Modular Phosphole-Methano-Bridged-Phosphine(Borane) Ligands. Application to Rhodium-Catalyzed Reactions
Nguyen, Duc Hanh; Bayardon, Jérôme; Salomon-Bertrand, Christine; Jugé, Sylvain; Kalck, Philippe; Daran, Jean-Claude; Urrutigoity, Martine; Gouygou, Maryse; Organometallics 31 (2012) 857–; doi:10.1021/om2008265

data_4067852
_publ_section_title
;
 Modular Phosphole-Methano-Bridged-Phosphine(Borane) Ligands. Application
 to Rhodium-Catalyzed Reactions
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              857
_journal_paper_doi               10.1021/om2008265
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C37 H39 B2 F4 P2 Rh'
_chemical_formula_sum            'C37 H39 B2 F4 P2 Rh'
_chemical_formula_weight         746.15
_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-97
_cell_angle_alpha                86.543(3)
_cell_angle_beta                 76.688(3)
_cell_angle_gamma                84.720(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5502(4)
_cell_length_b                   11.3776(4)
_cell_length_c                   14.6834(6)
_cell_measurement_reflns_used    10839
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.4120
_cell_measurement_theta_min      2.6850
_cell_volume                     1706.51(11)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       '\w and \f'
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16841
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm, 
CrysAlis RED (Oxford Diffraction, 2009).
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       box
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7342
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.501
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0559P)^2^+1.4108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                6086
_reflns_number_total             7342
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2008265_si_002.cif
_cod_data_source_block           10b
_cod_database_code               4067852