Mechanophotonic aspects of a room temperature phosphorescent flexible organic microcrystal
Kumar, Avulu Vinod; Rohullah, Mehdi; Ravi, Jada; Godumala, Mallesham; Annadhasan, Mari; Chandrasekar, Rajadurai; CrystEngComm 23 (2021) 5774–5779; doi:10.1039/D1CE00475A

data_7243029
_publ_section_title
;
 Mechanophotonic aspects of a room temperature phosphorescent flexible
 organic microcrystal
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              5774
_journal_page_last               5779
_journal_paper_doi               10.1039/D1CE00475A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C29 H16 F6 N2 S'
_chemical_formula_sum            'C29 H16 F6 N2 S'
_chemical_formula_weight         538.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-04-03 deposited with the CCDC.	2021-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.502(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6615(7)
_cell_length_b                   4.8528(2)
_cell_length_c                   39.0056(17)
_cell_measurement_reflns_used    5492
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      25.9280
_cell_measurement_theta_min      2.0920
_cell_volume                     2370.31(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.933
_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      3.00  29.00   0.50    9.20    --   16.22  30.00  30.00   52
  2  \w     55.00  87.00   0.50    9.20    --   16.22  30.00  30.00   64
  3  \w     -1.00  25.00   0.50    9.20    --   16.22  77.00 -60.00   52
  4  \w     56.00  86.00   0.50    9.20    --   16.22  77.00 -60.00   60
  5  \w     44.00  69.00   0.50    9.20    --   16.22 170.00 -16.00   50
  6  \w     64.00  90.00   0.50    9.20    --   16.22  30.00-150.00   52
  7  \w      6.00  32.00   0.50    9.20    --   16.22  30.00-150.00   52
  8  \w    -57.00 -32.00   0.50    9.20    --  -14.97 115.00-158.00   50
  9  \w    -81.00   7.00   0.50    9.20    --  -14.97 -30.00-150.00  176
 10  \w    -36.00  -1.00   0.50    9.20    --   16.22 -94.00-150.00   70
 11  \w    -57.00  38.00   0.50    9.20    --   16.22 -30.00-150.00  190
 12  \w     41.00  66.00   0.50    9.20    --   16.22-170.00 -31.00   50
 13  \w      9.00  35.00   0.50    9.20    --   16.22 -94.00   0.00   52
 14  \w     10.00  64.00   0.50    9.20    --   16.22-125.00 -30.00  108
 15  \w    -36.00  -9.00   0.50    9.20    --   16.22 -94.00   0.00   54
 16  \w    -93.00 -68.00   0.50    9.20    --  -14.97-170.00 -31.00   50
 17  \w     10.00  35.00   0.50    9.20    --   16.22-115.00 111.00   50
 18  \w    -27.00  17.00   0.50    9.20    --  -14.97 -94.00 150.00   88
 19  \w    -85.00   6.00   0.50    9.20    --  -14.97 -30.00 120.00  182
 20  \w    -67.00 -41.00   0.50    9.20    --  -14.97 125.00  90.00   52
 21  \w    -85.00 -60.00   0.50    9.20    --  -14.97 170.00 -16.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0303422000
_diffrn_orient_matrix_UB_12      -0.0216382000
_diffrn_orient_matrix_UB_13      0.0165735000
_diffrn_orient_matrix_UB_21      0.0477754000
_diffrn_orient_matrix_UB_22      0.0114126000
_diffrn_orient_matrix_UB_23      -0.0073468000
_diffrn_orient_matrix_UB_31      0.0007103000
_diffrn_orient_matrix_UB_32      0.1442130000
_diffrn_orient_matrix_UB_33      0.0030708000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2037
_diffrn_reflns_av_unetI/netI     0.2345
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            21184
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.949
_diffrn_reflns_theta_min         2.112
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       Monoclinic
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         4812
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.2165
_refine_ls_R_factor_gt           0.0903
_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^)+(0.1095P)^2^+1.5165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1965
_refine_ls_wR_factor_ref         0.3128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1959
_reflns_number_total             4812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00475a3.cif
_cod_data_source_block           rc34
_cod_depositor_comments          'Adding full bibliography for 7243029.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7243029
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N F S'
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.960
_reflns_odcompleteness_completeness 98.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F5A-F4A \\sim F5A-F6A \\sim F4A-F6A
 with sigma of 0.04
 C1A-C2 \\sim C1A-F5A \\sim C1A-F4A \\sim C1A-F6A
 with sigma of 0.02
 F5B-F6B \\sim F5B-F4B \\sim F6B-F4B
 with sigma of 0.04
 C1B-C2 \\sim C1B-F5B \\sim C1B-F6B \\sim C1B-F4B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1A, F5A, C2, F4A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, F4B, F5B, F6B, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F5B)=Sof(C1B)=Sof(F6B)=Sof(F4B)=1-FVAR(1)
 Sof(C1A)=Sof(F5A)=Sof(F4A)=Sof(F6A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C5(H5), C12(H12), C25(H25), C21(H21), C16(H16), C15(H15), C10(H10),
 C7(H7), C28(H28), C3(H3), C26(H26), C18(H18), C20(H20), C27(H27), C19(H19)
;
_shelx_res_checksum              25872
_shelx_hkl_checksum              81844
_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 5.341
_oxdiff_exptl_absorpt_empirical_full_min 0.151