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_1556640
_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         'C35 H36 Cl N3 O4'
_chemical_formula_sum            'C35 H36 Cl N3 O4'
_chemical_formula_weight         598.12
_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     dual
_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                92.541(3)
_cell_angle_beta                 91.378(4)
_cell_angle_gamma                109.089(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3765(4)
_cell_length_b                   9.2524(4)
_cell_length_c                   21.5856(8)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    298.0(2)
_cell_measurement_theta_max      21.0940
_cell_measurement_theta_min      2.7020
_cell_volume                     1578.08(12)
_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_temperature      298.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  46.00   0.30   10.00    --   29.89  54.00  90.00  380
  2  \w     29.00  54.80   0.30   10.00    --   29.89  54.00-180.00   86
  3  \w    -66.00 115.80   0.30   10.00    --   29.89  54.00 -30.00  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      -0.0219656000
_diffrn_orient_matrix_UB_12      -0.0016793000
_diffrn_orient_matrix_UB_13      -0.0320278000
_diffrn_orient_matrix_UB_21      -0.0596378000
_diffrn_orient_matrix_UB_22      0.0371297000
_diffrn_orient_matrix_UB_23      0.0072194000
_diffrn_orient_matrix_UB_31      0.0632701000
_diffrn_orient_matrix_UB_32      0.0722461000
_diffrn_orient_matrix_UB_33      -0.0024095000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8206
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.565
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89723
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1462
_refine_ls_R_factor_gt           0.0700
_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^)+(0.1108P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.2598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2279
_reflns_number_total             5532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp9b09326_si_003.cif
_cod_data_source_block           7-(o)m-cl
_cod_database_code               1556640
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.968
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1Aa,H1Ab,H1Ac} of C1A, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, {H29a,H29b,H29c} of C29, {H21a,H21b,H21c} of C21
2. Uiso/Uaniso restraints and constraints
Uanis(C2A)
3. Others
 Sof(H3bc)=Sof(H3bd)=Sof(C1B)=Sof(H1Ba)=Sof(H1Bb)=Sof(H1Bc)=Sof(C2B)=Sof(H2Ba)=
 Sof(H2Bb)=1-FVAR(1)
 Sof(H3aa)=Sof(H3ab)=Sof(C2A)=Sof(H2Aa)=Sof(H2Ab)=Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=
 Sof(H1Ac)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C4(H4a,H4b), C5(H5a,H5b), C7(H7a,H7b), C3(H3aa,H3ab), C2A(H2Aa,
 H2Ab)
4.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C14(H14), C18(H18), C24(H24), C31(H31), C27(H27), C13(H13),
 C35(H35), C16(H16), C9(H9), C32(H32), C10(H10), C17(H17), C34(H34)
4.c Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C29(H29a,H29b,H29c), C1A(H1Aa,H1Ab,H1Ac)
4.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_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 1.097
_oxdiff_exptl_absorpt_empirical_full_min 0.942