Intermolecular Hydroacylation: High Activity Rhodium Catalysts Containing Small-Bite-Angle Diphosphine Ligands
Adrian B. Chaplin; Joel F. Hooper; Andrew S. Weller; Michael C. Willis; Journal of the American Chemical Society 134 (2012) 4885–4897; doi:10.1021/ja211649a

data_4117649
_publ_section_title
;
 Intermolecular Hydroacylation: High Activity Rhodium Catalysts Containing
 Small-Bite-Angle Diphosphine Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4885
_journal_page_last               4897
_journal_paper_doi               10.1021/ja211649a
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C27 H47 F P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C59 H59 B F25 P2 Rh'
_chemical_formula_weight         1418.72
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                90.00
_cell_angle_beta                 113.8213(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.1637(2)
_cell_length_b                   12.7303(2)
_cell_length_c                   22.4993(3)
_cell_measurement_reflns_used    8446
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.575
_cell_measurement_theta_min      5.097
_cell_volume                     6069.41(14)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12887
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         5.14
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), 5687 Friedel pairs'
_refine_ls_abs_structure_Flack   0.597(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         12882
_refine_ls_number_restraints     509
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+5.8912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                11210
_reflns_number_total             12882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211649a_si_001_2.cif
_cod_data_source_block           1b-177abc10
_cod_original_cell_volume        6069.41(13)
_cod_database_code               4117649