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_4029026
_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            'C13 H20 Li N O'
_chemical_formula_weight         213.24
_chemical_name_common            ccs09jul12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 97.819(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3268(14)
_cell_length_b                   9.5932(16)
_cell_length_c                   14.897(2)
_cell_measurement_reflns_used    2196
_cell_measurement_temperature    198.(2)
_cell_measurement_theta_max      20.7553
_cell_measurement_theta_min      2.5330
_cell_volume                     1320.5(3)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7103
_diffrn_reflns_theta_full        21.83
_diffrn_reflns_theta_max         21.83
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.460
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.1051
_refine_ls_shift/su_max          4.194
_refine_ls_shift/su_mean         0.170
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1167P)^2^+3.3567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2539
_refine_ls_wR_factor_ref         0.2883
_reflns_number_gt                1061
_reflns_number_total             1573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo402498z_si_002.cif
_cod_data_source_block           958145
_cod_original_cell_volume        1320.5(4)
_cod_database_code               4029026
_shelx_res_checksum              81400
_shelx_hkl_checksum              35072