Rhodium-Hydrido-Benzylamine-Triphenylphosphine Complexes: Solid-State and Solution Structures and Implications in Catalyzed Imine Hydrogenation
Paolo Marcazzan; Brian O. Patrick; Brian R. James; Inorganic Chemistry 43 (2004) 6838–6841; doi:10.1021/ic049227b

data_4311753
_publ_section_title
;
 Rhodium-Hydrido-Benzylamine-Triphenylphosphine Complexes: Solid-State and
 Solution Structures and Implications in Catalyzed Imine Hydrogenation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6838
_journal_page_last               6841
_journal_paper_doi               10.1021/ic049227b
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C52 H54 Cl4 F6 N2 P3 Rh'
_chemical_formula_weight         1158.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 95.948(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7776(9)
_cell_length_b                   21.9566(14)
_cell_length_c                   19.2997(14)
_cell_measurement_reflns_used    14423
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      1.85
_cell_volume                     5806.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.071
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6625
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8158
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0011(2)
_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   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6625
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0600
_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^)+0.0996P^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1681
_reflns_number_gt                4488
_reflns_number_total             6625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049227bsi20040614_043101.cif
_cod_data_source_block           bj372
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4311753