Reversible Intramolecular Single-Electron Oxidative Addition Involving a Hemilabile Noninnocent Ligand
Hübner, Ralph; Weber, Sebastian; Strobel, Sabine; Sarkar, Biprajit; Záliš, Stanislav; Kaim, Wolfgang; Organometallics 30 (2011) 1414–; doi:10.1021/om100969q

data_4063829
_publ_section_title
;
 Reversible Intramolecular Single-Electron Oxidative Addition Involving a
 Hemilabile Noninnocent Ligand
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1414
_journal_paper_doi               10.1021/om100969q
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C31 H42 Ir N O S'
_chemical_formula_sum            'C31 H42 Ir N O S'
_chemical_formula_weight         668.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 113.0960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7134(1)
_cell_length_b                   22.2774(3)
_cell_length_c                   13.2353(2)
_cell_measurement_reflns_used    7398
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      0.41
_cell_volume                     2905.64(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       CCD
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14102
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    4.690
_exptl_absorpt_correction_T_max  0.8275
_exptl_absorpt_correction_T_min  0.6612
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Scalepack (W. Minor & Z. Otwinowski)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'coars shape'
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.411
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.00025(5)
_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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         7238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0210P)^2^+1.6278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0512
_reflns_number_gt                5917
_reflns_number_total             7238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100969q_si_001.cif
_cod_data_source_block           c:\crystal\x-red\rhaug09d
_cod_original_cell_volume        2905.64(6)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4063829