# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1735 data_General _audit_creation_date 'Sat Oct 30 10:41:16 1999' _audit_creation_method 'by teXsan' _audit_update_record ? #----------------------------------------------------------------------- # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #----------------------------------------------------------------------- # SUBMISSION DETAILS _publ_contact_author_name ' Yugen Zhang' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' zhangyg@ustc.edu.cn ' _publ_contact_author_fax ' 86-551-3631760 ' _publ_contact_author_phone ' 86-551-3603018 ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' J. of Chem. Soc., Dalton Trans.' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #----------------------------------------------------------------------- # TITLE AND AUTHOR LIST _publ_section_title ; Thermodynamically controlled products: novel motif of metallohelicates stabilized by inter- and intra-helix hydrogen bonds ; _publ_section_title_footnote ; ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' Yugen Zhang ' ; ; ; Dept. of Chem., Univ. of Sci. & Tech. of China, Hefei, Anhui 230026, PRC ; _publ_section_synopsis ; ENTER SYNOPSIS ; #----------------------------------------------------------------------- # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES 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. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #----------------------------------------------------------------------- data_I _audit_creation_method Sir _chemical_name_systematic ; [Zn(maleic)(thiourea)(H2O)]2.4H2O ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum ' C5 H12 Zn N2 O7 S ' _chemical_formula_weight 309.60 _chemical_melting_point ? _chemical_compound_source ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P-1(No.2) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.087(9) _cell_length_b 9.859(10) _cell_length_c 6.87(1) _cell_angle_alpha 108.65(8) _cell_angle_beta 96.21(5) _cell_angle_gamma 97.77(9) _cell_volume 570(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.802 _exptl_crystal_density_method ? _exptl_crystal_F_000 316.00 _exptl_absorpt_coefficient_mu 2.357 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; A single crystal was set up on a R-AXISII diffractometer with graphite monocromated Mo-Ka radiation. The data were collected to a maximun 2q value of 50.3 o. A laser-stimulated fluorescence image plate was used as a two-dimensional area detector. The structure was solved by Patterson methods using the SAPI and refined by full-matrix least squares. ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku RAXIS-II' _diffrn_measurement_method 'image plate' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 4 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1841 _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_reflns_theta_min 4.0 _diffrn_reflns_theta_max 25 _reflns_number_total 1841 _reflns_number_observed 1741 _reflns_observed_criterion >3sigma(I) _computing_data_collection '' _computing_cell_refinement '' _computing_data_reduction 'teXsan' _computing_structure_solution 'SAPI' _computing_structure_refinement 'teXsan' _computing_molecular_graphics 'ORTEPII' _computing_publication_material 'WORD96' _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/\s^2^(Fo)=1/\[sc^2^(Fo)+(p^2^/4)Fo^2^] where p=0.0700' _atom_sites_solution_primary 'Patterson (SAPI)' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method noref _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 1741 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.072 _refine_ls_wR_factor_ref 0.119 _refine_ls_goodness_of_fit_ref 2.95 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.00 _refine_ls_shift/esd_mean ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn(1) Zn 0.31123(7) 0.23485(6) 0.24432(9) 2.74(2) Uani 1 d . . S(1) S 0.1309(2) 0.0895(2) 0.3328(3) 3.24(4) Uani 1 d . . O(1) O 0.2496(5) 0.4254(5) 0.2439(6) 3.24(9) Uani 1 d . . O(2) O 0.2386(5) 0.4336(5) 0.5702(7) 3.25(9) Uani 1 d . . O(3) O 0.4802(5) 0.7046(5) 0.6107(7) 3.31(9) Uani 1 d . . O(4) O 0.4503(5) 0.9338(4) 0.7622(7) 3.51(9) Uani 1 d . . O(5) O 0.3153(5) 0.1613(4) -0.0667(6) 3.00(9) Uani 1 d . . O(6) O 0.4812(7) 0.3640(7) 0.8360(8) 5.8(1) Uani 1 d . . O(7) O 0.8334(9) 0.4412(6) 0.0491(8) 5.8(2) Uani 1 d . . N(1) N 0.2677(6) -0.1282(6) 0.1338(9) 3.4(1) Uani 1 d . . N(2) N 0.0168(6) -0.1900(6) 0.1417(8) 3.2(1) Uani 1 d . . C(1) C 0.2253(7) 0.4893(6) 0.4292(9) 2.9(1) Uani 1 d . . C(2) C 0.1621(7) 0.6267(6) 0.4678(9) 2.8(1) Uani 1 d . . C(3) C 0.3989(7) 0.8040(6) 0.6516(9) 2.9(1) Uani 1 d . . C(4) C 0.2359(7) 0.7620(7) 0.5662(9) 2.9(1) Uani 1 d . . C(5) C 0.1417(6) -0.0896(6) 0.1901(9) 2.7(1) Uani 1 d . . H(1) H 0.3422 0.0686 -0.1297 3.5587 Uiso 1 calc R . H(2) H 0.2930 0.2191 -0.1484 3.5587 Uiso 1 calc R . H(3) H 0.3583 -0.0596 0.1691 3.7930 Uiso 1 calc R . H(4) H 0.2706 -0.2297 0.0648 3.7930 Uiso 1 calc R . H(5) H -0.0765 -0.1640 0.1781 3.7666 Uiso 1 calc R . H(6) H 0.0184 -0.2912 0.0694 3.7666 Uiso 1 calc R . H(7) H 0.0560 0.6174 0.4164 3.0833 Uiso 1 calc R . H(8) H 0.1786 0.8393 0.5815 3.5024 Uiso 1 calc R . 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 Zn(1) 0.0371(6) 0.0311(6) 0.0335(6) 0.0075(4) 0.0050(4) 0.0073(4) S(1) 0.045(1) 0.0343(9) 0.0446(10) 0.0102(3) 0.0162(7) 0.0106(7) O(1) 0.055(3) 0.036(2) 0.028(2) 0.009(2) 0.009(2) 0.005(2) O(2) 0.054(3) 0.035(2) 0.034(2) 0.010(2) 0.009(2) 0.010(2) O(3) 0.038(2) 0.039(2) 0.040(2) 0.013(2) 0.001(2) 0.002(2) O(4) 0.047(3) 0.035(2) 0.043(2) 0.010(2) 0.011(2) 0.001(2) O(5) 0.045(2) 0.034(2) 0.032(2) 0.012(2) 0.007(2) 0.006(2) O(6) 0.075(4) 0.083(4) 0.043(3) -0.031(3) 0.013(3) 0.010(2) O(7) 0.134(6) 0.055(3) 0.040(3) 0.042(3) 0.020(3) 0.013(2) N(1) 0.037(3) 0.037(3) 0.052(3) 0.009(2) 0.010(2) 0.010(2) N(2) 0.035(3) 0.039(3) 0.042(3) 0.004(2) 0.003(2) 0.009(2) C(1) 0.036(3) 0.030(3) 0.036(3) 0.001(2) 0.011(2) 0.002(2) C(2) 0.038(3) 0.036(3) 0.033(3) 0.007(2) 0.007(2) 0.010(2) C(3) 0.039(3) 0.035(3) 0.030(3) 0.010(2) 0.012(2) 0.003(2) C(4) 0.036(3) 0.040(3) 0.034(3) 0.011(3) 0.009(2) 0.010(3) C(5) 0.034(3) 0.035(3) 0.035(3) 0.008(2) 0.003(2) 0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Zn(1) O(3) 1.961(5) Zn(1) O(1) 2.033(4) Zn(1) O(5) 2.032(4) Zn(1) S(1) 2.291(2) S(1) C(5) 1.746(6) O(1) C(1) 1.286(7) O(2) C(1) 1.261(7) O(3) C(3) 1.285(7) O(4) C(3) 1.254(7) N(1) C(5) 1.313(8) N(2) C(5) 1.336(7) C(1) C(2) 1.500(8) C(4) C(2) 1.330(8) C(3) C(4) 1.484(9) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O(1) Zn(1) S(1) 112.7(1) O(3) Zn(1) S(1) 123.2(1) O(5) Zn(1) S(1) 111.4(1) O(3) Zn(1) O(1) 103.3(2) O(1) Zn(1) O(5) 94.0(2) O(3) Zn(1) O(5) 108.1(2) C(5) S(1) Zn(1) 106.1(2) C(1) O(1) Zn(1) 106.0(4) C(3) O(3) Zn(1) 115.1(4) N(1) C(5) N(2) 119.7(5) N(1) C(5) S(1) 122.5(4) N(2) C(5) S(1) 117.8(4) O(1) C(1) O(2) 122.5(5) O(1) C(1) C(2) 117.4(5) O(2) C(1) C(2) 119.7(5) C(1) C(2) C(4) 127.0(6) C(2) C(4) C(3) 125.5(6) O(3) C(3) O(4) 123.2(6) O(3) C(3) C(4) 118.1(5) O(4) C(3) C(4) 118.7(5) _refine_diff_density_max 0.72 _refine_diff_density_min -1.49 _refine_diff_density_rms ? #================================================END #CRYSDATA of complex (II) data_II _audit_creation_method Sir _chemical_name_systematic ; [Zn(maleic)(thiourea)2]n ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum ' C6 H10 Zn N4 O4 S2 ' _chemical_formula_weight 331.67 _chemical_melting_point ? _chemical_compound_source ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca(No.61) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '1/2+x, 1/2-y, -z' '-x, 1/2+y, 1/2-z' '1/2-x, -y, 1/2+z' '-x, -y, -z' '1/2-x, 1/2+y, z' 'x, 1/2-y, 1/2+z' '1/2+x, y, 1/2-z' _cell_length_a 14.48(1) _cell_length_b 15.64(1) _cell_length_c 10.957(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2481(1) _cell_formula_units_Z 8 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method ? _exptl_crystal_F_000 1344.00 _exptl_absorpt_coefficient_mu 2.324 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; A single crystal was set up on a R-AXISII diffractometer with graphite monocromated Mo-Ka radiation. The data were collected to a maximun 2q value of 50.3 o. A laser-stimulated fluorescence image plate was used as a two-dimensional area detector. The structure was solved by Direct Methods(SIR92) and expanded using Fourier techniques. ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku RAXIS-II' _diffrn_measurement_method 'image plate' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 4 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2272 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_reflns_theta_min 4.0 _diffrn_reflns_theta_max 25 _reflns_number_total 2272 _reflns_number_observed 2101 _reflns_observed_criterion >3sigma(I) _computing_data_collection '' _computing_cell_refinement '' _computing_data_reduction 'teXsan' _computing_structure_solution 'Sir92' _computing_structure_refinement 'teXsan' _computing_molecular_graphics 'ORTEPII' _computing_publication_material 'WORD96' _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/\s^2^(Fo)=1/\[sc^2^(Fo)+(p^2^/4)Fo^2^] where p=0.0800' _atom_sites_solution_primary 'Direct Methods (SIR92)' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method noref _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 2101 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.052 _refine_ls_wR_factor_ref 0.079 _refine_ls_goodness_of_fit_ref 1.48 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/esd_max 0.01 _refine_ls_shift/esd_mean ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn(1) Zn 0.35013(3) 0.12902(3) 0.89679(4) 2.77(2) Uani 1 d . . S(1) S 0.32254(8) 0.23467(6) 0.75384(8) 2.97(2) Uani 1 d . . S(2) S 0.47834(7) 0.15848(7) 1.02450(8) 2.96(2) Uani 1 d . . O(1) O 0.3849(2) 0.0193(2) 0.8257(2) 3.12(6) Uani 1 d . . O(2) O 0.3226(2) 0.0448(2) 0.6425(2) 2.96(5) Uani 1 d . . O(3) O 0.3431(2) -0.0694(2) 0.3763(3) 3.14(6) Uani 1 d . . O(4) O 0.2473(2) -0.1175(2) 0.5210(2) 3.26(6) Uani 1 d . . N(1) N 0.3494(3) 0.3374(2) 0.9481(3) 3.25(7) Uani 1 d . . N(2) N 0.3074(3) 0.4018(2) 0.7692(3) 3.25(7) Uani 1 d . . N(3) N 0.5603(3) 0.1659(3) 0.8062(3) 3.74(8) Uani 1 d . . N(4) N 0.6337(2) 0.0864(3) 0.9524(3) 3.36(7) Uani 1 d . . C(1) C 0.3743(3) 0.0032(2) 0.7113(3) 2.85(8) Uani 1 d . . C(2) C 0.4279(3) -0.0719(3) 0.6653(3) 3.35(8) Uani 1 d . . C(3) C 0.4076(3) -0.1137(3) 0.5642(3) 3.16(8) Uani 1 d . . C(4) C 0.3274(3) -0.0965(2) 0.4822(3) 2.73(8) Uani 1 d . . C(5) C 0.3271(3) 0.3314(3) 0.8306(3) 2.59(8) Uani 1 d . . C(6) C 0.5639(3) 0.1345(3) 0.9185(4) 3.00(9) Uani 1 d . . H(1) H 0.3646 0.2896 0.9952 3.9473 Uiso 1 calc R . H(2) H 0.3524 0.3940 0.9868 3.9473 Uiso 1 calc R . H(3) H 0.3095 0.4573 0.8074 3.5755 Uiso 1 calc R . H(4) H 0.2903 0.3991 0.6849 3.5755 Uiso 1 calc R . H(5) H 0.5095 0.2012 0.7828 4.1039 Uiso 1 calc R . H(6) H 0.6065 0.1518 0.7490 4.1039 Uiso 1 calc R . H(7) H 0.6378 0.0638 1.0314 3.8059 Uiso 1 calc R . H(8) H 0.6813 0.0719 0.8931 3.8059 Uiso 1 calc R . H(9) H 0.4806 -0.0887 0.7105 3.5071 Uiso 1 calc R . H(10) H 0.4465 -0.1630 0.5476 3.5408 Uiso 1 calc R . 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 Zn(1) 0.0454(4) 0.0297(4) 0.0301(4) 0.0007(2) -0.0008(2) 0.0001(2) S(1) 0.0551(6) 0.0290(6) 0.0286(5) 0.0004(4) -0.0026(4) -0.0012(4) S(2) 0.0402(6) 0.0418(6) 0.0307(5) 0.0042(4) 0.0003(4) -0.0020(4) O(1) 0.059(2) 0.033(1) 0.027(1) 0.004(1) -0.003(1) -0.004(1) O(2) 0.045(1) 0.034(1) 0.033(1) 0.001(1) -0.002(1) 0.002(1) O(3) 0.050(2) 0.035(2) 0.034(1) 0.002(1) 0.005(1) 0.003(1) O(4) 0.048(2) 0.044(2) 0.032(1) -0.007(1) 0.002(1) -0.001(1) N(1) 0.071(3) 0.032(2) 0.029(2) 0.005(2) -0.009(2) 0.000(1) N(2) 0.059(2) 0.030(2) 0.034(2) 0.002(2) -0.004(2) -0.001(1) N(3) 0.052(2) 0.054(2) 0.037(2) 0.010(2) 0.010(2) 0.004(2) N(4) 0.042(2) 0.046(2) 0.039(2) 0.006(2) 0.002(1) 0.003(2) C(1) 0.042(2) 0.031(2) 0.035(2) -0.003(2) -0.001(2) 0.000(2) C(2) 0.047(2) 0.042(2) 0.038(2) 0.009(2) -0.006(2) -0.001(2) C(3) 0.048(2) 0.041(2) 0.032(2) 0.005(2) -0.002(2) -0.003(2) C(4) 0.049(2) 0.024(2) 0.031(2) 0.007(2) -0.003(2) -0.006(2) C(5) 0.038(2) 0.030(2) 0.031(2) -0.002(2) 0.001(1) 0.001(2) C(6) 0.047(2) 0.034(2) 0.033(2) 0.000(2) 0.004(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Zn(1) O(4) 1.968(3) Zn(1) O(1) 1.951(3) Zn(1) S(2) 2.370(2) Zn(1) S(1) 2.312(2) S(1) C(5) 1.732(4) S(2) C(6) 1.739(4) O(1) C(1) 1.288(4) O(2) C(1) 1.246(5) O(3) C(4) 1.256(5) O(4) C(4) 1.278(5) N(1) C(5) 1.330(5) N(2) C(5) 1.321(5) N(3) C(6) 1.326(5) N(4) C(6) 1.315(6) C(1) C(2) 1.496(6) C(3) C(2) 1.319(6) C(3) C(4) 1.493(5) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle S(1) Zn(1) S(2) 113.35(4) O(1) Zn(1) S(1) 113.77(8) O(4) Zn(1) S(1) 114.22(9) S(2) Zn(1) O(1) 101.79(9) S(2) Zn(1) O(4) 99.85(9) O(1) Zn(1) O(4) 112.4(1) C(5) S(1) Zn(1) 106.8(1) C(6) S(2) Zn(1) 97.0(2) C(1) O(1) Zn(1) 122.0(2) C(4) O(4) Zn(1) 116.4(2) N(1) C(5) N(2) 119.1(4) N(1) C(5) S(1) 122.7(3) N(2) C(5) S(1) 118.2(3) N(3) C(6) S(2) 120.8(3) N(4) C(6) S(2) 118.9(3) N(3) C(6) N(4) 120.2(4) O(1) C(1) O(2) 124.0(4) O(1) C(1) C(2) 114.8(3) O(2) C(1) C(2) 121.2(3) C(1) C(2) C(3) 123.9(4) C(2) C(3) C(4) 126.0(4) O(3) C(4) O(4) 123.9(4) O(3) C(4) C(3) 118.4(4) O(4) C(4) C(3) 117.4(3) _refine_diff_density_max 0.60 _refine_diff_density_min -1.17 _refine_diff_density_rms ? #================================================END data_Z903 #----------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C10 H16 Cd N4 O10 S2 ' _chemical_formula_moiety 'C10 H16 Cd N4 O10 S2 ' _chemical_formula_weight 528.79 _chemical_melting_point ? #----------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 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 _cell_length_a 5.804(2) _cell_length_b 24.97(2) _cell_length_c 6.190(5) _cell_angle_alpha 90 _cell_angle_beta 92.90(6) _cell_angle_gamma 90 _cell_volume 895(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 173.2 #----------------------------------------------------------------------- _exptl_crystal_description 'prism' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.513 _exptl_absorpt_correction_type none #----------------------------------------------------------------------- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type ? _diffrn_reflns_number 1401 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25.07 _diffrn_measured_fraction_theta_max 0.8759 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.8759 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 #----------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1391 _reflns_number_gt 1365 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.0995 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1365 _refine_ls_number_parameters 124 _refine_ls_goodness_of_fit_ref 1.788 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00203|Fo|^2^]' _refine_ls_shift/su_max 0.0021 _refine_diff_density_max 0.70 _refine_diff_density_min -1.43 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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) ; '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) ; 'N' 'N' 0.006 0.003 ;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) ; 'Cd' 'Cd' -0.807 1.202 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Cd(1) Cd 0.0000 0.0000 0.0000 0.0393(3) Uani 1.00 d S . . S(1) S 0.2119(3) 0.06925(6) 0.2576(3) 0.0408(5) Uani 1.00 d . . . O(1) O -0.2987(8) 0.0539(2) -0.1612(8) 0.043(1) Uani 1.00 d . . . O(2) O -0.0859(8) 0.1270(2) -0.1936(8) 0.042(1) Uani 1.00 d . . . O(3) O -0.1426(7) 0.2231(2) -0.2073(9) 0.049(1) Uani 1.00 d . . . O(4) O -0.4343(8) 0.2806(2) -0.2180(9) 0.047(1) Uani 1.00 d . . . O(5) O 0.282(1) 0.0065(2) -0.271(1) 0.043(1) Uani 1.00 d . . . N(1) N 0.0992(10) 0.1722(2) 0.298(1) 0.046(2) Uani 1.00 d . . . N(2) N -0.2065(8) 0.1136(2) 0.300(1) 0.047(2) Uani 1.00 d . . . C(1) C 0.023(1) 0.1222(3) 0.286(1) 0.041(2) Uani 1.00 d . . . C(2) C -0.280(1) 0.1038(3) -0.189(1) 0.041(2) Uani 1.00 d . . . C(3) C -0.5009(10) 0.1356(2) -0.213(1) 0.040(2) Uani 1.00 d . . . C(4) C -0.532(1) 0.1884(3) -0.223(1) 0.043(2) Uani 1.00 d . . . C(5) C -0.364(1) 0.2339(3) -0.215(1) 0.046(2) Uani 1.00 d . . . H(1) H -0.6352 0.1147 -0.2218 0.0471 Uiso 1.00 calc . . . H(2) H -0.6891 0.1999 -0.2294 0.0542 Uiso 1.00 calc . . . H(3) H 0.4241 -0.0115 -0.2551 0.0488 Uiso 1.00 calc . . . H(4) H 0.2474 0.0274 -0.4002 0.0488 Uiso 1.00 calc . . . H(5) H -0.0001 0.2019 0.3120 0.0582 Uiso 1.00 calc . . . H(6) H 0.2627 0.1791 0.2842 0.0582 Uiso 1.00 calc . . . H(7) H -0.3102 0.1436 0.3183 0.0530 Uiso 1.00 calc . . . H(8) H -0.2690 0.0787 0.2950 0.0530 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 Cd(1) 0.0388(6) 0.0353(5) 0.0438(6) 0.0009(2) 0.0019(4) -0.0014(2) S(1) 0.0392(9) 0.0358(9) 0.047(1) 0.0023(6) 0.0000(7) -0.0016(6) O(1) 0.041(2) 0.033(2) 0.053(3) 0.000(2) -0.007(2) 0.000(2) O(2) 0.041(2) 0.037(2) 0.048(3) 0.003(2) 0.005(2) 0.001(2) O(3) 0.038(2) 0.040(2) 0.068(4) 0.002(2) 0.001(2) 0.001(2) O(4) 0.053(3) 0.029(2) 0.060(3) 0.001(2) 0.007(2) -0.001(2) O(5) 0.044(3) 0.038(2) 0.047(3) -0.003(2) 0.003(2) 0.004(2) N(1) 0.046(3) 0.037(3) 0.055(4) 0.000(2) 0.005(3) 0.000(2) N(2) 0.037(3) 0.039(3) 0.065(4) -0.006(2) 0.002(2) -0.003(2) C(1) 0.044(3) 0.039(3) 0.040(4) -0.003(3) -0.003(3) -0.001(3) C(2) 0.038(3) 0.047(4) 0.038(3) 0.001(3) 0.003(2) -0.004(3) C(3) 0.031(3) 0.036(3) 0.051(4) -0.001(2) -0.005(3) -0.002(3) C(4) 0.045(3) 0.034(3) 0.050(4) 0.003(3) 0.005(3) 0.005(3) C(5) 0.042(3) 0.042(3) 0.053(4) -0.002(3) 0.003(3) 0.005(3) #----------------------------------------------------------------------- _computing_data_collection '.' _computing_cell_refinement '.' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #----------------------------------------------------------------------- _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 Cd(1) S(1) 2.617(2) . . yes Cd(1) S(1) 2.617(2) . 3_555 yes Cd(1) O(1) 2.374(4) . . yes Cd(1) O(1) 2.374(4) . 3_555 yes Cd(1) O(5) 2.405(7) . . yes Cd(1) O(5) 2.405(7) . 3_555 yes S(1) C(1) 1.733(7) . . yes O(1) C(2) 1.266(8) . . yes O(2) C(2) 1.268(8) . . yes O(3) C(5) 1.309(8) . . yes O(4) C(5) 1.238(8) . . yes N(1) C(1) 1.327(8) . . yes N(2) C(1) 1.354(9) . . yes C(2) C(3) 1.508(8) . . yes C(3) C(4) 1.333(9) . . yes C(4) C(5) 1.497(9) . . 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 S(1) Cd(1) S(1) 180.0 . 1_555 3_555 yes S(1) Cd(1) O(1) 101.1(1) . 1_555 1_555 yes S(1) Cd(1) O(1) 78.9(1) . 1_555 3_555 yes S(1) Cd(1) O(5) 93.7(1) . 1_555 1_555 yes S(1) Cd(1) O(5) 86.3(1) . 1_555 3_555 yes S(1) Cd(1) O(1) 78.9(1) . 3_555 1_555 yes S(1) Cd(1) O(1) 101.1(1) . 3_555 3_555 yes S(1) Cd(1) O(5) 86.3(1) . 3_555 1_555 yes S(1) Cd(1) O(5) 93.7(1) . 3_555 3_555 yes O(1) Cd(1) O(1) 180.0 . 1_555 3_555 yes O(1) Cd(1) O(5) 100.2(2) . 1_555 1_555 yes O(1) Cd(1) O(5) 79.8(2) . 1_555 3_555 yes O(1) Cd(1) O(5) 79.8(2) . 3_555 1_555 yes O(1) Cd(1) O(5) 100.2(2) . 3_555 3_555 yes O(5) Cd(1) O(5) 180.0 . 1_555 3_555 yes Cd(1) S(1) C(1) 106.6(2) . 1_555 1_555 yes Cd(1) O(1) C(2) 123.4(4) . 1_555 1_555 yes S(1) C(1) N(1) 120.8(5) . 1_555 1_555 yes S(1) C(1) N(2) 121.1(5) . 1_555 1_555 yes N(1) C(1) N(2) 118.1(6) . 1_555 1_555 yes O(1) C(2) O(2) 122.4(5) . 1_555 1_555 yes O(1) C(2) C(3) 116.9(5) . 1_555 1_555 yes O(2) C(2) C(3) 120.6(5) . 1_555 1_555 yes C(2) C(3) C(4) 129.6(5) . 1_555 1_555 yes C(3) C(4) C(5) 131.5(6) . 1_555 1_555 yes O(3) C(5) O(4) 121.2(6) . 1_555 1_555 yes O(3) C(5) C(4) 118.8(6) . 1_555 1_555 yes O(4) C(5) C(4) 120.0(6) . 1_555 1_555 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 Cd(1) S(1) 2.617(2) . . ? Cd(1) S(1) 2.617(2) . 3_555 ? S(1) O(5) 3.321(6) . 1_556 ? S(1) O(5) 3.493(6) . 3_655 ? S(1) N(2) 3.550(5) . 1_655 ? O(1) O(5) 2.761(7) . 1_455 ? O(2) N(2) 3.192(8) . 1_554 ? O(2) C(1) 3.315(9) . 1_554 ? O(2) C(3) 3.410(7) . 1_655 ? O(2) N(1) 3.561(8) . 1_554 ? O(2) C(4) 3.575(8) . 1_655 ? O(3) N(1) 2.967(7) . 4_554 ? O(3) O(3) 3.374(4) . 4_555 ? O(3) O(3) 3.374(4) . 4_554 ? O(3) C(5) 3.505(9) . 4_554 ? O(3) O(4) 3.511(7) . 4_554 ? O(3) C(5) 3.531(10) . 4_555 ? O(3) O(4) 3.545(8) . 4_555 ? O(4) N(2) 2.952(7) . 4_554 ? O(4) N(1) 2.959(7) . 4_454 ? O(4) C(5) 3.139(10) . 4_555 ? O(4) C(5) 3.147(10) . 4_554 ? O(4) C(4) 3.236(9) . 4_555 ? O(4) C(4) 3.244(9) . 4_554 ? O(4) N(1) 3.309(8) . 4_554 ? O(4) O(4) 3.453(4) . 4_555 ? O(4) O(4) 3.453(4) . 4_554 ? O(4) C(1) 3.594(8) . 4_554 ? O(5) C(3) 3.474(7) . 1_655 ? O(5) C(2) 3.537(8) . 1_655 ? N(1) C(5) 3.564(9) . 4_555 ? N(1) C(4) 3.591(9) . 1_656 ? N(2) C(2) 3.219(10) . 1_556 ? N(2) C(3) 3.581(10) . 1_556 ? C(5) C(5) 3.198(3) . 4_555 ? C(5) C(5) 3.198(3) . 4_554 ? #=END #For Complex IV data_ZZ-8 #----------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C11 H20 Cd2 N6 O10 S3 ' _chemical_formula_moiety 'C11 H20 Cd2 N6 O10 S3 ' _chemical_formula_weight 717.31 _chemical_melting_point ? #----------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 8.238(6) _cell_length_b 8.134(6) _cell_length_c 34.57(5) _cell_angle_alpha 90 _cell_angle_beta 92.51(5) _cell_angle_gamma 90 _cell_volume 2314(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 173.2 #----------------------------------------------------------------------- _exptl_crystal_description 'needle' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.059 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.170 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.477 _exptl_absorpt_correction_T_max 0.648 #----------------------------------------------------------------------- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type ? _diffrn_reflns_number 3485 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 0.8540 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.8540 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 #----------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3485 _reflns_number_gt 3431 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.0832 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3431 _refine_ls_number_parameters 289 _refine_ls_goodness_of_fit_ref 1.892 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00160|Fo|^2^]' _refine_ls_shift/su_max 0.0244 _refine_diff_density_max 1.30 _refine_diff_density_min -2.33 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;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) ; 'Cd' 'Cd' -0.807 1.202 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #----------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Cd(1) Cd 0.35178(4) 0.24243(5) 0.80500(1) 0.0285(2) Uani 1.00 d . . . Cd(2) Cd -0.07634(4) 0.19424(5) 0.938736(9) 0.0298(2) Uani 1.00 d . . . S(1) S 0.5849(1) 0.3783(2) 0.76723(3) 0.0327(4) Uani 1.00 d . . . S(2) S 0.1488(1) 0.0409(2) 0.97458(3) 0.0328(3) Uani 1.00 d . . . S(3) S -0.3491(1) 0.2826(2) 0.96002(4) 0.0343(4) Uani 1.00 d . . . O(1) O 0.2070(4) 0.5044(5) 0.81270(10) 0.0360(10) Uani 1.00 d . . . O(2) O 0.3625(4) 0.4076(5) 0.86126(10) 0.0363(10) Uani 1.00 d . . . O(3) O 0.1115(4) 0.0988(6) 0.8214(1) 0.048(1) Uani 1.00 d . . . O(4) O 0.2039(5) 0.2208(5) 0.7472(1) 0.038(1) Uani 1.00 d . . . O(5) O 0.0307(4) 0.3784(5) 0.8948(1) 0.0381(10) Uani 1.00 d . . . O(6) O 0.0678(5) 0.4723(5) 0.9546(1) 0.042(1) Uani 1.00 d . . . O(7) O -0.0998(4) 0.0409(5) 0.88212(9) 0.0326(9) Uani 1.00 d . . . O(8) O -0.2627(4) -0.1069(5) 0.9185(1) 0.0334(10) Uani 1.00 d . . . O(9) O -0.4624(4) 0.0735(5) 0.8483(1) 0.0327(9) Uani 1.00 d . . . O(10) O -0.5555(4) -0.0260(5) 0.79177(10) 0.0359(10) Uani 1.00 d . . . N(1) N 0.8761(5) 0.4975(7) 0.7856(1) 0.038(1) Uani 1.00 d . . . N(2) N 0.7736(5) 0.3363(6) 0.8325(1) 0.037(1) Uani 1.00 d . . . N(3) N 0.3110(4) 0.1150(6) 0.9103(1) 0.034(1) Uani 1.00 d . . . N(4) N 0.4290(5) -0.0717(6) 0.9529(1) 0.037(1) Uani 1.00 d . . . N(5) N -0.4056(6) 0.5567(6) 0.9188(1) 0.044(1) Uani 1.00 d . . . N(6) N -0.2619(6) 0.5920(6) 0.9763(1) 0.043(1) Uani 1.00 d . . . C(1) C 0.7555(5) 0.4035(7) 0.7978(1) 0.031(1) Uani 1.00 d . . . C(2) C 0.2665(6) 0.5147(7) 0.8469(1) 0.031(1) Uani 1.00 d . . . C(3) C 0.2197(6) 0.6612(7) 0.8709(1) 0.033(1) Uani 1.00 d . . . C(4) C 0.1388(5) 0.6496(7) 0.9031(1) 0.034(1) Uani 1.00 d . . . C(5) C 0.0755(5) 0.4896(7) 0.9185(1) 0.029(1) Uani 1.00 d . . . C(6) C 0.3067(5) 0.0294(7) 0.9432(1) 0.028(1) Uani 1.00 d . . . C(7) C -0.3352(5) 0.4957(7) 0.9512(1) 0.028(1) Uani 1.00 d . . . C(8) C -0.1984(6) -0.0748(7) 0.8874(1) 0.030(1) Uani 1.00 d . . . C(9) C -0.2302(6) -0.1922(7) 0.8529(2) 0.037(1) Uani 1.00 d . . . C(10) C -0.3476(7) -0.1788(7) 0.8261(2) 0.035(1) Uani 1.00 d . . . C(11) C -0.4628(5) -0.0370(6) 0.8218(1) 0.030(1) Uani 1.00 d . . . H(1) H 0.0144 0.1598 0.8272 0.0563 Uiso 1.00 calc . . . H(2) H 0.1082 -0.0172 0.8225 0.0563 Uiso 1.00 calc . . . H(3) H 0.1298 0.3027 0.7394 0.0485 Uiso 1.00 calc . . . H(4) H 0.2191 0.1260 0.7311 0.0485 Uiso 1.00 calc . . . H(5) H 0.9688 0.5204 0.8010 0.0461 Uiso 1.00 calc . . . H(6) H 0.8648 0.5474 0.7598 0.0461 Uiso 1.00 calc . . . H(7) H 0.8666 0.3587 0.8490 0.0423 Uiso 1.00 calc . . . H(8) H 0.6888 0.2681 0.8427 0.0423 Uiso 1.00 calc . . . H(9) H 0.2230 0.1888 0.9024 0.0400 Uiso 1.00 calc . . . H(10) H 0.3995 0.1041 0.8941 0.0400 Uiso 1.00 calc . . . H(11) H 0.4318 -0.1368 0.9767 0.0413 Uiso 1.00 calc . . . H(12) H 0.5203 -0.0835 0.9368 0.0413 Uiso 1.00 calc . . . H(13) H -0.3994 0.6720 0.9147 0.0524 Uiso 1.00 calc . . . H(14) H -0.4574 0.4867 0.9009 0.0524 Uiso 1.00 calc . . . H(15) H -0.2123 0.5492 0.9992 0.0498 Uiso 1.00 calc . . . H(16) H -0.2582 0.7080 0.9713 0.0498 Uiso 1.00 calc . . . H(17) H 0.2544 0.7675 0.8617 0.0440 Uiso 1.00 calc . . . H(18) H 0.1180 0.7503 0.9163 0.0375 Uiso 1.00 calc . . . H(19) H -0.1566 -0.2797 0.8514 0.0418 Uiso 1.00 calc . . . H(20) H -0.3608 -0.2655 0.8062 0.0438 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 Cd(1) 0.0295(3) 0.0306(4) 0.0252(3) 0.0011(1) 0.0001(2) 0.0000(1) Cd(2) 0.0295(3) 0.0322(4) 0.0278(3) 0.0012(1) 0.0017(2) 0.0011(1) S(1) 0.0294(6) 0.0423(9) 0.0264(6) -0.0014(5) -0.0003(4) 0.0022(5) S(2) 0.0320(6) 0.0394(8) 0.0275(6) 0.0039(5) 0.0061(4) 0.0053(5) S(3) 0.0329(7) 0.0336(8) 0.0368(7) 0.0029(5) 0.0043(5) 0.0040(5) O(1) 0.033(2) 0.043(2) 0.031(2) 0.000(2) -0.002(1) 0.001(2) O(2) 0.035(2) 0.042(2) 0.032(2) -0.002(2) 0.000(1) -0.001(2) O(3) 0.038(2) 0.060(3) 0.046(2) -0.016(2) 0.014(2) -0.007(2) O(4) 0.045(2) 0.041(2) 0.027(2) 0.008(2) -0.007(2) -0.006(2) O(5) 0.043(2) 0.038(2) 0.033(2) -0.005(2) -0.006(1) 0.001(2) O(6) 0.056(2) 0.043(2) 0.026(2) -0.004(2) 0.000(1) -0.001(2) O(7) 0.035(2) 0.030(2) 0.033(2) -0.005(2) 0.007(1) -0.003(1) O(8) 0.036(2) 0.031(2) 0.033(2) 0.004(2) 0.005(1) 0.001(1) O(9) 0.036(2) 0.031(2) 0.032(2) 0.001(2) 0.003(1) -0.008(1) O(10) 0.039(2) 0.033(2) 0.034(2) -0.003(2) -0.004(1) 0.000(2) N(1) 0.031(2) 0.050(3) 0.033(2) -0.008(2) -0.001(2) 0.003(2) N(2) 0.034(2) 0.036(3) 0.039(2) -0.009(2) -0.011(2) 0.005(2) N(3) 0.026(2) 0.044(3) 0.033(2) 0.006(2) 0.008(1) 0.008(2) N(4) 0.037(2) 0.039(3) 0.037(2) 0.000(2) 0.009(2) 0.009(2) N(5) 0.060(3) 0.032(3) 0.038(2) 0.000(2) -0.010(2) -0.001(2) N(6) 0.058(3) 0.028(3) 0.042(3) 0.003(2) -0.008(2) -0.009(2) C(1) 0.032(2) 0.032(3) 0.028(2) 0.004(2) 0.003(2) -0.003(2) C(2) 0.042(3) 0.028(3) 0.023(2) -0.004(2) 0.003(2) 0.004(2) C(3) 0.034(2) 0.032(3) 0.034(3) -0.003(2) -0.005(2) 0.001(2) C(4) 0.028(2) 0.038(3) 0.035(3) 0.000(2) 0.002(2) -0.003(2) C(5) 0.015(2) 0.034(3) 0.037(3) -0.004(2) 0.004(2) 0.000(2) C(6) 0.033(2) 0.028(3) 0.022(2) -0.011(2) 0.001(2) 0.000(2) C(7) 0.019(2) 0.030(3) 0.035(2) 0.001(2) 0.005(2) -0.002(2) C(8) 0.032(2) 0.027(3) 0.032(3) 0.001(2) -0.002(2) 0.002(2) C(9) 0.036(3) 0.039(3) 0.034(3) 0.006(2) -0.004(2) 0.001(2) C(10) 0.045(3) 0.024(3) 0.036(3) 0.001(2) 0.000(2) -0.007(2) C(11) 0.028(2) 0.026(3) 0.035(3) 0.000(2) 0.002(2) 0.000(2) #----------------------------------------------------------------------- _computing_data_collection '.' _computing_cell_refinement '.' _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 ? _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 Cd(1) S(1) 2.614(2) . . yes Cd(1) O(1) 2.462(4) . . yes Cd(1) O(2) 2.362(4) . . yes Cd(1) O(3) 2.388(4) . . yes Cd(1) O(4) 2.300(3) . . yes Cd(1) O(9) 2.505(4) . 1_655 yes Cd(1) O(10) 2.364(4) . 1_655 yes Cd(2) S(2) 2.516(2) . . yes Cd(2) S(3) 2.500(2) . . yes Cd(2) O(5) 2.334(4) . . yes Cd(2) O(6) 2.601(4) . . yes Cd(2) O(7) 2.321(3) . . yes S(1) C(1) 1.733(4) . . yes S(2) C(6) 1.732(5) . . yes S(3) C(7) 1.764(6) . . yes O(1) C(2) 1.261(6) . . yes O(2) C(2) 1.264(6) . . yes O(5) C(5) 1.266(7) . . yes O(6) C(5) 1.257(6) . . yes O(7) C(8) 1.262(6) . . yes O(8) C(8) 1.247(6) . . yes O(9) C(11) 1.283(6) . . yes O(10) C(11) 1.266(6) . . yes N(1) C(1) 1.336(7) . . yes N(2) C(1) 1.321(7) . . yes N(3) C(6) 1.337(6) . . yes N(4) C(6) 1.332(7) . . yes N(5) C(7) 1.334(7) . . yes N(6) C(7) 1.299(7) . . yes C(2) C(3) 1.513(8) . . yes C(3) C(4) 1.325(7) . . yes C(4) C(5) 1.508(8) . . yes C(8) C(9) 1.540(7) . . yes C(9) C(10) 1.315(7) . . yes C(10) C(11) 1.497(7) . . yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Cd(1) O(1) 93.33(9) . 1_555 1_555 yes S(1) Cd(1) O(2) 99.73(10) . 1_555 1_555 yes S(1) Cd(1) O(3) 163.8(1) . 1_555 1_555 yes S(1) Cd(1) O(4) 88.4(1) . 1_555 1_555 yes S(1) Cd(1) O(9) 95.02(10) . 1_555 1_655 yes S(1) Cd(1) O(10) 92.48(10) . 1_555 1_655 yes O(1) Cd(1) O(2) 54.5(1) . 1_555 1_555 yes O(1) Cd(1) O(3) 89.3(1) . 1_555 1_555 yes O(1) Cd(1) O(4) 85.4(1) . 1_555 1_555 yes O(1) Cd(1) O(9) 134.1(1) . 1_555 1_655 yes O(1) Cd(1) O(10) 169.2(1) . 1_555 1_655 yes O(2) Cd(1) O(3) 94.8(1) . 1_555 1_555 yes O(2) Cd(1) O(4) 139.2(1) . 1_555 1_555 yes O(2) Cd(1) O(9) 79.6(1) . 1_555 1_655 yes O(2) Cd(1) O(10) 133.1(1) . 1_555 1_655 yes O(3) Cd(1) O(4) 75.9(2) . 1_555 1_555 yes O(3) Cd(1) O(9) 94.6(1) . 1_555 1_655 yes O(3) Cd(1) O(10) 82.7(1) . 1_555 1_655 yes O(4) Cd(1) O(9) 139.8(1) . 1_555 1_655 yes O(4) Cd(1) O(10) 85.7(1) . 1_555 1_655 yes O(9) Cd(1) O(10) 54.2(1) . 1_655 1_655 yes S(2) Cd(2) S(3) 130.56(5) . 1_555 1_555 yes S(2) Cd(2) O(5) 110.33(10) . 1_555 1_555 yes S(2) Cd(2) O(6) 90.43(10) . 1_555 1_555 yes S(2) Cd(2) O(7) 100.44(9) . 1_555 1_555 yes S(3) Cd(2) O(5) 112.1(1) . 1_555 1_555 yes S(3) Cd(2) O(6) 95.5(1) . 1_555 1_555 yes S(3) Cd(2) O(7) 111.09(9) . 1_555 1_555 yes O(5) Cd(2) O(6) 52.9(1) . 1_555 1_555 yes O(5) Cd(2) O(7) 79.4(1) . 1_555 1_555 yes O(6) Cd(2) O(7) 131.6(1) . 1_555 1_555 yes Cd(1) S(1) C(1) 109.8(2) . 1_555 1_555 yes Cd(2) S(2) C(6) 106.1(2) . 1_555 1_555 yes Cd(2) S(3) C(7) 99.6(1) . 1_555 1_555 yes Cd(1) O(1) C(2) 89.3(3) . 1_555 1_555 yes Cd(1) O(2) C(2) 93.9(3) . 1_555 1_555 yes Cd(2) O(5) C(5) 98.3(3) . 1_555 1_555 yes Cd(2) O(6) C(5) 86.1(3) . 1_555 1_555 yes Cd(2) O(7) C(8) 108.0(3) . 1_555 1_555 yes Cd(1) O(9) C(11) 88.5(3) . 1_455 1_555 yes Cd(1) O(10) C(11) 95.4(3) . 1_455 1_555 yes S(1) C(1) N(1) 118.0(4) . 1_555 1_555 yes S(1) C(1) N(2) 124.2(4) . 1_555 1_555 yes N(1) C(1) N(2) 117.8(4) . 1_555 1_555 yes O(1) C(2) O(2) 122.3(5) . 1_555 1_555 yes O(1) C(2) C(3) 118.0(4) . 1_555 1_555 yes O(2) C(2) C(3) 119.7(4) . 1_555 1_555 yes C(2) C(3) C(4) 123.8(5) . 1_555 1_555 yes C(3) C(4) C(5) 123.5(5) . 1_555 1_555 yes O(5) C(5) O(6) 122.4(5) . 1_555 1_555 yes O(5) C(5) C(4) 118.9(4) . 1_555 1_555 yes O(6) C(5) C(4) 118.7(5) . 1_555 1_555 yes S(2) C(6) N(3) 123.6(4) . 1_555 1_555 yes S(2) C(6) N(4) 117.2(4) . 1_555 1_555 yes N(3) C(6) N(4) 119.2(4) . 1_555 1_555 yes S(3) C(7) N(5) 118.8(4) . 1_555 1_555 yes S(3) C(7) N(6) 120.6(4) . 1_555 1_555 yes N(5) C(7) N(6) 120.6(5) . 1_555 1_555 yes O(7) C(8) O(8) 125.5(5) . 1_555 1_555 yes O(7) C(8) C(9) 116.1(4) . 1_555 1_555 yes O(8) C(8) C(9) 118.2(5) . 1_555 1_555 yes C(8) C(9) C(10) 126.1(5) . 1_555 1_555 yes C(9) C(10) C(11) 125.2(5) . 1_555 1_555 yes O(9) C(11) O(10) 121.3(4) . 1_555 1_555 yes O(9) C(11) C(10) 119.2(4) . 1_555 1_555 yes O(10) C(11) C(10) 119.5(4) . 1_555 1_555 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 Cd(1) S(1) 2.614(2) . . ? Cd(1) O(9) 2.505(4) . 1_655 ? Cd(2) S(2) 2.516(2) . . ? Cd(2) S(3) 2.500(2) . . ? Cd(2) O(6) 2.601(4) . . ? S(2) S(2) 3.149(3) . 3_557 ? S(2) N(6) 3.539(5) . 3_567 ? S(3) N(4) 3.416(5) . 1_455 ? S(3) N(3) 3.499(4) . 1_455 ? S(3) C(6) 3.532(5) . 1_455 ? S(3) N(4) 3.551(5) . 3_557 ? O(1) O(4) 2.840(5) . 2_556 ? O(1) N(1) 2.844(5) . 1_455 ? O(3) N(2) 3.424(6) . 1_455 ? O(4) O(10) 2.722(5) . 2_456 ? O(5) N(2) 2.972(5) . 1_455 ? O(6) N(6) 2.864(6) . 3_567 ? O(6) O(6) 3.410(8) . 3_567 ? O(7) N(2) 3.105(6) . 1_455 ? O(8) N(4) 2.866(6) . 1_455 ? O(8) N(5) 2.979(7) . 1_545 ? O(8) N(6) 3.162(7) . 1_545 ? O(8) C(7) 3.486(7) . 1_545 ? O(9) N(3) 2.921(5) . 1_455 ? O(9) N(2) 2.957(6) . 1_455 ? O(10) N(1) 3.119(6) . 2_546 ? N(1) C(10) 3.536(7) . 1_665 ? N(1) C(9) 3.567(8) . 1_665 ? N(4) N(5) 3.538(8) . 1_645 ? N(5) C(9) 3.426(8) . 1_565 ? N(5) C(3) 3.542(7) . 1_455 ? C(4) C(8) 3.592(7) . 1_565 ? #-----------------------------------------------------------------------