Cluster Core Controlled Reactions of Substitution of Terminal Bromide Ligands by Triphenylphosphine in Octahedral Rhenium Chalcobromide Complexes
Michael A. Shestopalov; Yuri V. Mironov; Konstantin A. Brylev; Svetlana G. Kozlova; Vladimir E. Fedorov; Hartmut Spies; Hans-Jürgen Pietzsch; Holger Stephan; Gerhard Geipel; Gerd Bernhard; Journal of the American Chemical Society 129 (2007) 3714–3721; doi:10.1021/ja0668062

data_4109199
_publ_contact_author_address
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 3,
Novosibirsk 90,
630090 Russia
;
_publ_contact_author_email       fed@che.nsk.su
_publ_contact_author_fax         '007 383 3309489'
_publ_contact_author_name        'Prof. Vladimir E. Fedorov'
_publ_contact_author_phone       '007 383 3309253'
_publ_section_title
;
 Cluster Core Controlled Reactions of Substitution of Terminal Bromide
 Ligands by Triphenylphosphine in Octahedral Rhenium Chalcobromide
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3714
_journal_page_last               3721
_journal_paper_doi               10.1021/ja0668062
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         trans-[{Re6S8}(PPh3)4Br2]
_chemical_formula_sum            'C72 H60 Br2 P4 Re6 S8'
_chemical_formula_weight         2582.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 101.7800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4001(3)
_cell_length_b                   16.1927(4)
_cell_length_c                   19.1937(5)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.51
_cell_volume                     3772.76(16)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27083
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.20
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.993
_exptl_absorpt_correction_T_max  0.3338
_exptl_absorpt_correction_T_min  0.1278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.321
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.175
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         7705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0446P)^2^+0.1481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0790
_reflns_number_gt                6241
_reflns_number_total             7705
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja0668062si20061208_071712_2.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        3772.75(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4109199