Captured at last: a catalyst-substrate adduct and a Rh-dihydride solvate in the asymmetric hydrogenation by a Rh-monophosphine catalyst
Ilya D. Gridnev; Elisabetta Alberico; Serafino Gladiali; Chem.Commun. 48 (2012) 2186–; doi:10.1039/c2cc17335b

data_7107373
_publ_section_title
;
 Captured at last: a catalyst-substrate adduct and a Rh-dihydride solvate
 in the asymmetric hydrogenation by a Rh-monophosphine catalyst
;
_journal_coden_Cambridge         0182
_journal_name_full               Chem.Commun.
_journal_page_first              2186
_journal_paper_doi               10.1039/c2cc17335b
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C66 H53 Cl9 F6 P2 Rh Sb'
_chemical_formula_sum            'C66 H53 Cl9 F6 P2 Rh Sb'
_chemical_formula_weight         1565.82
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.1730(13)
_cell_length_b                   22.609(3)
_cell_length_c                   25.378(3)
_cell_measurement_reflns_used    4303
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.01
_cell_volume                     6410.7(14)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR2002 (Burla, et al., 2003)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            47979
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3128.00
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.070
_refine_diff_density_max         3.060
_refine_diff_density_min         -2.420
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 6601 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     820
_refine_ls_number_reflns         14590
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 1.7100\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                12632
_reflns_number_total             14633
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c2cc17335b.txt
_cod_data_source_block           global
_cod_original_cell_volume        6410.7(13)
_cod_database_code               7107373