Structures of Lithium N-Monosubstituted Anilides: Trisolvated Monomer to Tetrasolvated Dimer.
Su, Chicheung; Guang, Jie; Williard, Paul G.; The Journal of organic chemistry 79 (2014) 1032–; doi:10.1021/jo402498z

data_4029029
_publ_section_title
;
 Structures of Lithium N-Monosubstituted Anilides: Trisolvated Monomer to
 Tetrasolvated Dimer.
;
_journal_issue                   3
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1032
_journal_paper_doi               10.1021/jo402498z
_journal_volume                  79
_journal_year                    2014
_chemical_formula_sum            'C32 H52 Li2 N2 O3'
_chemical_formula_weight         526.64
_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
_cell_angle_alpha                90
_cell_angle_beta                 103.175(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.898(4)
_cell_length_b                   14.874(6)
_cell_length_c                   17.747(5)
_cell_measurement_temperature    198.(2)
_cell_volume                     3315.1(19)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      198.(2)
_diffrn_measured_fraction_theta_full 0.873
_diffrn_measured_fraction_theta_max 0.873
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5887
_diffrn_reflns_theta_full        19.63
_diffrn_reflns_theta_max         19.63
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_process_details
;
;
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.286
_refine_ls_abs_structure_details
;
Flack x determined using 1255 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   2.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         4555
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0830
_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^)+(0.1333P)^2^+2.5890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2254
_reflns_number_gt                3638
_reflns_number_total             4555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo402498z_si_002.cif
_cod_data_source_block           958152
_cod_depositor_comments
;

2020-10-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        3315.(2)
_cod_original_formula_sum        'C16 H26 Li N O1.50'
_cod_original_formula_units_Z    8
_cod_original_formula_weight     263.32
_cod_database_code               4029029
_shelx_res_checksum              9843
_shelx_hkl_checksum              68779