Understanding the remarkable difference in liquid crystal behaviour between secondary and tertiary amides: the synthesis and characterisation of new benzanilide-based liquid crystal dimers.
Imrie, Corrie T.; Strachan, Grant James; Harrison, William T.; Storey, John M. D.; Physical Chemistry Chemical Physics  (2021) –; doi:10.1039/D1CP01125A

data_7242746
_publ_section_title
;
 Understanding the remarkable difference in liquid crystal behaviour
 between secondary and tertiary amides: the synthesis and characterisation
 of new benzanilide-based liquid crystal dimers.
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D1CP01125A
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C47 H41 N3 O2'
_chemical_formula_sum            'C47 H41 N3 O2'
_chemical_formula_weight         679.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-07-16 deposited with the CCDC.	2021-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.551(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   31.5211(4)
_cell_length_b                   14.7867(2)
_cell_length_c                   33.4555(5)
_cell_measurement_reflns_used    25292
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.9630
_cell_measurement_theta_min      2.9980
_cell_volume                     14401.1(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            129158
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.063
_diffrn_reflns_theta_min         2.860
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystAlisPro
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             5760
_exptl_crystal_preparation       'Liquid crystal precursor'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 9087 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.23(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1593
_refine_ls_number_reflns         26665
_refine_ls_number_restraints     538
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1276P)^2^+19.2313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2115
_refine_ls_wR_factor_ref         0.2221
_reflns_Friedel_coverage         0.978
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                22766
_reflns_number_total             26665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp01125a2.cif
_cod_data_source_block           b52b
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7242746
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.943
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              20577