Photochemical and time resolved spectroscopic studies of intermediates relevant to iridium-catalyzed methanol carbonylation: photoinduced CO migratory insertion.
Volpe, Maurizio; Wu, Guang; Iretskii, Alexei; Ford, Peter C.; Inorganic chemistry 45 (2006) 1861–1870; doi:10.1021/ic0513033

data_4340153
_publ_section_title
;
 Photochemical and time resolved spectroscopic studies of intermediates
 relevant to iridium-catalyzed methanol carbonylation: photoinduced CO
 migratory insertion.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1861
_journal_page_last               1870
_journal_paper_doi               10.1021/ic0513033
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C27 H23 As I3 Ir O2'
_chemical_formula_weight         1027.27
_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                71.549(2)
_cell_angle_beta                 85.826(2)
_cell_angle_gamma                70.565(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5278(15)
_cell_length_b                   12.0524(17)
_cell_length_c                   12.4234(17)
_cell_measurement_temperature    110(1)
_cell_volume                     1409.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(1)
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'CCd area detector'
_diffrn_measurement_method       'Omega Scan'
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10838
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    9.211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.960
_refine_diff_density_min         -2.829
_refine_diff_density_rms         0.238
_refine_ls_extinction_coef       0.0011(2)
_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   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5980
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0769P)^2^+1.3354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                4337
_reflns_number_total             5980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Pub.CIF
_cod_data_source_block           '[Ir(C(O)CH3)(CO)I3]2[AsPh4]2'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4340153