Photo-and thermoresponsive N-salicylideneaniline derivatives: solid-state studies and structural aspects
Hulushe, Siya T.; Malan, Frederick P.; Hosten, Eric C.; Lobb, Kevin A.; Khanye, Setshaba D.; Watkins, Gareth M.; New Journal of Chemistry  (2022) –; doi:10.1039/D1NJ03056F

data_7061988
_publ_section_title
;
 Photo-and thermoresponsive N-salicylideneaniline derivatives: solid-state
 studies and structural aspects
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/D1NJ03056F
_journal_year                    2022
_chemical_formula_moiety         'C13 H9 Br N2 O3'
_chemical_formula_sum            'C13 H8 Br N2 O3'
_chemical_formula_weight         320.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-25
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.05 svn.r3537 for Rigaku Oxford Diffraction, GUI svn.r5625)
;
_audit_update_record
;
2022-03-04 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.2470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.59950(10)
_cell_length_b                   11.5868(2)
_cell_length_c                   14.0731(2)
_cell_measurement_reflns_used    12463
_cell_measurement_temperature    299.95(13)
_cell_measurement_theta_max      78.5800
_cell_measurement_theta_min      3.1410
_cell_volume                     1235.79(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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      air
_diffrn_ambient_temperature      299.95(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_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     30.00 119.00   0.50    0.05    --   46.83  63.00-104.00  178
  2  \w     24.00 119.00   0.50    0.05    --   46.83  77.00 -60.00  190
  3  \w     24.00 119.00   0.50    0.05    --   46.83  77.00  30.00  190
  4  \w     24.00 119.00   0.50    0.05    --   46.83  77.00 150.00  190
  5  \w    -64.00  26.00   0.50    0.05    --  -46.83  63.00-104.00  180
  6  \w     -5.00  29.00   0.50    0.05    --  -46.83  19.00  30.00   68
  7  \w     -5.00  29.00   0.50    0.05    --  -46.83  19.00-120.00   68
  8  \w     -5.00  29.00   0.50    0.05    --  -46.83  19.00-150.00   68
  9  \w     93.00 178.00   0.50    0.07    --  110.25  63.00-104.00  170
 10  \w     94.00 178.00   0.50    0.07    --  110.25  61.00-180.00  168
 11  \w     98.00 178.00   0.50    0.07    --  110.25  45.00-150.00  160
 12  \w     97.00 175.00   0.50    0.07    --  110.25  15.00-180.00  156
 13  \w     98.00 178.00   0.50    0.07    --  110.25  45.00 -60.00  160
 14  \w     98.00 178.00   0.50    0.07    --  110.25  30.00  90.00  160
 15  \w     38.00 106.00   0.50    0.07    --  110.25 -94.00 -90.00  136
 16  \w     38.00 106.00   0.50    0.07    --  110.25 -94.00-180.00  136
 17  \w     18.00  95.00   0.50    0.05    --   46.83-125.00 -30.00  154
 18  \w     38.00 106.00   0.50    0.07    --  110.25 -94.00   0.00  136
 19  \w     38.00  80.00   0.50    0.07    --  110.25 -61.00  60.00   84
 20  \w     38.00  85.00   0.50    0.07    --  110.25 -63.00 119.00   94
 21  \w     38.00 133.00   0.50    0.07    --  110.25 -77.00   0.00  190
 22  \w     38.00  80.00   0.50    0.07    --  110.25 -61.00 -90.00   84
 23  \w     38.00  80.00   0.50    0.07    --  110.25 -61.00   0.00   84
 24  \w    -25.00  64.00   0.50    0.05    --   46.83 -63.00 119.00  178
 25  \w   -175.00-110.00   0.50    0.07    -- -102.00 -77.00  90.00  130
 26  \w   -118.00 -30.00   0.50    0.05    --  -46.83 -63.00 119.00  176
 27  \w   -175.00 -85.00   0.50    0.07    -- -102.00 -63.00 119.00  180
 28  \w   -167.00 -88.00   0.50    0.07    -- -102.00 -15.00   0.00  158
 29  \w    -77.00 -29.00   0.50    0.07    -- -102.00  63.00-104.00   96
 30  \w    -72.00 -29.00   0.50    0.07    -- -102.00  61.00  30.00   86
 31  \w    -72.00 -29.00   0.50    0.07    -- -102.00  61.00  60.00   86
 32  \w    -72.00 -29.00   0.50    0.07    -- -102.00  61.00  90.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0971505000
_diffrn_orient_matrix_UB_12      0.0960874000
_diffrn_orient_matrix_UB_13      0.0507843000
_diffrn_orient_matrix_UB_21      0.1627433000
_diffrn_orient_matrix_UB_22      0.0165617000
_diffrn_orient_matrix_UB_23      0.0706498000
_diffrn_orient_matrix_UB_31      0.0733924000
_diffrn_orient_matrix_UB_32      0.0903984000
_diffrn_orient_matrix_UB_33      -0.0669445000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15577
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.657
_diffrn_reflns_theta_min         4.950
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_F_000             636
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2596
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.4774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2372
_reflns_number_total             2596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03056f3.cif
_cod_data_source_block           sh36_300b_auto
_cod_database_code               7061988
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C10 H10 N4 O4 Br'
_diffrn_oxdiff_digest_frames
;
010f92fff3b06126a72b392c26ce056799000473cfb
;
_diffrn_oxdiff_digest_hkl
;
01db5c8e36fff3d65d3be19ddd639682f72558
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C2(H2), C5(H5), C10(H10), C4(H4), C13(H13), C11(H11), C12(H12)
2.b Idealised tetrahedral OH refined as rotating group:
 O19(H19)
;
_shelx_res_checksum              27172
_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 1.877
_oxdiff_exptl_absorpt_empirical_full_min 0.688