Mechanistic Study of Rhodium/xantphos-Catalyzed Methanol Carbonylation
Williams, Gary L.; Parks, Christopher M.; Smith, C. Robert; Adams, Harry; Haynes, Anthony; Meijer, Anthony J. H. M.; Sunley, Glenn J.; Gaemers, Sander; Organometallics 30 (2011) 6166–; doi:10.1021/om2006968

data_4065298
_publ_section_title
;
 Mechanistic Study of Rhodium/xantphos-Catalyzed Methanol Carbonylation
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6166
_journal_paper_doi               10.1021/om2006968
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C46.5 H46 B F4 O2 P2 Rh'
_chemical_formula_weight         888.49
_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                 100.902(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.755(3)
_cell_length_b                   31.222(6)
_cell_length_c                   16.892(3)
_cell_measurement_reflns_used    3557
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.681
_cell_measurement_theta_min      4.61
_cell_volume                     8677(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      150(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.2225
_diffrn_reflns_av_sigmaI/netI    0.2610
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            84602
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.9449
_exptl_absorpt_correction_T_min  0.8266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.135
_refine_diff_density_min         -1.791
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         15273
_refine_ls_number_restraints     769
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.1852
_refine_ls_R_factor_gt           0.0834
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1073P)^2^+0.4118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1933
_refine_ls_wR_factor_ref         0.2287
_reflns_number_gt                5478
_reflns_number_total             15273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2006968_si_002.cif
_cod_data_source_block           iah242m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2025-11-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C93 H92 B2 F8 O4 P4 Rh2'
_cod_original_formula_weight         1776.99
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4065298