Supplementary Information (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal ' ChemComm' loop_ _publ_author_name 'Nakamura, Takayoshi' 'Akutagawa, T.' 'Hasegawa, Tatsuo' 'Nishihara, Sadafumi' _publ_contact_author_name 'Prof Takayoshi Nakamura' _publ_contact_author_address ; Research Institute for Electronic Science Hokkaido University N12W6, Kita-ku Sapporo Hokkaido 060-0812 JAPAN ; _publ_contact_author_email ' tnaka@imd.es.hokudai.ac.jp ' _publ_section_title ; Formation of Molecular Spin Ladder Induced by Supramolecular Cation Structure ; _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, M., Giacovazzo, C, Guagliardi, A., Polidori, G., (1994). J. Appl. Cryst. 27, 435 Burnett, M. N. & Johnson, C. K. (1996). ORTEP-III. Report ORNL-6895, Oak Ridge National Laboratory, Tennessee, USA. Higashi, T. (1995). Program for Abosrption Correction, Rigaku Corporation, Tokyo, Japan. Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. PROCESS-AUTO(1998). Automatic Data Acquisition and Processing Package for Imaging Plate Diffractometer. Rigaku Corporation, Tokyo, Japan. ; data_1 _database_code_CSD 176980 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Mar 22 21:02:01 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ORTEP-III #------------------------------------------------------------------------------ _chemical_compound_source 'synthesized by the authors, see text' _chemical_name_common ? _chemical_formula_weight 809.82 _chemical_formula_analytical ? _chemical_formula_sum 'C24 H32 N Ni O6 S10 ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 14.217(1) _cell_length_b 16.666(2) _cell_length_c 8.1271(6) _cell_angle_alpha 97.120(2) _cell_angle_beta 92.599(3) _cell_angle_gamma 112.846(2) _cell_volume 1751.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 9986 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'block' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_meas 'not measured' _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'Rigaku' _diffrn_measurement_method \w-scan _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 14477 _reflns_number_observed 5677 _reflns_number_total 7594 _reflns_observed_criterion F^2^>3.0\s(F^2^) _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni(1) Ni 0.59516(2) 0.95347(2) 0.10993(4) 0.04312(10) Uani 1.00 d . . . S(1) S 0.49447(5) 0.81793(5) 0.11518(10) 0.0544(2) Uani 1.00 d . . . S(2) S 0.50170(6) 0.64761(5) -0.0497(1) 0.0582(2) Uani 1.00 d . . . S(3) S 0.58768(7) 0.54305(6) -0.2696(1) 0.0814(3) Uani 1.00 d . . . S(4) S 0.67666(7) 0.73895(5) -0.2183(1) 0.0643(2) Uani 1.00 d . . . S(5) S 0.68702(6) 0.91814(5) -0.06733(9) 0.0549(2) Uani 1.00 d . . . S(6) S 0.70034(6) 1.08867(5) 0.1201(1) 0.0580(2) Uani 1.00 d . . . S(7) S 0.69569(7) 1.25852(5) 0.2966(1) 0.0688(2) Uani 1.00 d . . . S(8) S 0.6065(1) 1.36028(6) 0.5181(1) 0.0888(3) Uani 1.00 d . . . S(9) S 0.50995(7) 1.16550(5) 0.43909(10) 0.0600(2) Uani 1.00 d . . . S(10) S 0.49947(6) 0.98849(5) 0.2767(1) 0.0566(2) Uani 1.00 d . . . O(1) O 1.1370(2) 0.8857(2) 0.2840(3) 0.0862(8) Uani 1.00 d . . . O(2) O 0.9453(2) 0.8928(2) 0.3137(3) 0.0827(8) Uani 1.00 d . . . O(3) O 0.7645(2) 0.7339(2) 0.2433(3) 0.0682(7) Uani 1.00 d . . . O(4) O 0.7906(2) 0.5783(1) 0.2648(3) 0.0670(6) Uani 1.00 d . . . O(5) O 0.9730(2) 0.5633(2) 0.2005(3) 0.0860(9) Uani 1.00 d . . . O(6) O 1.1472(2) 0.7217(2) 0.2870(4) 0.097(1) Uani 1.00 d . . . N(1) N 0.9541(2) 0.7255(2) 1.1526(3) 0.0508(6) Uani 1.00 d . . . C(1) C 0.5481(2) 0.7615(2) -0.0148(3) 0.0459(7) Uani 1.00 d . . . C(2) C 0.5886(2) 0.6383(2) -0.1838(4) 0.0572(8) Uani 1.00 d . . . C(3) C 0.6311(2) 0.8056(2) -0.0921(3) 0.0480(7) Uani 1.00 d . . . C(4) C 0.6448(2) 1.1444(2) 0.2458(3) 0.0484(7) Uani 1.00 d . . . C(5) C 0.6044(3) 1.2664(2) 0.4213(4) 0.0622(9) Uani 1.00 d . . . C(6) C 0.5578(2) 1.1009(2) 0.3129(3) 0.0477(7) Uani 1.00 d . . . C(7) C 1.1236(4) 0.9616(3) 0.3576(6) 0.116(2) Uani 1.00 d . . . C(8) C 1.0321(5) 0.9642(3) 0.2733(6) 0.107(2) Uani 1.00 d . . . C(9) C 0.8511(4) 0.8871(3) 0.2390(5) 0.096(2) Uani 1.00 d . . . C(10) C 0.7659(3) 0.8173(3) 0.3081(5) 0.084(1) Uani 1.00 d . . . C(11) C 0.6953(2) 0.6652(3) 0.3205(4) 0.076(1) Uani 1.00 d . . . C(12) C 0.6912(2) 0.5788(3) 0.2412(4) 0.078(1) Uani 1.00 d . . . C(13) C 0.7922(4) 0.4960(2) 0.2007(5) 0.088(1) Uani 1.00 d . . . C(14) C 0.8924(4) 0.4957(3) 0.2604(5) 0.100(2) Uani 1.00 d . . . C(15) C 1.0719(5) 0.5673(4) 0.2568(7) 0.119(2) Uani 1.00 d . . . C(16) C 1.1516(4) 0.6441(5) 0.2042(7) 0.126(2) Uani 1.00 d . . . C(17) C 1.2357(3) 0.8001(5) 0.2703(7) 0.119(2) Uani 1.00 d . . . C(18) C 1.2224(3) 0.8768(5) 0.3595(6) 0.125(2) Uani 1.00 d . . . C(19) C 0.9519(2) 0.7173(2) 0.9710(3) 0.0490(7) Uani 1.00 d . . . C(20) C 1.0320(3) 0.7717(3) 0.9022(4) 0.090(1) Uani 1.00 d . . . C(21) C 1.0299(3) 0.7610(4) 0.7295(5) 0.124(2) Uani 1.00 d . . . C(22) C 0.9494(3) 0.6975(3) 0.6316(4) 0.097(1) Uani 1.00 d . . . C(23) C 0.8684(3) 0.6432(3) 0.7017(4) 0.071(1) Uani 1.00 d . . . C(24) C 0.8701(2) 0.6524(2) 0.8731(4) 0.0594(9) Uani 1.00 d . . . H(1) H 1.1153 0.9589 0.4733 0.1221 Uiso 1.00 calc . . . H(2) H 1.1839 1.0131 0.3497 0.1221 Uiso 1.00 calc . . . H(3) H 1.0415 0.9604 0.1576 0.1312 Uiso 1.00 calc . . . H(4) H 1.0320 1.0204 0.3123 0.1312 Uiso 1.00 calc . . . H(5) H 0.8441 0.9426 0.2549 0.1114 Uiso 1.00 calc . . . H(6) H 0.8443 0.8699 0.1161 0.1114 Uiso 1.00 calc . . . H(7) H 0.7006 0.8193 0.2846 0.1091 Uiso 1.00 calc . . . H(8) H 0.7804 0.8276 0.4293 0.1091 Uiso 1.00 calc . . . H(9) H 0.7170 0.6761 0.4382 0.0925 Uiso 1.00 calc . . . H(10) H 0.6281 0.6676 0.3102 0.0925 Uiso 1.00 calc . . . H(11) H 0.6686 0.5682 0.1257 0.0939 Uiso 1.00 calc . . . H(12) H 0.6431 0.5317 0.2921 0.0939 Uiso 1.00 calc . . . H(13) H 0.7355 0.4490 0.2402 0.1058 Uiso 1.00 calc . . . H(14) H 0.7817 0.4856 0.0824 0.1058 Uiso 1.00 calc . . . H(15) H 0.8939 0.4399 0.2241 0.1218 Uiso 1.00 calc . . . H(16) H 0.8996 0.5057 0.3809 0.1218 Uiso 1.00 calc . . . H(17) H 1.0796 0.5719 0.3761 0.1443 Uiso 1.00 calc . . . H(18) H 1.0790 0.5141 0.2107 0.1443 Uiso 1.00 calc . . . H(19) H 1.1424 0.6432 0.0856 0.1483 Uiso 1.00 calc . . . H(20) H 1.2198 0.6460 0.2291 0.1483 Uiso 1.00 calc . . . H(21) H 1.2966 0.7938 0.3102 0.1331 Uiso 1.00 calc . . . H(22) H 1.2398 0.8030 0.1507 0.1331 Uiso 1.00 calc . . . H(23) H 1.2836 0.9296 0.3550 0.1437 Uiso 1.00 calc . . . H(24) H 1.2150 0.8705 0.4726 0.1437 Uiso 1.00 calc . . . H(25) H 1.0127 0.7172 1.1978 0.0607 Uiso 1.00 calc . . . H(26) H 0.9602 0.7832 1.1975 0.0607 Uiso 1.00 calc . . . H(27) H 0.8939 0.6831 1.1834 0.0607 Uiso 1.00 calc . . . H(28) H 1.0893 0.8173 0.9711 0.1063 Uiso 1.00 calc . . . H(29) H 1.0875 0.8007 0.6808 0.1529 Uiso 1.00 calc . . . H(30) H 0.9493 0.6906 0.5120 0.1171 Uiso 1.00 calc . . . H(31) H 0.8092 0.5972 0.6322 0.0838 Uiso 1.00 calc . . . H(32) H 0.8142 0.6133 0.9243 0.0724 Uiso 1.00 calc . . . 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(1) 0.0477(2) 0.0373(2) 0.0436(2) 0.0170(1) 0.0062(1) 0.0025(1) S(1) 0.0529(4) 0.0416(4) 0.0636(4) 0.0146(3) 0.0186(3) -0.0011(3) S(2) 0.0566(4) 0.0399(4) 0.0706(5) 0.0147(3) 0.0082(4) -0.0044(3) S(3) 0.0732(5) 0.0507(5) 0.1114(8) 0.0254(4) 0.0102(5) -0.0232(5) S(4) 0.0766(5) 0.0536(4) 0.0651(5) 0.0288(4) 0.0264(4) -0.0003(3) S(5) 0.0658(4) 0.0441(4) 0.0569(4) 0.0217(3) 0.0222(4) 0.0100(3) S(6) 0.0625(4) 0.0415(4) 0.0661(5) 0.0149(3) 0.0223(4) 0.0074(3) S(7) 0.0885(6) 0.0355(4) 0.0761(5) 0.0178(4) 0.0148(5) 0.0058(3) S(8) 0.1379(9) 0.0516(5) 0.0844(7) 0.0509(6) 0.0071(6) -0.0055(4) S(9) 0.0750(5) 0.0523(4) 0.0588(4) 0.0339(4) 0.0111(4) 0.0002(3) S(10) 0.0563(4) 0.0405(4) 0.0689(5) 0.0154(3) 0.0202(4) 0.0007(3) O(1) 0.061(1) 0.107(2) 0.059(1) 0.002(1) 0.000(1) 0.006(1) O(2) 0.090(2) 0.064(2) 0.082(2) 0.018(1) 0.001(1) 0.011(1) O(3) 0.060(1) 0.081(2) 0.061(1) 0.030(1) 0.007(1) -0.006(1) O(4) 0.067(1) 0.056(1) 0.063(1) 0.010(1) 0.007(1) 0.0073(10) O(5) 0.118(2) 0.095(2) 0.072(2) 0.069(2) 0.009(1) 0.023(1) O(6) 0.062(1) 0.160(3) 0.081(2) 0.048(2) 0.018(1) 0.040(2) N(1) 0.047(1) 0.061(1) 0.042(1) 0.018(1) 0.0068(10) 0.0088(10) C(1) 0.050(1) 0.039(1) 0.046(1) 0.017(1) 0.003(1) 0.000(1) C(2) 0.060(2) 0.048(2) 0.062(2) 0.024(1) 0.002(1) -0.009(1) C(3) 0.058(2) 0.046(1) 0.044(1) 0.025(1) 0.007(1) 0.002(1) C(4) 0.060(2) 0.034(1) 0.048(1) 0.016(1) 0.004(1) 0.006(1) C(5) 0.095(2) 0.047(2) 0.051(2) 0.038(2) -0.004(2) 0.001(1) C(6) 0.059(2) 0.043(1) 0.045(1) 0.025(1) 0.003(1) 0.003(1) C(7) 0.098(3) 0.093(3) 0.090(3) -0.026(3) 0.031(3) -0.018(2) C(8) 0.146(4) 0.059(2) 0.099(3) 0.020(3) 0.038(3) 0.014(2) C(9) 0.143(4) 0.077(3) 0.080(3) 0.064(3) -0.017(3) -0.007(2) C(10) 0.084(2) 0.103(3) 0.079(2) 0.060(2) -0.005(2) -0.011(2) C(11) 0.052(2) 0.109(3) 0.056(2) 0.022(2) 0.015(2) 0.003(2) C(12) 0.055(2) 0.087(3) 0.065(2) 0.001(2) 0.008(2) 0.003(2) C(13) 0.119(3) 0.050(2) 0.078(2) 0.015(2) 0.008(2) 0.010(2) C(14) 0.162(4) 0.068(2) 0.083(3) 0.059(3) -0.001(3) 0.020(2) C(15) 0.140(4) 0.142(5) 0.126(4) 0.107(4) 0.006(4) 0.034(4) C(16) 0.109(4) 0.201(7) 0.118(4) 0.110(5) 0.024(3) 0.042(4) C(17) 0.051(2) 0.220(7) 0.096(3) 0.046(3) 0.023(2) 0.086(4) C(18) 0.046(2) 0.197(6) 0.083(3) -0.011(3) -0.008(2) 0.042(3) C(19) 0.045(1) 0.062(2) 0.040(1) 0.021(1) 0.004(1) 0.011(1) C(20) 0.064(2) 0.118(3) 0.046(2) -0.010(2) 0.004(2) 0.017(2) C(21) 0.083(3) 0.177(5) 0.051(2) -0.018(3) 0.012(2) 0.031(3) C(22) 0.086(3) 0.144(4) 0.040(2) 0.025(3) 0.005(2) 0.011(2) C(23) 0.067(2) 0.090(2) 0.050(2) 0.028(2) -0.005(2) 0.000(2) C(24) 0.055(2) 0.068(2) 0.050(2) 0.019(1) 0.005(1) 0.010(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5677 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs ? _refine_ls_wR_factor_ref 0.1183 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs ? _refine_ls_goodness_of_fit_ref 1.693 _refine_ls_shift/su_max 0.0012 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.43 _refine_diff_density_max 0.28 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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(1) S(1) 2.1615(7) . . yes Ni(1) S(5) 2.1644(7) . . yes Ni(1) S(6) 2.1554(8) . . yes Ni(1) S(10) 2.1486(7) . . yes S(1) C(1) 1.722(3) . . yes S(2) C(1) 1.730(3) . . yes S(2) C(2) 1.723(3) . . yes S(3) C(2) 1.648(3) . . yes S(4) C(2) 1.725(3) . . yes S(4) C(3) 1.744(3) . . yes S(5) C(3) 1.709(3) . . yes S(6) C(4) 1.713(3) . . yes S(7) C(4) 1.739(3) . . yes S(7) C(5) 1.717(3) . . yes S(8) C(5) 1.650(3) . . yes S(9) C(5) 1.726(3) . . yes S(9) C(6) 1.741(3) . . yes S(10) C(6) 1.708(3) . . yes O(1) C(7) 1.416(6) . . yes O(1) C(18) 1.402(6) . . yes O(2) C(8) 1.428(5) . . yes O(2) C(9) 1.409(5) . . yes O(3) C(10) 1.417(4) . . yes O(3) C(11) 1.425(4) . . yes O(4) C(12) 1.420(4) . . yes O(4) C(13) 1.415(4) . . yes O(5) C(14) 1.416(5) . . yes O(5) C(15) 1.433(5) . . yes O(6) C(16) 1.407(7) . . yes O(6) C(17) 1.446(6) . . yes N(1) C(19) 1.463(3) . . yes C(1) C(3) 1.356(4) . . yes C(4) C(6) 1.348(4) . . yes C(7) C(8) 1.462(7) . . yes C(9) C(10) 1.505(6) . . yes C(11) C(12) 1.482(5) . . yes C(13) C(14) 1.486(6) . . yes C(15) C(16) 1.470(8) . . yes C(17) C(18) 1.470(8) . . yes C(19) C(20) 1.347(4) . . yes C(19) C(24) 1.372(4) . . yes C(20) C(21) 1.391(5) . . yes C(21) C(22) 1.353(6) . . yes C(22) C(23) 1.360(5) . . yes C(23) C(24) 1.380(4) . . yes #------------------------------------------------------------------------------ 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 S(3) S(8) 3.420(1) . 1_544 ? S(5) C(9) 3.555(4) . . ? S(9) C(3) 3.574(3) . 2_675 ? O(1) N(1) 2.946(3) . 1_554 ? O(1) C(20) 3.373(4) . 1_554 ? O(2) N(1) 2.982(3) . 1_554 ? O(3) N(1) 2.877(3) . 1_554 ? O(4) N(1) 2.927(3) . 1_554 ? O(4) C(22) 3.518(4) . . ? O(4) C(23) 3.573(4) . . ? O(5) N(1) 2.888(3) . 1_554 ? O(5) C(19) 3.447(4) . 1_554 ? O(6) N(1) 2.934(3) . 1_554 ? N(1) C(9) 3.547(5) . 1_556 ? N(1) C(16) 3.590(5) . 1_556 ? #------------------------------------------------------------------------------ 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 S(1) Ni(1) S(5) 93.42(3) . 1_555 1_555 yes S(1) Ni(1) S(6) 176.29(3) . 1_555 1_555 yes S(1) Ni(1) S(10) 86.48(3) . 1_555 1_555 yes S(5) Ni(1) S(6) 87.45(3) . 1_555 1_555 yes S(5) Ni(1) S(10) 177.45(3) . 1_555 1_555 yes S(6) Ni(1) S(10) 92.81(3) . 1_555 1_555 yes Ni(1) S(1) C(1) 102.01(9) . 1_555 1_555 yes C(1) S(2) C(2) 97.3(1) . 1_555 1_555 yes C(2) S(4) C(3) 97.8(1) . 1_555 1_555 yes Ni(1) S(5) C(3) 101.47(9) . 1_555 1_555 yes Ni(1) S(6) C(4) 102.30(9) . 1_555 1_555 yes C(4) S(7) C(5) 97.7(1) . 1_555 1_555 yes C(5) S(9) C(6) 97.1(1) . 1_555 1_555 yes Ni(1) S(10) C(6) 102.54(10) . 1_555 1_555 yes C(7) O(1) C(18) 112.9(4) . 1_555 1_555 yes C(8) O(2) C(9) 113.5(4) . 1_555 1_555 yes C(10) O(3) C(11) 111.8(3) . 1_555 1_555 yes C(12) O(4) C(13) 112.3(3) . 1_555 1_555 yes C(14) O(5) C(15) 112.2(3) . 1_555 1_555 yes C(16) O(6) C(17) 113.0(4) . 1_555 1_555 yes S(1) C(1) S(2) 122.5(2) . 1_555 1_555 yes S(1) C(1) C(3) 120.5(2) . 1_555 1_555 yes S(2) C(1) C(3) 117.0(2) . 1_555 1_555 yes S(2) C(2) S(3) 123.3(2) . 1_555 1_555 yes S(2) C(2) S(4) 113.0(1) . 1_555 1_555 yes S(3) C(2) S(4) 123.6(2) . 1_555 1_555 yes S(4) C(3) S(5) 122.6(2) . 1_555 1_555 yes S(4) C(3) C(1) 114.9(2) . 1_555 1_555 yes S(5) C(3) C(1) 122.5(2) . 1_555 1_555 yes S(6) C(4) S(7) 123.2(2) . 1_555 1_555 yes S(6) C(4) C(6) 121.0(2) . 1_555 1_555 yes S(7) C(4) C(6) 115.7(2) . 1_555 1_555 yes S(7) C(5) S(8) 124.1(2) . 1_555 1_555 yes S(7) C(5) S(9) 113.2(2) . 1_555 1_555 yes S(8) C(5) S(9) 122.7(2) . 1_555 1_555 yes S(9) C(6) S(10) 122.5(2) . 1_555 1_555 yes S(9) C(6) C(4) 116.3(2) . 1_555 1_555 yes S(10) C(6) C(4) 121.2(2) . 1_555 1_555 yes O(1) C(7) C(8) 108.8(4) . 1_555 1_555 yes O(2) C(8) C(7) 107.5(4) . 1_555 1_555 yes O(2) C(9) C(10) 108.2(3) . 1_555 1_555 yes O(3) C(10) C(9) 108.4(3) . 1_555 1_555 yes O(3) C(11) C(12) 109.8(3) . 1_555 1_555 yes O(4) C(12) C(11) 108.6(3) . 1_555 1_555 yes O(4) C(13) C(14) 108.3(3) . 1_555 1_555 yes O(5) C(14) C(13) 109.6(3) . 1_555 1_555 yes O(5) C(15) C(16) 109.1(4) . 1_555 1_555 yes O(6) C(16) C(15) 109.4(4) . 1_555 1_555 yes O(6) C(17) C(18) 108.3(4) . 1_555 1_555 yes O(1) C(18) C(17) 110.0(4) . 1_555 1_555 yes N(1) C(19) C(20) 119.4(3) . 1_555 1_555 yes N(1) C(19) C(24) 119.7(2) . 1_555 1_555 yes C(20) C(19) C(24) 120.8(3) . 1_555 1_555 yes C(19) C(20) C(21) 118.6(3) . 1_555 1_555 yes C(20) C(21) C(22) 121.1(3) . 1_555 1_555 yes C(21) C(22) C(23) 120.1(3) . 1_555 1_555 yes C(22) C(23) C(24) 119.4(3) . 1_555 1_555 yes C(19) C(24) C(23) 120.0(3) . 1_555 1_555 yes #==END data_2 _database_code_CSD 176981 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Dec 20 18:30:06 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ORTEP-III #------------------------------------------------------------------------------ _chemical_compound_source 'synthesized by the authors, see text' _chemical_name_common ? _chemical_formula_weight 1623.63 _chemical_formula_analytical ? _chemical_formula_sum 'C46 H64 N4 Ni2 O12 S20' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 13.1321(4) _cell_length_b 16.3032(5) _cell_length_c 17.6903(5) _cell_angle_alpha 73.5786(9) _cell_angle_beta 76.2712(8) _cell_angle_gamma 82.426(1) _cell_volume 3520.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 26974 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'needle' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_meas 'not measured' _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type multi-scan _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device_type 'Rigaku' _diffrn_measurement_method \w-scan _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 55511 _reflns_number_observed 8095 _reflns_number_total 16043 _reflns_observed_criterion F^2^>3.0\s(F^2^) _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ni' 'Ni' 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni(1) Ni 0.09250(4) -0.41156(3) -0.08839(3) 0.0420(1) Uani 1.00 d . . . Ni(2) Ni 0.88698(3) -0.07761(3) -0.41387(3) 0.0418(1) Uani 1.00 d . . . S(1) S 0.17429(9) -0.48348(7) 0.00421(6) 0.0611(3) Uani 1.00 d . . . S(2) S 0.15247(9) -0.47564(8) 0.17666(7) 0.0655(3) Uani 1.00 d . . . S(3) S 0.0623(1) -0.40573(10) 0.31731(7) 0.0782(4) Uani 1.00 d . . . S(4) S -0.01388(9) -0.34215(8) 0.16333(7) 0.0628(3) Uani 1.00 d . . . S(5) S -0.00460(8) -0.33705(7) -0.01108(6) 0.0543(3) Uani 1.00 d . . . S(6) S 0.00842(8) -0.34138(7) -0.18097(6) 0.0560(3) Uani 1.00 d . . . S(7) S 0.02811(8) -0.35494(7) -0.35177(6) 0.0548(3) Uani 1.00 d . . . S(8) S 0.12250(9) -0.42677(9) -0.49166(7) 0.0701(4) Uani 1.00 d . . . S(9) S 0.19585(8) -0.48703(7) -0.33696(6) 0.0572(3) Uani 1.00 d . . . S(10) S 0.19120(8) -0.48638(7) -0.16491(6) 0.0546(3) Uani 1.00 d . . . S(11) S 0.98892(8) -0.13701(7) -0.33107(6) 0.0568(3) Uani 1.00 d . . . S(12) S 0.97130(8) -0.13715(7) -0.15648(6) 0.0551(3) Uani 1.00 d . . . S(13) S 0.86818(9) -0.08836(8) -0.00538(7) 0.0675(4) Uani 1.00 d . . . S(14) S 0.77547(8) -0.03487(8) -0.15178(6) 0.0595(3) Uani 1.00 d . . . S(15) S 0.77478(8) -0.02489(7) -0.32527(6) 0.0561(3) Uani 1.00 d . . . S(16) S 0.78756(8) -0.01520(7) -0.49802(6) 0.0548(3) Uani 1.00 d . . . S(17) S 0.80521(9) -0.01606(8) -0.67195(6) 0.0635(3) Uani 1.00 d . . . S(18) S 0.9056(1) -0.07060(9) -0.82089(7) 0.0812(4) Uani 1.00 d . . . S(19) S 0.99891(8) -0.12224(8) -0.67522(7) 0.0607(3) Uani 1.00 d . . . S(20) S 0.99634(7) -0.13338(7) -0.50105(6) 0.0550(3) Uani 1.00 d . . . O(1) O 0.5219(4) -0.2179(2) -0.6475(2) 0.095(1) Uani 1.00 d . . . O(2) O 0.3548(3) -0.2082(2) -0.5197(3) 0.089(1) Uani 1.00 d . . . O(3) O 0.3601(2) -0.2985(2) -0.3636(3) 0.085(1) Uani 1.00 d . . . O(4) O 0.5557(3) -0.3532(2) -0.3242(2) 0.083(1) Uani 1.00 d . . . O(5) O 0.7317(2) -0.3535(2) -0.4453(2) 0.0666(10) Uani 1.00 d . . . O(6) O 0.7193(3) -0.2577(2) -0.5998(2) 0.082(1) Uani 1.00 d . . . O(7) O 0.4520(2) -0.1773(2) -0.1576(2) 0.0719(10) Uani 1.00 d . . . O(8) O 0.2657(2) -0.1450(2) -0.0536(2) 0.0624(9) Uani 1.00 d . . . O(9) O 0.2489(2) -0.2210(2) 0.1096(2) 0.075(1) Uani 1.00 d . . . O(10) O 0.4281(3) -0.2733(2) 0.1782(2) 0.078(1) Uani 1.00 d . . . O(11) O 0.6112(2) -0.3032(2) 0.0681(2) 0.076(1) Uani 1.00 d . . . O(12) O 0.6346(2) -0.2297(2) -0.0957(2) 0.0665(10) Uani 1.00 d . . . N(1) N 0.4686(2) -0.6653(2) -0.5096(2) 0.0441(8) Uani 1.00 d . . . N(2) N 0.5445(2) -0.8319(2) -0.0076(2) 0.0431(8) Uani 1.00 d . . . N(3) N 0.5750(5) -0.4949(4) -0.1012(3) 0.136(2) Uani 1.00 d . . . N(4) N 0.4705(5) -0.0290(4) -0.3880(3) 0.116(2) Uani 1.00 d . . . C(1) C 0.1159(3) -0.4415(2) 0.0841(2) 0.048(1) Uani 1.00 d . . . C(2) C 0.0667(3) -0.4079(3) 0.2240(2) 0.057(1) Uani 1.00 d . . . C(3) C 0.0371(3) -0.3784(2) 0.0771(2) 0.046(1) Uani 1.00 d . . . C(4) C 0.0658(3) -0.3856(2) -0.2594(2) 0.045(1) Uani 1.00 d . . . C(5) C 0.1151(3) -0.4234(3) -0.3988(2) 0.052(1) Uani 1.00 d . . . C(6) C 0.1454(3) -0.4484(2) -0.2524(2) 0.044(1) Uani 1.00 d . . . C(7) C 0.9244(3) -0.1081(2) -0.2452(2) 0.0423(10) Uani 1.00 d . . . C(8) C 0.8720(3) -0.0865(2) -0.0998(2) 0.049(1) Uani 1.00 d . . . C(9) C 0.8311(3) -0.0592(2) -0.2426(2) 0.044(1) Uani 1.00 d . . . C(10) C 0.8517(3) -0.0456(2) -0.5830(2) 0.046(1) Uani 1.00 d . . . C(11) C 0.9039(3) -0.0696(3) -0.7277(2) 0.057(1) Uani 1.00 d . . . C(12) C 0.9430(3) -0.0967(2) -0.5842(2) 0.045(1) Uani 1.00 d . . . C(13) C 0.4298(7) -0.1596(4) -0.6562(4) 0.115(3) Uani 1.00 d . . . C(14) C 0.3379(6) -0.1979(4) -0.5959(6) 0.126(3) Uani 1.00 d . . . C(15) C 0.2609(4) -0.2253(4) -0.4586(5) 0.114(3) Uani 1.00 d . . . C(16) C 0.2843(4) -0.2311(4) -0.3812(5) 0.108(2) Uani 1.00 d . . . C(17) C 0.3792(5) -0.3142(4) -0.2844(4) 0.104(2) Uani 1.00 d . . . C(18) C 0.4602(5) -0.3832(4) -0.2722(3) 0.102(2) Uani 1.00 d . . . C(19) C 0.6440(5) -0.4109(4) -0.3123(3) 0.103(2) Uani 1.00 d . . . C(20) C 0.7389(4) -0.3699(4) -0.3641(4) 0.100(2) Uani 1.00 d . . . C(21) C 0.8203(3) -0.3148(3) -0.4999(4) 0.093(2) Uani 1.00 d . . . C(22) C 0.8112(4) -0.3080(4) -0.5828(4) 0.097(2) Uani 1.00 d . . . C(23) C 0.7079(6) -0.2432(5) -0.6808(4) 0.112(3) Uani 1.00 d . . . C(24) C 0.6150(8) -0.1817(4) -0.6947(3) 0.118(3) Uani 1.00 d . . . C(25) C 0.3706(4) -0.1185(3) -0.1848(3) 0.081(2) Uani 1.00 d . . . C(26) C 0.2685(4) -0.1474(3) -0.1336(3) 0.078(2) Uani 1.00 d . . . C(27) C 0.1673(3) -0.1664(3) -0.0016(4) 0.082(2) Uani 1.00 d . . . C(28) C 0.1695(3) -0.1604(4) 0.0791(4) 0.087(2) Uani 1.00 d . . . C(29) C 0.2462(4) -0.2274(4) 0.1905(3) 0.089(2) Uani 1.00 d . . . C(30) C 0.3236(5) -0.2969(4) 0.2188(3) 0.091(2) Uani 1.00 d . . . C(31) C 0.5072(6) -0.3377(4) 0.1994(3) 0.095(2) Uani 1.00 d . . . C(32) C 0.6108(5) -0.3115(4) 0.1501(4) 0.094(2) Uani 1.00 d . . . C(33) C 0.7103(4) -0.2938(3) 0.0182(4) 0.081(2) Uani 1.00 d . . . C(34) C 0.7062(3) -0.2965(3) -0.0644(4) 0.078(2) Uani 1.00 d . . . C(35) C 0.6315(4) -0.2258(4) -0.1751(3) 0.084(2) Uani 1.00 d . . . C(36) C 0.5549(4) -0.1570(4) -0.2045(3) 0.086(2) Uani 1.00 d . . . C(37) C 0.4040(3) -0.5173(2) -0.5087(2) 0.050(1) Uani 1.00 d . . . C(38) C 0.4847(3) -0.5800(2) -0.5044(2) 0.0395(10) Uani 1.00 d . . . C(39) C 0.5807(3) -0.5636(2) -0.4958(3) 0.050(1) Uani 1.00 d . . . C(40) C 0.5890(3) -0.9868(2) 0.0221(3) 0.053(1) Uani 1.00 d . . . C(41) C 0.5216(2) -0.9187(2) -0.0043(2) 0.0373(9) Uani 1.00 d . . . C(42) C 0.4333(3) -0.9306(2) -0.0263(3) 0.052(1) Uani 1.00 d . . . C(43) C 0.5873(5) -0.5563(4) -0.0527(4) 0.091(2) Uani 1.00 d . . . C(44) C 0.6011(5) -0.6329(3) 0.0076(4) 0.109(2) Uani 1.00 d . . . C(45) C 0.5130(5) -0.0786(4) -0.4220(3) 0.083(2) Uani 1.00 d . . . C(46) C 0.5661(5) -0.1416(3) -0.4648(4) 0.096(2) Uani 1.00 d . . . H(1) H 0.3085 -0.3486 0.2072 0.1109 Uiso 1.00 calc . . . H(2) H 0.3157 -0.3107 0.2768 0.1109 Uiso 1.00 calc . . . H(3) H 0.2655 -0.1745 0.1979 0.1100 Uiso 1.00 calc . . . H(4) H 0.1770 -0.2375 0.2244 0.1100 Uiso 1.00 calc . . . H(5) H 0.1113 -0.1279 -0.0225 0.0988 Uiso 1.00 calc . . . H(6) H 0.1518 -0.2235 0.0011 0.0988 Uiso 1.00 calc . . . H(7) H 0.1016 -0.1711 0.1145 0.1090 Uiso 1.00 calc . . . H(8) H 0.1838 -0.1029 0.0756 0.1090 Uiso 1.00 calc . . . H(9) H 0.3799 -0.0622 -0.1804 0.0964 Uiso 1.00 calc . . . H(10) H 0.3728 -0.1130 -0.2409 0.0964 Uiso 1.00 calc . . . H(11) H 0.2629 -0.2057 -0.1357 0.0915 Uiso 1.00 calc . . . H(12) H 0.2119 -0.1128 -0.1541 0.0915 Uiso 1.00 calc . . . H(13) H 0.7367 -0.2398 0.0152 0.0974 Uiso 1.00 calc . . . H(14) H 0.7611 -0.3383 0.0399 0.0974 Uiso 1.00 calc . . . H(15) H 0.6830 -0.3518 -0.0607 0.0946 Uiso 1.00 calc . . . H(16) H 0.7746 -0.2920 -0.0989 0.0946 Uiso 1.00 calc . . . H(17) H 0.7001 -0.2192 -0.2109 0.1019 Uiso 1.00 calc . . . H(18) H 0.6095 -0.2804 -0.1786 0.1019 Uiso 1.00 calc . . . H(19) H 0.5572 -0.1466 -0.2619 0.1113 Uiso 1.00 calc . . . H(20) H 0.5724 -0.1029 -0.1984 0.1113 Uiso 1.00 calc . . . H(21) H 0.5043 -0.3499 0.2580 0.1103 Uiso 1.00 calc . . . H(22) H 0.4911 -0.3921 0.1929 0.1103 Uiso 1.00 calc . . . H(23) H 0.6654 -0.3524 0.1686 0.1149 Uiso 1.00 calc . . . H(24) H 0.6221 -0.2575 0.1582 0.1149 Uiso 1.00 calc . . . H(25) H 0.4058 -0.2648 -0.2745 0.1245 Uiso 1.00 calc . . . H(26) H 0.3177 -0.3283 -0.2405 0.1245 Uiso 1.00 calc . . . H(27) H 0.4406 -0.4331 -0.2850 0.1293 Uiso 1.00 calc . . . H(28) H 0.4687 -0.4052 -0.2160 0.1293 Uiso 1.00 calc . . . H(29) H 0.4413 -0.1045 -0.6506 0.1387 Uiso 1.00 calc . . . H(30) H 0.4186 -0.1487 -0.7113 0.1387 Uiso 1.00 calc . . . H(31) H 0.3248 -0.2510 -0.6028 0.1433 Uiso 1.00 calc . . . H(32) H 0.2737 -0.1598 -0.6018 0.1433 Uiso 1.00 calc . . . H(33) H 0.2046 -0.1822 -0.4687 0.1260 Uiso 1.00 calc . . . H(34) H 0.2345 -0.2797 -0.4557 0.1260 Uiso 1.00 calc . . . H(35) H 0.2205 -0.2408 -0.3377 0.1267 Uiso 1.00 calc . . . H(36) H 0.3080 -0.1780 -0.3812 0.1267 Uiso 1.00 calc . . . H(37) H 0.8253 -0.2584 -0.4945 0.1087 Uiso 1.00 calc . . . H(38) H 0.8840 -0.3481 -0.4894 0.1087 Uiso 1.00 calc . . . H(39) H 0.8102 -0.3638 -0.5889 0.1138 Uiso 1.00 calc . . . H(40) H 0.8725 -0.2820 -0.6202 0.1138 Uiso 1.00 calc . . . H(41) H 0.7712 -0.2222 -0.7188 0.1272 Uiso 1.00 calc . . . H(42) H 0.6963 -0.2961 -0.6909 0.1272 Uiso 1.00 calc . . . H(43) H 0.6137 -0.1631 -0.7511 0.1378 Uiso 1.00 calc . . . H(44) H 0.6250 -0.1297 -0.6798 0.1378 Uiso 1.00 calc . . . H(45) H 0.6503 -0.4288 -0.2565 0.1254 Uiso 1.00 calc . . . H(46) H 0.6398 -0.4634 -0.3273 0.1254 Uiso 1.00 calc . . . H(47) H 0.8011 -0.4030 -0.3538 0.1193 Uiso 1.00 calc . . . H(48) H 0.7401 -0.3154 -0.3506 0.1193 Uiso 1.00 calc . . . H(49) H 0.5308 -0.7026 -0.5053 0.0529 Uiso 1.00 calc . . . H(50) H 0.4124 -0.6904 -0.4673 0.0529 Uiso 1.00 calc . . . H(51) H 0.4512 -0.6620 -0.5602 0.0529 Uiso 1.00 calc . . . H(52) H 0.6111 -0.8176 -0.0425 0.0518 Uiso 1.00 calc . . . H(53) H 0.4917 -0.7910 -0.0274 0.0518 Uiso 1.00 calc . . . H(54) H 0.5466 -0.8280 0.0449 0.0518 Uiso 1.00 calc . . . H(55) H 0.6248 -0.6205 0.0521 0.1299 Uiso 1.00 calc . . . H(56) H 0.5376 -0.6612 0.0320 0.1299 Uiso 1.00 calc . . . H(57) H 0.6538 -0.6735 -0.0113 0.1299 Uiso 1.00 calc . . . H(58) H 0.5717 -0.1972 -0.4284 0.1117 Uiso 1.00 calc . . . H(59) H 0.5288 -0.1458 -0.5040 0.1117 Uiso 1.00 calc . . . H(60) H 0.6360 -0.1263 -0.4929 0.1117 Uiso 1.00 calc . . . H(62) H 0.3369 -0.5300 -0.5151 0.0597 Uiso 1.00 calc . . . H(63) H 0.6365 -0.6081 -0.4926 0.0615 Uiso 1.00 calc . . . H(65) H 0.6512 -0.9769 0.0374 0.0637 Uiso 1.00 calc . . . H(68) H 0.3870 -0.8816 -0.0452 0.0623 Uiso 1.00 calc . . . 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(1) 0.0453(3) 0.0410(3) 0.0420(3) -0.0030(2) -0.0141(2) -0.0106(2) Ni(2) 0.0405(2) 0.0429(3) 0.0422(3) -0.0017(2) -0.0137(2) -0.0080(2) S(1) 0.0761(7) 0.0607(7) 0.0498(6) 0.0193(6) -0.0269(5) -0.0194(5) S(2) 0.0745(7) 0.0780(8) 0.0453(6) 0.0071(6) -0.0230(5) -0.0149(5) S(3) 0.0799(8) 0.115(1) 0.0447(6) -0.0140(8) -0.0109(6) -0.0282(7) S(4) 0.0591(6) 0.0805(8) 0.0508(6) 0.0018(6) -0.0082(5) -0.0264(6) S(5) 0.0518(5) 0.0631(7) 0.0496(6) 0.0096(5) -0.0176(4) -0.0178(5) S(6) 0.0602(6) 0.0619(6) 0.0503(6) 0.0185(5) -0.0218(5) -0.0233(5) S(7) 0.0546(5) 0.0667(7) 0.0494(6) 0.0107(5) -0.0234(4) -0.0215(5) S(8) 0.0687(7) 0.0990(9) 0.0543(7) 0.0080(7) -0.0236(5) -0.0362(6) S(9) 0.0623(6) 0.0626(7) 0.0525(6) 0.0137(5) -0.0182(5) -0.0272(5) S(10) 0.0626(6) 0.0531(6) 0.0496(6) 0.0150(5) -0.0224(5) -0.0154(5) S(11) 0.0531(5) 0.0704(7) 0.0486(6) 0.0196(5) -0.0207(4) -0.0207(5) S(12) 0.0576(6) 0.0618(6) 0.0536(6) 0.0142(5) -0.0278(5) -0.0224(5) S(13) 0.0702(7) 0.0901(9) 0.0548(7) 0.0064(7) -0.0264(5) -0.0334(6) S(14) 0.0569(6) 0.0725(7) 0.0552(6) 0.0165(6) -0.0207(5) -0.0287(5) S(15) 0.0507(5) 0.0666(7) 0.0493(6) 0.0159(5) -0.0200(4) -0.0138(5) S(16) 0.0516(5) 0.0665(7) 0.0472(6) 0.0131(5) -0.0189(4) -0.0172(5) S(17) 0.0679(7) 0.0767(8) 0.0475(6) 0.0130(6) -0.0250(5) -0.0165(5) S(18) 0.1030(10) 0.0969(10) 0.0485(7) 0.0011(8) -0.0196(6) -0.0270(7) S(19) 0.0575(6) 0.0721(7) 0.0532(6) 0.0008(6) -0.0071(5) -0.0237(5) S(20) 0.0457(5) 0.0676(7) 0.0529(6) 0.0098(5) -0.0183(4) -0.0174(5) O(1) 0.143(3) 0.058(2) 0.095(3) -0.018(2) -0.058(3) -0.006(2) O(2) 0.069(2) 0.064(2) 0.151(4) 0.009(2) -0.064(2) -0.026(2) O(3) 0.063(2) 0.062(2) 0.128(3) 0.000(2) 0.000(2) -0.041(2) O(4) 0.088(2) 0.086(2) 0.069(2) -0.012(2) -0.017(2) -0.007(2) O(5) 0.048(2) 0.068(2) 0.093(2) -0.008(1) -0.031(2) -0.021(2) O(6) 0.081(2) 0.085(2) 0.077(2) -0.016(2) 0.005(2) -0.030(2) O(7) 0.067(2) 0.080(2) 0.063(2) -0.003(2) -0.022(1) -0.004(2) O(8) 0.044(1) 0.067(2) 0.083(2) -0.006(1) -0.021(1) -0.024(2) O(9) 0.074(2) 0.081(2) 0.065(2) -0.007(2) 0.003(2) -0.024(2) O(10) 0.102(2) 0.062(2) 0.072(2) -0.003(2) -0.028(2) -0.012(2) O(11) 0.065(2) 0.076(2) 0.094(2) 0.013(2) -0.036(2) -0.024(2) O(12) 0.060(2) 0.062(2) 0.075(2) 0.011(2) -0.011(1) -0.022(2) N(1) 0.043(2) 0.030(2) 0.066(2) -0.001(1) -0.020(1) -0.016(1) N(2) 0.042(2) 0.035(2) 0.057(2) -0.002(1) -0.017(1) -0.014(1) N(3) 0.144(5) 0.168(6) 0.066(4) 0.010(5) -0.006(3) -0.007(4) N(4) 0.143(5) 0.126(5) 0.063(3) 0.006(4) 0.001(3) -0.025(3) C(1) 0.053(2) 0.047(2) 0.047(2) -0.006(2) -0.015(2) -0.011(2) C(2) 0.054(2) 0.073(3) 0.046(2) -0.015(2) -0.005(2) -0.019(2) C(3) 0.046(2) 0.051(2) 0.044(2) -0.011(2) -0.006(2) -0.015(2) C(4) 0.049(2) 0.051(2) 0.038(2) -0.002(2) -0.014(2) -0.015(2) C(5) 0.049(2) 0.058(3) 0.052(2) -0.005(2) -0.016(2) -0.018(2) C(6) 0.045(2) 0.044(2) 0.046(2) 0.000(2) -0.013(2) -0.014(2) C(7) 0.047(2) 0.042(2) 0.042(2) 0.002(2) -0.021(2) -0.011(2) C(8) 0.054(2) 0.054(2) 0.047(2) -0.002(2) -0.019(2) -0.018(2) C(9) 0.046(2) 0.044(2) 0.045(2) -0.001(2) -0.017(2) -0.012(2) C(10) 0.051(2) 0.049(2) 0.041(2) -0.003(2) -0.015(2) -0.009(2) C(11) 0.066(3) 0.056(3) 0.049(2) -0.008(2) -0.012(2) -0.012(2) C(12) 0.045(2) 0.047(2) 0.044(2) -0.003(2) -0.009(2) -0.011(2) C(13) 0.182(7) 0.062(4) 0.126(5) 0.014(4) -0.113(5) -0.005(3) C(14) 0.138(6) 0.056(3) 0.214(8) 0.003(4) -0.131(6) -0.007(4) C(15) 0.046(3) 0.071(4) 0.235(9) 0.014(3) -0.050(4) -0.046(5) C(16) 0.048(3) 0.086(4) 0.198(7) 0.002(3) -0.005(4) -0.069(5) C(17) 0.103(4) 0.118(5) 0.091(5) -0.037(4) 0.022(4) -0.049(4) C(18) 0.115(5) 0.101(5) 0.072(4) -0.026(4) 0.002(3) -0.002(3) C(19) 0.123(5) 0.098(4) 0.082(4) 0.014(4) -0.049(4) 0.000(3) C(20) 0.092(4) 0.112(5) 0.114(5) 0.011(4) -0.069(4) -0.026(4) C(21) 0.043(2) 0.082(4) 0.166(6) -0.011(3) -0.022(3) -0.048(4) C(22) 0.064(3) 0.088(4) 0.135(5) -0.023(3) 0.019(3) -0.046(4) C(23) 0.148(6) 0.108(5) 0.077(4) -0.053(5) 0.019(4) -0.038(4) C(24) 0.219(9) 0.083(4) 0.057(4) -0.031(6) -0.035(4) -0.011(3) C(25) 0.086(3) 0.088(4) 0.069(3) 0.003(3) -0.034(3) -0.008(3) C(26) 0.077(3) 0.087(4) 0.085(4) 0.010(3) -0.048(3) -0.028(3) C(27) 0.046(2) 0.094(4) 0.115(4) -0.010(3) -0.018(3) -0.038(3) C(28) 0.046(2) 0.087(4) 0.119(5) 0.004(3) 0.001(3) -0.032(3) C(29) 0.093(4) 0.088(4) 0.078(4) -0.014(3) 0.004(3) -0.023(3) C(30) 0.116(5) 0.090(4) 0.059(3) -0.034(4) 0.003(3) -0.011(3) C(31) 0.135(5) 0.081(4) 0.071(4) 0.007(4) -0.041(3) -0.012(3) C(32) 0.117(4) 0.088(4) 0.101(4) 0.039(4) -0.073(4) -0.042(3) C(33) 0.058(3) 0.064(3) 0.126(5) 0.015(2) -0.037(3) -0.026(3) C(34) 0.053(2) 0.067(3) 0.113(4) 0.021(2) -0.018(3) -0.030(3) C(35) 0.069(3) 0.091(4) 0.080(4) -0.003(3) 0.004(3) -0.022(3) C(36) 0.079(3) 0.112(4) 0.054(3) -0.023(3) -0.003(2) -0.002(3) C(37) 0.034(2) 0.041(2) 0.080(3) -0.002(2) -0.019(2) -0.022(2) C(38) 0.037(2) 0.030(2) 0.055(2) -0.002(2) -0.013(2) -0.016(2) C(39) 0.038(2) 0.034(2) 0.086(3) 0.008(2) -0.023(2) -0.024(2) C(40) 0.044(2) 0.044(2) 0.082(3) 0.001(2) -0.031(2) -0.022(2) C(41) 0.038(2) 0.033(2) 0.044(2) -0.001(2) -0.009(1) -0.014(2) C(42) 0.051(2) 0.035(2) 0.079(3) 0.007(2) -0.030(2) -0.017(2) C(43) 0.088(4) 0.108(5) 0.082(4) -0.012(4) -0.001(3) -0.043(4) C(44) 0.128(5) 0.055(3) 0.135(6) -0.018(4) -0.012(4) -0.017(3) C(45) 0.090(4) 0.084(4) 0.070(4) -0.022(3) -0.020(3) -0.001(3) C(46) 0.107(4) 0.064(3) 0.127(5) -0.016(3) -0.024(4) -0.040(3) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 8095 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs ? _refine_ls_wR_factor_ref 0.0943 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs ? _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_shift/su_max 0.0006 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.37 _refine_diff_density_max 0.31 #------------------------------------------------------------------------------ _geom_special_details ; ? ; 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(1) S(1) 2.151(1) . . yes Ni(1) S(5) 2.162(1) . . yes Ni(1) S(6) 2.162(1) . . yes Ni(1) S(10) 2.164(1) . . yes Ni(2) S(11) 2.159(1) . . yes Ni(2) S(15) 2.167(1) . . yes Ni(2) S(16) 2.161(1) . . yes Ni(2) S(20) 2.160(1) . . yes S(1) C(1) 1.718(4) . . yes S(2) C(1) 1.734(4) . . yes S(2) C(2) 1.713(4) . . yes S(3) C(2) 1.649(4) . . yes S(4) C(2) 1.735(4) . . yes S(4) C(3) 1.745(4) . . yes S(5) C(3) 1.702(4) . . yes S(6) C(4) 1.714(4) . . yes S(7) C(4) 1.739(4) . . yes S(7) C(5) 1.726(4) . . yes S(8) C(5) 1.639(4) . . yes S(9) C(5) 1.736(4) . . yes S(9) C(6) 1.739(4) . . yes S(10) C(6) 1.715(4) . . yes S(11) C(7) 1.713(4) . . yes S(12) C(7) 1.741(4) . . yes S(12) C(8) 1.717(4) . . yes S(13) C(8) 1.651(4) . . yes S(14) C(8) 1.731(4) . . yes S(14) C(9) 1.732(4) . . yes S(15) C(9) 1.715(4) . . yes S(16) C(10) 1.710(4) . . yes S(17) C(10) 1.742(4) . . yes S(17) C(11) 1.731(4) . . yes S(18) C(11) 1.648(4) . . yes S(19) C(11) 1.724(4) . . yes S(19) C(12) 1.744(4) . . yes S(20) C(12) 1.702(4) . . yes O(1) C(13) 1.447(7) . . yes O(1) C(24) 1.402(8) . . yes O(2) C(14) 1.377(8) . . yes O(2) C(15) 1.434(7) . . yes O(3) C(16) 1.401(7) . . yes O(3) C(17) 1.428(7) . . yes O(4) C(18) 1.419(6) . . yes O(4) C(19) 1.411(6) . . yes O(5) C(20) 1.410(6) . . yes O(5) C(21) 1.413(5) . . yes O(6) C(22) 1.411(7) . . yes O(6) C(23) 1.425(7) . . yes O(7) C(25) 1.416(6) . . yes O(7) C(36) 1.434(5) . . yes O(8) C(26) 1.419(5) . . yes O(8) C(27) 1.418(5) . . yes O(9) C(28) 1.431(6) . . yes O(9) C(29) 1.398(6) . . yes O(10) C(30) 1.436(6) . . yes O(10) C(31) 1.413(6) . . yes O(11) C(32) 1.418(6) . . yes O(11) C(33) 1.389(6) . . yes O(12) C(34) 1.419(5) . . yes O(12) C(35) 1.399(6) . . yes N(1) C(38) 1.465(4) . . yes N(2) C(41) 1.468(4) . . yes N(3) C(43) 1.141(8) . . yes N(4) C(45) 1.151(7) . . yes C(1) C(3) 1.362(5) . . yes C(4) C(6) 1.365(5) . . yes C(7) C(9) 1.370(5) . . yes C(10) C(12) 1.366(5) . . yes C(13) C(14) 1.481(9) . . yes C(15) C(16) 1.447(9) . . yes C(17) C(18) 1.450(9) . . yes C(19) C(20) 1.474(7) . . yes C(21) C(22) 1.472(8) . . yes C(23) C(24) 1.494(10) . . yes C(25) C(26) 1.479(6) . . yes C(27) C(28) 1.465(7) . . yes C(29) C(30) 1.480(8) . . yes C(31) C(32) 1.473(8) . . yes C(33) C(34) 1.487(7) . . yes C(35) C(36) 1.470(7) . . yes C(37) C(38) 1.373(5) . . yes C(37) C(39) 1.387(5) . 2_644 yes C(38) C(39) 1.373(4) . . yes C(40) C(41) 1.371(5) . . yes C(40) C(42) 1.393(5) . 2_635 yes C(41) C(42) 1.360(5) . . yes C(43) C(44) 1.418(8) . . yes C(45) C(46) 1.455(8) . . yes #------------------------------------------------------------------------------ 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 S(2) N(3) 3.531(6) . 2_645 ? S(3) S(8) 3.564(2) . 1_556 ? S(5) S(12) 3.566(2) . 1_455 ? S(6) S(12) 3.435(2) . 1_455 ? S(13) S(18) 3.509(2) . 1_556 ? S(17) N(4) 3.562(6) . 2_654 ? O(1) N(1) 2.911(5) . 2_644 ? O(2) N(1) 2.932(4) . 2_644 ? O(2) C(46) 3.534(6) . . ? O(3) N(1) 2.905(4) . 2_644 ? O(3) C(38) 3.580(5) . 2_644 ? O(4) N(1) 2.959(4) . 2_644 ? O(5) N(1) 2.881(4) . 2_644 ? O(5) C(37) 3.305(4) . 2_644 ? O(5) C(38) 3.550(4) . 2_644 ? O(6) N(1) 2.931(4) . 2_644 ? O(6) C(46) 3.551(7) . . ? O(7) N(2) 2.980(4) . 2_645 ? O(7) C(44) 3.485(6) . 2_645 ? O(8) N(2) 2.885(4) . 2_645 ? O(8) C(40) 3.291(4) . 2_645 ? O(8) C(41) 3.557(4) . 2_645 ? O(9) N(2) 2.962(4) . 2_645 ? O(10) N(2) 2.983(4) . 2_645 ? O(11) N(2) 2.949(4) . 2_645 ? O(12) N(2) 2.872(4) . 2_645 ? O(12) C(41) 3.546(4) . 2_645 ? N(1) C(46) 3.406(6) . 2_644 ? N(2) C(44) 3.517(6) . . ? N(3) C(43) 3.272(7) . 2_645 ? N(3) C(44) 3.360(9) . 2_645 ? N(3) C(19) 3.531(8) . . ? N(4) C(45) 3.293(6) . 2_654 ? N(4) C(46) 3.301(8) . 2_654 ? N(4) C(25) 3.475(7) . . ? C(43) C(43) 3.30(1) . 2_645 ? C(45) C(45) 3.24(1) . 2_654 ? #------------------------------------------------------------------------------ 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 S(1) Ni(1) S(5) 92.74(4) . 1_555 1_555 yes S(1) Ni(1) S(6) 178.87(5) . 1_555 1_555 yes S(1) Ni(1) S(10) 86.62(4) . 1_555 1_555 yes S(5) Ni(1) S(6) 87.48(4) . 1_555 1_555 yes S(5) Ni(1) S(10) 179.28(4) . 1_555 1_555 yes S(6) Ni(1) S(10) 93.17(4) . 1_555 1_555 yes S(11) Ni(2) S(15) 93.15(4) . 1_555 1_555 yes S(11) Ni(2) S(16) 178.44(5) . 1_555 1_555 yes S(11) Ni(2) S(20) 86.86(4) . 1_555 1_555 yes S(15) Ni(2) S(16) 87.02(4) . 1_555 1_555 yes S(15) Ni(2) S(20) 178.37(5) . 1_555 1_555 yes S(16) Ni(2) S(20) 93.01(4) . 1_555 1_555 yes Ni(1) S(1) C(1) 102.8(1) . 1_555 1_555 yes C(1) S(2) C(2) 97.8(2) . 1_555 1_555 yes C(2) S(4) C(3) 97.6(2) . 1_555 1_555 yes Ni(1) S(5) C(3) 102.5(1) . 1_555 1_555 yes Ni(1) S(6) C(4) 102.3(1) . 1_555 1_555 yes C(4) S(7) C(5) 98.3(2) . 1_555 1_555 yes C(5) S(9) C(6) 98.0(2) . 1_555 1_555 yes Ni(1) S(10) C(6) 102.1(1) . 1_555 1_555 yes Ni(2) S(11) C(7) 102.4(1) . 1_555 1_555 yes C(7) S(12) C(8) 98.1(2) . 1_555 1_555 yes C(8) S(14) C(9) 97.8(2) . 1_555 1_555 yes Ni(2) S(15) C(9) 102.2(1) . 1_555 1_555 yes Ni(2) S(16) C(10) 102.1(1) . 1_555 1_555 yes C(10) S(17) C(11) 97.7(2) . 1_555 1_555 yes C(11) S(19) C(12) 97.8(2) . 1_555 1_555 yes Ni(2) S(20) C(12) 102.4(1) . 1_555 1_555 yes C(13) O(1) C(24) 112.8(5) . 1_555 1_555 yes C(14) O(2) C(15) 112.5(5) . 1_555 1_555 yes C(16) O(3) C(17) 113.3(5) . 1_555 1_555 yes C(18) O(4) C(19) 113.6(5) . 1_555 1_555 yes C(20) O(5) C(21) 112.9(4) . 1_555 1_555 yes C(22) O(6) C(23) 114.1(5) . 1_555 1_555 yes C(25) O(7) C(36) 113.8(4) . 1_555 1_555 yes C(26) O(8) C(27) 112.2(4) . 1_555 1_555 yes C(28) O(9) C(29) 112.4(4) . 1_555 1_555 yes C(30) O(10) C(31) 113.6(4) . 1_555 1_555 yes C(32) O(11) C(33) 113.5(4) . 1_555 1_555 yes C(34) O(12) C(35) 112.1(4) . 1_555 1_555 yes S(1) C(1) S(2) 123.0(2) . 1_555 1_555 yes S(1) C(1) C(3) 120.5(3) . 1_555 1_555 yes S(2) C(1) C(3) 116.5(3) . 1_555 1_555 yes S(2) C(2) S(3) 123.1(3) . 1_555 1_555 yes S(2) C(2) S(4) 113.0(2) . 1_555 1_555 yes S(3) C(2) S(4) 123.9(3) . 1_555 1_555 yes S(4) C(3) S(5) 123.5(2) . 1_555 1_555 yes S(4) C(3) C(1) 115.0(3) . 1_555 1_555 yes S(5) C(3) C(1) 121.5(3) . 1_555 1_555 yes S(6) C(4) S(7) 123.3(2) . 1_555 1_555 yes S(6) C(4) C(6) 121.1(3) . 1_555 1_555 yes S(7) C(4) C(6) 115.6(3) . 1_555 1_555 yes S(7) C(5) S(8) 124.0(2) . 1_555 1_555 yes S(7) C(5) S(9) 112.2(2) . 1_555 1_555 yes S(8) C(5) S(9) 123.8(2) . 1_555 1_555 yes S(9) C(6) S(10) 122.8(2) . 1_555 1_555 yes S(9) C(6) C(4) 115.9(3) . 1_555 1_555 yes S(10) C(6) C(4) 121.4(3) . 1_555 1_555 yes S(11) C(7) S(12) 123.4(2) . 1_555 1_555 yes S(11) C(7) C(9) 121.3(3) . 1_555 1_555 yes S(12) C(7) C(9) 115.3(3) . 1_555 1_555 yes S(12) C(8) S(13) 123.6(2) . 1_555 1_555 yes S(12) C(8) S(14) 112.8(2) . 1_555 1_555 yes S(13) C(8) S(14) 123.7(2) . 1_555 1_555 yes S(14) C(9) S(15) 123.1(2) . 1_555 1_555 yes S(14) C(9) C(7) 115.9(3) . 1_555 1_555 yes S(15) C(9) C(7) 121.0(3) . 1_555 1_555 yes S(16) C(10) S(17) 123.1(2) . 1_555 1_555 yes S(16) C(10) C(12) 121.2(3) . 1_555 1_555 yes S(17) C(10) C(12) 115.7(3) . 1_555 1_555 yes S(17) C(11) S(18) 123.2(3) . 1_555 1_555 yes S(17) C(11) S(19) 113.0(2) . 1_555 1_555 yes S(18) C(11) S(19) 123.8(3) . 1_555 1_555 yes S(19) C(12) S(20) 122.9(2) . 1_555 1_555 yes S(19) C(12) C(10) 115.8(3) . 1_555 1_555 yes S(20) C(12) C(10) 121.2(3) . 1_555 1_555 yes O(1) C(13) C(14) 109.1(4) . 1_555 1_555 yes O(2) C(14) C(13) 109.1(5) . 1_555 1_555 yes O(2) C(15) C(16) 108.9(4) . 1_555 1_555 yes O(3) C(16) C(15) 110.0(5) . 1_555 1_555 yes O(3) C(17) C(18) 109.4(5) . 1_555 1_555 yes O(4) C(18) C(17) 107.6(4) . 1_555 1_555 yes O(4) C(19) C(20) 108.6(4) . 1_555 1_555 yes O(5) C(20) C(19) 108.8(4) . 1_555 1_555 yes O(5) C(21) C(22) 109.2(4) . 1_555 1_555 yes O(6) C(22) C(21) 110.5(4) . 1_555 1_555 yes O(6) C(23) C(24) 109.6(5) . 1_555 1_555 yes O(1) C(24) C(23) 110.5(5) . 1_555 1_555 yes O(7) C(25) C(26) 108.8(4) . 1_555 1_555 yes O(8) C(26) C(25) 108.6(4) . 1_555 1_555 yes O(8) C(27) C(28) 109.0(4) . 1_555 1_555 yes O(9) C(28) C(27) 109.1(4) . 1_555 1_555 yes O(9) C(29) C(30) 108.5(4) . 1_555 1_555 yes O(10) C(30) C(29) 109.8(4) . 1_555 1_555 yes O(10) C(31) C(32) 110.2(4) . 1_555 1_555 yes O(11) C(32) C(31) 108.9(4) . 1_555 1_555 yes O(11) C(33) C(34) 110.1(4) . 1_555 1_555 yes O(12) C(34) C(33) 109.4(4) . 1_555 1_555 yes O(12) C(35) C(36) 110.3(4) . 1_555 1_555 yes O(7) C(36) C(35) 108.9(4) . 1_555 1_555 yes C(38) C(37) C(39) 119.7(3) . 1_555 2_644 yes N(1) C(38) C(37) 119.7(3) . 1_555 1_555 yes N(1) C(38) C(39) 119.6(3) . 1_555 1_555 yes C(37) C(38) C(39) 120.7(3) . 1_555 1_555 yes C(41) C(40) C(42) 119.4(3) . 1_555 2_635 yes N(2) C(41) C(40) 119.3(3) . 1_555 1_555 yes N(2) C(41) C(42) 119.7(3) . 1_555 1_555 yes C(40) C(41) C(42) 121.0(3) . 1_555 1_555 yes N(3) C(43) C(44) 179.1(8) . 1_555 1_555 yes N(4) C(45) C(46) 179.6(6) . 1_555 1_555 yes #==END