Studies of C-S Bond Cleavage Reactions of Re(V) Dithiolates: Synthesis, Reactivity, and Mechanism
Ming Li; Arkady Ellern; James H. Espenson; Journal of the American Chemical Society 127 (2005) 10436–10447; doi:10.1021/ja0519334

data_4111804
_publ_section_title
;
 Studies of C-S Bond Cleavage Reactions of Re(V) Dithiolates: Synthesis,
 Reactivity, and Mechanism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10436
_journal_page_last               10447
_journal_paper_doi               10.1021/ja0519334
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C20 H19 Cl O P Re S2'
_chemical_formula_weight         592.09
_chemical_name_systematic
; 
 ? 
;
_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                 110.753(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.345(4)
_cell_length_b                   10.982(2)
_cell_length_c                   23.929(5)
_cell_measurement_reflns_used    931
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.24
_cell_volume                     4262.3(15)
_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      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.945
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16819
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    6.105
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_correction_T_min  0.21
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.406
_refine_diff_density_min         -1.919
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+38.9203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1052
_reflns_number_gt                3854
_reflns_number_total             5003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0519334si20050408_011828.cif
_cod_data_source_block           esp71
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4262.4(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4111804