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_4067851
_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         'C40 H40 P2'
_chemical_formula_sum            'C40 H40 P2'
_chemical_formula_weight         582.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7465(13)
_cell_length_b                   29.866(3)
_cell_length_c                   6.0097(5)
_cell_measurement_reflns_used    3522
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.2679
_cell_measurement_theta_min      3.1401
_cell_volume                     2287.8(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1672
_diffrn_reflns_av_sigmaI/netI    0.1228
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            16641
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.293
_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    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         4682
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1851
_refine_ls_R_factor_gt           0.1525
_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^)+(0.0000P)^2^+33.2279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3339
_refine_ls_wR_factor_ref         0.3495
_reflns_number_gt                3182
_reflns_number_total             4682
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om2008265_si_002.cif
_cod_data_source_block           5b
_cod_database_code               4067851