Mixed Aggregates of an Alkyl Lithium Reagent and a Chiral Lithium Amide Derived from N-Ethyl-O-triisopropylsilyl Valinol
Chicheung Su; Russell Hopson; Paul G. Williard; Journal of the American Chemical Society 135 (2013) 14367–14379; doi:10.1021/ja406912h

data_4120846
_publ_section_title
;
 Mixed Aggregates of an Alkyl Lithium Reagent and a Chiral Lithium Amide
 Derived from N-Ethyl-O-triisopropylsilyl Valinol
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14367
_journal_page_last               14379
_journal_paper_doi               10.1021/ja406912h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C42 H90 Li4 N2 O2 Si2'
_chemical_formula_weight         739.09
_chemical_name_common            ccs19feb`13
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_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
_cell_angle_alpha                84.247(5)
_cell_angle_beta                 82.647(5)
_cell_angle_gamma                80.286(5)
_cell_formula_units_Z            1
_cell_length_a                   8.8685(15)
_cell_length_b                   11.5116(18)
_cell_length_c                   12.3562(17)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    198.(2)
_cell_measurement_theta_max      26.0501
_cell_measurement_theta_min      2.7230
_cell_volume                     1229.1(3)
_computing_cell_refinement       'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      198.(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25239
_diffrn_reflns_theta_full        26.10
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.998
_exptl_crystal_description       chunk
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.302
_refine_ls_abs_structure_details
;
Flack x determined using 3846 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9277
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0827P)^2^+2.7446P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2239
_refine_ls_wR_factor_ref         0.2268
_reflns_number_gt                8585
_reflns_number_total             9277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja406912h_si_002.cif
_cod_data_source_block           I
_cod_database_code               4120846