Synthesis of Oxygen- and Sulfur-Bridged Dirhodium Complexes and Their Use As Catalysts in the Chemoselective Hydrogenation of Alkenes
Zhu, Chuan; Yukimura, Noriaki; Yamane, Motoki; Organometallics 29 (2010) 2098–; doi:10.1021/om100067r

data_4065682
_publ_section_title
;
 Synthesis of Oxygen- and Sulfur-Bridged Dirhodium Complexes and Their Use
 As Catalysts in the Chemoselective Hydrogenation of Alkenes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2098
_journal_paper_doi               10.1021/om100067r
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C50 H53 Cl7 O5 P2 Rh2'
_chemical_formula_weight         1249.83
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                79.908(8)
_cell_angle_beta                 79.935(8)
_cell_angle_gamma                80.945(8)
_cell_formula_units_Z            2
_cell_length_a                   13.389(4)
_cell_length_b                   13.783(4)
_cell_length_c                   14.458(4)
_cell_measurement_reflns_used    8705
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0402
_cell_volume                     2564.2(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0287
_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       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16324
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.7305
_exptl_absorpt_correction_T_min  0.6052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998) Private communication
;
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0333P)^2^+4.4785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0789
_reflns_number_gt                7782
_reflns_number_total             8705
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100067r_si_002.cif
_cod_data_source_block           m_O_Rh
_cod_original_cell_volume        2564.1(14)
_cod_database_code               4065682