Synthesis, Coordination to Rh(I), and Hydroformylation Catalysis of New β-Aminophosphines Bearing a Dangling Nitrogen Group: An Unusual Inversion of a Rh-Coordinated P Center
Jacques Andrieu; Philippe Richard; Jean-Michel Camus; Rinaldo Poli; Inorganic Chemistry 41 (2002) 3876–3885; doi:10.1021/ic011035i

data_4318231
_publ_contact_author_address
;
L.S.E.O. Facult\'e des Sciences,
6 Bd Gabriel 21000 Dijon, FRANCE
;
_publ_contact_author_email       Jacques.Andrieu@u-bourgogne.fr
_publ_contact_author_fax         +33-0380396073
_publ_contact_author_name        'Dr Jacques ANDRIEU'
_publ_contact_author_phone       +33-0380396880
_publ_section_title
;
 Synthesis, Coordination to Rh(I), and Hydroformylation Catalysis of New
 \b-Aminophosphines Bearing a Dangling Nitrogen Group: An Unusual
 Inversion of a Rh-Coordinated P Center
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3876
_journal_page_last               3885
_journal_paper_doi               10.1021/ic011035i
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C41 H45 Cl N2 O2.5 P Rh'
_chemical_formula_weight         775.12
_chemical_name_systematic
;
 ?
;
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.3710(10)
_cell_angle_beta                 82.5370(10)
_cell_angle_gamma                78.4730(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8621(4)
_cell_length_b                   12.7054(4)
_cell_length_c                   12.9551(5)
_cell_measurement_reflns_used    5985
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     1844.59(11)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius,1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett, 1996)'
_computing_publication_material  'SHELXL97 and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f scans (\k = 0) + additional \w scans'
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13427
_diffrn_reflns_theta_full        27.74
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.177
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0077(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.7958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                6479
_reflns_number_total             8258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic011035i_2.cif
_cod_data_source_block           p33s(compound1')
_cod_original_formula_sum        'C41 H45 Cl N2 O2.50 P Rh'
_cod_database_code               4318231