Key Role of the Lewis Base Position in Asymmetric Bifunctional Catalysis: Design and Evaluation of a New Ligand for Chiral Polymetallic Catalysts
Ikuo Fujimori; Tsuyoshi Mita; Keisuke Maki; Motoo Shiro; Akihiro Sato; Sanae Furusho; Motomu Kanai; Masakatsu Shibasaki; Journal of the American Chemical Society 128 (2006) 16438–16439; doi:10.1021/ja067003h

data_4111306
_publ_section_title
;
 Key Role of the Lewis Base Position in Asymmetric Bifunctional Catalysis:
 Design and Evaluation of a New Ligand for Chiral Polymetallic Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16438
_journal_page_last               16439
_journal_paper_doi               10.1021/ja067003h
_journal_volume                  128
_journal_year                    2006
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C96 H87 F8 Gd3 O18 P4, 6(C3 H5 N), 2(H2 O) '
_chemical_formula_sum            'C114 H121 F8 Gd3 N6 O20 P4'
_chemical_formula_weight         2642.87
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.4996(4)
_cell_length_b                   17.5151(4)
_cell_length_c                   39.0416(9)
_cell_measurement_reflns_used    170582
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      3.6
_cell_volume                     11282.7(5)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (R/MSC, Rigaku, 2005)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (R/MSC, Rigaku, 2005)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.110
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            326018
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    1.887
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             5324.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.80
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  11886 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.006(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     1412
_refine_ls_number_reflns         25844
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.0070
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0097P)^2^+14.8355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                24127
_reflns_number_total             25844
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja067003hsi20060929_083829.cif
_cod_data_source_block           '_SC0013raplt'
_cod_original_formula_sum        'C114 H121 F8 Gd3 N6 O20 P4 '
_cod_database_code               4111306