Lewis Acids and Lewis Acid-Functionalized Ligands in Rhodium-Catalyzed Methyl Acetate Carbonylation
Conifer, Christopher M.; Law, David J.; Sunley, Glenn J.; White, Andrew J. P.; Britovsek, George J. P.; Organometallics 30 (2011) 4060–; doi:10.1021/om200341t

data_4064793
_publ_section_title
;
 Lewis Acids and Lewis Acid-Functionalized Ligands in Rhodium-Catalyzed
 Methyl Acetate Carbonylation
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4060
_journal_paper_doi               10.1021/om200341t
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C44 H33 B O2 P2 Rh, F6 Sb, C H2 Cl2'
_chemical_formula_sum            'C45 H35 B Cl2 F6 O2 P2 Rh Sb'
_chemical_formula_weight         1090.04
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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
_cell_angle_beta                 110.0615(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4627(3)
_cell_length_b                   15.58519(17)
_cell_length_c                   15.9429(2)
_cell_measurement_reflns_used    25148
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.4600
_cell_measurement_theta_min      3.7499
_cell_volume                     4309.14(11)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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      173(2)
_diffrn_detector_area_resol_mean 15.9863
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            67443
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         32.54
_diffrn_reflns_theta_min         3.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) 
(compiled May  8 2007,13:10:02) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'Pale brown'
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.958
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         14435
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0586P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                9106
_reflns_number_total             14435
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200341t_si_002.cif
_cod_data_source_block           '[Rh(CO)2(BPP)](SbF6)'
_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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4064793