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_4311754
_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            'C50.5 H50 F6 N2 O0.5 P3 Rh'
_chemical_formula_weight         1002.74
_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                 124.853(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.3124(7)
_cell_length_b                   21.0184(5)
_cell_length_c                   18.1676(4)
_cell_measurement_reflns_used    22397
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.97
_cell_volume                     9185.3(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.843
_diffrn_measured_fraction_theta_max 0.843
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0741
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9302
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8219
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            irregular
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       red
_exptl_crystal_F_000             4120
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.240
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+0.0588P^2^+0.5327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                7083
_reflns_number_total             9302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049227bsi20040614_043132.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        9185.2(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C50.50 H50 F6 N2 O0.50 P3 Rh'
_cod_database_code               4311754