Enantiopure 1,2-bis(tert-butylmethylphosphino)benzene as a highly efficient ligand in rhodium-catalyzed asymmetric hydrogenation.
Tamura, Ken; Sugiya, Masashi; Yoshida, Kazuhiro; Yanagisawa, Akira; Imamoto, Tsuneo; Organic letters 12 (2010) 4400–4403; doi:10.1021/ol101936w

data_1503241
_publ_section_title
;
 Enantiopure 1,2-bis(tert-butylmethylphosphino)benzene as a highly
 efficient ligand in rhodium-catalyzed asymmetric hydrogenation.
;
_journal_issue                   19
_journal_name_full               'Organic letters'
_journal_page_first              4400
_journal_page_last               4403
_journal_paper_doi               10.1021/ol101936w
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety
;
'C24 H40 F6 P2 Rh Sb, C24 H40 F6 P2 Rh Sb, C4 H8 O2'
;
_chemical_formula_sum            'C52 H88 F12 O2 P4 Rh2 Sb2'
_chemical_formula_weight         1546.42
_chemical_name_common
;
(R,R)-1,2-Bis(tert-butylmethylphosphino)benzene(1,5-cyclooctadiene)rhodium(I) 
hexafluoroantiomonate 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.8880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3013(8)
_cell_length_b                   17.9217(15)
_cell_length_c                   18.9114(16)
_cell_measurement_reflns_used    3563
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.12
_cell_measurement_theta_min      2.20
_cell_volume                     3084.8(5)
_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      173
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17468
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    1.569
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_correction_T_min  0.7241
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.792
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10741
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.792
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0409
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                8594
_reflns_number_total             10741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol101936w_si_002.cif
_cod_data_source_block           yoshida01_p21
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               1503241