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_4122413
_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 H92 Li4 N4 O6'
_chemical_formula_weight         776.95
_chemical_name_common            ccs23feb13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8399(9)
_cell_length_b                   12.7510(10)
_cell_length_c                   36.398(3)
_cell_measurement_temperature    198.(2)
_cell_volume                     5030.9(7)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      198.(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26351
_diffrn_reflns_theta_full        18.56
_diffrn_reflns_theta_max         18.56
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_process_details
;
;
_exptl_crystal_density_diffrn    1.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.225
_refine_ls_abs_structure_details
;
Flack x determined using 1342 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   1.1(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         3760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0720
_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^)+(0.1284P)^2^+8.9802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2028
_reflns_number_gt                3419
_reflns_number_total             3760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja505179y_si_010.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4122407--4122413.cif.'
_cod_database_code               4122413
_shelx_res_checksum              56788
_shelx_hkl_checksum              90745