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_4065683
_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            'C49 H53 Cl3 O4 P2 Rh2 S'
_chemical_formula_weight         1112.08
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.584(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.427(6)
_cell_length_b                   24.331(10)
_cell_length_c                   14.036(6)
_cell_measurement_reflns_used    7873
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0402
_cell_volume                     4521(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26570
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_T_max  0.6742
_exptl_absorpt_correction_T_min  0.6168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998) Private communication
;
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.638
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0499P)^2^+13.9874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                6756
_reflns_number_total             7873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100067r_si_002.cif
_cod_data_source_block           m_S_Rh
_cod_original_cell_volume        4522(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4065683