Surface coating induced room-temperature phosphorescence in flexible organic single crystals.
Samadder, Prodipta; Naim, Khalid; Sahoo, Subash Chandra; Neelakandan, Prakash P.; Chemical science 15 (2024) 9258–9265; doi:10.1039/d4sc01708k

data_1571636
_publ_section_title
;
 Surface coating induced room-temperature phosphorescence in flexible
 organic single crystals.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              9258
_journal_page_last               9265
_journal_paper_doi               10.1039/d4sc01708k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C15 H14 O3'
_chemical_formula_sum            'C15 H14 O3'
_chemical_formula_weight         242.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-01
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289)
;
_audit_update_record
;
2023-10-05 deposited with the CCDC.	2024-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                76.429(3)
_cell_angle_beta                 78.195(3)
_cell_angle_gamma                70.242(4)
_cell_formula_units_Z            4
_cell_length_a                   9.5504(4)
_cell_length_b                   9.6216(4)
_cell_length_c                   14.9202(5)
_cell_measurement_reflns_used    6219
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1970
_cell_measurement_theta_min      3.3150
_cell_volume                     1242.47(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_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    -69.00  -2.00   0.50    8.00    --   -9.79 -57.00 -90.00  134
  2  \w    -64.00  -1.00   0.50    8.00    --   -9.79 -19.00  60.00  126
  3  \w    -48.00 -22.00   0.50    8.00    --   -9.79 125.00  30.00   52
  4  \w    -80.00  -1.00   0.50    8.00    --   -9.79 -19.00   0.00  158
  5  \w    -43.00   4.00   0.50    8.00    --   -9.79 -38.00-180.00   94
  6  \w    -58.00 -33.00   0.50    8.00    --   -9.79 125.00-150.00   50
  7  \w     14.00  54.00   0.50    8.00    --   -9.79  57.00   0.00   80
  8  \w      7.00  49.00   0.50    8.00    --   -9.79  19.00   0.00   84
  9  \w    -19.00  43.00   0.50    8.00    --   10.07 -99.00-150.00  124
 10  \w     42.00  72.00   0.50    8.00    --   10.07  38.00-120.00   60
 11  \w    -28.00   1.00   0.50    8.00    --   10.07 120.00 -94.67   58
 12  \w     21.00  55.00   0.50    8.00    --   10.07-125.00-180.00   68
 13  \w    -33.00  -4.00   0.50    8.00    --   10.07 127.00  81.44   58
 14  \w     13.00  58.00   0.50    8.00    --   10.07-125.00  60.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, 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      -0.0704564000
_diffrn_orient_matrix_UB_12      0.0446411000
_diffrn_orient_matrix_UB_13      0.0192416000
_diffrn_orient_matrix_UB_21      0.0347770000
_diffrn_orient_matrix_UB_22      0.0507573000
_diffrn_orient_matrix_UB_23      0.0064780000
_diffrn_orient_matrix_UB_31      -0.0131526000
_diffrn_orient_matrix_UB_32      0.0420867000
_diffrn_orient_matrix_UB_33      -0.0450020000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14173
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.308
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
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    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.021
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.154
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0613P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3200
_reflns_number_total             5034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01708k5.cif
_cod_data_source_block           scs-inst-jan31
_cod_depositor_comments
;
          Adding full bibliography for 1571636.cif.

2025-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C30 H28 O6'
_cod_original_formula_weight         484.52
_cod_original_formula_moiety         '2(C15 H14 O3)'
_cod_original_formula_units_Z            2
_cod_database_code               1571636
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N O B F'
_diffrn_oxdiff_ac3_digest_frames
;
01aafc86d3c829eee4bd00aa1588798eca01236171b
;
_diffrn_oxdiff_ac3_digest_hkl
;
0147df4e59e7bc99e335943cd38c9ec82f843b
;
_reflns_odcompleteness_completeness 99.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C21(H21), C29(H29), C19(H19), C7(H7), C22(H22), C25(H25),
 C3(H3), C4(H4), C28(H28), C13(H13), C18(H18), C26(H26), C10(H10), C11(H11)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C30(H30A,H30B,H30C), C15(H15A,H15B,H15C)
;
_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 1.287
_oxdiff_exptl_absorpt_empirical_full_min 0.734