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_4122411
_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            'C40 H88 Li4 N4 O6'
_chemical_formula_weight         748.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 105.542(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.037(5)
_cell_length_b                   10.268(4)
_cell_length_c                   17.665(6)
_cell_measurement_reflns_used    5371
_cell_measurement_temperature    198.(2)
_cell_measurement_theta_max      19.9748
_cell_measurement_theta_min      2.3167
_cell_volume                     2453.0(15)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12604
_diffrn_reflns_theta_full        20.05
_diffrn_reflns_theta_max         20.05
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_density_diffrn    1.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             832
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.141
_refine_ls_abs_structure_details
;
Flack x determined using 1617 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.8(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         4543
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          1.908
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+0.8744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                3925
_reflns_number_total             4543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja505179y_si_004.cif
_cod_data_source_block           I
_cod_depositor_comments
;
Adding full bibliography for 4122407--4122413.cif.

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C20 H44 Li2 N2 O3'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     374.45
_cod_database_code               4122411
_shelx_res_checksum              69523
_shelx_hkl_checksum              91586