C6 C 0.2539(6) -0.1875(7) 0.3134(3) 0.031(2) Uani 1 d . . C7 C 0.3034(7) -0.1459(7) 0.2483(4) 0.041(3) Uani 1 d . . C8 C 0.3111(7) -0.2243(8) 0.1909(4) 0.053(3) Uani 1 d . . H8A H 0.2823(7) -0.3052(8) 0.1929(4) 0.063 Uiso 1 calc R . C9 C 0.3597(7) -0.1849(10) 0.1323(4) 0.071(3) Uani 1 d . . H9A H 0.3640(7) -0.2392(10) 0.0951(4) 0.085 Uiso 1 calc R . C10 C 0.4029(7) -0.0648(9) 0.1275(5) 0.071(3) Uani 1 d . . H10A H 0.4336(7) -0.0362(9) 0.0869(5) 0.085 Uiso 1 calc R . C11 C 0.3992(7) 0.0116(8) 0.1846(5) 0.065(3) Uani 1 d . . H11A H 0.4322(7) 0.0905(8) 0.1833(5) 0.078 Uiso 1 calc R . C12 C 0.3480(7) -0.0266(8) 0.2425(5) 0.057(3) Uani 1 d . . H12A H 0.3429(7) 0.0287(8) 0.2792(5) 0.068 Uiso 1 calc R . N2 N 0.1625(5) -0.1429(6) 0.3371(3) 0.035(2) Uani 1 d . . N3 N 0.1019(5) -0.0610(6) 0.2989(3) 0.033(2) Uani 1 d . . C13 C 0.0073(6) -0.0307(7) 0.3272(3) 0.027(2) Uani 1 d . . N4 N -0.0598(5) 0.0432(6) 0.2895(3) 0.039(2) Uani 1 d . . N5 N -0.1554(5) 0.0727(6) 0.3226(3) 0.037(2) Uani 1 d . . N6 N -0.3302(5) 0.1217(6) 0.3926(3) 0.044(2) Uani 1 d . . C14 C -0.4205(6) 0.1385(8) 0.4296(4) 0.048(3) Uani 1 d . . H14A H -0.4225(6) 0.1068(8) 0.4740(4) 0.058 Uiso 1 calc R . C15 C -0.5119(7) 0.2018(8) 0.4040(4) 0.054(3) Uani 1 d . . H15A H -0.5741(7) 0.2121(8) 0.4309(4) 0.065 Uiso 1 calc R . C16 C -0.5097(7) 0.2494(8) 0.3380(4) 0.049(3) Uani 1 d . . H16A H -0.5698(7) 0.2929(8) 0.3202(4) 0.058 Uiso 1 calc R . C17 C -0.4171(6) 0.2311(7) 0.2998(4) 0.043(3) Uani 1 d . . H17A H -0.4121(6) 0.2648(7) 0.2560(4) 0.051 Uiso 1 calc R . C18 C -0.3313(7) 0.1621(7) 0.3270(4) 0.035(2) Uani 1 d . . C19 C -0.2313(7) 0.1315(8) 0.2897(4) 0.046(3) Uani 1 d . . C20 C -0.2244(5) 0.1589(6) 0.2149(3) 0.064(3) Uani 1 d D . C21 C -0.1640(8) 0.2568(8) 0.1870(3) 0.083(3) Uani 0.791(8) d PDU 1 H21A H -0.1250(8) 0.3110(8) 0.2157(3) 0.099 Uiso 0.791(8) calc PR 1 C22 C -0.1612(8) 0.2743(8) 0.1166(3) 0.084(3) Uani 0.791(8) d PDU 1 H22A H -0.1179(8) 0.3374(8) 0.0977(3) 0.101 Uiso 0.791(8) calc PR 1 C23 C -0.2241(7) 0.1965(8) 0.0747(4) 0.083(3) Uani 0.791(8) d PDU 1 H23A H -0.2236(7) 0.2103(8) 0.0277(4) 0.099 Uiso 0.791(8) calc PR 1 C24 C -0.2879(8) 0.0986(9) 0.1002(3) 0.077(3) Uani 0.791(8) d PDU 1 H24A H -0.3299(8) 0.0478(9) 0.0714(3) 0.092 Uiso 0.791(8) calc PR 1 C25 C -0.2863(8) 0.0798(9) 0.1711(3) 0.071(4) Uani 0.791(8) d PDU 1 H25A H -0.3267(8) 0.0140(9) 0.1897(3) 0.085 Uiso 0.791(8) calc PR 1 C21' C -0.1469(10) 0.2565(12) 0.2135(5) 0.085(6) Uani 0.209(8) d PDU 2 H21B H -0.1244(10) 0.2871(12) 0.2560(5) 0.103 Uiso 0.209(8) calc PR 2 C22' C -0.0988(10) 0.3141(18) 0.1566(4) 0.087(4) Uani 0.209(8) d PDU 2 H22B H -0.0364(10) 0.3647(18) 0.1582(4) 0.104 Uiso 0.209(8) calc PR 2 C23' C -0.1582(9) 0.2846(15) 0.0971(6) 0.085(4) Uani 0.209(8) d PDU 2 H23B H -0.1354(9) 0.3256(15) 0.0576(6) 0.102 Uiso 0.209(8) calc PR 2 C24' C -0.2470(12) 0.2023(15) 0.0888(5) 0.082(4) Uani 0.209(8) d PDU 2 H24B H -0.2849(12) 0.1899(15) 0.0479(5) 0.098 Uiso 0.209(8) calc PR 2 C25' C -0.2713(14) 0.1411(19) 0.1502(4) 0.081(4) Uani 0.209(8) d PDU 2 H25B H -0.3262(14) 0.0802(19) 0.1476(4) 0.097 Uiso 0.209(8) calc PR 2 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 Cu1 0.0327(6) 0.0458(6) 0.0392(6) 0.0005(6) 0.0075(5) 0.0066(6) Cu2 0.0279(6) 0.0583(7) 0.0338(5) 0.0062(6) 0.0083(5) 0.0071(6) Cl1 0.0516(15) 0.0557(14) 0.0502(13) 0.0150(12) 0.0153(12) 0.0050(13) Cl2 0.0408(13) 0.0528(14) 0.0372(11) 0.0016(11) 0.0115(10) -0.0039(12) S1 0.0320(13) 0.063(2) 0.0389(13) 0.0105(12) 0.0103(11) 0.0085(12) N1 0.021(4) 0.021(4) 0.059(4) 0.000(4) -0.008(3) 0.012(3) C1 0.032(5) 0.045(6) 0.077(7) 0.009(5) -0.008(5) 0.024(5) C2 0.052(6) 0.046(6) 0.083(7) 0.034(6) -0.029(5) 0.004(6) C3 0.037(6) 0.028(5) 0.106(8) 0.002(5) 0.012(5) 0.010(5) C4 0.036(5) 0.038(6) 0.067(6) -0.016(5) -0.004(5) 0.013(5) C5 0.035(5) 0.038(5) 0.040(5) -0.012(4) 0.012(4) 0.008(5) C6 0.023(5) 0.045(5) 0.026(4) -0.007(4) 0.008(4) 0.001(4) C7 0.042(5) 0.039(5) 0.042(5) -0.001(4) 0.016(4) 0.018(5) C8 0.035(5) 0.062(7) 0.061(6) -0.003(5) 0.021(5) -0.006(5) C9 0.069(7) 0.126(9) 0.018(4) -0.010(6) 0.028(4) 0.004(7) C10 0.047(6) 0.098(8) 0.068(6) 0.036(6) 0.031(5) 0.032(6) C11 0.059(6) 0.054(7) 0.084(7) 0.000(6) 0.043(5) -0.004(5) C12 0.053(6) 0.042(6) 0.076(6) -0.014(5) 0.024(5) -0.003(5) N2 0.033(4) 0.046(4) 0.024(4) -0.007(3) 0.003(3) 0.001(4) N3 0.015(4) 0.045(4) 0.040(4) 0.011(4) 0.007(3) 0.013(4) C13 0.024(5) 0.025(4) 0.031(4) -0.003(4) -0.010(4) -0.009(4) N4 0.033(4) 0.052(4) 0.033(4) 0.004(4) 0.013(3) 0.008(4) N5 0.024(4) 0.047(5) 0.038(4) -0.008(3) 0.009(3) 0.014(4) N6 0.036(4) 0.059(5) 0.038(4) 0.007(4) 0.009(4) 0.016(4) C14 0.030(5) 0.058(6) 0.057(6) 0.009(5) 0.010(5) 0.017(5) C15 0.043(6) 0.055(6) 0.066(6) 0.007(5) 0.021(5) 0.028(5) C16 0.034(5) 0.045(5) 0.067(6) 0.005(5) 0.003(5) 0.023(5) C17 0.029(5) 0.051(6) 0.049(5) 0.013(5) -0.008(4) 0.020(5) C18 0.040(5) 0.027(5) 0.039(5) -0.004(4) 0.001(4) 0.006(4) C19 0.031(5) 0.061(6) 0.047(5) 0.020(5) 0.013(4) 0.022(5) C20 0.070(7) 0.083(7) 0.039(5) 0.022(5) 0.026(5) 0.047(6) C21 0.097(7) 0.106(6) 0.046(5) 0.058(5) 0.041(5) 0.049(6) C22 0.091(6) 0.120(6) 0.041(5) 0.028(5) 0.022(5) 0.061(5) C23 0.091(6) 0.122(6) 0.035(5) 0.025(5) 0.022(5) 0.055(5) C24 0.083(6) 0.109(6) 0.040(5) -0.004(5) 0.000(5) 0.037(6) C25 0.086(7) 0.103(8) 0.025(5) 0.008(6) -0.002(6) 0.026(7) C21' 0.100(10) 0.113(10) 0.044(10) 0.054(10) 0.030(10) 0.065(10) C22' 0.096(8) 0.118(8) 0.047(8) 0.038(8) 0.028(8) 0.063(8) C23' 0.093(8) 0.120(8) 0.042(7) 0.023(8) 0.020(7) 0.060(8) C24' 0.091(7) 0.118(7) 0.036(7) 0.019(7) 0.017(7) 0.053(7) C25' 0.091(8) 0.118(8) 0.034(8) 0.010(8) 0.011(8) 0.045(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 Cu1 N2 1.947(6) . ? Cu1 N1 2.007(6) . ? Cu1 Cl1 2.219(2) . ? Cu1 S1 2.270(2) . ? Cu1 Cl2 2.724(2) 3_556 ? Cu2 N5 1.950(6) . ? Cu2 N6 2.029(6) . ? Cu2 Cl2 2.250(2) . ? Cu2 S1 2.286(2) . ? Cu2 Cl1 2.729(3) 3_556 ? Cl1 Cu2 2.729(3) 3_556 ? Cl2 Cu1 2.724(2) 3_556 ? S1 C13 1.786(7) . ? N1 C1 1.282(10) . ? N1 C5 1.406(9) . ? C1 C2 1.389(11) . ? C2 C3 1.375(12) . ? C3 C4 1.364(11) . ? C4 C5 1.363(10) . ? C5 C6 1.430(10) . ? C6 N2 1.295(9) . ? C6 C7 1.478(10) . ? C7 C12 1.383(11) . ? C7 C8 1.400(10) . ? C8 C9 1.357(10) . ? C9 C10 1.384(13) . ? C10 C11 1.380(12) . ? C11 C12 1.357(11) . ? N2 N3 1.359(8) . ? N3 C13 1.318(9) . ? C13 N4 1.347(9) . ? N4 N5 1.369(8) . ? N5 C19 1.282(10) . ? N6 C14 1.329(9) . ? N6 C18 1.352(9) . ? C14 C15 1.387(11) . ? C15 C16 1.384(11) . ? C16 C17 1.369(11) . ? C17 C18 1.377(10) . ? C18 C19 1.458(11) . ? C19 C20 1.491(9) . ? C20 C21 1.387(7) . ? C20 C25' 1.396(8) . ? C20 C21' 1.401(9) . ? C20 C25 1.413(7) . ? C21 C22 1.390(7) . ? C22 C23 1.388(8) . ? C23 C24 1.391(8) . ? C24 C25 1.398(7) . ? C21' C22' 1.400(9) . ? C22' C23' 1.398(9) . ? C23' C24' 1.397(9) . ? C24' C25' 1.397(9) . ? 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 Cu1 N1 82.2(3) . . ? N2 Cu1 Cl1 175.6(2) . . ? N1 Cu1 Cl1 95.7(2) . . ? N2 Cu1 S1 84.0(2) . . ? N1 Cu1 S1 161.2(2) . . ? Cl1 Cu1 S1 97.16(9) . . ? N2 Cu1 Cl2 90.2(2) . 3_556 ? N1 Cu1 Cl2 97.4(2) . 3_556 ? Cl1 Cu1 Cl2 93.96(8) . 3_556 ? S1 Cu1 Cl2 95.34(8) . 3_556 ? N5 Cu2 N6 81.1(2) . . ? N5 Cu2 Cl2 173.3(2) . . ? N6 Cu2 Cl2 96.2(2) . . ? N5 Cu2 S1 83.0(2) . . ? N6 Cu2 S1 160.2(2) . . ? Cl2 Cu2 S1 98.35(9) . . ? N5 Cu2 Cl1 93.1(2) . 3_556 ? N6 Cu2 Cl1 94.0(2) . 3_556 ? Cl2 Cu2 Cl1 93.14(8) . 3_556 ? S1 Cu2 Cl1 98.58(8) . 3_556 ? Cu1 Cl1 Cu2 86.59(8) . 3_556 ? Cu2 Cl2 Cu1 86.08(8) . 3_556 ? C13 S1 Cu1 95.0(3) . . ? C13 S1 Cu2 96.0(3) . . ? Cu1 S1 Cu2 163.71(11) . . ? C1 N1 C5 118.7(7) . . ? C1 N1 Cu1 130.9(6) . . ? C5 N1 Cu1 110.2(5) . . ? N1 C1 C2 125.6(8) . . ? C3 C2 C1 115.3(8) . . ? C4 C3 C2 121.1(8) . . ? C5 C4 C3 120.7(8) . . ? C4 C5 N1 118.5(7) . . ? C4 C5 C6 126.4(7) . . ? N1 C5 C6 115.1(6) . . ? N2 C6 C5 116.0(6) . . ? N2 C6 C7 123.6(7) . . ? C5 C6 C7 120.4(7) . . ? C12 C7 C8 116.8(7) . . ? C12 C7 C6 120.4(7) . . ? C8 C7 C6 122.8(7) . . ? C9 C8 C7 121.6(8) . . ? C8 C9 C10 120.6(9) . . ? C11 C10 C9 118.2(8) . . ? C12 C11 C10 121.0(9) . . ? C11 C12 C7 121.6(8) . . ? C6 N2 N3 120.0(6) . . ? C6 N2 Cu1 115.8(5) . . ? N3 N2 Cu1 123.9(5) . . ? C13 N3 N2 113.4(6) . . ? N3 C13 N4 116.1(6) . . ? N3 C13 S1 122.5(6) . . ? N4 C13 S1 121.4(5) . . ? C13 N4 N5 112.7(6) . . ? C19 N5 N4 118.8(6) . . ? C19 N5 Cu2 115.8(5) . . ? N4 N5 Cu2 125.3(5) . . ? C14 N6 C18 118.1(7) . . ? C14 N6 Cu2 129.5(5) . . ? C18 N6 Cu2 112.3(5) . . ? N6 C14 C15 121.9(8) . . ? C16 C15 C14 119.5(8) . . ? C17 C16 C15 118.5(8) . . ? C16 C17 C18 119.1(8) . . ? N6 C18 C17 122.5(7) . . ? N6 C18 C19 113.6(7) . . ? C17 C18 C19 123.8(7) . . ? N5 C19 C18 117.1(7) . . ? N5 C19 C20 122.8(7) . . ? C18 C19 C20 119.9(7) . . ? C25' C20 C21' 110.6(9) . . ? C21 C20 C25 119.2(6) . . ? C21 C20 C19 124.4(6) . . ? C25' C20 C19 146.6(8) . . ? C21' C20 C19 101.9(6) . . ? C25 C20 C19 116.4(6) . . ? C20 C21 C22 120.4(7) . . ? C23 C22 C21 119.1(8) . . ? C22 C23 C24 122.7(7) . . ? C23 C24 C25 117.2(8) . . ? C24 C25 C20 121.3(7) . . ? C22' C21' C20 128.5(10) . . ? C23' C22' C21' 110.3(10) . . ? C24' C23' C22' 129.0(11) . . ? C23' C24' C25' 111.1(11) . . ? C20 C25' C24' 128.8(11) . . ? _refine_diff_density_max 0.445 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.106 ##END## #####################