Dinuclear Oxidative Addition of N-H and S-H Bonds at Chromium. Reaction of .Cr(CO)3(C5Me5) with {o-(HA)C6H4S-Cr(CO)3(C5Me5)} (A = S, NH) Yielding [η2-o-(μ-A)C6H4S-Cr(C5Me5)]2 and H-Cr(CO)3(C5Me5)
Kengkaj Sukcharoenphon; Telvin D. Ju; Khalil A. Abboud; Carl D. Hoff; Inorganic Chemistry 41 (2002) 6769–6774; doi:10.1021/ic0204934

data_4319017
_publ_section_title
;
 Dinuclear Oxidative Addition of N-H and S-H Bonds at Chromium. Reaction
 of .Cr(CO)3(C5Me5) with {o-(HA)C6H4S-Cr(CO)3(C5Me5)} (A = S, NH) Yielding
 [\h2-o-(\m-A)C6H4S-Cr(C5Me5)]2 and H-Cr(CO)3(C5Me5)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6769
_journal_page_last               6774
_journal_paper_doi               10.1021/ic0204934
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H38 Cr2 S4'
_chemical_formula_weight         654.86
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                62.673(2)
_cell_angle_beta                 70.209(2)
_cell_angle_gamma                80.978(2)
_cell_formula_units_Z            1
_cell_length_a                   8.0712(3)
_cell_length_b                   10.3454(4)
_cell_length_c                   10.7893(5)
_cell_measurement_reflns_used    80
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     753.09(6)
_computing_cell_refinement       'Bruker SMART & SAINT (Bruker 1998)'
_computing_data_collection       'Bruker SMART (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6589
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  0.8818
_exptl_absorpt_correction_T_min  0.8107
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, SHELXTL (Bruker 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0186(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.3379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                3149
_reflns_number_total             3335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0204934_2.cif
_cod_data_source_block           ho29
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        753.09(5)
_cod_database_code               4319017