Synthesis and Characterization of Rhenium−Copper Sulfide Cluster Complexes [(Ph3P)2N][Re3(CuX)(μ3-S)4Cl6(PMe2Ph)3] (X = Cl, Br, I)
Iijima, Kazuya; Sunaga, Tomoaki; Hirose, Masaya; Saito, Taro; Inorganic Chemistry 45 (2006) 3452–3455; doi:10.1021/ic052135h

data_4332069
_publ_section_title
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 Synthesis and Characterization of Rhenium&#x2212;Copper Sulfide Cluster
 Complexes [(Ph3P)2N][Re3(CuX)(\m3-S)4Cl6(PMe2Ph)3] (X = Cl, Br, I)
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_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3452
_journal_page_last               3455
_journal_paper_doi               10.1021/ic052135h
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source        'local laboratory'
_chemical_formula_sum            'C62 H67 Cl11 Cu N P5 Re3 S4'
_chemical_formula_weight         2121.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.8650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1274(5)
_cell_length_b                   14.6445(6)
_cell_length_c                   45.975(2)
_cell_measurement_reflns_used    5972
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.26
_cell_volume                     7438.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0746
_diffrn_reflns_av_sigmaI/netI    0.0909
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            55368
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         0.89
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.802
_exptl_absorpt_correction_T_max  0.8928
_exptl_absorpt_correction_T_min  0.2359
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.89
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.727
_refine_diff_density_min         -2.271
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         18477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+14.4416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                12194
_reflns_number_total             18477
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic052135hsup3.cif
_cod_data_source_block           cu1227
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4332069