Carbon−Sulfur Bond Cleavage of Methyl-Substituted Thiophenes with Iridium(III)
Grochowski, Matthew R.; Brennessel, William W.; Jones, William D.; Organometallics 28 (2009) 2661–; doi:10.1021/om900114m

data_4069265
_publ_section_title
;
 Carbon&#x2212;Sulfur Bond Cleavage of Methyl-Substituted Thiophenes with
 Iridium(III)
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2661
_journal_paper_doi               10.1021/om900114m
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety
'C30 H45 Ir3 S2, 2(C10 H15 Cl3 Ir), 2(C6 H8 S)'
_chemical_formula_sum            'C62 H91 Cl6 Ir5 S4'
_chemical_formula_weight         2138.29
_chemical_name_common            jonmg01
_chemical_name_systematic
;
[(Cp*Ir)3(mu-S)2]+[Cp*IrCl3]2-, 2
;
_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                72.210(1)
_cell_angle_beta                 78.404(1)
_cell_angle_gamma                87.161(1)
_cell_formula_units_Z            2
_cell_length_a                   10.9688(9)
_cell_length_b                   16.3357(13)
_cell_length_c                   20.4096(16)
_cell_measurement_reflns_used    3925
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      33.02
_cell_measurement_theta_min      2.52
_cell_volume                     3410.8(5)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            60766
_diffrn_reflns_theta_full        32.03
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    10.113
_exptl_absorpt_correction_T_max  0.2966
_exptl_absorpt_correction_T_min  0.1102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.118
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     723
_refine_ls_number_reflns         23487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+1.2077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0508
_reflns_number_gt                20560
_reflns_number_total             23487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900114m_si_002.cif
_cod_data_source_block           jonmg01
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4069265