Synthesis of Amidolanthanides with New Chiral Biaryl-Based NNO Ligands and Their Use as Catalysts for Enantioselective Hydroamination/Cyclization
Qiuwen Wang; Li Xiang; Haibin Song; Guofu Zi; Inorganic Chemistry 47 (2008) 4319–4328; doi:10.1021/ic702461f

data_4304868
_publ_section_title
;
Synthesis of Amidolanthanides with New Chiral Biaryl-Based NNO Ligands and
Their Use as Catalysts for Enantioselective Hydroamination/Cyclization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4319
_journal_page_last               4328
_journal_paper_doi               10.1021/ic702461f
_journal_volume                  47
_journal_year                    2008
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C116.50 H126 N9 O4 Si2 Yb3'
_chemical_formula_sum            'C116.5 H126 N9 O4 Si2 Yb3'
_chemical_formula_weight         2291.56
_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                 100.426(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7699(8)
_cell_length_b                   22.0136(10)
_cell_length_c                   31.2361(18)
_cell_measurement_reflns_used    17796
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      1.4
_cell_volume                     9988.4(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        crystalclear
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_sigmaI/netI    0.1326
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            76143
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.869
_exptl_absorpt_correction_T_max  0.9448
_exptl_absorpt_correction_T_min  0.8939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4632
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.696
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2401
_refine_ls_number_reflns         35126
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0711
_refine_ls_shift/su_max          0.128
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                29813
_reflns_number_total             35126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702461f-file003_6.cif
_cod_data_source_block           compound10
_cod_original_formula_sum        'C116.50 H126 N9 O4 Si2 Yb3'
_cod_database_code               4304868