Substitution of the Terminal Chloride Ligands of [Re6S8Cl6]4- with Triethylphosphine: Photophysical and Electrochemical Properties of a New Series of [Re6S8]2+ Based Clusters
Lisa F. Szczepura; David L. Cedeño; Dean B. Johnson; Robert McDonald; Stanley A. Knott; Kristen M. Jeans; Jessica L. Durham; Inorganic Chemistry 49 (2010) 11386–11394; doi:10.1021/ic101348h

data_4317290
_publ_section_title
;
 Substitution of the Terminal Chloride Ligands of [Re6S8Cl6]4- with
 Triethylphosphine: Photophysical and Electrochemical Properties of a New
 Series of [Re6S8]2+ Based Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11386
_journal_page_last               11394
_journal_paper_doi               10.1021/ic101348h
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C12 H30 Cl4 P2 Re6 S8, 2(C16 H36 N), 3(C7 H8)'
_chemical_formula_sum            'C65 H126 Cl4 N2 P2 Re6 S8'
_chemical_formula_weight         2513.10
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 96.316(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.186(3)
_cell_length_b                   19.144(2)
_cell_length_c                   18.3863(19)
_cell_measurement_reflns_used    7202
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.23
_cell_volume                     8461.5(16)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36905
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    8.946
_exptl_absorpt_correction_T_max  0.3286
_exptl_absorpt_correction_T_min  0.0693
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4824
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.501
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         9687
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+22.9912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                8144
_reflns_number_total             9687
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101348h_si_002_1.cif
_cod_data_source_block           isu0805
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        8461.6(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4317290