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_7062001
_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         'C14 H8 F3 N2 O3'
_chemical_formula_sum            'C14 H8 F3 N2 O3'
_chemical_formula_weight         309.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-07
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.05 svn.r3537 for Rigaku Oxford Diffraction, GUI svn.r5625)
;
_audit_update_record
;
2022-07-18 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.790(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3168(6)
_cell_length_b                   6.7716(3)
_cell_length_c                   14.2320(5)
_cell_measurement_reflns_used    4246
_cell_measurement_temperature    299.97(12)
_cell_measurement_theta_max      77.4950
_cell_measurement_theta_min      3.2120
_cell_volume                     1320.94(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.97a (Rigaku OD, 2021)'
_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      299.97(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.901
_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     35.00 119.00   0.50    0.28    --   46.82  42.00  32.00  168
  2  \w     24.00 120.00   0.50    0.28    --   46.82  77.00  90.00  192
  3  \w     24.00 118.00   0.50    0.28    --   46.82  77.00 -60.00  188
  4  \w     79.00 178.00   0.50    1.13    --  110.25 125.00-120.00  198
  5  \w     98.00 178.00   0.50    1.13    --  110.25  42.00  32.00  160
  6  \w    -27.00  13.00   0.50    0.28    --   46.82 -19.00  60.00   80
  7  \w    -25.00  48.00   0.50    0.28    --   46.82 -42.00-119.00  146
  8  \w     38.00  80.00   0.50    1.13    --  110.25 -61.00 -60.00   84
  9  \w     38.00  80.00   0.50    1.13    --  110.25 -61.00-120.00   84
 10  \w     38.00  80.00   0.50    1.13    --  110.25 -61.00-180.00   84
 11  \w     38.00 106.00   0.50    1.13    --  110.25 -94.00-180.00  136
 12  \w     38.00 111.00   0.50    1.13    --  110.25-125.00-180.00  146
 13  \w     38.00 106.00   0.50    1.13    --  110.25 -94.00-120.00  136
 14  \w     38.00 106.00   0.50    1.13    --  110.25 -94.00 -60.00  136
 15  \w     38.00 111.00   0.50    1.13    --  110.25-125.00  30.00  146
 16  \w    -40.00  25.00   0.50    0.28    --  -46.82  42.00  32.00  130
 17  \w     -5.00  29.00   0.50    0.28    --  -46.82  19.00 150.00   68
 18  \w     -5.00  29.00   0.50    0.28    --  -46.82  19.00-150.00   68
 19  \w     -5.00  29.00   0.50    0.28    --  -46.82  19.00-180.00   68
 20  \w   -119.00 -24.00   0.50    0.28    --  -46.82 -77.00-180.00  190
 21  \w   -174.00 -89.00   0.50    1.13    -- -102.00 -42.00-119.00  170
 22  \w   -119.00 -34.00   0.50    0.28    --  -46.82 -42.00-119.00  170
 23  \w   -174.00 -89.00   0.50    1.13    -- -102.00 -45.00 150.00  170
 24  \w    -72.00 -29.00   0.50    1.13    -- -102.00  61.00  60.00   86
 25  \w    -72.00 -29.00   0.50    1.13    -- -102.00  61.00 120.00   86
 26  \w    -72.00 -29.00   0.50    1.13    -- -102.00  61.00 150.00   86
 27  \w   -125.00 -29.00   0.50    1.13    -- -102.00  77.00  60.00  192
 28  \w    -72.00 -29.00   0.50    1.13    -- -102.00  61.00-150.00   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      -0.0597759000
_diffrn_orient_matrix_UB_12      -0.0795797000
_diffrn_orient_matrix_UB_13      -0.1008986000
_diffrn_orient_matrix_UB_21      -0.0944711000
_diffrn_orient_matrix_UB_22      0.0748930000
_diffrn_orient_matrix_UB_23      0.0191172000
_diffrn_orient_matrix_UB_31      0.0117094000
_diffrn_orient_matrix_UB_32      0.1995032000
_diffrn_orient_matrix_UB_33      -0.0473329000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6419
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         83.762
_diffrn_reflns_theta_min         3.244
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.97a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       platelets
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.212
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0655
_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^)+(0.1432P)^2^+0.2926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2135
_refine_ls_wR_factor_ref         0.2377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1180
_reflns_number_total             1460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03056f3.cif
_cod_data_source_block           sh01_300_auto
_cod_depositor_comments
;

2024-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         154.61
_cod_original_formula_moiety         'C7 H4.5 F1.5 N O1.5'
_cod_original_formula_units_Z            8
_cod_original_formula_sum        'C7 H4 F1.50 N O1.50'
_cod_database_code               7062001
_diffrn_oxdiff_digest_frames
;
01f203b30d18f3ebd198937fdf4ca71d820005189e0
;
_diffrn_oxdiff_digest_hkl
;
0146843d9690de31a3e2cd2921f9e33b6824e5
;
_reflns_odcompleteness_completeness 98.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C18(H18), C9(H9), C2(H2), C14(H14), C13(H13), C17(H17), C19(H19)
;
_shelx_res_checksum              22811
_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 4.388
_oxdiff_exptl_absorpt_empirical_full_min 0.571