Tetrakis(μ~3~-thiourea)bis(μ~2~-thiourea)octakis(thiourea)hexacopper(I) hexakis(perchlorate)
S. Athimoolam; J. Kumar; V. Ramakrishnan; R. K. Rajaram; Acta Crystallographica Section E 61 (2005) m2014–m2017; doi:10.1107/S1600536805028588

data_2206969
_publ_section_title
;
 Tetrakis(\m~3~-thiourea)bis(\m~2~-thiourea)octakis(thiourea)hexacopper(I)
 hexakis(perchlorate)
;
_journal_coeditor_code           HG6222
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2014
_journal_page_last               m2017
_journal_paper_doi               10.1107/S1600536805028588
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Cu6 (C H4 N2 S)14] (Cl O4)6'
_chemical_formula_moiety         'C14 H56 Cu6 N28 S14 6+ , 6Cl O4 -'
_chemical_formula_sum            'C14 H56 Cl6 Cu6 N28 O24 S14'
_chemical_formula_weight         2043.65
_chemical_name_systematic
;
Tetrakis(\m~3~-thiourea)bis(\m~2~-thiourea)octakis(thiourea)hexacopper(I)
hexaperchlorate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.30(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.229(2)
_cell_length_b                   15.363(3)
_cell_length_c                   27.639(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.59
_cell_measurement_theta_min      11.19
_cell_volume                     7304(2)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'SHELXTL/PC and PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  SHELXTL/PC
_computing_structure_solution    'SHELXTL/PC (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius MACH3'
_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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            7120
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.416
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            White
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_meas      1.845
_exptl_crystal_density_method
'flotation using a mixture of CCl~4~ and CHBr~3~'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.221
_refine_diff_density_min         -0.864
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs'
_refine_ls_abs_structure_Flack   0.015(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         6610
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0685P)^2^+13.3767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                5203
_reflns_number_total             6610
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6222.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2206969
_cod_database_fobs_code          2206969