Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemsitry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Hirotsu, Masakazu' 'Kobayashi, Atsushi' 'Konno, Takumi' 'Yoshimura, Takashi' _publ_contact_author_name 'Prof Takumi Konno' _publ_contact_author_address ; Department of Chemistry Overseas Graduate School of Science Osaka University Toyonaka Osaka 560-0043 JAPAN ; _publ_contact_author_email 'KONNO@CH.WANI.OSAKA-U.AC.JP' publ_contact_author_phone '+ 81-6-6850-5765' _publ_contact_author_fax '+ 81-6-6850-5765' _publ_section_title ; Rhodium (III) complexes with thiolate and thioether ligands derived from fac(S)-[Rh(aet)3] (aet = 2-aminoethanethiolate): selective formation, characterization and properties ; data_[1](ClO4)2(H2O) _database_code_CSD 172537 #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 576.28 _chemical_formula_analytical ? _chemical_formula_sum 'C8 H24 Cl2 N3 O9 Rh S3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 9.368(2) _cell_length_b 16.306(2) _cell_length_c 13.167(1) _cell_angle_alpha 90 _cell_angle_beta 96.413(10) _cell_angle_gamma 90 _cell_volume 1998.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _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 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1168.00 _exptl_absorpt_coefficient_mu 1.479 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_correction_T_min 0.906 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -3.02 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5032 _reflns_number_total 4753 _reflns_number_observed 4095 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.011 _diffrn_reflns_av_sigmaI/netI 0.031 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.01703 _diffrn_orient_matrix_UB_12 -0.02030 _diffrn_orient_matrix_UB_13 -0.06930 _diffrn_orient_matrix_UB_21 0.00048 _diffrn_orient_matrix_UB_22 -0.05776 _diffrn_orient_matrix_UB_23 0.02555 _diffrn_orient_matrix_UB_31 -0.10607 _diffrn_orient_matrix_UB_32 -0.00352 _diffrn_orient_matrix_UB_33 -0.01965 #------------------------------------------------------------------------------ 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 32 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 8 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 12 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 36 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Rh 0 4 -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 12 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_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 _atom_site_occupancy _atom_site_refinement_flags Rh1 0.71781(2) 0.22756(1) 0.24567(2) 0.02171(6) Uani d . 1.00 . Cl1 0.72511(8) -0.03010(5) 0.07117(6) 0.0375(2) Uani d . 1.00 . Cl2 0.22445(9) 0.08928(5) 0.38739(6) 0.0406(2) Uani d . 1.00 . S1 0.61361(8) 0.21088(5) 0.39734(5) 0.0304(2) Uani d . 1.00 . S2 0.89733(8) 0.30279(5) 0.33436(5) 0.0283(2) Uani d . 1.00 . S3 0.60567(8) 0.34837(5) 0.20100(5) 0.0292(2) Uani d . 1.00 . O1 0.6861(3) -0.0472(2) 0.1703(2) 0.084(1) Uani d . 1.00 . O2 0.6352(3) -0.0692(2) -0.0064(2) 0.090(1) Uani d . 1.00 . O3 0.8705(3) -0.0539(2) 0.0658(2) 0.0700(9) Uani d . 1.00 . O4 0.7143(3) 0.0575(1) 0.0580(2) 0.0563(8) Uani d . 1.00 . O5 0.1310(3) 0.0196(2) 0.3827(2) 0.0706(10) Uani d . 1.00 . O6 0.2987(3) 0.0901(2) 0.2977(2) 0.0700(9) Uani d . 1.00 . O7 0.3247(3) 0.0859(2) 0.4756(2) 0.0730(10) Uani d . 1.00 . O8 0.1387(3) 0.1607(2) 0.3882(2) 0.091(1) Uani d . 1.00 . O9 0.0692(3) 0.1198(2) 0.1318(2) 0.0654(9) Uani d . 1.00 . N1 0.8155(3) 0.1135(2) 0.2825(2) 0.0316(7) Uani d . 1.00 . N2 0.8376(3) 0.2396(2) 0.1176(2) 0.0292(7) Uani d . 1.00 . N3 0.5278(3) 0.1742(2) 0.1708(2) 0.0303(7) Uani d . 1.00 . C1 0.7984(4) 0.0825(2) 0.3867(3) 0.043(1) Uani d . 1.00 . C2 0.6514(4) 0.1018(2) 0.4121(3) 0.041(1) Uani d . 1.00 . C3 0.9373(4) 0.3107(2) 0.1297(2) 0.0348(9) Uani d . 1.00 . C4 1.0183(3) 0.3114(2) 0.2352(2) 0.0340(9) Uani d . 1.00 . C5 0.4210(3) 0.2364(2) 0.1269(2) 0.0343(9) Uani d . 1.00 . C6 0.4226(3) 0.3110(2) 0.1948(2) 0.0338(9) Uani d . 1.00 . C7 0.8166(4) 0.4063(2) 0.3325(3) 0.0358(9) Uani d . 1.00 . C8 0.6538(4) 0.4056(2) 0.3180(2) 0.0345(9) Uani d . 1.00 . H1 0.819(3) 0.025(2) 0.387(2) 0.035(9) Uiso calc . 1.00 . H2 0.877(4) 0.112(2) 0.436(3) 0.07(1) Uiso calc . 1.00 . H3 0.590(3) 0.067(2) 0.356(2) 0.06(1) Uiso calc . 1.00 . H4 0.649(3) 0.090(2) 0.471(2) 0.038(10) Uiso calc . 1.00 . H5 0.883(3) 0.363(2) 0.120(2) 0.037(9) Uiso calc . 1.00 . H6 1.005(3) 0.308(2) 0.081(2) 0.038(9) Uiso calc . 1.00 . H7 1.069(3) 0.360(2) 0.251(2) 0.039(9) Uiso calc . 1.00 . H8 1.077(3) 0.265(2) 0.250(2) 0.039(9) Uiso calc . 1.00 . H9 0.328(3) 0.212(2) 0.119(2) 0.039(9) Uiso calc . 1.00 . H10 0.443(3) 0.252(2) 0.065(2) 0.037(9) Uiso calc . 1.00 . H11 0.367(3) 0.351(2) 0.166(2) 0.026(8) Uiso calc . 1.00 . H12 0.408(3) 0.298(2) 0.260(2) 0.027(8) Uiso calc . 1.00 . H13 0.864(3) 0.436(2) 0.277(2) 0.035(8) Uiso calc . 1.00 . H14 0.854(3) 0.426(2) 0.393(2) 0.038(9) Uiso calc . 1.00 . H15 0.611(3) 0.381(2) 0.375(2) 0.027(8) Uiso calc . 1.00 . H16 0.614(3) 0.458(2) 0.312(2) 0.041(9) Uiso calc . 1.00 . H17 0.776(4) 0.083(2) 0.243(2) 0.05(1) Uiso calc . 1.00 . H18 0.906(4) 0.117(2) 0.269(3) 0.08(1) Uiso calc . 1.00 . H19 0.784(3) 0.244(2) 0.066(2) 0.04(1) Uiso calc . 1.00 . H20 0.893(4) 0.186(2) 0.118(2) 0.06(1) Uiso calc . 1.00 . H21 0.497(4) 0.145(2) 0.218(2) 0.05(1) Uiso calc . 1.00 . H22 0.550(3) 0.139(2) 0.124(2) 0.05(1) Uiso calc . 1.00 . 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 Rh1 0.0232(1) 0.0244(1) 0.0176(1) -0.00091(9) 0.00232(8) -0.00258(9) Cl1 0.0341(4) 0.0423(5) 0.0348(4) 0.0018(4) -0.0013(3) -0.0060(3) Cl2 0.0397(4) 0.0421(5) 0.0397(4) 0.0026(4) 0.0031(4) 0.0041(4) S1 0.0333(4) 0.0363(4) 0.0225(3) -0.0015(3) 0.0076(3) -0.0015(3) S2 0.0280(4) 0.0327(4) 0.0238(3) -0.0041(3) 0.0009(3) -0.0031(3) S3 0.0306(4) 0.0292(4) 0.0275(4) 0.0018(3) 0.0019(3) -0.0018(3) O1 0.106(3) 0.089(2) 0.063(2) -0.022(2) 0.036(2) 0.019(2) O2 0.071(2) 0.080(2) 0.108(2) 0.007(2) -0.036(2) -0.055(2) O3 0.040(1) 0.092(2) 0.076(2) 0.024(2) -0.001(1) -0.008(2) O4 0.077(2) 0.043(1) 0.048(1) 0.011(1) 0.006(1) -0.002(1) O5 0.070(2) 0.064(2) 0.080(2) -0.025(2) 0.018(2) -0.008(2) O6 0.053(2) 0.115(3) 0.043(1) -0.021(2) 0.012(1) -0.005(2) O7 0.069(2) 0.102(2) 0.044(2) -0.016(2) -0.011(1) 0.013(2) O8 0.099(3) 0.059(2) 0.117(3) 0.036(2) 0.020(2) 0.012(2) O9 0.057(2) 0.073(2) 0.065(2) 0.027(1) 0.004(1) -0.014(1) N1 0.035(2) 0.031(1) 0.029(1) 0.000(1) 0.005(1) -0.003(1) N2 0.030(1) 0.037(2) 0.021(1) 0.002(1) 0.003(1) -0.001(1) N3 0.030(1) 0.034(1) 0.027(1) -0.003(1) 0.001(1) -0.007(1) C1 0.051(2) 0.041(2) 0.039(2) 0.008(2) 0.010(2) 0.012(2) C2 0.052(2) 0.041(2) 0.033(2) 0.002(2) 0.014(2) 0.011(2) C3 0.036(2) 0.039(2) 0.031(2) -0.003(2) 0.011(1) 0.002(1) C4 0.028(2) 0.040(2) 0.035(2) -0.005(2) 0.008(1) -0.004(1) C5 0.028(2) 0.045(2) 0.028(2) -0.002(1) -0.002(1) -0.004(1) C6 0.028(2) 0.041(2) 0.032(2) 0.005(1) 0.000(1) -0.001(1) C7 0.038(2) 0.031(2) 0.038(2) -0.004(1) 0.005(2) -0.012(1) C8 0.039(2) 0.029(2) 0.036(2) 0.002(1) 0.005(1) -0.010(1) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0039(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4095 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0262 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0248 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.574 _refine_ls_shift/esd_max 0.0402 _refine_ls_shift/esd_mean 0.0016 _refine_diff_density_min -0.38 _refine_diff_density_max 0.37 #------------------------------------------------------------------------------ _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 RH1 S1 2.3347(7) 1_555 1_555 yes RH1 S2 2.2930(7) 1_555 1_555 yes RH1 S3 2.2785(8) 1_555 1_555 yes RH1 N1 2.106(3) 1_555 1_555 yes RH1 N2 2.137(2) 1_555 1_555 yes RH1 N3 2.122(3) 1_555 1_555 yes CL1 O1 1.422(3) 1_555 1_555 yes CL1 O2 1.402(2) 1_555 1_555 yes CL1 O3 1.426(2) 1_555 1_555 yes CL1 O4 1.441(2) 1_555 1_555 yes CL2 O5 1.432(3) 1_555 1_555 yes CL2 O6 1.436(2) 1_555 1_555 yes CL2 O7 1.411(2) 1_555 1_555 yes CL2 O8 1.416(3) 1_555 1_555 yes S1 C2 1.820(4) 1_555 1_555 yes S2 C4 1.827(3) 1_555 1_555 yes S2 C7 1.848(3) 1_555 1_555 yes S3 C6 1.813(3) 1_555 1_555 yes S3 C8 1.815(3) 1_555 1_555 yes N1 C1 1.487(4) 1_555 1_555 yes N2 C3 1.486(4) 1_555 1_555 yes N3 C5 1.494(4) 1_555 1_555 yes C1 C2 1.488(5) 1_555 1_555 yes C3 C4 1.507(4) 1_555 1_555 yes C5 C6 1.509(4) 1_555 1_555 yes C7 C8 1.516(4) 1_555 1_555 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 RH1 S2 88.83(3) 1_555 1_555 1_555 yes S1 RH1 S3 95.55(3) 1_555 1_555 1_555 yes S1 RH1 N1 84.98(8) 1_555 1_555 1_555 yes S1 RH1 N2 173.02(8) 1_555 1_555 1_555 yes S1 RH1 N3 86.59(8) 1_555 1_555 1_555 yes S2 RH1 S3 87.69(3) 1_555 1_555 1_555 yes S2 RH1 N1 94.61(8) 1_555 1_555 1_555 yes S2 RH1 N2 86.15(7) 1_555 1_555 1_555 yes S2 RH1 N3 170.09(7) 1_555 1_555 1_555 yes S3 RH1 N1 177.66(8) 1_555 1_555 1_555 yes S3 RH1 N2 89.10(8) 1_555 1_555 1_555 yes S3 RH1 N3 84.01(7) 1_555 1_555 1_555 yes N1 RH1 N2 90.6(1) 1_555 1_555 1_555 yes N1 RH1 N3 93.7(1) 1_555 1_555 1_555 yes N2 RH1 N3 99.1(1) 1_555 1_555 1_555 yes O1 CL1 O2 112.6(2) 1_555 1_555 1_555 yes O1 CL1 O3 109.7(2) 1_555 1_555 1_555 yes O1 CL1 O4 106.5(2) 1_555 1_555 1_555 yes O2 CL1 O3 109.8(2) 1_555 1_555 1_555 yes O2 CL1 O4 109.5(2) 1_555 1_555 1_555 yes O3 CL1 O4 108.5(2) 1_555 1_555 1_555 yes O5 CL2 O6 108.8(2) 1_555 1_555 1_555 yes O5 CL2 O7 110.6(2) 1_555 1_555 1_555 yes O5 CL2 O8 107.9(2) 1_555 1_555 1_555 yes O6 CL2 O7 109.8(2) 1_555 1_555 1_555 yes O6 CL2 O8 109.0(2) 1_555 1_555 1_555 yes O7 CL2 O8 110.6(2) 1_555 1_555 1_555 yes RH1 S1 C2 96.4(1) 1_555 1_555 1_555 yes RH1 S2 C4 98.9(1) 1_555 1_555 1_555 yes RH1 S2 C7 101.9(1) 1_555 1_555 1_555 yes C4 S2 C7 101.9(2) 1_555 1_555 1_555 yes RH1 S3 C6 97.3(1) 1_555 1_555 1_555 yes RH1 S3 C8 99.3(1) 1_555 1_555 1_555 yes C6 S3 C8 110.8(2) 1_555 1_555 1_555 yes RH1 N1 C1 115.1(2) 1_555 1_555 1_555 yes RH1 N1 H17 104(2) 1_555 1_555 1_555 no RH1 N1 H18 107(2) 1_555 1_555 1_555 no C1 N1 H17 108(2) 1_555 1_555 1_555 no C1 N1 H18 114(2) 1_555 1_555 1_555 no H17 N1 H18 106(3) 1_555 1_555 1_555 no RH1 N2 C3 111.5(2) 1_555 1_555 1_555 yes RH1 N2 H19 109(2) 1_555 1_555 1_555 no RH1 N2 H20 102(1) 1_555 1_555 1_555 no C3 N2 H19 110(2) 1_555 1_555 1_555 no C3 N2 H20 110(1) 1_555 1_555 1_555 no H19 N2 H20 110(2) 1_555 1_555 1_555 no RH1 N3 C5 113.1(2) 1_555 1_555 1_555 yes RH1 N3 H21 102(2) 1_555 1_555 1_555 no RH1 N3 H22 110(2) 1_555 1_555 1_555 no C5 N3 H21 113(2) 1_555 1_555 1_555 no C5 N3 H22 111(2) 1_555 1_555 1_555 no H21 N3 H22 104(2) 1_555 1_555 1_555 no N1 C1 C2 109.5(3) 1_555 1_555 1_555 yes N1 C1 H1 107(1) 1_555 1_555 1_555 no N1 C1 H2 105(1) 1_555 1_555 1_555 no C2 C1 H1 113(1) 1_555 1_555 1_555 no C2 C1 H2 112(1) 1_555 1_555 1_555 no H1 C1 H2 108(2) 1_555 1_555 1_555 no S1 C2 C1 110.9(3) 1_555 1_555 1_555 yes S1 C2 H3 111(1) 1_555 1_555 1_555 no S1 C2 H4 108(2) 1_555 1_555 1_555 no C1 C2 H3 99(1) 1_555 1_555 1_555 no C1 C2 H4 106(2) 1_555 1_555 1_555 no H3 C2 H4 118(2) 1_555 1_555 1_555 no N2 C3 C4 110.5(3) 1_555 1_555 1_555 yes N2 C3 H5 110(1) 1_555 1_555 1_555 no N2 C3 H6 110(1) 1_555 1_555 1_555 no C4 C3 H5 108(1) 1_555 1_555 1_555 no C4 C3 H6 108(1) 1_555 1_555 1_555 no H5 C3 H6 108(2) 1_555 1_555 1_555 no S2 C4 C3 111.7(2) 1_555 1_555 1_555 yes S2 C4 H7 104(1) 1_555 1_555 1_555 no S2 C4 H8 100(1) 1_555 1_555 1_555 no C3 C4 H7 113(1) 1_555 1_555 1_555 no C3 C4 H8 113(1) 1_555 1_555 1_555 no H7 C4 H8 111(2) 1_555 1_555 1_555 no N3 C5 C6 110.8(2) 1_555 1_555 1_555 yes N3 C5 H9 108(1) 1_555 1_555 1_555 no N3 C5 H10 109(1) 1_555 1_555 1_555 no C6 C5 H9 110(1) 1_555 1_555 1_555 no C6 C5 H10 108(1) 1_555 1_555 1_555 no H9 C5 H10 108(2) 1_555 1_555 1_555 no S3 C6 C5 104.2(2) 1_555 1_555 1_555 yes S3 C6 H11 106(1) 1_555 1_555 1_555 no S3 C6 H12 106(1) 1_555 1_555 1_555 no C5 C6 H11 111(1) 1_555 1_555 1_555 no C5 C6 H12 112(1) 1_555 1_555 1_555 no H11 C6 H12 115(2) 1_555 1_555 1_555 no S2 C7 C8 113.6(2) 1_555 1_555 1_555 yes S2 C7 H13 103(1) 1_555 1_555 1_555 no S2 C7 H14 101(1) 1_555 1_555 1_555 no C8 C7 H13 115(1) 1_555 1_555 1_555 no C8 C7 H14 113(1) 1_555 1_555 1_555 no H13 C7 H14 107(2) 1_555 1_555 1_555 no S3 C8 C7 105.1(2) 1_555 1_555 1_555 yes S3 C8 H15 110(1) 1_555 1_555 1_555 no S3 C8 H16 109(1) 1_555 1_555 1_555 no C7 C8 H15 113(1) 1_555 1_555 1_555 no C7 C8 H16 113(1) 1_555 1_555 1_555 no H15 C8 H16 104(2) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ #===END data_[3](ClO4)3(H2O) _database_code_CSD 172538 #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1385.57 _chemical_formula_analytical ? _chemical_formula_sum 'C18 H58 Cl6 N6 O26 Rh2 S6 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 19.181(4) _cell_length_b 14.374(4) _cell_length_c 20.233(4) _cell_angle_alpha 90 _cell_angle_beta 116.93(1) _cell_angle_gamma 90 _cell_volume 4973(1) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 14.2 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2816.00 _exptl_absorpt_coefficient_mu 1.320 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.920 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -3.40 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 12212 _reflns_number_total 11869 _reflns_number_observed 6702 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.131 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02084 _diffrn_orient_matrix_UB_12 -0.00382 _diffrn_orient_matrix_UB_13 -0.03715 _diffrn_orient_matrix_UB_21 0.05420 _diffrn_orient_matrix_UB_22 -0.00732 _diffrn_orient_matrix_UB_23 0.04108 _diffrn_orient_matrix_UB_31 -0.00690 _diffrn_orient_matrix_UB_32 -0.06908 _diffrn_orient_matrix_UB_33 -0.00230 #------------------------------------------------------------------------------ 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 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 232 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 104 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 24 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 24 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 24 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Rh 0 8 -1.118 0.919 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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 _atom_site_occupancy _atom_site_refinement_flags Rh1 0.91824(3) 0.22527(3) 0.60954(3) 0.0270(1) Uani d . 1.00 . Rh2 0.68122(3) 0.24351(4) 0.11210(3) 0.0311(1) Uani d . 1.00 . Cl1 0.8224(1) 0.4866(1) 0.4111(1) 0.0543(6) Uani d . 1.00 . Cl2 0.4404(1) 0.4551(1) 0.0638(1) 0.0434(5) Uani d . 1.00 . Cl3 0.5611(1) 0.2300(1) 0.31725(10) 0.0459(5) Uani d . 1.00 . Cl4 0.8692(1) -0.0186(1) 0.4155(1) 0.0445(5) Uani d . 1.00 . Cl5 0.4447(1) 0.0162(2) 0.1074(1) 0.0665(8) Uani d . 1.00 . Cl6 0.7567(1) -0.2069(2) 0.1909(1) 0.0612(7) Uani d . 1.00 . S1 0.8921(1) 0.3834(1) 0.6088(1) 0.0426(5) Uani d . 1.00 . S2 0.9716(1) 0.2000(1) 0.73733(9) 0.0406(5) Uani d . 1.00 . S3 0.79406(10) 0.1731(1) 0.58312(10) 0.0367(5) Uani d . 1.00 . S4 0.7457(1) 0.3845(1) 0.1448(1) 0.0464(6) Uani d . 1.00 . S5 0.7486(1) 0.1842(1) 0.0507(1) 0.0486(6) Uani d . 1.00 . S6 0.7535(1) 0.1655(1) 0.2241(1) 0.0455(6) Uani d . 1.00 . O1 0.8667(4) 0.5545(4) 0.4635(3) 0.089(2) Uani d . 1.00 . O2 0.7892(4) 0.5261(4) 0.3386(3) 0.075(2) Uani d . 1.00 . O3 0.7620(4) 0.4541(4) 0.4285(4) 0.103(3) Uani d . 1.00 . O4 0.8732(4) 0.4105(4) 0.4155(3) 0.081(2) Uani d . 1.00 . O5 0.4950(3) 0.5301(4) 0.0864(3) 0.075(2) Uani d . 1.00 . O6 0.3728(3) 0.4797(4) -0.0012(3) 0.086(2) Uani d . 1.00 . O7 0.4737(3) 0.3752(4) 0.0467(3) 0.080(2) Uani d . 1.00 . O8 0.4223(4) 0.4342(4) 0.1210(3) 0.092(3) Uani d . 1.00 . O9 0.5960(4) 0.2968(4) 0.3747(3) 0.087(2) Uani d . 1.00 . O10 0.5029(3) 0.2719(5) 0.2540(3) 0.098(3) Uani d . 1.00 . O11 0.6198(3) 0.1930(5) 0.3003(3) 0.083(2) Uani d . 1.00 . O12 0.5309(4) 0.1579(5) 0.3439(4) 0.101(3) Uani d . 1.00 . O13 0.9151(4) 0.0638(4) 0.4291(4) 0.082(2) Uani d . 1.00 . O14 0.7901(3) 0.0013(5) 0.3704(3) 0.089(2) Uani d . 1.00 . O15 0.8941(3) -0.0861(4) 0.3794(3) 0.079(2) Uani d . 1.00 . O16 0.8788(4) -0.0541(4) 0.4849(3) 0.075(2) Uani d . 1.00 . O17 0.4859(4) 0.1004(5) 0.1253(5) 0.120(3) Uani d . 1.00 . O18 0.3812(6) 0.0184(6) 0.0409(4) 0.175(4) Uani d . 1.00 . O19 0.4914(5) -0.0585(6) 0.1095(6) 0.158(4) Uani d . 1.00 . O20 0.4164(5) -0.0009(7) 0.1574(5) 0.158(5) Uani d . 1.00 . O21 0.7930(7) -0.1433(9) 0.1675(7) 0.243(8) Uani d . 1.00 . O22 0.7109(4) -0.2605(8) 0.1336(4) 0.185(4) Uani d . 1.00 . O23 0.8112(7) -0.2535(9) 0.2379(6) 0.272(6) Uani d . 1.00 . O24 0.7156(5) -0.1599(5) 0.2216(5) 0.120(4) Uani d . 1.00 . O25 0.5210(3) 0.2472(5) 0.4780(3) 0.072(2) Uani d . 1.00 . O26 0.5397(4) -0.2123(5) 0.0538(4) 0.106(3) Uani d . 1.00 . N1 1.0310(3) 0.2686(4) 0.6278(3) 0.038(2) Uani d . 1.00 . N2 0.9465(3) 0.0843(4) 0.6045(3) 0.040(2) Uani d . 1.00 . N3 0.8747(3) 0.2355(4) 0.4934(3) 0.036(2) Uani d . 1.00 . N4 0.6130(3) 0.2940(4) 0.1615(3) 0.049(2) Uani d . 1.00 . N5 0.6067(3) 0.3040(4) 0.0096(3) 0.046(2) Uani d . 1.00 . N6 0.6137(4) 0.1204(4) 0.0790(3) 0.049(2) Uani d . 1.00 . C1 0.9828(4) 0.4281(5) 0.6131(5) 0.053(2) Uani d . 1.00 . C2 1.0492(4) 0.3646(5) 0.6582(4) 0.054(3) Uani d . 1.00 . C3 0.8996(5) 0.4223(6) 0.6962(5) 0.065(3) Uani d . 1.00 . C4 1.0104(4) 0.0845(5) 0.7388(4) 0.050(2) Uani d . 1.00 . C5 0.9586(4) 0.0303(5) 0.6712(4) 0.049(2) Uani d . 1.00 . C6 0.8968(5) 0.1744(6) 0.7651(4) 0.067(3) Uani d . 1.00 . C7 0.7581(4) 0.1534(5) 0.4848(4) 0.045(2) Uani d . 1.00 . C8 0.7876(4) 0.2263(5) 0.4510(3) 0.044(2) Uani d . 1.00 . C9 0.7314(4) 0.2653(6) 0.5829(4) 0.062(3) Uani d . 1.00 . C10 0.6796(5) 0.4430(5) 0.1723(4) 0.053(3) Uani d . 1.00 . C11 0.6498(5) 0.3756(6) 0.2116(4) 0.061(3) Uani d . 1.00 . C12 0.8345(4) 0.3752(6) 0.2327(4) 0.063(3) Uani d . 1.00 . C13 0.6781(5) 0.2148(6) -0.0423(4) 0.058(3) Uani d . 1.00 . C14 0.6417(5) 0.3058(6) -0.0434(4) 0.058(3) Uani d . 1.00 . C15 0.8287(5) 0.2591(6) 0.0626(4) 0.065(3) Uani d . 1.00 . C16 0.6904(5) 0.0637(5) 0.2033(4) 0.056(3) Uani d . 1.00 . C17 0.6571(5) 0.0388(5) 0.1240(4) 0.055(3) Uani d . 1.00 . C18 0.8404(5) 0.1128(6) 0.2276(5) 0.064(3) Uani d . 1.00 . H1 0.9779 0.4323 0.5643 0.0631 Uiso calc . 1.00 . H2 0.9930 0.4881 0.6352 0.0631 Uiso calc . 1.00 . H3 1.0570 0.3644 0.7080 0.0643 Uiso calc . 1.00 . H4 1.0953 0.3858 0.6566 0.0643 Uiso calc . 1.00 . H5 1.0608 0.0900 0.7409 0.0596 Uiso calc . 1.00 . H6 1.0147 0.0523 0.7815 0.0596 Uiso calc . 1.00 . H7 0.9096 0.0195 0.6710 0.0587 Uiso calc . 1.00 . H8 0.9825 -0.0276 0.6712 0.0587 Uiso calc . 1.00 . H9 0.7754 0.0941 0.4774 0.0534 Uiso calc . 1.00 . H10 0.7026 0.1549 0.4614 0.0534 Uiso calc . 1.00 . H11 0.7640 0.2842 0.4516 0.0533 Uiso calc . 1.00 . H12 0.7740 0.2095 0.4012 0.0533 Uiso calc . 1.00 . H13 0.7064 0.4928 0.2048 0.0633 Uiso calc . 1.00 . H14 0.6366 0.4669 0.1295 0.0633 Uiso calc . 1.00 . H15 0.6120 0.4057 0.2225 0.0737 Uiso calc . 1.00 . H16 0.6921 0.3549 0.2564 0.0737 Uiso calc . 1.00 . H17 0.7037 0.2180 -0.0729 0.0691 Uiso calc . 1.00 . H18 0.6385 0.1684 -0.0608 0.0691 Uiso calc . 1.00 . H19 0.6019 0.3181 -0.0920 0.0692 Uiso calc . 1.00 . H20 0.6804 0.3532 -0.0290 0.0692 Uiso calc . 1.00 . H21 0.7201 0.0128 0.2323 0.0671 Uiso calc . 1.00 . H22 0.6490 0.0769 0.2154 0.0671 Uiso calc . 1.00 . H23 0.6225 -0.0124 0.1140 0.0663 Uiso calc . 1.00 . H24 0.6980 0.0225 0.1120 0.0663 Uiso calc . 1.00 . H25 0.9456 0.3972 0.7354 0.0778 Uiso calc . 1.00 . H26 0.9021 0.4883 0.6983 0.0778 Uiso calc . 1.00 . H27 0.8551 0.4019 0.7012 0.0778 Uiso calc . 1.00 . H28 0.8715 0.2304 0.7671 0.0798 Uiso calc . 1.00 . H29 0.8596 0.1331 0.7303 0.0798 Uiso calc . 1.00 . H30 0.9199 0.1460 0.8127 0.0798 Uiso calc . 1.00 . H31 0.7448 0.2828 0.6325 0.0747 Uiso calc . 1.00 . H32 0.7376 0.3173 0.5571 0.0747 Uiso calc . 1.00 . H33 0.6786 0.2449 0.5591 0.0747 Uiso calc . 1.00 . H34 0.8237 0.3405 0.2669 0.0757 Uiso calc . 1.00 . H35 0.8740 0.3447 0.2248 0.0757 Uiso calc . 1.00 . H36 0.8519 0.4357 0.2520 0.0757 Uiso calc . 1.00 . H37 0.8712 0.2490 0.1102 0.0782 Uiso calc . 1.00 . H38 0.8447 0.2457 0.0256 0.0782 Uiso calc . 1.00 . H39 0.8124 0.3222 0.0584 0.0782 Uiso calc . 1.00 . H40 0.8596 0.0672 0.2657 0.0770 Uiso calc . 1.00 . H41 0.8283 0.0841 0.1813 0.0770 Uiso calc . 1.00 . H42 0.8792 0.1592 0.2376 0.0770 Uiso calc . 1.00 . H43 1.0687 0.2272 0.6619 0.0452 Uiso calc . 1.00 . H44 1.0336 0.2668 0.5820 0.0452 Uiso calc . 1.00 . H45 0.9050 0.0565 0.5625 0.0482 Uiso calc . 1.00 . H46 0.9932 0.0818 0.5992 0.0482 Uiso calc . 1.00 . H47 0.8893 0.2944 0.4823 0.0426 Uiso calc . 1.00 . H48 0.8979 0.1876 0.4776 0.0426 Uiso calc . 1.00 . H49 0.5635 0.3125 0.1235 0.0590 Uiso calc . 1.00 . H50 0.6060 0.2453 0.1898 0.0590 Uiso calc . 1.00 . H51 0.5595 0.2693 -0.0121 0.0554 Uiso calc . 1.00 . H52 0.5957 0.3661 0.0180 0.0554 Uiso calc . 1.00 . H53 0.5676 0.1290 0.0847 0.0593 Uiso calc . 1.00 . H54 0.5999 0.1085 0.0284 0.0593 Uiso calc . 1.00 . 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 Rh1 0.0255(3) 0.0276(3) 0.0264(3) 0.0019(2) 0.0105(2) -0.0004(2) Rh2 0.0290(3) 0.0362(3) 0.0290(3) 0.0042(2) 0.0140(2) 0.0039(2) Cl1 0.075(2) 0.040(1) 0.051(1) 0.010(1) 0.031(1) 0.0092(9) Cl2 0.044(1) 0.042(1) 0.045(1) 0.0040(9) 0.0203(9) 0.0038(8) Cl3 0.0413(10) 0.057(1) 0.041(1) 0.0049(10) 0.0206(8) 0.0053(9) Cl4 0.044(1) 0.046(1) 0.044(1) 0.0006(9) 0.0206(9) -0.0102(9) Cl5 0.062(2) 0.071(2) 0.068(2) 0.002(1) 0.031(1) -0.019(1) Cl6 0.044(1) 0.089(2) 0.051(1) 0.002(1) 0.022(1) -0.011(1) S1 0.041(1) 0.0329(10) 0.050(1) 0.0036(8) 0.0168(9) -0.0008(9) S2 0.041(1) 0.049(1) 0.0285(9) 0.0051(9) 0.0129(8) 0.0000(8) S3 0.0292(9) 0.040(1) 0.040(1) -0.0023(8) 0.0140(8) -0.0007(8) S4 0.046(1) 0.046(1) 0.048(1) -0.0032(10) 0.0222(10) -0.0029(9) S5 0.055(1) 0.049(1) 0.052(1) 0.009(1) 0.034(1) 0.0060(10) S6 0.040(1) 0.058(1) 0.038(1) 0.0079(10) 0.0177(9) 0.0111(9) O1 0.081(5) 0.073(5) 0.077(5) 0.008(4) 0.004(4) -0.021(4) O2 0.094(5) 0.085(5) 0.039(3) 0.020(4) 0.024(3) 0.021(3) O3 0.129(6) 0.066(5) 0.160(7) 0.005(4) 0.106(6) 0.028(5) O4 0.112(6) 0.063(4) 0.085(5) 0.041(4) 0.060(4) 0.025(4) O5 0.065(4) 0.062(4) 0.099(5) -0.025(3) 0.037(4) -0.007(4) O6 0.069(4) 0.077(5) 0.064(4) 0.017(4) -0.011(3) -0.001(4) O7 0.071(4) 0.073(4) 0.090(5) 0.030(4) 0.031(4) -0.006(4) O8 0.151(7) 0.088(5) 0.075(5) -0.049(5) 0.085(5) -0.022(4) O9 0.097(5) 0.073(5) 0.084(5) -0.004(4) 0.036(4) -0.021(4) O10 0.069(4) 0.132(6) 0.076(4) 0.048(5) 0.018(4) 0.051(5) O11 0.057(4) 0.127(6) 0.076(4) 0.023(4) 0.037(4) -0.002(4) O12 0.124(6) 0.081(5) 0.125(6) -0.023(5) 0.081(5) 0.014(4) O13 0.113(6) 0.052(4) 0.107(5) -0.028(4) 0.073(5) -0.024(4) O14 0.060(4) 0.130(6) 0.064(4) 0.034(4) 0.016(3) -0.001(4) O15 0.070(4) 0.075(4) 0.106(5) -0.003(3) 0.052(4) -0.046(4) O16 0.102(5) 0.069(4) 0.047(4) -0.023(4) 0.027(4) -0.003(3) O17 0.102(6) 0.095(6) 0.183(8) -0.039(5) 0.082(6) -0.063(6) O18 0.24(1) 0.104(7) 0.068(5) -0.011(7) -0.032(6) -0.016(5) O19 0.120(7) 0.108(7) 0.28(1) 0.013(6) 0.117(8) -0.050(7) O20 0.163(9) 0.20(1) 0.172(9) -0.004(8) 0.127(8) -0.011(8) O21 0.29(1) 0.25(1) 0.35(2) -0.14(1) 0.28(1) -0.13(1) O22 0.080(6) 0.35(1) 0.140(7) -0.084(8) 0.061(5) -0.167(9) O23 0.24(1) 0.21(1) 0.180(10) 0.17(1) -0.070(9) -0.005(10) O24 0.176(8) 0.076(5) 0.186(8) -0.012(5) 0.150(7) -0.023(5) O25 0.058(4) 0.117(5) 0.050(3) 0.004(4) 0.033(3) 0.000(4) O26 0.057(4) 0.102(6) 0.123(6) -0.009(4) 0.010(4) -0.016(5) N1 0.030(3) 0.039(3) 0.042(3) -0.001(3) 0.016(3) -0.001(3) N2 0.037(3) 0.037(3) 0.041(4) 0.004(3) 0.012(3) -0.004(3) N3 0.035(3) 0.041(3) 0.028(3) -0.004(3) 0.011(2) 0.000(3) N4 0.039(4) 0.061(4) 0.048(4) 0.009(3) 0.020(3) 0.008(3) N5 0.046(4) 0.048(4) 0.040(4) 0.007(3) 0.016(3) 0.008(3) N6 0.051(4) 0.050(4) 0.043(4) -0.006(3) 0.018(3) 0.004(3) C1 0.046(5) 0.035(4) 0.073(6) -0.004(4) 0.024(4) 0.005(4) C2 0.047(5) 0.046(5) 0.070(6) -0.015(4) 0.029(5) -0.007(4) C3 0.066(6) 0.055(5) 0.077(6) -0.001(5) 0.036(5) -0.024(5) C4 0.045(5) 0.058(5) 0.038(4) 0.022(4) 0.011(4) 0.016(4) C5 0.057(5) 0.033(4) 0.052(5) 0.005(4) 0.020(4) 0.005(4) C6 0.065(6) 0.101(7) 0.049(5) 0.017(5) 0.039(5) 0.021(5) C7 0.041(4) 0.042(4) 0.041(4) -0.002(4) 0.010(4) -0.010(3) C8 0.035(4) 0.056(5) 0.029(4) -0.002(4) 0.002(3) 0.002(4) C9 0.038(4) 0.063(6) 0.086(6) -0.001(4) 0.028(4) -0.025(5) C10 0.053(5) 0.044(5) 0.060(5) 0.009(4) 0.024(4) -0.005(4) C11 0.073(6) 0.067(6) 0.051(5) 0.022(5) 0.034(5) -0.007(5) C12 0.036(5) 0.080(6) 0.055(5) -0.009(5) 0.004(4) -0.017(5) C13 0.072(6) 0.073(6) 0.032(4) 0.000(5) 0.027(4) 0.002(4) C14 0.067(6) 0.072(6) 0.036(4) 0.011(5) 0.026(4) 0.016(4) C15 0.065(6) 0.065(6) 0.089(6) 0.005(5) 0.055(5) 0.012(5) C16 0.055(5) 0.051(5) 0.061(6) 0.006(4) 0.026(5) 0.028(4) C17 0.064(6) 0.043(5) 0.057(5) 0.003(4) 0.025(5) 0.014(4) C18 0.050(5) 0.086(7) 0.063(6) 0.034(5) 0.032(5) 0.037(5) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.00003(1) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6702 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0487 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0347 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.572 _refine_ls_shift/esd_max 0.0149 _refine_ls_shift/esd_mean 0.0008 _refine_diff_density_min -0.55 _refine_diff_density_max 0.75 #------------------------------------------------------------------------------ _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 RH1 S1 2.326(2) 1_555 1_555 yes RH1 S2 2.338(2) 1_555 1_555 yes RH1 S3 2.317(2) 1_555 1_555 yes RH1 N1 2.116(5) 1_555 1_555 yes RH1 N2 2.112(6) 1_555 1_555 yes RH1 N3 2.113(5) 1_555 1_555 yes RH2 S4 2.309(2) 1_555 1_555 yes RH2 S5 2.322(2) 1_555 1_555 yes RH2 S6 2.339(2) 1_555 1_555 yes RH2 N4 2.104(6) 1_555 1_555 yes RH2 N5 2.101(5) 1_555 1_555 yes RH2 N6 2.115(6) 1_555 1_555 yes CL1 O1 1.408(6) 1_555 1_555 yes CL1 O2 1.427(5) 1_555 1_555 yes CL1 O3 1.433(6) 1_555 1_555 yes CL1 O4 1.441(6) 1_555 1_555 yes CL2 O5 1.426(5) 1_555 1_555 yes CL2 O6 1.411(5) 1_555 1_555 yes CL2 O7 1.431(6) 1_555 1_555 yes CL2 O8 1.384(5) 1_555 1_555 yes CL3 O9 1.420(6) 1_555 1_555 yes CL3 O10 1.399(5) 1_555 1_555 yes CL3 O11 1.420(6) 1_555 1_555 yes CL3 O12 1.407(6) 1_555 1_555 yes CL4 O13 1.426(6) 1_555 1_555 yes CL4 O14 1.401(6) 1_555 1_555 yes CL4 O15 1.421(5) 1_555 1_555 yes CL4 O16 1.426(6) 1_555 1_555 yes CL5 O17 1.401(7) 1_555 1_555 yes CL5 O18 1.346(7) 1_555 1_555 yes CL5 O19 1.388(8) 1_555 1_555 yes CL5 O20 1.369(8) 1_555 1_555 yes CL6 O21 1.359(10) 1_555 1_555 yes CL6 O22 1.338(7) 1_555 1_555 yes CL6 O23 1.243(8) 1_555 1_555 yes CL6 O24 1.380(6) 1_555 1_555 yes S1 C1 1.820(8) 1_555 1_555 yes S1 C3 1.798(8) 1_555 1_555 yes S2 C4 1.815(8) 1_555 1_555 yes S2 C6 1.799(8) 1_555 1_555 yes S3 C7 1.809(7) 1_555 1_555 yes S3 C9 1.788(8) 1_555 1_555 yes S4 C10 1.807(8) 1_555 1_555 yes S4 C12 1.826(8) 1_555 1_555 yes S5 C13 1.806(8) 1_555 1_555 yes S5 C15 1.800(8) 1_555 1_555 yes S6 C16 1.822(8) 1_555 1_555 yes S6 C18 1.804(8) 1_555 1_555 yes N1 C2 1.486(9) 1_555 1_555 yes N2 C5 1.480(8) 1_555 1_555 yes N3 C8 1.499(8) 1_555 1_555 yes N4 C11 1.501(10) 1_555 1_555 yes N5 C14 1.501(9) 1_555 1_555 yes N6 C17 1.486(9) 1_555 1_555 yes C1 C2 1.49(1) 1_555 1_555 yes C4 C5 1.495(10) 1_555 1_555 yes C7 C8 1.495(10) 1_555 1_555 yes C10 C11 1.52(1) 1_555 1_555 yes C13 C14 1.48(1) 1_555 1_555 yes C16 C17 1.48(1) 1_555 1_555 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 RH1 S2 98.27(7) 1_555 1_555 1_555 yes S1 RH1 S3 96.80(7) 1_555 1_555 1_555 yes S1 RH1 N1 85.1(2) 1_555 1_555 1_555 yes S1 RH1 N2 175.2(2) 1_555 1_555 1_555 yes S1 RH1 N3 87.1(2) 1_555 1_555 1_555 yes S2 RH1 S3 95.40(7) 1_555 1_555 1_555 yes S2 RH1 N1 87.2(1) 1_555 1_555 1_555 yes S2 RH1 N2 84.9(2) 1_555 1_555 1_555 yes S2 RH1 N3 174.4(2) 1_555 1_555 1_555 yes S3 RH1 N1 176.5(2) 1_555 1_555 1_555 yes S3 RH1 N2 86.4(2) 1_555 1_555 1_555 yes S3 RH1 N3 85.3(1) 1_555 1_555 1_555 yes N1 RH1 N2 91.5(2) 1_555 1_555 1_555 yes N1 RH1 N3 91.8(2) 1_555 1_555 1_555 yes N2 RH1 N3 89.7(2) 1_555 1_555 1_555 yes S4 RH2 S5 96.85(8) 1_555 1_555 1_555 yes S4 RH2 S6 97.88(7) 1_555 1_555 1_555 yes S4 RH2 N4 86.0(2) 1_555 1_555 1_555 yes S4 RH2 N5 87.5(2) 1_555 1_555 1_555 yes S4 RH2 N6 175.5(2) 1_555 1_555 1_555 yes S5 RH2 S6 96.48(7) 1_555 1_555 1_555 yes S5 RH2 N4 176.0(2) 1_555 1_555 1_555 yes S5 RH2 N5 85.3(2) 1_555 1_555 1_555 yes S5 RH2 N6 86.2(2) 1_555 1_555 1_555 yes S6 RH2 N4 85.9(2) 1_555 1_555 1_555 yes S6 RH2 N5 174.1(2) 1_555 1_555 1_555 yes S6 RH2 N6 85.1(2) 1_555 1_555 1_555 yes N4 RH2 N5 92.0(2) 1_555 1_555 1_555 yes N4 RH2 N6 90.9(2) 1_555 1_555 1_555 yes N5 RH2 N6 89.4(2) 1_555 1_555 1_555 yes O1 CL1 O2 109.5(4) 1_555 1_555 1_555 yes O1 CL1 O3 108.7(4) 1_555 1_555 1_555 yes O1 CL1 O4 108.6(4) 1_555 1_555 1_555 yes O2 CL1 O3 110.4(4) 1_555 1_555 1_555 yes O2 CL1 O4 109.8(4) 1_555 1_555 1_555 yes O3 CL1 O4 109.7(4) 1_555 1_555 1_555 yes O5 CL2 O6 109.9(4) 1_555 1_555 1_555 yes O5 CL2 O7 109.9(4) 1_555 1_555 1_555 yes O5 CL2 O8 108.7(4) 1_555 1_555 1_555 yes O6 CL2 O7 107.4(4) 1_555 1_555 1_555 yes O6 CL2 O8 111.2(4) 1_555 1_555 1_555 yes O7 CL2 O8 109.7(4) 1_555 1_555 1_555 yes O9 CL3 O10 110.0(4) 1_555 1_555 1_555 yes O9 CL3 O11 108.7(4) 1_555 1_555 1_555 yes O9 CL3 O12 107.9(4) 1_555 1_555 1_555 yes O10 CL3 O11 109.4(4) 1_555 1_555 1_555 yes O10 CL3 O12 111.8(4) 1_555 1_555 1_555 yes O11 CL3 O12 109.0(4) 1_555 1_555 1_555 yes O13 CL4 O14 110.4(4) 1_555 1_555 1_555 yes O13 CL4 O15 110.2(4) 1_555 1_555 1_555 yes O13 CL4 O16 108.3(4) 1_555 1_555 1_555 yes O14 CL4 O15 108.7(4) 1_555 1_555 1_555 yes O14 CL4 O16 109.4(4) 1_555 1_555 1_555 yes O15 CL4 O16 109.8(4) 1_555 1_555 1_555 yes O17 CL5 O18 112.8(6) 1_555 1_555 1_555 yes O17 CL5 O19 112.3(5) 1_555 1_555 1_555 yes O17 CL5 O20 109.4(5) 1_555 1_555 1_555 yes O18 CL5 O19 109.2(6) 1_555 1_555 1_555 yes O18 CL5 O20 105.1(6) 1_555 1_555 1_555 yes O19 CL5 O20 107.7(6) 1_555 1_555 1_555 yes O21 CL6 O22 108.9(6) 1_555 1_555 1_555 yes O21 CL6 O23 104.1(8) 1_555 1_555 1_555 yes O21 CL6 O24 108.4(6) 1_555 1_555 1_555 yes O22 CL6 O23 110.2(7) 1_555 1_555 1_555 yes O22 CL6 O24 112.8(5) 1_555 1_555 1_555 yes O23 CL6 O24 112.0(7) 1_555 1_555 1_555 yes RH1 S1 C1 98.4(2) 1_555 1_555 1_555 yes RH1 S1 C3 112.1(3) 1_555 1_555 1_555 yes C1 S1 C3 101.2(4) 1_555 1_555 1_555 yes RH1 S2 C4 97.5(2) 1_555 1_555 1_555 yes RH1 S2 C6 111.5(3) 1_555 1_555 1_555 yes C4 S2 C6 100.8(4) 1_555 1_555 1_555 yes RH1 S3 C7 98.3(2) 1_555 1_555 1_555 yes RH1 S3 C9 112.4(3) 1_555 1_555 1_555 yes C7 S3 C9 101.1(4) 1_555 1_555 1_555 yes RH2 S4 C10 97.9(3) 1_555 1_555 1_555 yes RH2 S4 C12 110.9(3) 1_555 1_555 1_555 yes C10 S4 C12 102.1(4) 1_555 1_555 1_555 yes RH2 S5 C13 97.6(3) 1_555 1_555 1_555 yes RH2 S5 C15 110.9(3) 1_555 1_555 1_555 yes C13 S5 C15 100.7(4) 1_555 1_555 1_555 yes RH2 S6 C16 96.9(2) 1_555 1_555 1_555 yes RH2 S6 C18 111.8(3) 1_555 1_555 1_555 yes C16 S6 C18 100.2(4) 1_555 1_555 1_555 yes RH1 N1 C2 112.0(4) 1_555 1_555 1_555 yes RH1 N1 H43 108.8(4) 1_555 1_555 1_555 no RH1 N1 H44 108.8(4) 1_555 1_555 1_555 no C2 N1 H43 108.8(5) 1_555 1_555 1_555 no C2 N1 H44 108.8(6) 1_555 1_555 1_555 no H43 N1 H44 109.5(5) 1_555 1_555 1_555 no RH1 N2 C5 113.4(4) 1_555 1_555 1_555 yes RH1 N2 H45 108.5(4) 1_555 1_555 1_555 no RH1 N2 H46 108.5(4) 1_555 1_555 1_555 no C5 N2 H45 108.5(6) 1_555 1_555 1_555 no C5 N2 H46 108.5(5) 1_555 1_555 1_555 no H45 N2 H46 109.5(5) 1_555 1_555 1_555 no RH1 N3 C8 114.0(4) 1_555 1_555 1_555 yes RH1 N3 H47 108.3(4) 1_555 1_555 1_555 no RH1 N3 H48 108.3(4) 1_555 1_555 1_555 no C8 N3 H47 108.3(5) 1_555 1_555 1_555 no C8 N3 H48 108.3(5) 1_555 1_555 1_555 no H47 N3 H48 109.5(5) 1_555 1_555 1_555 no RH2 N4 C11 112.8(5) 1_555 1_555 1_555 yes RH2 N4 H49 108.6(4) 1_555 1_555 1_555 no RH2 N4 H50 108.6(4) 1_555 1_555 1_555 no C11 N4 H49 108.6(6) 1_555 1_555 1_555 no C11 N4 H50 108.6(6) 1_555 1_555 1_555 no H49 N4 H50 109.5(6) 1_555 1_555 1_555 no RH2 N5 C14 112.8(4) 1_555 1_555 1_555 yes RH2 N5 H51 108.6(4) 1_555 1_555 1_555 no RH2 N5 H52 108.6(4) 1_555 1_555 1_555 no C14 N5 H51 108.6(6) 1_555 1_555 1_555 no C14 N5 H52 108.6(6) 1_555 1_555 1_555 no H51 N5 H52 109.5(6) 1_555 1_555 1_555 no RH2 N6 C17 111.9(5) 1_555 1_555 1_555 yes RH2 N6 H53 108.9(5) 1_555 1_555 1_555 no RH2 N6 H54 108.9(4) 1_555 1_555 1_555 no C17 N6 H53 108.9(6) 1_555 1_555 1_555 no C17 N6 H54 108.9(6) 1_555 1_555 1_555 no H53 N6 H54 109.5(6) 1_555 1_555 1_555 no S1 C1 C2 110.2(5) 1_555 1_555 1_555 yes S1 C1 H1 109.3(6) 1_555 1_555 1_555 no S1 C1 H2 109.3(6) 1_555 1_555 1_555 no C2 C1 H1 109.3(7) 1_555 1_555 1_555 no C2 C1 H2 109.3(7) 1_555 1_555 1_555 no H1 C1 H2 109.5(7) 1_555 1_555 1_555 no N1 C2 C1 109.8(6) 1_555 1_555 1_555 yes N1 C2 H3 109.4(7) 1_555 1_555 1_555 no N1 C2 H4 109.4(7) 1_555 1_555 1_555 no C1 C2 H3 109.4(7) 1_555 1_555 1_555 no C1 C2 H4 109.4(7) 1_555 1_555 1_555 no H3 C2 H4 109.5(7) 1_555 1_555 1_555 no S1 C3 H25 109.5(6) 1_555 1_555 1_555 no S1 C3 H26 109.5(7) 1_555 1_555 1_555 no S1 C3 H27 109.5(6) 1_555 1_555 1_555 no H25 C3 H26 109.5(8) 1_555 1_555 1_555 no H25 C3 H27 109.5(9) 1_555 1_555 1_555 no H26 C3 H27 109.5(8) 1_555 1_555 1_555 no S2 C4 C5 111.3(5) 1_555 1_555 1_555 yes S2 C4 H5 109.0(6) 1_555 1_555 1_555 no S2 C4 H6 109.0(6) 1_555 1_555 1_555 no C5 C4 H5 109.0(7) 1_555 1_555 1_555 no C5 C4 H6 109.0(7) 1_555 1_555 1_555 no H5 C4 H6 109.5(7) 1_555 1_555 1_555 no N2 C5 C4 109.0(6) 1_555 1_555 1_555 yes N2 C5 H7 109.6(6) 1_555 1_555 1_555 no N2 C5 H8 109.6(7) 1_555 1_555 1_555 no C4 C5 H7 109.6(7) 1_555 1_555 1_555 no C4 C5 H8 109.6(7) 1_555 1_555 1_555 no H7 C5 H8 109.5(7) 1_555 1_555 1_555 no S2 C6 H28 109.5(7) 1_555 1_555 1_555 no S2 C6 H29 109.5(6) 1_555 1_555 1_555 no S2 C6 H30 109.5(6) 1_555 1_555 1_555 no H28 C6 H29 109.5(8) 1_555 1_555 1_555 no H28 C6 H30 109.5(8) 1_555 1_555 1_555 no H29 C6 H30 109.5(9) 1_555 1_555 1_555 no S3 C7 C8 111.0(5) 1_555 1_555 1_555 yes S3 C7 H9 109.1(5) 1_555 1_555 1_555 no S3 C7 H10 109.1(6) 1_555 1_555 1_555 no C8 C7 H9 109.1(7) 1_555 1_555 1_555 no C8 C7 H10 109.1(6) 1_555 1_555 1_555 no H9 C7 H10 109.5(7) 1_555 1_555 1_555 no N3 C8 C7 110.7(5) 1_555 1_555 1_555 yes N3 C8 H11 109.2(6) 1_555 1_555 1_555 no N3 C8 H12 109.2(6) 1_555 1_555 1_555 no C7 C8 H11 109.2(7) 1_555 1_555 1_555 no C7 C8 H12 109.2(7) 1_555 1_555 1_555 no H11 C8 H12 109.5(6) 1_555 1_555 1_555 no S3 C9 H31 109.5(6) 1_555 1_555 1_555 no S3 C9 H32 109.5(6) 1_555 1_555 1_555 no S3 C9 H33 109.5(6) 1_555 1_555 1_555 no H31 C9 H32 109.5(8) 1_555 1_555 1_555 no H31 C9 H33 109.5(8) 1_555 1_555 1_555 no H32 C9 H33 109.5(8) 1_555 1_555 1_555 no S4 C10 C11 110.3(5) 1_555 1_555 1_555 yes S4 C10 H13 109.3(6) 1_555 1_555 1_555 no S4 C10 H14 109.3(6) 1_555 1_555 1_555 no C11 C10 H13 109.3(7) 1_555 1_555 1_555 no C11 C10 H14 109.3(7) 1_555 1_555 1_555 no H13 C10 H14 109.5(7) 1_555 1_555 1_555 no N4 C11 C10 108.5(6) 1_555 1_555 1_555 yes N4 C11 H15 109.7(8) 1_555 1_555 1_555 no N4 C11 H16 109.7(7) 1_555 1_555 1_555 no C10 C11 H15 109.7(8) 1_555 1_555 1_555 no C10 C11 H16 109.7(8) 1_555 1_555 1_555 no H15 C11 H16 109.5(8) 1_555 1_555 1_555 no S4 C12 H34 109.5(6) 1_555 1_555 1_555 no S4 C12 H35 109.5(6) 1_555 1_555 1_555 no S4 C12 H36 109.5(7) 1_555 1_555 1_555 no H34 C12 H35 109.5(9) 1_555 1_555 1_555 no H34 C12 H36 109.5(8) 1_555 1_555 1_555 no H35 C12 H36 109.5(8) 1_555 1_555 1_555 no S5 C13 C14 110.9(6) 1_555 1_555 1_555 yes S5 C13 H17 109.1(6) 1_555 1_555 1_555 no S5 C13 H18 109.1(6) 1_555 1_555 1_555 no C14 C13 H17 109.1(7) 1_555 1_555 1_555 no C14 C13 H18 109.1(8) 1_555 1_555 1_555 no H17 C13 H18 109.5(7) 1_555 1_555 1_555 no N5 C14 C13 109.6(6) 1_555 1_555 1_555 yes N5 C14 H19 109.5(7) 1_555 1_555 1_555 no N5 C14 H20 109.5(7) 1_555 1_555 1_555 no C13 C14 H19 109.5(8) 1_555 1_555 1_555 no C13 C14 H20 109.4(8) 1_555 1_555 1_555 no H19 C14 H20 109.5(8) 1_555 1_555 1_555 no S5 C15 H37 109.5(6) 1_555 1_555 1_555 no S5 C15 H38 109.5(7) 1_555 1_555 1_555 no S5 C15 H39 109.5(6) 1_555 1_555 1_555 no H37 C15 H38 109.5(8) 1_555 1_555 1_555 no H37 C15 H39 109.5(9) 1_555 1_555 1_555 no H38 C15 H39 109.5(8) 1_555 1_555 1_555 no S6 C16 C17 111.1(5) 1_555 1_555 1_555 yes S6 C16 H21 109.1(6) 1_555 1_555 1_555 no S6 C16 H22 109.1(6) 1_555 1_555 1_555 no C17 C16 H21 109.1(8) 1_555 1_555 1_555 no C17 C16 H22 109.1(7) 1_555 1_555 1_555 no H21 C16 H22 109.5(7) 1_555 1_555 1_555 no N6 C17 C16 108.7(6) 1_555 1_555 1_555 yes N6 C17 H23 109.7(7) 1_555 1_555 1_555 no N6 C17 H24 109.7(7) 1_555 1_555 1_555 no C16 C17 H23 109.7(7) 1_555 1_555 1_555 no C16 C17 H24 109.7(7) 1_555 1_555 1_555 no H23 C17 H24 109.5(8) 1_555 1_555 1_555 no S6 C18 H40 109.5(6) 1_555 1_555 1_555 no S6 C18 H41 109.5(6) 1_555 1_555 1_555 no S6 C18 H42 109.5(7) 1_555 1_555 1_555 no H40 C18 H41 109.5(9) 1_555 1_555 1_555 no H40 C18 H42 109.5(8) 1_555 1_555 1_555 no H41 C18 H42 109.5(8) 1_555 1_555 1_555 no #------------------------------------------------------------------------------