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_4112293
_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            'C6 H6 I4 Ir2 O4'
_chemical_formula_weight         1034.11
_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
_cell_angle_alpha                103.18(2)
_cell_angle_beta                 111.12(2)
_cell_angle_gamma                90.38(2)
_cell_formula_units_Z            1
_cell_length_a                   6.693(2)
_cell_length_b                   7.7050(10)
_cell_length_c                   8.731(2)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.079
_cell_measurement_theta_min      13.170
_cell_volume                     406.99(18)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1806
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        6.51
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    23.913
_exptl_absorpt_correction_T_max  0.206
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.219
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.811
_refine_diff_density_min         -3.136
_refine_diff_density_rms         0.603
_refine_ls_extinction_coef       0.0179(21)
_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_all   1.083
_refine_ls_goodness_of_fit_obs   1.094
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_restrained_S_obs      1.094
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_obs          0.0548
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1202P)^2^+4.4890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1585
_refine_ls_wR_factor_obs         0.1557
_reflns_number_observed          1339
_reflns_number_total             1414
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja039464ysi20031106_124155.cif
_cod_data_source_block           tgredo2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1202P)^2^+4.4890P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1202P)^2^+4.4890P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        407.0(2)
_cod_database_code               4112293