Photoswitchable Bent-Core Nematic Liquid Crystals with Methylated Azobenzene Wing Exhibiting Optic-Field-Enhanced Fréedericksz Transition Effect
Begum, Nazma; Kaur, Supreet; Xiang, Ying; Yin, Heng; Mohiuddin, Golam; Rao, Nandiraju V. S.; Pal, Santanu Kumar; The Journal of Physical Chemistry C  (2019) –; doi:10.1021/acs.jpcc.9b09326

data_1556641
_publ_section_title
;
 Photoswitchable Bent-Core Nematic Liquid Crystals with Methylated
 Azobenzene Wing Exhibiting Optic-Field-Enhanced Fr\'eedericksz Transition
 Effect
;
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_paper_doi               10.1021/acs.jpcc.9b09326
_journal_year                    2019
_chemical_formula_moiety         'C33 H32 Cl N3 O4'
_chemical_formula_sum            'C33 H32 Cl N3 O4'
_chemical_formula_weight         570.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.120(7)
_cell_angle_beta                 99.083(8)
_cell_angle_gamma                95.775(6)
_cell_formula_units_Z            2
_cell_length_a                   8.2760(7)
_cell_length_b                   9.9957(6)
_cell_length_c                   17.6584(19)
_cell_measurement_reflns_used    1985
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      32.2680
_cell_measurement_theta_min      2.9340
_cell_volume                     1434.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -68.00  27.10   0.30   20.00    --   29.89  54.00  30.00  317
  2  \w     81.00 106.80   0.30   20.00    --   29.89  54.00-180.00   86
  3  \w    -68.00 113.80   0.30   20.00    --   29.89  54.00 -90.00  606
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0647544000
_diffrn_orient_matrix_UB_12      0.0000581000
_diffrn_orient_matrix_UB_13      0.0219536000
_diffrn_orient_matrix_UB_21      0.0578040000
_diffrn_orient_matrix_UB_22      0.0002177000
_diffrn_orient_matrix_UB_23      0.0342528000
_diffrn_orient_matrix_UB_31      0.0087940000
_diffrn_orient_matrix_UB_32      0.0713306000
_diffrn_orient_matrix_UB_33      0.0006208000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10905
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.715
_diffrn_reflns_theta_min         2.591
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         8876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0698P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5555
_reflns_number_total             8876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp9b09326_si_002.cif
_cod_data_source_block           5-mm-cl
_cod_database_code               1556641
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C29(H29a,H29b), C31(H31a,H31b), C30(H30a,H30b), C32(H32a,H32b)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C5(H5), C20(H20), C6(H6), C27(H27), C19(H19), C3(H3a), C11(H11),
 C28(H28), C25(H25), C8(H8), C22(H22), C9(H9), C2(H2)
2.c Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C13(H13a,H13b,H13c), C33(H33a,H33b,H33c)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.379
_oxdiff_exptl_absorpt_empirical_full_min 0.709