# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1629 data_9/05268B _publ_contact_author_name 'Dr Timothy J. R. Weakley' _publ_contact_author_address ;Department of Chemistry, University of Oregon, Eugene, OR 97403-1253 USA ; _publ_contact_author_email 'tweakley@oregon.uoregon.edu' _publ_contact_author_fax '01(541)3464643' _publ_contact_author_phone '01(541)3464620' _publ_section_title ;Ni(II)-induced activation of carbon-nitrogen single bond of coordinated ligand by hydroxylated substrates: generation of mono- and binuclear complexes of modified ligand frameworks. ; _publ_author_name ;S.Bhattacharyya, D.Ghosh, A.Endo, K.Shimuzu, T.J.R.Weakley, and M.Chaudhury ; _publ_section_references ;Cromer, D.T. & Waber, J.T. (1974). In International Tables for X-Ray Crystallography, vol. IV, pp. 71, 148. Kynoch Press, Birmingham, England. Enraf-Nonius (1993). CAD4/PC diffractometer software version 1.2. Enraf-Nonius, Delft, The Netherlands Molecular Structure Corporation (1989). TEXSAN structure analysis software, version 5.0. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Molecular Structure Corporation (1997). TeXsan structure analysis software, version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D.C. & Mathews, F.S. (1963). Acta Crystallogr., A24, 351-359. Stout, G.H. & Jensen, L.H. (1968). In X-Ray Structure Determination: A Practical Guide; Macmillan Co., London, p. 411. Walker, N. & Stuart, D. (1983). Acta Crystallogr., A39, 158-166. ; #-------------------------------------------------------------------- data_(1)_C18H29ClN4NiO5S2 _audit_creation_date 'Tue May 7 12:36:30 1996' _audit_creation_method 'from TEXRAY.INF file' _computing_data_collection 'CAD4/PC (Enraf-Nonius, 1993)' _computing_cell_refinement 'CAD4/PC (Enraf-Nonius, 1993)' _computing_data_reduction 'TEXSAN (Molecular Structure Corp., 1989)' _computing_structure_solution 'TEXSAN (Molecular Structure Corp., 1989)' _computing_structure_refinement 'TEXSAN (Molecular Structure Corp., 1989)' _computing_publication_material 'TEXSAN (Molecular Structure Corp., 1989)' _cell_length_a 11.779(4) _cell_length_b 13.233(3) _cell_length_c 14.732(3) _cell_angle_alpha 90 _cell_angle_beta 100.03(2) _cell_angle_gamma 90 _cell_volume 2261(1) _cell_formula_units_Z 4 _cell_measurement_temperature 294.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.0 _cell_measurement_theta_max 14.0 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz '+x, +y, +z' '-x,1/2+y,1/2-z' '-x, -y, -z' '+x,1/2-y,1/2+z' _exptl_crystal_description 'amber-yellow prism' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 539.72 _chemical_formula_sum 'C18 H29 Cl N4 Ni O5 S2 ' _chemical_formula_moiety 'C18 H29 N4 Ni O S2 1+, Cl O4 1-' _exptl_crystal_F_000 1128.00 _exptl_absorpt_coefficient_mu 1.19 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_max 1.374 _exptl_absorpt_correction_T_min 0.686 _diffrn_special_details none _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'sealed X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -0.60 _diffrn_reflns_number 3856 _reflns_number_total 3643 _reflns_number_observed 2238 _reflns_observed_criterion 'I>3\s(I)' _diffrn_reflns_av_R_equivalents 0.091 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25.0 _diffrn_orient_matrix_UB_11 0.02541 _diffrn_orient_matrix_UB_12 0.04209 _diffrn_orient_matrix_UB_13 0.05621 _diffrn_orient_matrix_UB_21 0.00223 _diffrn_orient_matrix_UB_22 0.06103 _diffrn_orient_matrix_UB_23 -0.03972 _diffrn_orient_matrix_UB_31 -0.08235 _diffrn_orient_matrix_UB_32 0.01467 _diffrn_orient_matrix_UB_33 0.00369 loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 72 0.002 0.002 'Cromer & Waber (1974)' H 0 116 0.000 0.000 'Cromer & Waber (1974)' N 0 16 0.004 0.003 'Cromer & Waber (1974)' S 0 8 0.110 0.124 'Cromer & Waber (1974)' Ni 0 4 0.285 1.113 'Cromer & Waber (1974)' Cl 0 4 0.132 0.159 'Cromer & Waber (1974)' O 0 20 0.008 0.006 'Cromer & Waber (1974)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ;w = 4F~o~^2^/[\s^2^(I)+(0.02I)^2^] ; _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00 _refine_ls_abs_structure_details 'not applicable' _refine_ls_number_reflns 2238 _refine_ls_number_parameters 280 _refine_ls_R_factor_obs 0.044 _refine_ls_wR_factor_obs 0.045 _refine_ls_goodness_of_fit_obs 1.80 _refine_ls_shift/esd_max 0.021 _refine_diff_density_max 0.52 _refine_diff_density_min -0.34 loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Ni 0.64179(6) 0.22743(6) 0.41254(5) 0.0315(2) Uij ? ? Cl -0.0348(1) -0.0657(2) 0.2349(1) 0.0587(6) Uij ? ? S1 0.4696(1) 0.1977(1) 0.3482(1) 0.0441(5) Uij ? ? S2 0.2941(1) 0.0346(1) 0.3162(1) 0.0561(6) Uij ? ? O1 0.7116(3) 0.3107(3) 0.5989(3) 0.055(1) Uij ? ? O2 -0.0155(5) -0.0015(5) 0.1622(4) 0.104(2) Uij ? ? O3 -0.1489(4) -0.0839(6) 0.2333(5) 0.146(3) Uij ? ? O4 0.0075(6) -0.0187(6) 0.3188(4) 0.138(3) Uij ? ? O5 0.0238(6) -0.1545(6) 0.2305(5) 0.158(4) Uij ? ? N1 0.6903(4) 0.0938(3) 0.4207(3) 0.035(1) Uij ? ? N2 0.7984(3) 0.2628(3) 0.4751(3) 0.035(1) Uij ? ? N3 0.6181(3) 0.3706(3) 0.4028(3) 0.036(1) Uij ? ? N4 0.7178(4) 0.4219(4) 0.4298(3) 0.039(2) Uij ? ? C1 0.2167(5) 0.1509(5) 0.2928(5) 0.067(3) Uij ? ? C2 0.4391(5) 0.0713(4) 0.3512(4) 0.040(2) Uij ? ? C3 0.5140(5) -0.0033(4) 0.3762(4) 0.038(2) Uij ? ? C4 0.4838(5) -0.1133(5) 0.3748(5) 0.056(2) Uij ? ? C5 0.5958(6) -0.1707(5) 0.4041(5) 0.058(2) Uij ? ? C6 0.6914(5) -0.0931(5) 0.4224(5) 0.055(2) Uij ? ? C7 0.6360(5) 0.0087(4) 0.4076(4) 0.041(2) Uij ? ? C8 0.8187(5) 0.0848(4) 0.4524(5) 0.045(2) Uij ? ? C9 0.8733(5) 0.1847(4) 0.4421(4) 0.042(2) Uij ? ? C10 0.9993(5) 0.1888(5) 0.4868(5) 0.059(2) Uij ? ? C11 0.8235(5) 0.3649(5) 0.4442(5) 0.050(2) Uij ? ? C12 0.8068(5) 0.2603(5) 0.5756(4) 0.054(2) Uij ? ? C13 0.5369(5) 0.4426(5) 0.3889(4) 0.047(2) Uij ? ? C14 0.5878(5) 0.5372(5) 0.4060(5) 0.059(2) Uij ? ? C15 0.7028(5) 0.5225(5) 0.4319(5) 0.050(2) Uij ? ? C16 0.4102(5) 0.4248(5) 0.3602(5) 0.063(2) Uij ? ? C17 0.8005(6) 0.5940(5) 0.4596(5) 0.064(2) Uij ? ? C18 0.7208(6) 0.3174(6) 0.6968(5) 0.072(3) Uij ? ? H1 0.8341 0.0647 0.5153 0.0541 Uiso ? ? H2 0.8490 0.0358 0.4159 0.0541 Uiso ? ? H3 0.8700 0.1957 0.3779 0.0509 Uiso ? ? H4 1.0060 0.1784 0.5513 0.0707 Uiso ? ? H5 1.0406 0.1375 0.4613 0.0707 Uiso ? ? H6 1.0303 0.2530 0.4758 0.0707 Uiso ? ? H7 0.8788 0.3969 0.4898 0.0601 Uiso ? ? H8 0.8529 0.3608 0.3881 0.0601 Uiso ? ? H9 0.8074 0.1922 0.5961 0.0651 Uiso ? ? H10 0.8758 0.2929 0.6040 0.0651 Uiso ? ? H11 0.5490 0.6004 0.4006 0.0704 Uiso ? ? H12 0.3708 0.4878 0.3544 0.0753 Uiso ? ? H13 0.3965 0.3907 0.3025 0.0753 Uiso ? ? H14 0.3828 0.3846 0.4053 0.0753 Uiso ? ? H15 0.8380 0.5787 0.5204 0.0765 Uiso ? ? H16 0.8538 0.5876 0.4184 0.0765 Uiso ? ? H17 0.7719 0.6612 0.4575 0.0765 Uiso ? ? H18 0.7240 0.2513 0.7223 0.0864 Uiso ? ? H19 0.7890 0.3533 0.7218 0.0864 Uiso ? ? H20 0.6556 0.3521 0.7112 0.0864 Uiso ? ? H21 0.2264 0.1909 0.3471 0.0800 Uiso ? ? H22 0.2455 0.1866 0.2456 0.0800 Uiso ? ? H23 0.1371 0.1369 0.2731 0.0800 Uiso ? ? H24 0.4325 -0.1264 0.4166 0.0670 Uiso ? ? H25 0.4486 -0.1331 0.3145 0.0670 Uiso ? ? H26 0.5927 -0.2084 0.4585 0.0696 Uiso ? ? H27 0.6087 -0.2152 0.3564 0.0696 Uiso ? ? H28 0.7312 -0.0989 0.4841 0.0666 Uiso ? ? H29 0.7440 -0.1027 0.3811 0.0666 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni 0.0336(4) 0.0312(4) 0.0302(4) -0.0022(3) 0.0073(3) 0.0010(4) Cl 0.0504(10) 0.068(1) 0.059(1) -0.0013(9) 0.0133(9) -0.007(1) S1 0.0401(8) 0.0370(9) 0.053(1) -0.0039(7) 0.0012(8) 0.0016(8) S2 0.0429(9) 0.053(1) 0.071(1) -0.0132(8) 0.0079(9) -0.0068(10) O1 0.065(3) 0.066(3) 0.037(3) 0.005(2) 0.015(2) 0.000(2) O2 0.130(5) 0.102(5) 0.079(5) -0.010(4) 0.017(4) 0.034(4) O3 0.055(4) 0.202(8) 0.179(7) -0.031(4) 0.016(4) 0.018(6) O4 0.166(6) 0.175(7) 0.079(5) -0.078(5) 0.031(5) -0.045(5) O5 0.191(7) 0.148(7) 0.159(8) 0.088(6) 0.093(6) 0.036(6) N1 0.036(2) 0.030(3) 0.038(3) -0.001(2) 0.008(2) 0.000(2) N2 0.039(2) 0.032(3) 0.034(3) -0.001(2) 0.008(2) 0.002(2) N3 0.029(2) 0.032(3) 0.044(3) -0.004(2) 0.003(2) -0.001(3) N4 0.040(3) 0.033(3) 0.043(4) -0.003(2) 0.005(2) 0.002(3) C1 0.042(4) 0.070(5) 0.084(6) -0.011(4) 0.001(4) -0.003(4) C2 0.043(3) 0.035(4) 0.043(4) -0.005(3) 0.014(3) -0.009(3) C3 0.047(3) 0.033(4) 0.035(4) -0.009(3) 0.013(3) -0.006(3) C4 0.063(4) 0.036(4) 0.070(5) -0.007(3) 0.017(4) -0.009(4) C5 0.080(5) 0.035(4) 0.062(5) -0.006(4) 0.020(4) -0.003(4) C6 0.059(4) 0.039(4) 0.069(5) 0.006(3) 0.012(4) 0.000(4) C7 0.050(4) 0.030(4) 0.046(4) 0.005(3) 0.016(3) -0.002(3) C8 0.043(3) 0.038(4) 0.054(5) 0.001(3) 0.010(3) -0.005(3) C9 0.040(3) 0.041(4) 0.046(4) 0.001(3) 0.009(3) -0.001(3) C10 0.043(3) 0.063(5) 0.071(5) 0.003(3) 0.010(3) 0.005(4) C11 0.042(4) 0.046(4) 0.061(5) -0.009(3) 0.005(3) 0.008(4) C12 0.053(3) 0.065(5) 0.044(4) 0.005(3) 0.004(3) -0.001(4) C13 0.047(4) 0.037(4) 0.053(5) 0.003(3) 0.001(3) -0.005(3) C14 0.058(4) 0.033(4) 0.078(6) 0.005(3) -0.007(4) -0.006(4) C15 0.057(4) 0.035(4) 0.057(5) -0.005(3) 0.007(4) 0.005(3) C16 0.053(4) 0.039(4) 0.090(6) 0.006(3) -0.003(4) -0.009(4) C17 0.066(4) 0.041(4) 0.078(6) -0.010(4) -0.003(4) -0.003(4) C18 0.099(5) 0.083(6) 0.037(5) -0.001(5) 0.019(4) -0.001(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S1 2.121(2) ? ? yes Ni N1 1.855(5) ? ? yes Ni N2 1.969(4) ? ? yes Ni N3 1.917(5) ? ? yes Cl O2 1.417(5) ? ? no Cl O3 1.362(5) ? ? no Cl O4 1.396(6) ? ? no Cl O5 1.371(6) ? ? no S1 C2 1.713(6) ? ? yes S2 C1 1.792(7) ? ? yes S2 C2 1.763(5) ? ? yes O1 C12 1.397(7) ? ? yes O1 C18 1.429(7) ? ? yes N1 C7 1.293(7) ? ? yes N1 C8 1.508(7) ? ? yes N2 C9 1.494(7) ? ? yes N2 C11 1.473(7) ? ? yes N2 C12 1.467(7) ? ? yes N3 N4 1.354(6) ? ? yes N3 C13 1.341(7) ? ? yes N4 C11 1.440(7) ? ? yes N4 C15 1.344(7) ? ? yes C2 C3 1.332(8) ? ? yes C3 C4 1.498(8) ? ? yes C3 C7 1.440(7) ? ? yes C4 C5 1.518(9) ? ? yes C5 C6 1.513(9) ? ? yes C6 C7 1.495(8) ? ? yes C8 C9 1.491(8) ? ? yes C9 C10 1.516(8) ? ? yes C13 C14 1.391(8) ? ? yes C13 C16 1.498(8) ? ? yes C14 C15 1.356(8) ? ? yes C15 C17 1.490(8) ? ? yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni N1 96.4(1) ? ? ? yes S1 Ni N2 176.5(1) ? ? ? yes S1 Ni N3 92.0(1) ? ? ? yes N1 Ni N2 86.8(2) ? ? ? yes N1 Ni N3 170.4(2) ? ? ? yes N2 Ni N3 85.0(2) ? ? ? yes O2 Cl O3 112.4(4) ? ? ? no O2 Cl O4 108.9(4) ? ? ? no O2 Cl O5 109.3(4) ? ? ? no O3 Cl O4 107.1(5) ? ? ? no O3 Cl O5 110.5(5) ? ? ? no O4 Cl O5 108.7(5) ? ? ? no Ni S1 C2 111.0(2) ? ? ? no C1 S2 C2 104.8(3) ? ? ? no C12 O1 C18 110.7(5) ? ? ? no Ni N1 C7 133.0(4) ? ? ? no Ni N1 C8 112.1(3) ? ? ? no C7 N1 C8 114.8(5) ? ? ? no Ni N2 C9 104.0(3) ? ? ? no Ni N2 C11 107.2(3) ? ? ? no Ni N2 C12 111.1(3) ? ? ? no C9 N2 C11 111.8(4) ? ? ? no C9 N2 C12 111.9(5) ? ? ? no C11 N2 C12 110.6(5) ? ? ? no Ni N3 N4 111.5(3) ? ? ? no Ni N3 C13 143.6(4) ? ? ? no N4 N3 C13 104.3(5) ? ? ? no N3 N4 C11 117.6(5) ? ? ? no N3 N4 C15 113.2(5) ? ? ? no C11 N4 C15 128.9(5) ? ? ? no S1 C2 S2 117.2(3) ? ? ? no S1 C2 C3 126.8(5) ? ? ? no S2 C2 C3 116.0(5) ? ? ? no C2 C3 C4 124.9(6) ? ? ? no C2 C3 C7 125.7(5) ? ? ? no C4 C3 C7 109.4(5) ? ? ? no C3 C4 C5 106.8(5) ? ? ? no C4 C5 C6 107.1(5) ? ? ? no C5 C6 C7 107.0(5) ? ? ? no N1 C7 C3 125.7(5) ? ? ? no N1 C7 C6 124.8(5) ? ? ? no C3 C7 C6 109.5(5) ? ? ? no N1 C8 C9 109.0(5) ? ? ? no N2 C9 C8 106.9(4) ? ? ? no N2 C9 C10 115.0(5) ? ? ? no C8 C9 C10 113.2(5) ? ? ? no N2 C11 N4 108.1(4) ? ? ? no O1 C12 N2 108.7(5) ? ? ? no N3 C13 C14 109.8(5) ? ? ? no N3 C13 C16 125.5(5) ? ? ? no C14 C13 C16 124.7(5) ? ? ? no C13 C14 C15 107.5(6) ? ? ? no N4 C15 C14 105.3(5) ? ? ? no N4 C15 C17 122.5(6) ? ? ? no C14 C15 C17 132.3(6) ? ? ? no #====END data_(2)_C16H25ClN4NiO4S2 _audit_creation_date '1998-11-23' _audit_creation_method 'by teXsan v1.7' _computing_data_collection 'CAD4/PC (Enraf-Nonius, 1993)' _computing_cell_refinement 'CAD4/PC (Enraf-Nonius, 1993)' _computing_data_reduction 'TEXSAN (Molecular Structure Corp., 1997)' _computing_structure_solution 'TEXSAN (Molecular Structure Corp., 1997)' _computing_structure_refinement 'TEXSAN (Molecular Structure Corp., 1997)' _computing_publication_material 'TEXSAN (Molecular Structure Corp., 1997)' _cell_length_a 7.8562(12) _cell_length_b 20.9125(16) _cell_length_c 12.7270(13) _cell_angle_alpha 90 _cell_angle_beta 99.381(11) _cell_angle_gamma 90 _cell_volume 2063.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.0 _cell_measurement_theta_max 14.9 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' _exptl_crystal_description 'tablet' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 495.67 _chemical_formula_sum 'C16 H25 Cl N4 Ni O4 S2 ' _chemical_formula_moiety 'C16 H25 N4 Ni S2 1+, Cl O4 1-' _exptl_crystal_F_000 1032.00 _exptl_absorpt_coefficient_mu 1.30 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.800 _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'sealed X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Enraf-Nonius CAD-4 diffractometer' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1.9 _diffrn_reflns_number 4026 _reflns_number_total 3744 _reflns_number_gt 2940 _reflns_threshold_expression 'I>1.5\s(I)' _diffrn_reflns_av_R_equivalents 0.012 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00417 _diffrn_orient_matrix_UB_12 0.03784 _diffrn_orient_matrix_UB_13 0.04838 _diffrn_orient_matrix_UB_21 0.01349 _diffrn_orient_matrix_UB_22 -0.02916 _diffrn_orient_matrix_UB_23 0.06304 _diffrn_orient_matrix_UB_31 0.12821 _diffrn_orient_matrix_UB_32 0.00186 _diffrn_orient_matrix_UB_33 0.00486 loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 64 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 100 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 4 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 16 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni 0 4 0.285 1.113 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 16 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 8 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ;w = 4F~o~^2^/[\s^2^(I)+(0.02I)^2^] ; _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0.000 _refine_ls_abs_structure_details 'not applicable' _refine_ls_number_reflns 2940 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_number_constraints 50 _refine_ls_R_factor_all 0.066 _refine_ls_R_factor_gt 0.048 _refine_ls_wR_factor_all 0.062 _refine_ls_wR_factor_ref 0.061 _refine_ls_goodness_of_fit_all 2.49 _refine_ls_goodness_of_fit_ref 2.73 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 _refine_diff_density_min -0.61 _refine_diff_density_max 0.92 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni 0.72087(8) 0.52096(3) 0.59243(4) 0.03454(16) 1.000 . Uani d ? Cl 0.8659(2) 0.12343(7) 0.59630(12) 0.0672(5) 1.000 . Uani d ? S1 0.72427(18) 0.53427(5) 0.42627(9) 0.0452(3) 1.000 . Uani d ? S2 0.71293(20) 0.63479(6) 0.25931(9) 0.0548(4) 1.000 . Uani d ? O1 0.9238(8) 0.0736(3) 0.6612(6) 0.160(3) 1.000 . Uani d ? O2 0.9840(8) 0.1678(3) 0.5912(8) 0.218(4) 1.000 . Uani d ? O3 0.7285(10) 0.1503(4) 0.6290(11) 0.266(6) 1.000 . Uani d ? O4 0.803(2) 0.1021(6) 0.5088(6) 0.382(8) 1.000 . Uani d ? N1 0.6621(5) 0.60506(16) 0.6228(3) 0.0374(10) 1.000 . Uani d ? N2 0.7387(5) 0.50723(18) 0.7445(3) 0.0438(11) 1.000 . Uani d ? N3 0.7738(5) 0.43114(17) 0.5883(3) 0.0389(11) 1.000 . Uani d ? N4 0.7718(5) 0.40230(18) 0.6858(3) 0.0432(12) 1.000 . Uani d ? C1 0.7973(7) 0.5659(3) 0.2011(4) 0.0582(17) 1.000 . Uani d ? C2 0.7013(6) 0.6134(2) 0.3917(3) 0.0387(13) 1.000 . Uani d ? C3 0.6716(6) 0.6623(2) 0.4562(4) 0.0433(14) 1.000 . Uani d ? C4 0.6503(8) 0.7315(2) 0.4224(4) 0.0569(16) 1.000 . Uani d ? C5 0.6536(10) 0.7690(3) 0.5229(4) 0.082(2) 1.000 . Uani d ? C6 0.6156(8) 0.7227(2) 0.6064(4) 0.0596(17) 1.000 . Uani d ? C7 0.6516(6) 0.6568(2) 0.5648(3) 0.0387(13) 1.000 . Uani d ? C8 0.6402(7) 0.6137(2) 0.7357(3) 0.0450(14) 1.000 . Uani d ? C9 0.6175(7) 0.5506(2) 0.7845(4) 0.0492(15) 1.000 . Uani d ? C10 0.6393(8) 0.5522(3) 0.9057(3) 0.0583(17) 1.000 . Uani d ? C11 0.7171(7) 0.4396(2) 0.7688(4) 0.0495(15) 1.000 . Uani d ? C12 0.8196(6) 0.3838(2) 0.5263(4) 0.0427(13) 1.000 . Uani d ? C13 0.8404(7) 0.3268(2) 0.5839(4) 0.0522(16) 1.000 . Uani d ? C14 0.8106(7) 0.3401(2) 0.6848(4) 0.0485(15) 1.000 . Uani d ? C15 0.8436(8) 0.3913(2) 0.4138(4) 0.0561(16) 1.000 . Uani d ? C16 0.8157(9) 0.2985(3) 0.7807(5) 0.0704(20) 1.000 . Uani d ? H1 0.7211 0.5308 0.2034 0.070 1.000 . Uiso c ? H2 0.8059 0.5752 0.1291 0.070 1.000 . Uiso c ? H3 0.9081 0.5552 0.2389 0.070 1.000 . Uiso c ? H4 0.7410 0.7444 0.3860 0.068 1.000 . Uiso c ? H5 0.5426 0.7376 0.3774 0.068 1.000 . Uiso c ? H6 0.7657 0.7863 0.5438 0.098 1.000 . Uiso c ? H7 0.5714 0.8027 0.5132 0.098 1.000 . Uiso c ? H8 0.6875 0.7306 0.6726 0.072 1.000 . Uiso c ? H9 0.4981 0.7262 0.6150 0.072 1.000 . Uiso c ? H10 0.7394 0.6335 0.7750 0.054 1.000 . Uiso c ? H11 0.5419 0.6398 0.7383 0.054 1.000 . Uiso c ? H12 0.5042 0.5360 0.7579 0.059 1.000 . Uiso c ? H13 0.6253 0.5101 0.9311 0.070 1.000 . Uiso c ? H14 0.7524 0.5670 0.9325 0.070 1.000 . Uiso c ? H15 0.5570 0.5797 0.9291 0.070 1.000 . Uiso c ? H16 0.7835 0.4290 0.8357 0.059 1.000 . Uiso c ? H17 0.5986 0.4317 0.7718 0.059 1.000 . Uiso c ? H18 0.8699 0.2864 0.5580 0.063 1.000 . Uiso c ? H19 0.8740 0.3513 0.3869 0.067 1.000 . Uiso c ? H20 0.7388 0.4060 0.3726 0.067 1.000 . Uiso c ? H21 0.9324 0.4215 0.4096 0.067 1.000 . Uiso c ? H22 0.7052 0.2979 0.8018 0.084 1.000 . Uiso c ? H23 0.8471 0.2562 0.7641 0.084 1.000 . Uiso c ? H24 0.8983 0.3148 0.8372 0.084 1.000 . Uiso c ? H25 0.8519 0.5194 0.7767 0.053 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni 0.0469(4) 0.0322(3) 0.0246(3) -0.0012(3) 0.0059(2) -0.0004(2) Cl 0.0773(11) 0.0544(9) 0.0661(9) -0.0034(8) 0.0004(8) 0.0112(7) S1 0.0755(9) 0.0338(6) 0.0268(6) -0.0015(6) 0.0094(6) -0.0009(5) S2 0.0873(11) 0.0471(7) 0.0306(6) -0.0031(7) 0.0119(6) 0.0068(5) O1 0.132(5) 0.137(5) 0.215(7) 0.018(4) 0.038(5) 0.113(5) O2 0.089(5) 0.098(5) 0.450(14) -0.019(4) -0.006(6) 0.116(7) O3 0.105(6) 0.170(8) 0.527(19) 0.040(6) 0.060(8) 0.074(10) O4 0.72(3) 0.350(15) 0.065(5) -0.160(17) 0.023(9) -0.085(7) N1 0.049(2) 0.036(2) 0.028(2) -0.000(2) 0.008(2) -0.002(2) N2 0.060(3) 0.044(2) 0.029(2) 0.003(2) 0.011(2) 0.004(2) N3 0.053(3) 0.035(2) 0.030(2) -0.000(2) 0.010(2) 0.002(2) N4 0.058(3) 0.041(2) 0.031(2) 0.001(2) 0.009(2) 0.004(2) C1 0.073(4) 0.065(4) 0.041(3) -0.005(3) 0.023(3) -0.002(3) C2 0.049(3) 0.038(2) 0.028(2) -0.007(2) 0.004(2) 0.002(2) C3 0.056(3) 0.036(3) 0.038(3) -0.005(2) 0.004(2) 0.001(2) C4 0.090(4) 0.036(3) 0.045(3) -0.001(3) 0.010(3) 0.006(2) C5 0.151(7) 0.040(3) 0.057(4) 0.005(4) 0.024(4) 0.002(3) C6 0.093(5) 0.039(3) 0.048(3) 0.004(3) 0.016(3) -0.004(2) C7 0.045(3) 0.035(2) 0.035(2) -0.004(2) 0.004(2) -0.004(2) C8 0.064(3) 0.043(3) 0.029(2) 0.001(2) 0.011(2) -0.006(2) C9 0.068(4) 0.047(3) 0.034(3) -0.002(3) 0.014(2) -0.006(2) C10 0.085(4) 0.060(3) 0.033(3) 0.003(3) 0.020(3) -0.001(2) C11 0.068(4) 0.047(3) 0.036(3) -0.003(3) 0.015(2) 0.004(2) C12 0.050(3) 0.039(3) 0.038(3) 0.000(2) 0.004(2) -0.003(2) C13 0.066(4) 0.035(3) 0.055(3) 0.005(3) 0.008(3) -0.001(2) C14 0.064(4) 0.036(3) 0.044(3) -0.002(2) 0.002(2) 0.005(2) C15 0.082(4) 0.045(3) 0.043(3) 0.011(3) 0.016(3) -0.009(2) C16 0.102(5) 0.049(3) 0.060(4) 0.003(3) 0.012(3) 0.016(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S1 2.138(2) . . yes Ni N1 1.874(4) . . yes Ni N2 1.939(4) . . yes Ni N3 1.926(4) . . yes Cl O1 1.361(5) . . no Cl O2 1.322(6) . . no Cl O3 1.342(9) . . no Cl O4 1.226(7) . . no S1 C2 1.714(4) . . yes S2 C1 1.796(5) . . yes S2 C2 1.760(4) . . yes N1 C7 1.304(5) . . yes N1 C8 1.485(5) . . yes N2 C9 1.465(6) . . yes N2 C11 1.463(6) . . yes N3 N4 1.381(5) . . yes N3 C12 1.351(6) . . yes N4 C11 1.434(6) . . yes N4 C14 1.336(6) . . yes C2 C3 1.355(6) . . yes C3 C4 1.512(6) . . yes C3 C7 1.421(6) . . yes C4 C5 1.498(7) . . yes C5 C6 1.504(7) . . yes C6 C7 1.519(6) . . yes C8 C9 1.481(6) . . yes C9 C10 1.524(6) . . yes C12 C13 1.393(6) . . yes C12 C15 1.483(6) . . yes C13 C14 1.371(7) . . yes C14 C16 1.495(7) . . yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni N1 97.18(11) . . . yes S1 Ni N2 175.08(13) . . . yes S1 Ni N3 93.59(10) . . . yes N1 Ni N2 85.03(15) . . . yes N1 Ni N3 169.09(14) . . . yes N2 Ni N3 84.36(15) . . . yes O1 Cl O2 113.6(4) . . . no O1 Cl O3 109.8(6) . . . no O1 Cl O4 108.5(7) . . . no O2 Cl O3 109.1(5) . . . no O2 Cl O4 113.1(7) . . . no O3 Cl O4 102.1(9) . . . no Ni S1 C2 111.22(15) . . . no C1 S2 C2 105.7(2) . . . no Ni N1 C7 131.0(3) . . . no Ni N1 C8 112.6(3) . . . no C7 N1 C8 116.1(4) . . . no Ni N2 C9 108.0(3) . . . no Ni N2 C11 111.2(3) . . . no C9 N2 C11 114.9(4) . . . no Ni N3 N4 111.6(3) . . . no Ni N3 C12 144.1(3) . . . no N4 N3 C12 104.3(4) . . . no N3 N4 C11 118.2(4) . . . no N3 N4 C14 112.4(4) . . . no C11 N4 C14 129.2(4) . . . no S1 C2 S2 118.2(3) . . . no S1 C2 C3 126.5(3) . . . no S2 C2 C3 115.4(3) . . . no C2 C3 C4 124.9(4) . . . no C2 C3 C7 125.8(4) . . . no C4 C3 C7 109.2(4) . . . no C3 C4 C5 105.8(4) . . . no C4 C5 C6 106.8(4) . . . no C5 C6 C7 105.6(4) . . . no N1 C7 C3 127.7(4) . . . no N1 C7 C6 123.5(4) . . . no C3 C7 C6 108.8(4) . . . no N1 C8 C9 109.8(4) . . . no N2 C9 C8 106.0(4) . . . no N2 C9 C10 113.1(4) . . . no C8 C9 C10 113.8(4) . . . no N2 C11 N4 108.1(4) . . . no N3 C12 C13 109.8(4) . . . no N3 C12 C15 125.0(4) . . . no C13 C12 C15 125.1(4) . . . no C12 C13 C14 107.2(4) . . . no N4 C14 C13 106.3(4) . . . no N4 C14 C16 122.3(5) . . . no C13 C14 C16 131.4(5) . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S2 C6 3.574(5) . 4_564 no S2 C5 3.586(6) . 4_564 no O1 N2 3.059(7) . 2_746 no O1 C1 3.149(8) . 4 no O1 C15 3.454(9) . 4 no O1 C8 3.563(9) . 2_746 no O1 C9 3.590(8) . 2_746 no O2 C13 3.508(8) . . no O2 C8 3.568(8) . 2_746 no O2 C4 3.589(8) . 3_766 no O3 C10 3.513(10) . 2_646 no O4 C11 3.143(8) . 4_554 no O4 C16 3.585(12) . 4_554 no N4 C1 3.520(7) . 3_766 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ni S1 C2 S2 . . . . 176.5(2) no Ni S1 C2 C3 . . . . -4.7(5) no Ni N1 C7 C3 . . . . 4.8(8) no Ni N1 C7 C6 . . . . -174.8(4) no Ni N1 C8 C9 . . . . -17.4(5) no Ni N2 C9 C8 . . . . -45.4(4) no Ni N2 C9 C10 . . . . -170.8(4) no Ni N2 C11 N4 . . . . 27.5(5) no Ni N3 N4 C11 . . . . 5.7(5) no Ni N3 N4 C14 . . . . -179.1(3) no Ni N3 C12 C13 . . . . 178.3(4) no Ni N3 C12 C15 . . . . -1.9(9) no S1 Ni N1 C7 . . . . -8.7(4) no S1 Ni N1 C8 . . . . 177.6(3) no S1 Ni N2 C9 . . . . 146.8(13) no S1 Ni N2 C11 . . . . -86.2(15) no S1 Ni N3 N4 . . . . -175.9(3) no S1 Ni N3 C12 . . . . 7.6(6) no S1 C2 S2 C1 . . . . -13.0(4) no S1 C2 C3 C4 . . . . -179.4(4) no S1 C2 C3 C7 . . . . -0.9(8) no S2 C2 C3 C4 . . . . -0.6(7) no S2 C2 C3 C7 . . . . 177.9(4) no N1 Ni S1 C2 . . . . 7.4(2) no N1 Ni N2 C9 . . . . 29.9(3) no N1 Ni N2 C11 . . . . 156.8(4) no N1 Ni N3 N4 . . . . -5.0(10) no N1 Ni N3 C12 . . . . 178.5(7) no N1 C7 C3 C2 . . . . 1.9(8) no N1 C7 C3 C4 . . . . -179.5(5) no N1 C7 C6 C5 . . . . 167.7(5) no N1 C8 C9 N2 . . . . 40.4(5) no N1 C8 C9 C10 . . . . 165.4(4) no N2 Ni S1 C2 . . . . -109.1(14) no N2 Ni N1 C7 . . . . 166.9(5) no N2 Ni N1 C8 . . . . -6.8(3) no N2 Ni N3 N4 . . . . 8.6(3) no N2 Ni N3 C12 . . . . -167.9(6) no N2 C11 N4 N3 . . . . -21.9(6) no N2 C11 N4 C14 . . . . 163.9(5) no N3 Ni S1 C2 . . . . -174.3(2) no N3 Ni N1 C7 . . . . -179.5(7) no N3 Ni N1 C8 . . . . 6.8(10) no N3 Ni N2 C9 . . . . -147.6(3) no N3 Ni N2 C11 . . . . -20.7(3) no N3 N4 C14 C13 . . . . 0.3(6) no N3 N4 C14 C16 . . . . -179.6(5) no N3 C12 C13 C14 . . . . -1.5(6) no N4 N3 C12 C13 . . . . 1.6(5) no N4 N3 C12 C15 . . . . -178.5(5) no N4 C11 N2 C9 . . . . 150.6(4) no N4 C14 C13 C12 . . . . 0.7(6) no C1) S2 C2 C3 . . . . 168.1(4) no C2 C3 C4 C5 . . . . -169.6(6) no C2 C3 C7 C6 . . . . -178.5(5) no C3 C4 C5 C6 . . . . -18.9(7) no C3 C7 N1 C8 . . . . 178.4(5) no C3 C7 C6 C5 . . . . -11.9(6) no C4 C3 C7 C6 . . . . 0.2(6) no C4 C5 C6 C7 . . . . 19.0(7) no C5 C4 C3 C7 . . . . 11.7(6) no C6 C7 N1 C8 . . . . -1.2(7) no C7 N1 C8 C9 . . . . 167.8(4) no C8 C9 N2 C11 . . . . -170.1(4) no C10 C9 N2 C11 . . . . 64.4(6) no C11 N4 N3 C12 . . . . -176.4(4) no C11 N4 C14 C13 . . . . 174.8(5) no C11 N4 C14 C16 . . . . -5.2(9) no C12 N3 N4 C14 . . . . -1.2(5) no C12 C13 C14 C16 . . . . -179.3(6) no C14 C13 C12 C15 . . . . 178.7(5) no #====END data_(3)_C25H41ClN6Ni2O4S4 _audit_creation_date 'Tue Apr 7 14:18:10 1998' _audit_creation_method 'from TEXRAY.INF file' _computing_data_collection 'CAD4/PC (Enraf-Nonius, 1993)' _computing_cell_refinement 'CAD4/PC (Enraf-Nonius, 1993)' _computing_data_reduction 'TEXSAN (Molecular Structure Corp., 1989)' _computing_structure_solution 'TEXSAN (Molecular Structure Corp., 1989)' _computing_structure_refinement 'TEXSAN (Molecular Structure Corp., 1989)' _computing_publication_material 'TEXSAN (Molecular Structure Corp., 1989)' _cell_length_a 18.732(2) _cell_length_b 11.284(1) _cell_length_c 16.048(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3392(1) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.0 _cell_measurement_theta_max 16.0 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I b a 2 ' _symmetry_Int_Tables_number 45 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y,1/2+z' ' -x, -y, +z' '1/2-x,1/2-y,1/2+z' ' -x, +y,1/2+z' '1/2-x,1/2+y, +z' ' +x, -y,1/2+z' '1/2+x,1/2-y, +z' _exptl_crystal_description 'prism' _exptl_crystal_colour 'rose-pink' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 770.73 _chemical_formula_sum 'C25 H41 Cl N6 Ni2 O4 S4 ' _chemical_formula_moiety 'C24 H41 N6 Ni2 S4 1+, Cl O4 1-' _chemical_formula_structural '(Ni2 (C10 H9 N2 S2 )2 (C5 H7 N2 )) (Cl O4 )' _exptl_crystal_F_000 1608.00 _exptl_absorpt_coefficient_mu 1.47 _exptl_absorpt_correction_type none _diffrn_special_details none _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'sealed X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Enraf-Nonius CAD-4 diffractometer' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0.6 _diffrn_reflns_number 1686 _reflns_number_total 1686 _reflns_number_observed 1312 _reflns_observed_criterion 'I>1.5s\(I)' _diffrn_reflns_av_R_equivalents 'no equivalent rflns measured' _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25.0 _diffrn_orient_matrix_UB_11 0.00069 _diffrn_orient_matrix_UB_12 -0.02206 _diffrn_orient_matrix_UB_13 0.08069 _diffrn_orient_matrix_UB_21 0.01309 _diffrn_orient_matrix_UB_22 0.04758 _diffrn_orient_matrix_UB_23 0.03563 _diffrn_orient_matrix_UB_31 -0.06091 _diffrn_orient_matrix_UB_32 0.00995 _diffrn_orient_matrix_UB_33 0.00854 loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 100 0.002 0.002 'Cromer & Waber (1974)' H 0 164 0.000 0.000 'Cromer & Waber (1974)' Cl 0 4 0.132 0.159 'Cromer & Waber (1974)' N 0 24 0.004 0.003 'Cromer & Waber (1974)' Ni 0 8 0.285 1.113 'Cromer & Waber (1974)' O 0 16 0.008 0.006 'Cromer & Waber (1974)' S 0 16 0.110 0.124 'Cromer & Waber (1974)' _refine_special_details ;The anion was disordered over two sites ca. 0.4 \%A from a crystal diad axis. Its atoms were refined isotropically with site occupancy factors of 0.5. Hydrogen atoms were included at calculated positions [d(C---H) = 0.95 \%A; U(H) = 1.2U~eq~(C)]. The value of a secondary extinction parameter (Stout & Jensen, 1968) was predicted to be negative and was fixed at zero. Refinement of the structure of opposite polarity led to no significant changes in standard deviations or residuals. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ;w = 4F~o~^2^/[\s^2^(I)+(0.02I)^2^] ; _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1312 _refine_ls_number_parameters 187 _refine_ls_R_factor_obs 0.041 _refine_ls_wR_factor_obs 0.042 _refine_ls_goodness_of_fit_obs 2.17 _refine_ls_shift/esd_max 0.034 _refine_diff_density_max 0.44 _refine_diff_density_min -0.46 loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom Ni 0.44274(4) 0.38918(6) 0.5000 0.0394(2) Uij ? ? Cl 0.4811(2) 0.0002(6) 0.8484(3) 0.072(1) Uij ? ? S1 0.35143(9) 0.5014(2) 0.4910(2) 0.0517(5) Uij ? ? S2 0.2295(1) 0.5953(3) 0.5895(2) 0.0913(10) Uij ? ? O1 0.5410(10) 0.073(2) 0.905(2) 0.140(7) Uij ? ? O2 0.485(1) 0.116(1) 0.855(1) 0.127(6) Uij ? ? O3 0.535(1) 0.020(3) 0.768(2) 0.22(1) Uij ? ? O4 0.578(2) -0.032(3) 0.849(2) 0.23(1) Uij ? ? N1 0.4212(3) 0.3198(5) 0.6024(4) 0.047(2) Uij ? ? N2 0.5238(3) 0.2844(4) 0.4956(5) 0.052(2) Uij ? ? N3 0.4738(3) 0.4592(4) 0.3981(3) 0.035(2) Uij ? ? C1 0.2190(6) 0.658(1) 0.4902(9) 0.118(5) Uij ? ? C2 0.3012(4) 0.4968(7) 0.5798(5) 0.053(2) Uij ? ? C3 0.3133(5) 0.4263(8) 0.6478(5) 0.060(3) Uij ? ? C4 0.2676(5) 0.423(1) 0.7243(6) 0.091(4) Uij ? ? C5 0.2916(9) 0.318(1) 0.7715(8) 0.139(6) Uij ? ? C6 0.3609(6) 0.2755(10) 0.7377(6) 0.087(3) Uij ? ? C7 0.3687(5) 0.3413(8) 0.6547(5) 0.057(3) Uij ? ? C8 0.4728(6) 0.2237(9) 0.6230(6) 0.078(3) Uij ? ? C9 0.5414(6) 0.2443(9) 0.5798(6) 0.088(4) Uij ? ? C10 0.5928(7) 0.1404(9) 0.5830(8) 0.097(4) Uij ? ? C11 0.5000 0.5000 0.2666(5) 0.044(3) Uij ? ? C12 0.4567(3) 0.4320(6) 0.3187(4) 0.039(2) Uij ? ? C13 0.4001(5) 0.3445(8) 0.3006(5) 0.058(3) Uij ? ? H1 0.5126 0.2178 0.4618 0.0629 Uiso ? ? H2 0.5634 0.3252 0.4725 0.0629 Uiso ? ? H3 0.2619 0.6966 0.4743 0.1416 Uiso ? ? H4 0.2082 0.5972 0.4511 0.1416 Uiso ? ? H5 0.1810 0.7137 0.4913 0.1416 Uiso ? ? H6 0.2741 0.4928 0.7563 0.1093 Uiso ? ? H7 0.2187 0.4152 0.7095 0.1093 Uiso ? ? H8 0.2973 0.3387 0.8285 0.1665 Uiso ? ? H9 0.2570 0.2569 0.7667 0.1665 Uiso ? ? H10 0.3989 0.2949 0.7744 0.1043 Uiso ? ? H11 0.3598 0.1922 0.7291 0.1043 Uiso ? ? H12 0.4807 0.2225 0.6814 0.0939 Uiso ? ? H13 0.4537 0.1497 0.6057 0.0939 Uiso ? ? H14 0.5641 0.3088 0.6072 0.1051 Uiso ? ? H15 0.5714 0.0733 0.5575 0.1161 Uiso ? ? H16 0.6354 0.1604 0.5541 0.1161 Uiso ? ? H17 0.6038 0.1226 0.6394 0.1161 Uiso ? ? H18 0.5000 0.5000 0.2074 0.0534 Uiso ? ? H19 0.3561 0.3714 0.3232 0.0695 Uiso ? ? H20 0.3954 0.3354 0.2420 0.0695 Uiso ? ? H21 0.4124 0.2705 0.3249 0.0695 Uiso ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni 0.0519(4) 0.0360(4) 0.0305(4) -0.0027(4) -0.0018(6) 0.0001(6) S1 0.0555(9) 0.0518(9) 0.048(1) 0.0054(8) 0.017(1) 0.005(1 S2 0.080(2) 0.109(2) 0.085(2) 0.015(2) 0.039(2) -0.012(2) N1 0.066(4) 0.040(4) 0.036(4) -0.017(3) -0.008(3) 0.006(3) N2 0.065(3) 0.041(3) 0.051(3) 0.004(3) -0.018(4) -0.008(4) N3 0.039(3) 0.037(3) 0.030(3) 0.003(2) -0.002(2) -0.003(2) C1 0.114(8) 0.148(10) 0.092(9) 0.068(7) 0.021(9) 0.037(10) C2 0.054(4) 0.059(4) 0.047(5) -0.014(4) 0.015(4) -0.013(4) C3 0.065(5) 0.073(6) 0.043(5) -0.025(5) 0.012(4) -0.014(4) C4 0.097(8) 0.127(9) 0.049(6) -0.042(7) 0.016(5) -0.011(6) C5 0.20(2) 0.14(1) 0.072(8) 0.01(1) 0.071(9) 0.026(8) C6 0.119(8) 0.103(8) 0.039(4) -0.053(7) -0.016(6) 0.014(5) C7 0.083(6) 0.063(5) 0.025(4) -0.038(5) -0.010(4) 0.005(4) C8 0.094(7) 0.076(6) 0.065(6) -0.020(6) -0.025(6) 0.021(5) C9 0.116(9) 0.084(7) 0.062(6) 0.012(6) -0.017(6) 0.022(6) C10 0.120(8) 0.074(7) 0.096(8) 0.026(6) -0.035(7) 0.011(6) C11 0.056(5) 0.055(6) 0.023(6) 0.002(7) 0.0000 0.0000 C12 0.039(4) 0.040(4) 0.038(4) 0.010(3) -0.003(3) -0.010(3) C13 0.066(6) 0.066(5) 0.042(5) 0.005(4) -0.016(4) -0.014(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S1 2.133(2) ? ? yes Ni N1 1.865(6) ? ? yes Ni N2 1.925(5) ? ? yes Ni N3 1.907(5) ? ? yes Cl Cl 0.709(8) ? ? no Cl O1 1.30(2) ? ? no Cl O2 1.46(2) ? ? no Cl O3 1.34(3) ? ? no Cl O4 1.17(3) ? ? no S1 C2 1.709(7) ? ? yes S2 C1 1.75(1) ? ? yes S2 C2 1.750(9) ? ? yes O1 O2 1.41(2) ? ? yes O1 O4 1.64(3) ? ? yes O2 O4 1.52(3) ? ? yes O3 O3 1.38(5) ? ? yes O3 O4 1.65(4) ? ? yes N1 C7 1.32(1) ? ? yes N1 C8 1.49(1) ? ? yes N2 C9 1.46(1) ? ? yes N3 N3 1.347(10) ? 2_665 yes N3 C12 1.348(8) ? ? yes C2 C3 1.37(1) ? ? yes C3 C4 1.50(1) ? ? yes C3 C7 1.42(1) ? ? yes C4 C5 1.47(2) ? ? yes C5 C6 1.49(2) ? ? yes C6 C7 1.53(1) ? ? yes C8 C9 1.48(1) ? ? yes C9 C10 1.52(1) ? ? yes C11 C12 1.396(9) ? ? yes C12 C13 1.48(1) ? ? yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni N1 97.8(2) ? ? ? yes S1 Ni N2 173.8(3) ? ? ? yes S1 Ni N3 86.6(2) ? ? ? yes N1 Ni N2 86.9(3) ? ? ? yes N1 Ni N3 174.8(3) ? ? ? yes N2 Ni N3 89.0(3) ? ? ? yes O1 Cl O2 96.2(10) ? ? ? no O1 Cl O3 119(1) ? ? ? no O1 Cl O4 118(1) ? ? ? no O2 Cl O3 105(1) ? ? ? no O2 Cl O4 98(2) ? ? ? no O3 Cl O4 101(1) ? ? ? no Ni S1 C2 111.5(3) ? ? ? no C1 S2 C2 105.2(4) ? ? ? no Ni N1 C7 130.3(6) ? ? ? no Ni N1 C8 111.1(6) ? ? ? no C7 N1 C8 118.6(7) ? ? ? no Ni N2 C9 109.5(6) ? ? ? no Ni N3 N3 120.4(2) ? ? ? no Ni N3 C12 130.0(5) ? ? ? no N3 N3 C12 109.2(4) ? ? ? no S1 C2 S2 118.5(5) ? ? ? no S1 C2 C3 126.2(7) ? ? ? no S2 C2 C3 115.2(6) ? ? ? no C2 C3 C4 125.0(9) ? ? ? no C2 C3 C7 125.3(7) ? ? ? no C4 C3 C7 109.7(9) ? ? ? no C3 C4 C5 105.5(10) ? ? ? no C4 C5 C6 109.8(9) ? ? ? no C5 C6 C7 104.1(10) ? ? ? no N1 C7 C3 128.4(7) ? ? ? no N1 C7 C6 122.5(9) ? ? ? no C3 C7 C6 109.0(8) ? ? ? no N1 C8 C9 110.2(8) ? ? ? no N2 C9 C8 106.6(8) ? ? ? no N2 C9 C10 114.4(9) ? ? ? no C8 C9 C10 114.5(9) ? ? ? no C12 C11 C12 106.3(8) ? ? ? no N3 C12 C11 107.6(6) ? ? ? no N3 C12 C13 120.6(6) ? ? ? no C11 C12 C13 131.8(7) ? ? ? no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni S1 C2 S2 172.9(3) ? ? ? ? no Ni S1 C2 C3 -3.8(8) ? ? ? ? no Ni N1 C7 C3 -1(1) ? ? ? ? no Ni N1 C7 C6 -178.7(5) ? ? ? ? no Ni N1 C8 C9 25.2(8) ? ? ? ? no Ni N2 C9 C8 39.1(9) ? ? ? ? no Ni N2 C9 C10 166.7(7) ? ? ? ? no Ni N3 N3 C12 174.0(3) ? ? ? ? no Ni N3 C12 C11 -173.1(3) ? ? ? ? no Ni N3 C12 C13 7.6(9) ? ? ? ? no S1 Ni N1 C7 -4.6(7) ? ? ? ? no S1 Ni N1 C8 173.7(5) ? ? ? ? no S1 Ni N2 C9 -160(2) ? ? ? ? no S1 Ni N3 N3 104.1(6) ? ? ? ? no S1 Ni N3 C12 -83.9(6) ? ? ? ? no S1 C2 S2 C1 10.9(7) ? ? ? ? no S1 C2 C3 C4 -178.9(7) ? ? ? ? no S1 C2 C3 C7 -2(1) ? ? ? ? no S2 C2 C3 C4 4(1) ? ? ? ? no S2 C2 C3 C7 -179.1(6) ? ? ? ? no N1 Ni S1 C2 5.9(3) ? ? ? ? no N1 Ni N2 C9 -21.3(6) ? ? ? ? no N1 Ni N3 N3 -42(3) ? ? ? ? no N1 Ni N3 C12 130(3) ? ? ? ? no N1 C7 C3 C2 6(1) ? ? ? ? no N1 C7 C3 C4 -177.3(7) ? ? ? ? no N1 C7 C6 C5 -174.2(9) ? ? ? ? no N1 C8 C9 N2 -41(1) ? ? ? ? no N1 C8 C9 C10 -168.9(8) ? ? ? ? no N2 Ni S1 C2 144(2) ? ? ? ? no N2 Ni N1 C7 179.5(7) ? ? ? ? no N2 Ni N1 C8 -2.2(5) ? ? ? ? no N2 Ni N3 N3 -80.2(6) ? ? ? ? no N2 Ni N3 C12 91.8(6) ? ? ? ? no N3 Ni S1 C2 -171.2(3) ? ? ? ? no N3 Ni N1 C7 141(3) ? ? ? ? no N3 Ni N1 C8 -40(3) ? ? ? ? no N3 Ni N2 C9 155.4(6) ? ? ? ? no N3 N3 C12 C11 -0.4(8) ? ? ? ? no N3 N3 C12 C13 -179.8(6) ? ? ? ? no N3 C12 C11 C12 0.1(3) ? ? ? ? no C1 S2 C2 C3 -172.1(7) ? ? ? ? no C2 C3 C4 C5 168(1) ? ? ? ? no C2 C3 C7 C6 -176.2(8) ? ? ? ? no C3 C4 C5 C6 14(1) ? ? ? ? no C3 C7 N1 C8 -179.1(7) ? ? ? ? no C3 C7 C6 C5 7(1) ? ? ? ? no C4 C3 C7 C6 0.8(9) ? ? ? ? no C4 C5 C6 C7 -13(1) ? ? ? ? no C5 C4 C3 C7 -9(1) ? ? ? ? no C6 C7 N1 C8 3(1) ? ? ? ? no C7 N1 C8 C9 -156.2(8) ? ? ? ? no C12 C11 C12 C13 179.4(9) ? ? ? ? no #====END