Charge-Transfer Spectra of Structurally Characterized Mixed-Valence Thiolate-Bridged Cu(I)/Cu(II) Cluster Complexes
Robert T. Stibrany; Ronald Fikar; Mark Brader; Marc N. Potenza; Joseph A. Potenza; Harvey J. Schugar; Inorganic Chemistry 41 (2002) 5203–5215; doi:10.1021/ic020156v

data_4318549
_publ_section_title
;
 Charge-Transfer Spectra of Structurally Characterized Mixed-Valence
 Thiolate-Bridged Cu(I)/Cu(II) Cluster Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5203
_journal_page_last               5215
_journal_paper_doi               10.1021/ic020156v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C52 H84 Cl2 Cu5 N6.5 O4 S6'
_chemical_formula_weight         1445.22
_chemical_name_common            R,R-7Cl.solvate
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.312(2)
_cell_length_b                   19.312(2)
_cell_length_c                   19.312(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     7202.5(13)
_computing_cell_refinement       'CAD4 (Enraf Nonius, 1985'
_computing_data_collection       'CAD4 (Enraf Nonius, 1985'
_computing_data_reduction        'local programs'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1976) and ORTEP32 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       'scintillation counter'
_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  0.0509
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3750
_diffrn_reflns_theta_full        19.96
_diffrn_reflns_theta_max         19.96
_diffrn_reflns_theta_min         2.11
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.741
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psicalc
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_meas      1.36(1)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       'hexagonal block'
_exptl_crystal_F_000             2994
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1255
_refine_ls_number_restraints     253
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                996
_reflns_number_total             1255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020156v_4.cif
_cod_data_source_block           R,R-7
_cod_database_code               4318549