Enantioselective Hydroamination/Cyclization Catalyzed by Organolanthanide Amides Derived from a New Chiral Ligand, (S)-2-(Pyrrol-2-ylmethyleneamino)-2′-(dimethylamino)-1,1′-binaphthyl
Zi, Guofu; Xiang, Li; Song, Haibin; Organometallics 27 (2008) 1242–; doi:10.1021/om701058k

data_4070828
_publ_section_title
;
 Enantioselective Hydroamination/Cyclization Catalyzed by Organolanthanide
 Amides Derived from a New Chiral Ligand,
 (S)-2-(Pyrrol-2-ylmethyleneamino)-2&#x2032;-(dimethylamino)-1,1&#x2032;-binaphthyl
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1242
_journal_paper_doi               10.1021/om701058k
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C67 H70 N7 Si2 Y'
_chemical_formula_sum            'C67 H70 N7 Si2 Y'
_chemical_formula_weight         1118.39
_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                   11.4444(10)
_cell_length_b                   21.5082(16)
_cell_length_c                   24.216(2)
_cell_measurement_reflns_used    13824
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      1.7
_cell_volume                     5960.7(8)
_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 14.63
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            52865
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_T_max  0.9196
_exptl_absorpt_correction_T_min  0.8652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         12997
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0656
_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^)+(0.0197P)^2^+1.0476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1135
_reflns_number_gt                12104
_reflns_number_total             12997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701058k-file003.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        5960.6(8)
_cod_database_code               4070828