Chiral-at-metal organolanthanides: enantioselective aminoalkene hydroamination/cyclisation with non-cyclopentadienyls
Peter Scott; Kevin M. Gillespie; Paul D. Knight; Colin Morton; O.Paul N; Chemical communications (Cambridge, England)  (2003) –; doi:10.1039/b305105f

data_7103785
_publ_section_title
;
Chiral-at-metal organolanthanides: enantioselective
aminoalkene hydroamination/cyclisation with non-cyclopentadienyls
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/b305105f
_journal_year                    2003
_chemical_formula_moiety         '[YL2{N(SiMe2H)2}(THF)]'
_chemical_formula_sum            'C46 H64 N3 O3 Si2 Y'
_chemical_formula_weight         852.09
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 95.16(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.92(2)
_cell_length_b                   17.51(3)
_cell_length_c                   16.80(2)
_cell_measurement_reflns_used    6479
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.93
_cell_measurement_theta_min      2.57
_cell_volume                     4666(12)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens SMART diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3069
_diffrn_reflns_av_sigmaI/netI    0.3744
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20959
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  0.9003
_exptl_absorpt_correction_T_min  0.7660
_exptl_absorpt_correction_type   Semi-empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         6070
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.3134
_refine_ls_R_factor_gt           0.1607
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.1302P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3003
_refine_ls_wR_factor_ref         0.3725
_reflns_number_gt                2094
_reflns_number_total             6070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305105f.txt
_cod_data_source_block           po10_[YL2{N(SiMe2H)2}(THF)]
_cod_original_sg_symbol_H-M      P2(1)/a
_cod_database_code               7103785