Deformation-induced phosphorescence shift in a 2D elastically flexible organic single crystal: Role of chalcogen-centered weak interactions
Bhandary, Subhrajyoti; Van Deun, Rik; Kaczmarek, Anna Marta; Van Hecke, Kristof; Chemical Science  (2022) –; doi:10.1039/D2SC03729G

data_1567475
_publ_section_title
;
 Deformation-induced phosphorescence shift in a 2D elastically flexible
 organic single crystal: Role of chalcogen-centered weak interactions
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC03729G
_journal_year                    2022
_chemical_formula_moiety         'C12 H7 Br S'
_chemical_formula_sum            'C12 H7 Br S'
_chemical_formula_weight         263.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-04-13 deposited with the CCDC.	2022-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.9868(3)
_cell_length_b                   12.1976(7)
_cell_length_c                   20.4470(11)
_cell_measurement_reflns_used    1540
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      69.1530
_cell_measurement_theta_min      4.1690
_cell_volume                     994.33(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      290(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_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      6.00  82.00   1.00    2.00    --   41.16 -99.00 -90.00   76
  2  \w    -47.00 129.00   1.00    2.00    --   41.16   0.00  90.00  176
  3  \w     34.00 135.00   1.00    6.00    --  106.28 -61.00 -60.00  101
  4  \w    103.00 178.00   1.00    6.00    --  106.28  77.00  90.00   75
  5  \w     97.00 178.00   1.00    6.00    --  106.28 125.00   0.00   81
  6  \w     30.00 139.00   1.00    6.00    --  106.28 -77.00-150.00  109
  7  \w    103.00 178.00   1.00    6.00    --  106.28  77.00 -30.00   75
  8  \w   -114.00 -13.00   1.00    2.00    --  -41.16 -57.00 -90.00  101
  9  \w   -114.00 -13.00   1.00    2.00    --  -41.16 -57.00-180.00  101
 10  \w     77.00 128.00   1.00    6.00    --  106.28  61.00 -90.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1787730000
_diffrn_orient_matrix_UB_12      0.0563873000
_diffrn_orient_matrix_UB_13      0.0576504000
_diffrn_orient_matrix_UB_21      -0.3006895000
_diffrn_orient_matrix_UB_22      0.0257531000
_diffrn_orient_matrix_UB_23      -0.0447299000
_diffrn_orient_matrix_UB_31      -0.1632410000
_diffrn_orient_matrix_UB_32      -0.1100954000
_diffrn_orient_matrix_UB_33      0.0189606000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4820
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.054
_diffrn_reflns_theta_min         4.220
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.182
_exptl_absorpt_correction_T_max  0.05805
_exptl_absorpt_correction_T_min  0.00429
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.590
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.204
_refine_ls_abs_structure_details
;
 Flack x determined using 286 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.1028
_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^)+(0.1989P)^2^+0.5506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2940
_refine_ls_wR_factor_ref         0.3580
_reflns_Friedel_coverage         0.527
_reflns_Friedel_fraction_full    0.871
_reflns_Friedel_fraction_max     0.807
_reflns_number_gt                1288
_reflns_number_total             1831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03729g8.cif
_cod_data_source_block           dbs-br-nat-bent
_cod_original_cell_volume        994.33(10)
_cod_database_code               1567475
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 Br1 S1 H8'
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.267
_reflns_odcompleteness_completeness 97.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C9(H9), C2(H2), C3(H3), C10(H10), C11(H11)
;
_shelx_res_checksum              41431
_olex2_date_sample_data_collection 2022-03-03
_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 9.058
_oxdiff_exptl_absorpt_empirical_full_min 0.407