Structure and molecular packing in smectic BCr and Ad phases of Schiff base liquid crystal compounds through analyses of layer spacing, entropy and crystal structure
Yamamura, Yasuhisa; Murakoshi, Takahito; Iwagaki, Sakiko; Osiecka, Natalia; Galewski, Zbigniew; Saitoh, Hideki; Hishida, Mafumi; Massalska-Arodz, Maria; SAITO, Kazuya; Phys. Chem. Chem. Phys.  (2017) –; doi:10.1039/C7CP03863A

data_7228621
_publ_section_title
;
 Structure and molecular packing in smectic BCr and Ad phases of Schiff
 base liquid crystal compounds through analyses of layer spacing, entropy
 and crystal structure
;
_journal_name_full               'Phys. Chem. Chem. Phys.'
_journal_paper_doi               10.1039/C7CP03863A
_journal_year                    2017
_chemical_formula_iupac          'C18 H20 Cl N1 O1'
_chemical_formula_moiety         'C18 H20 Cl N O'
_chemical_formula_sum            'C18 H20 Cl N O'
_chemical_formula_weight         301.81
_chemical_name_common            4-chlorobenzylidene-4'-pentyloxyaniline
_chemical_name_systematic        4-chlorobenzylidene-4'-pentyloxyaniline
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2017-03-28 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1002(3)
_cell_length_b                   7.3335(4)
_cell_length_c                   36.4538(18)
_cell_measurement_reflns_used    3922
_cell_measurement_temperature    295.(2)
_cell_measurement_theta_max      22.7969
_cell_measurement_theta_min      1.1029
_cell_volume                     1630.79(14)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 v2014.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \W scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            10115
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.12
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.345
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.112
_refine_diff_density_min         -0.144
_refine_ls_abs_structure_details
;
Flack x determined using 914 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3309
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0584P)^2^+0.0894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                2553
_reflns_number_total             3309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cp03863a2.cif
_cod_data_source_block           I
_cod_database_code               7228621
_shelx_res_checksum              68006