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_4111802
_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            'C34.5 H29.5 O P Re S3'
_chemical_formula_weight         773.43
_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                 121.374(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.844(6)
_cell_length_b                   9.5051(16)
_cell_length_c                   22.643(4)
_cell_measurement_reflns_used    958
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      3.01
_cell_volume                     6219.0(19)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29006
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    4.188
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.929
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7711
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+7.9321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                6237
_reflns_number_total             7711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0519334si20050408_011727.cif
_cod_data_source_block           esp57
_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        6219.1(18)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C34.50 H29.50 O P Re S3'
_cod_database_code               4111802