 
data_s 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H4 Cu3 O8 S' 
_chemical_formula_weight          354.71 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cu'  'Cu'   0.3201   1.2651 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z' 
 'x+1/2, -y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, y, -z-1/2' 
 'x, -y-1/2, z' 
 '-x-1/2, y-1/2, z-1/2' 
 
_cell_length_a                    8.2583(4) 
_cell_length_b                    6.0512(3) 
_cell_length_c                    12.0063(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      599.99(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.927 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              684 
_exptl_absorpt_coefficient_mu     10.890 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5084 
_diffrn_reflns_av_R_equivalents   0.0255 
_diffrn_reflns_av_sigmaI/netI     0.0228 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -6 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.99 
_diffrn_reflns_theta_max          33.36 
_reflns_number_total              1190 
_reflns_number_gt                 1046 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0142P)²+0.5465P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0082(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          1190 
_refine_ls_number_parameters      75 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0229 
_refine_ls_R_factor_gt            0.0176 
_refine_ls_wR_factor_ref          0.0437 
_refine_ls_wR_factor_gt           0.0419 
_refine_ls_goodness_of_fit_ref    1.115 
_refine_ls_restrained_S_all       1.115 
_refine_ls_shift/su_max           0.004 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
H3 H 0.775(6) 0.7500 1.251(4) 0.056(16) Uiso 1 2 d S . . 
H1 H 0.651(5) 0.2500 0.989(3) 0.035(12) Uiso 1 2 d S . . 
H2 H 1.007(4) 0.012(5) 0.846(3) 0.048(11) Uiso 1 1 d . . . 
O4 O 0.6977(2) 0.7500 0.97788(15) 0.0143(3) Uani 1 2 d S . . 
O5 O 0.53120(14) 0.9527(2) 0.84824(11) 0.0119(2) Uani 1 1 d . . . 
O6 O 0.7620(2) 0.7500 0.78264(15) 0.0127(3) Uani 1 2 d S . . 
O1 O 0.7188(2) 0.2500 1.02531(14) 0.0100(3) Uani 1 2 d S . . 
O3 O 0.7013(2) 0.7500 1.22136(14) 0.0102(3) Uani 1 2 d S . . 
O2 O 1.04665(15) 0.00658(19) 0.89805(10) 0.0090(2) Uani 1 1 d . . . 
Cu1 Cu 0.99520(3) 0.2500 1.00119(2) 0.00835(8) Uani 1 2 d S . . 
Cu2 Cu 0.71009(2) 0.49710(3) 1.125862(16) 0.00871(7) Uani 1 1 d . . . 
S3 S 0.63035(6) 0.7500 0.86429(4) 0.00674(11) Uani 1 2 d S . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
O4 0.0211(9) 0.0121(8) 0.0095(8) 0.000 -0.0050(6) 0.000 
O5 0.0083(5) 0.0093(5) 0.0182(6) 0.0018(4) 0.0009(4) 0.0018(4) 
O6 0.0104(7) 0.0136(9) 0.0141(8) 0.000 0.0045(6) 0.000 
O1 0.0105(7) 0.0097(8) 0.0098(7) 0.000 -0.0006(6) 0.000 
O3 0.0121(7) 0.0091(8) 0.0096(8) 0.000 -0.0007(6) 0.000 
O2 0.0105(5) 0.0087(5) 0.0079(5) -0.0002(4) -0.0002(4) -0.0002(4) 
Cu1 0.01027(13) 0.00473(13) 0.01005(14) 0.000 0.00310(9) 0.000 
Cu2 0.00837(11) 0.00642(11) 0.01134(11) -0.00114(7) 0.00222(6) -0.00015(7) 
S3 0.0065(2) 0.0065(2) 0.0072(2) 0.000 -0.00005(17) 0.000 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
O4 S3 1.4727(18) . ? 
O4 Cu2 2.3472(14) 7_575 ? 
O4 Cu2 2.3472(14) . ? 
O5 S3 1.4872(13) . ? 
O5 Cu2 2.0346(12) 3_657 ? 
O6 S3 1.4640(17) . ? 
O6 Cu2 2.4150(14) 2_664 ? 
O6 Cu2 2.4150(14) 8_765 ? 
O1 Cu2 1.9231(11) . ? 
O1 Cu2 1.9231(11) 7_565 ? 
O1 Cu1 2.3007(17) . ? 
O3 Cu2 1.9136(10) 7_575 ? 
O3 Cu2 1.9136(10) . ? 
O2 Cu1 1.9706(12) . ? 
O2 Cu1 1.9984(12) 5_757 ? 
O2 Cu2 2.0301(12) 3_747 ? 
Cu1 O2 1.9706(12) 7_565 ? 
Cu1 O2 1.9984(12) 3_757 ? 
Cu1 O2 1.9984(12) 5_757 ? 
Cu1 Cu1 3.02677(16) 5_767 ? 
Cu1 Cu1 3.02677(15) 5_757 ? 
Cu2 O2 2.0301(12) 3_757 ? 
Cu2 O5 2.0346(12) 3_647 ? 
Cu2 O6 2.4150(14) 2_665 ? 
Cu2 Cu2 2.9905(4) 7_565 ? 
S3 O5 1.4872(13) 7_575 ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
S3 O4 Cu2 135.84(5) . 7_575 ? 
S3 O4 Cu2 135.84(5) . . ? 
Cu2 O4 Cu2 81.38(6) 7_575 . ? 
S3 O5 Cu2 128.93(8) . 3_657 ? 
S3 O6 Cu2 126.35(7) . 2_664 ? 
S3 O6 Cu2 126.35(7) . 8_765 ? 
Cu2 O6 Cu2 76.51(5) 2_664 8_765 ? 
Cu2 O1 Cu2 102.07(8) . 7_565 ? 
Cu2 O1 Cu1 96.68(6) . . ? 
Cu2 O1 Cu1 96.68(6) 7_565 . ? 
Cu2 O3 Cu2 106.21(8) 7_575 . ? 
Cu1 O2 Cu1 99.39(5) . 5_757 ? 
Cu1 O2 Cu2 108.86(6) . 3_747 ? 
Cu1 O2 Cu2 103.58(6) 5_757 3_747 ? 
O2 Cu1 O2 96.74(7) . 7_565 ? 
O2 Cu1 O2 176.75(4) . 3_757 ? 
O2 Cu1 O2 80.61(5) 7_565 3_757 ? 
O2 Cu1 O2 80.61(5) . 5_757 ? 
O2 Cu1 O2 176.75(4) 7_565 5_757 ? 
O2 Cu1 O2 101.96(7) 3_757 5_757 ? 
O2 Cu1 O1 107.04(5) . . ? 
O2 Cu1 O1 107.04(5) 7_565 . ? 
O2 Cu1 O1 75.65(4) 3_757 . ? 
O2 Cu1 O1 75.65(5) 5_757 . ? 
O2 Cu1 Cu1 137.36(4) . 5_767 ? 
O2 Cu1 Cu1 40.65(4) 7_565 5_767 ? 
O2 Cu1 Cu1 39.97(3) 3_757 5_767 ? 
O2 Cu1 Cu1 141.90(4) 5_757 5_767 ? 
O1 Cu1 Cu1 91.556(10) . 5_767 ? 
O2 Cu1 Cu1 40.65(4) . 5_757 ? 
O2 Cu1 Cu1 137.36(4) 7_565 5_757 ? 
O2 Cu1 Cu1 141.90(4) 3_757 5_757 ? 
O2 Cu1 Cu1 39.97(3) 5_757 5_757 ? 
O1 Cu1 Cu1 91.556(10) . 5_757 ? 
Cu1 Cu1 Cu1 176.81(2) 5_767 5_757 ? 
O3 Cu2 O1 177.93(6) . . ? 
O3 Cu2 O2 95.72(6) . 3_757 ? 
O1 Cu2 O2 84.03(6) . 3_757 ? 
O3 Cu2 O5 88.68(6) . 3_647 ? 
O1 Cu2 O5 91.72(6) . 3_647 ? 
O2 Cu2 O5 173.98(5) 3_757 3_647 ? 
O3 Cu2 O4 86.01(5) . . ? 
O1 Cu2 O4 91.91(5) . . ? 
O2 Cu2 O4 85.28(6) 3_757 . ? 
O5 Cu2 O4 99.15(6) 3_647 . ? 
O3 Cu2 O6 91.82(5) . 2_665 ? 
O1 Cu2 O6 90.25(5) . 2_665 ? 
O2 Cu2 O6 91.91(5) 3_757 2_665 ? 
O5 Cu2 O6 83.83(6) 3_647 2_665 ? 
O4 Cu2 O6 176.26(5) . 2_665 ? 
O3 Cu2 Cu2 143.10(4) . 7_565 ? 
O1 Cu2 Cu2 38.97(4) . 7_565 ? 
O2 Cu2 Cu2 91.62(3) 3_757 7_565 ? 
O5 Cu2 Cu2 82.41(4) 3_647 7_565 ? 
O4 Cu2 Cu2 130.69(3) . 7_565 ? 
O6 Cu2 Cu2 51.75(3) 2_665 7_565 ? 
O6 S3 O4 109.86(11) . . ? 
O6 S3 O5 108.79(6) . 7_575 ? 
O4 S3 O5 109.14(7) . 7_575 ? 
O6 S3 O5 108.79(6) . . ? 
O4 S3 O5 109.14(7) . . ? 
O5 S3 O5 111.11(10) 7_575 . ? 
 
_diffrn_measured_fraction_theta_max    0.943 
_diffrn_reflns_theta_full              33.36 
_diffrn_measured_fraction_theta_full   0.943 
_refine_diff_density_max    0.532 
_refine_diff_density_min   -0.502 
_refine_diff_density_rms    0.129 
