New Rhodacarborane−Phosphoramidite Catalyst System for Enantioselective Hydrogenation of Functionalized Olefins and Molecular Structure of the Chiral Catalyst Precursor [3,3-{(S)-PipPhos}2-3-H-1,2-(o-xylylene)-closo-3,1,2-RhC2B9H9]
Alekseev, Leonid S.; Lyubimov, Sergey E.; Dolgushin, Fedor M.; Novikov, Valentin V.; Davankov, Vadim A.; Chizhevsky, Igor T.; Organometallics 30 (2011) 1942–; doi:10.1021/om101201e

data_4064238
_publ_section_title
;
 New Rhodacarborane&#x2212;Phosphoramidite Catalyst System for
 Enantioselective Hydrogenation of Functionalized Olefins and Molecular
 Structure of the Chiral Catalyst Precursor
 [3,3-{(S)-PipPhos}2-3-H-1,2-(o-xylylene)-closo-3,1,2-RhC2B9H9]
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1942
_journal_paper_doi               10.1021/om101201e
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety
'C60 H62 B9 N2 O4 P2 Rh, 2(C H2 Cl2), 0.25(H2 O)'
_chemical_formula_sum            'C62 H66.5 B9 Cl4 N2 O4.25 P2 Rh'
_chemical_formula_weight         1311.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.117(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1963(19)
_cell_length_b                   16.434(2)
_cell_length_c                   27.847(4)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.47
_cell_measurement_theta_min      2.34
_cell_volume                     6480.0(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.783
_diffrn_measured_fraction_theta_max 0.783
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            22577
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2698
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1525
_refine_ls_number_reflns         22637
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+3.5161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                19624
_reflns_number_total             22637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101201e_si_002.cif
_cod_data_source_block           twina5
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6480.1(15)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C62 H66.50 B9 Cl4 N2 O4.25 P2 Rh'
_cod_database_code               4064238