Methylation-effect in Prolonging the Pure Organic Room Temperature Phosphorescence Lifetime
Mao, Zhu; Yang, Zhan; Fan, Zhenguo; Ubba, Eethamukkala; Li, Wenlang; Li, Yang; Zhao, Juan; Yang, Zhiyong; Aldred, Matthew Phillip; Chi, Zhenguo; Chemical Science  (2018) –; doi:10.1039/C8SC03019G

data_1550021
_publ_section_title
;
 Methylation-effect in Prolonging the Pure Organic Room Temperature
 Phosphorescence Lifetime
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC03019G
_journal_year                    2018
_chemical_formula_moiety         'C27 H23 N O2 S'
_chemical_formula_sum            'C27 H23 N O2 S'
_chemical_formula_weight         425.52
_chemical_name_systematic        3M
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2018-03-28 deposited with the CCDC.
2018-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.148(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.0963(7)
_cell_length_b                   12.9096(3)
_cell_length_c                   15.8774(4)
_cell_measurement_reflns_used    6949
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.9270
_cell_measurement_theta_min      4.0210
_cell_volume                     4242.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5826
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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    -25.00  21.00   1.00    5.02    --   42.74 -77.00-120.00   46
  2  \w     22.00  49.00   1.00    5.02    --   42.74 -99.00 -60.00   27
  3  \w     37.00 121.00   1.00   12.10    --  107.32-125.00  30.00   84
  4  \w     68.00 104.00   1.00   12.10    --  107.32 -94.00 120.00   36
  5  \w     55.00 129.00   1.00   12.10    --  107.32 -61.00  90.00   74
  6  \w     89.00 132.00   1.00   12.10    --  107.32  30.00 150.00   43
  7  \w    110.00 160.00   1.00   12.10    --  107.32 125.00 150.00   50
  8  \w     83.00 175.00   1.00   12.10    --  107.32  45.00-120.00   92
  9  \w     99.00 178.00   1.00   12.10    --  107.32 125.00-180.00   79
 10  \w     99.00 126.00   1.00   12.10    --  107.32 125.00-120.00   27
 11  \w     98.00 165.00   1.00   12.10    --  107.32  30.00-180.00   67
 12  \w     79.00 106.00   1.00   12.10    --  107.32 -94.00-150.00   27
 13  \w     65.00 137.00   1.00   12.10    --  107.32 -77.00-180.00   72
 14  \w     35.00 124.00   1.00   12.10    --  107.32 -30.00-150.00   89
 15  \w     33.00  64.00   1.00   12.10    --  107.32 -94.00 120.00   31
 16  \w    -91.00  -6.00   1.00    5.02    --  -40.50 125.00-150.00   85
 17  \w   -110.00 -14.00   1.00    5.02    --  -40.50 -57.00   0.00   96
 18  \w   -110.00  -9.00   1.00    5.02    --  -40.50 -77.00 120.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0388107000
_diffrn_orient_matrix_UB_12      -0.0999590000
_diffrn_orient_matrix_UB_13      -0.0257531000
_diffrn_orient_matrix_UB_21      -0.0605387000
_diffrn_orient_matrix_UB_22      0.0651983000
_diffrn_orient_matrix_UB_23      -0.0355102000
_diffrn_orient_matrix_UB_31      0.0194046000
_diffrn_orient_matrix_UB_32      0.0031678000
_diffrn_orient_matrix_UB_33      -0.0885376000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14320
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.409
_diffrn_reflns_theta_min         4.036
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0606P)^2^+3.0836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3867
_reflns_number_total             4269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc03019g2.cif
_cod_data_source_block           17060204
_cod_database_code               1550021
_chemical_oxdiff_formula         CHONS
_chemical_oxdiff_usercomment     tCSCz
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C006(H006), C00C(H00C), C00D(H00D), C00E(H00E), C00G(H00G), C00I(H00I),
 C00J(H00J), C00K(H00K), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00U(H00U)
2.b Idealised Me refined as rotating group:
 C00S(H00A,H00B,H00F), C00T(H00H,H00L,H00M), C00V(H00S,H00T,H00V)
;
_shelx_res_checksum              45852
_shelx_shelxl_version_number     2014/7
_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 1.684
_oxdiff_exptl_absorpt_empirical_full_min 0.558