Remarkably Stable Chiral Zirconium Complexes for Asymmetric Mannich-Type Reactions
Kowichiro Saruhashi; Shū Kobayashi; Journal of the American Chemical Society 128 (2006) 11232–11235; doi:10.1021/ja062776r

data_4110843
_publ_section_title
;
 Remarkably Stable Chiral Zirconium Complexes for Asymmetric Mannich-Type
 Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11232
_journal_page_last               11235
_journal_paper_doi               10.1021/ja062776r
_journal_volume                  128
_journal_year                    2006
_chemical_absolute_configuration ad
_chemical_formula_sum            'C120 H60 Br12 O16 Zr4'
_chemical_formula_weight         3081.51
_space_group_IT_number           209
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      209
_symmetry_space_group_name_Hall  'F 4 2 3'
_symmetry_space_group_name_H-M   'F 4 3 2'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   32.163(5)
_cell_length_b                   32.163(5)
_cell_length_c                   32.163(5)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      3.1
_cell_volume                     33271(9)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            71835
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_exptl_absorpt_coefficient_mu    3.178
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             11904.00
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.44
_refine_diff_density_min         -0.66
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  966 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.513
_refine_ls_number_parameters     68
_refine_ls_number_reflns         2444
_refine_ls_R_factor_gt           0.1126
_refine_ls_shift/su_max          0.1530
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3523
_reflns_number_gt                1985
_reflns_number_total             2444
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja062776rsi20060628_075108.cif
_cod_data_source_block           x
_cod_original_formula_sum        'C120 H60 Br12 O16 Zr4 '
_cod_database_code               4110843