Chiral lithium diamides derived from linked N-isopropyl valinol or alaninol.
Su, Chicheung; Guang, Jie; Li, Weibin; Wu, Kuiwang; Hopson, Russell; Williard, Paul G.; Journal of the American Chemical Society 136 (2014) 11735–11747; doi:10.1021/ja505179y

data_4122407
_publ_section_title
;
 Chiral lithium diamides derived from linked N-isopropyl valinol or
 alaninol.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11735
_journal_page_last               11747
_journal_paper_doi               10.1021/ja505179y
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C42 H88 Li4 N4 O6'
_chemical_formula_weight         772.92
_chemical_name_common            ccs21feb13
_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                101.548(4)
_cell_angle_beta                 93.004(4)
_cell_angle_gamma                100.111(4)
_cell_formula_units_Z            1
_cell_length_a                   9.1291(13)
_cell_length_b                   10.2451(15)
_cell_length_c                   13.7745(17)
_cell_measurement_temperature    198.(2)
_cell_volume                     1237.5(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      198.(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14854
_diffrn_reflns_theta_full        20.39
_diffrn_reflns_theta_max         20.39
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.185
_refine_ls_abs_structure_details
;
Flack x determined using 2080 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         4734
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0659P)^2^+0.4970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1160
_reflns_number_gt                4447
_reflns_number_total             4734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja505179y_si_009.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4122407--4122413.cif.'
_cod_database_code               4122407
_shelx_res_checksum              12262
_shelx_hkl_checksum              86820