Structural Understanding, Photoswitchability, and Supergelation of a New Class of Four Ring-Based Bent-Shaped Liquid Crystal.
Begum, Nazma; Kaur, Supreet; Mohiuddin, Golam; Nandi, Rajib; Gupta, Santosh Prasad; Rao, Nandiraju V. S.; Pal, Santanu Kumar; The journal of physical chemistry. B  (2019) –; doi:10.1021/acs.jpcb.9b01456

data_1551028
_publ_section_title
;
 Structural Understanding, Photoswitchability, and Supergelation of a New
 Class of Four Ring-Based Bent-Shaped Liquid Crystal.
;
_journal_name_full               'The journal of physical chemistry. B'
_journal_paper_doi               10.1021/acs.jpcb.9b01456
_journal_year                    2019
_chemical_formula_moiety         'C39 H43 Cl2 N3 O4'
_chemical_formula_sum            'C39 H43 Cl2 N3 O4'
_chemical_formula_weight         688.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                88.713(12)
_cell_angle_beta                 87.642(12)
_cell_angle_gamma                72.098(13)
_cell_formula_units_Z            2
_cell_length_a                   7.2493(10)
_cell_length_b                   9.8263(14)
_cell_length_c                   26.749(4)
_cell_measurement_reflns_used    799
_cell_measurement_temperature    298.0(2)
_cell_measurement_theta_max      24.1460
_cell_measurement_theta_min      2.6560
_cell_volume                     1811.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7f (Rigaku OD, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -67.00  27.00   0.50   10.00    --   29.89  54.00  30.00  188
  2  \w    -52.00 -26.00   0.50   10.00    --   29.89  54.00 120.00   52
  3  \w     44.00  70.00   0.50   10.00    --   29.89  54.00 120.00   52
  4  \w    -67.00 115.00   0.50   10.00    --   29.89  54.00 -90.00  364
;
_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      0.0691700000
_diffrn_orient_matrix_UB_12      0.0132589000
_diffrn_orient_matrix_UB_13      0.0156319000
_diffrn_orient_matrix_UB_21      0.0547986000
_diffrn_orient_matrix_UB_22      0.0109020000
_diffrn_orient_matrix_UB_23      -0.0214490000
_diffrn_orient_matrix_UB_31      -0.0529033000
_diffrn_orient_matrix_UB_32      0.0738932000
_diffrn_orient_matrix_UB_33      0.0000784000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.1118
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            9628
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.053
_diffrn_reflns_theta_min         2.646
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79341
_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    1.263
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.1761
_refine_ls_R_factor_gt           0.0706
_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^)+(0.0715P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.2344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2320
_reflns_number_total             6405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp9b01456_si_005.cif
_cod_data_source_block           nb-azo_rt
_cod_database_code               1551028
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C25 N4 O4 H23'
_reflns_odcompleteness_completeness 96.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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:
 C7(H7A,H7B), C10(H10A,H10B), C9(H9A,H9B), C6(H6A,H6B), C12(H12A,H12B),
 C11(H11A,H11B), C5(H5A,H5B), C3(H3A,H3B), C8(H8A,H8B), C4(H4A,H4B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C29(H29), C19(H19), C30(H30), C21(H21), C14(H14), C39(H39),
 C22(H22), C23(H23), C18(H18), C38(H38), C15(H15), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C1(H1A,H1B,H1C)
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 1.219
_oxdiff_exptl_absorpt_empirical_full_min 0.863