Studies of synthesis, structural features of Cu(I) thiophene-2-thiocarboxylates and unprecedented desulfurization of Cu(II) thiocarboxylate complexes.
Singh, Suryabhan; Chaturvedi, Jyotsna; Bhattacharya, Subrato; Dalton transactions (Cambridge, England : 2003) 41 (2012) 424–431; doi:10.1039/c1dt10629e

data_7017494
_publ_section_title
;
 Studies of synthesis, structural features of Cu(I)
 thiophene-2-thiocarboxylates and unprecedented desulfurization of Cu(II)
 thiocarboxylate complexes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              424
_journal_page_last               431
_journal_paper_doi               10.1039/c1dt10629e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C22 H14 Cu N2 O5 S2'
_chemical_formula_weight         514.04
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.567(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5195(10)
_cell_length_b                   13.8376(12)
_cell_length_c                   14.5830(12)
_cell_measurement_temperature    293(2)
_cell_volume                     2120.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.850
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10879
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76032
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             1044
_exptl_crystal_recrystallization_method Methanol
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         2.861
_refine_diff_density_min         -0.965
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8141
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.1081
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1981P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2794
_refine_ls_wR_factor_ref         0.2986
_reflns_number_gt                5115
_reflns_number_total             8141
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10629e.txt
_cod_data_source_block           phencuta
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7017494