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_4340154
_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            'C13 H13 I2 Ir N2 O2'
_chemical_formula_weight         675.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.7620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0999(4)
_cell_length_b                   10.0552(4)
_cell_length_c                   17.2639(7)
_cell_measurement_temperature    115(1)
_cell_volume                     1678.77(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      117(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14505
_diffrn_reflns_theta_full        28.71
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    11.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Dark-yellow
_exptl_crystal_density_diffrn    2.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.645
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.00014(3)
_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   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+3.0912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0580
_reflns_number_gt                3323
_reflns_number_total             3981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Pub.CIF
_cod_data_source_block           mer,trans[Ir(C(O)CH3)(CO)(py)2I2]
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4340154