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_7103786
_publ_section_title
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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         '[SmL4{N(SiMe2H)}]'
_chemical_formula_sum            'C57 H92 N3 O2 Si2 Sm'
_chemical_formula_weight         1057.87
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.030(2)
_cell_angle_beta                 101.798(3)
_cell_angle_gamma                94.828(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1290(13)
_cell_length_b                   14.1565(17)
_cell_length_c                   19.349(2)
_cell_measurement_reflns_used    11143
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.83
_cell_volume                     2904.7(6)
_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 0.885
_diffrn_measured_fraction_theta_max 0.885
_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  0.0661
_diffrn_reflns_av_sigmaI/netI    0.1349
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28296
_diffrn_reflns_theta_full        29.22
_diffrn_reflns_theta_max         29.22
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.9377
_exptl_absorpt_correction_T_min  0.6965
_exptl_absorpt_correction_type   Semi-empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1122
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.163
_refine_diff_density_min         -2.170
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         13972
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0431P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                9141
_reflns_number_total             13972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305105f.txt
_cod_data_source_block           po17_[SmL4{N(SiMe2H)}]
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7103786