Promotion of Iridium-Catalyzed Methanol Carbonylation: Mechanistic Studies of the Cativa Process
Anthony Haynes; Peter M. Maitlis; George E. Morris; Glenn J. Sunley; Harry Adams; Peter W. Badger; Craig M. Bowers; David B. Cook; Paul I. P. Elliott; Talit Ghaffar; Helena Green; Tim R. Griffin; Marc Payne; Jean M. Pearson; Michael J. Taylor; Paul W. Vickers; Rob J. Watt; Journal of the American Chemical Society 126 (2004) 2847–2861; doi:10.1021/ja039464y

data_4112294
_publ_section_title
;
 Promotion of Iridium-Catalyzed Methanol Carbonylation: Mechanistic
 Studies of the Cativa Process
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2847
_journal_page_last               2861
_journal_paper_doi               10.1021/ja039464y
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C28 H23 As I3 Ir O3'
_chemical_formula_weight         1055.28
_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                 110.277(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.351(3)
_cell_length_b                   16.500(4)
_cell_length_c                   15.971(4)
_cell_measurement_reflns_used    116
_cell_measurement_temperature    100(2)
_cell_volume                     3053.1(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19149
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    8.509
_exptl_absorpt_correction_T_max  0.2681
_exptl_absorpt_correction_T_min  0.1244
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.296
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.946
_refine_diff_density_min         -1.435
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0418P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                5870
_reflns_number_total             7319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039464ysi20031106_124248.cif
_cod_data_source_block           iah89m
_cod_original_cell_volume        3053.1(12)
_cod_database_code               4112294