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_4304865
_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         'C100 H136 N12 O4 Si8 Y4'
_chemical_formula_sum            'C100 H136 N12 O4 Si8 Y4'
_chemical_formula_weight         2150.57
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5736(7)
_cell_length_b                   19.1832(10)
_cell_length_c                   45.840(3)
_cell_measurement_reflns_used    17768
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     11056.7(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1154
_diffrn_reflns_av_sigmaI/netI    0.1096
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            88689
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    2.217
_exptl_absorpt_correction_T_max  0.8785
_exptl_absorpt_correction_T_min  0.7466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1184
_refine_ls_number_reflns         21744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                17567
_reflns_number_total             21744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702461f-file003_3.cif
_cod_data_source_block           compound7
_cod_original_cell_volume        11056.7(10)
_cod_database_code               4304865