X-ray diffraction study of copper(I) thiourea complexes formed in sulfate-containing acid solutions
Piro, O. E.; Piatti, R. C. V.; Bolzán, A. E.; Salvarezza, R. C.; Arvia, A. J.; Acta Crystallographica Section B 56 (2000) 993–997; doi:10.1107/S0108768100008028

data_2102186
_publ_section_title
;
 X-ray diffraction study of copper(I) thiourea complexes formed in
 sulfate-containing acid solutions
;
_journal_coeditor_code           CA0005
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              993
_journal_page_last               997
_journal_paper_doi               10.1107/S0108768100008028
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Cu4(C H4 N2 S)12](S O4)2,2H2 O'
_chemical_formula_moiety         'C12 H48 Cu4 N24 S12 4+, 2(O4 S 2-), 2(H2 O)'
_chemical_formula_sum            'C12 H52 Cu4 N24 O10 S14'
_chemical_formula_weight         1395.78
_chemical_name_systematic
;
 hexa(thiourea)dicopper(I) sulphate monohydrate 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                64.843(10)
_cell_angle_beta                 76.119(10)
_cell_angle_gamma                66.059(10)
_cell_formula_units_Z            1
_cell_length_a                   11.079(2)
_cell_length_b                   11.2620(10)
_cell_length_c                   12.195(2)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.7
_cell_measurement_theta_min      13.5
_cell_volume                     1254.6(4)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_data_reduction        'SDP (Frenz, 1983)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6343
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        1.4
_diffrn_standards_interval_time  30
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    2.322
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_hydrogen_treatment    isotropic
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_obs          0.0255
_refine_ls_shift/esd_max         -0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.7410P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0676
_refine_ls_wR_factor_obs         0.0646
_reflns_number_observed          5184
_reflns_number_total             5781
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ca0005.cif
_cod_data_source_block           sulph
_cod_depositor_comments
;

2019-10-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C6 H26 Cu2 N12 O5 S7'
_cod_original_formula_weight         697.89
_cod_original_formula_moiety         'C6 H24 Cu2 N12 S6 2+,O4 S 2-,H2 O'
_cod_original_formula_iupac          '[Cu2(C H4 N2 S)6](S O4),H2 O'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        1254.6(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2102186