Two precatalysts for application in asymmetric homogeneous hydrogenation
Meißner, Antje; Pribbenow, Cornelia; Drexler, Hans-Joachim; Heller, Detlef; Acta Crystallographica Section C 70 (2014) 941–944; doi:10.1107/S205322961401910X

data_2019652
_publ_section_title
;
 Two precatalysts for application in asymmetric homogeneous hydrogenation
;
_journal_coeditor_code           EG3166
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              941
_journal_page_last               944
_journal_paper_doi               10.1107/S205322961401910X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Rh (C34 H36 P2) (C7 H8)] B F4'
_chemical_formula_moiety         'C41 H44 P2 Rh +, B F4 -'
_chemical_formula_sum            'C41 H44 B F4 P2 Rh'
_chemical_formula_weight         788.42
_chemical_name_systematic
'[(1<i>R</i>,1'<i>R</i>,2<i>R</i>,2'<i>R</i>)-2,2'-Bis(diphenylphosphanyl)-1,1'-dicyclopentane](\h^4^-norbornadiene)rhodium(I) tetrafluoroborate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.17(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.002(2)
_cell_length_b                   9.0293(18)
_cell_length_c                   39.251(8)
_cell_measurement_reflns_used    16122
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.00
_cell_volume                     3530.4(12)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2005)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'rotation method'
_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  0.0871
_diffrn_reflns_av_sigmaI/netI    0.1088
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            38678
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.8969
_exptl_absorpt_correction_T_min  0.4531
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_refine_diff_density_max         2.804
_refine_diff_density_min         -1.092
_refine_ls_abs_structure_details 'Flack (1983), with 5782 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         12426
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0481P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                7748
_reflns_number_total             12426
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3166sup1.cif
_cod_data_source_block           RhBICPnbdBF4
_cod_depositor_comments
'Adding full bibliography for 2019652--2019653.cif.'
_cod_database_code               2019652
_cod_database_fobs_code          2019652