One-step synthesis of cyclic compounds towards easy room-temperature phosphorescence and deep blue thermally activated delayed fluorescence.
Hu, Yingyuan; Wang, Zhenfeng; Jiang, Xiaofang; Cai, Xinyi; Su, Shi-Jian; Huang, Fei; Cao, Yong; Chemical communications (Cambridge, England) 54 (2018) 7850–7853; doi:10.1039/c8cc03833c

data_7121855
_publ_section_title
;
 One-step synthesis of cyclic compounds towards easy room-temperature
 phosphorescence and deep blue thermally activated delayed fluorescence.
;
_journal_issue                   56
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7850
_journal_page_last               7853
_journal_paper_doi               10.1039/c8cc03833c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C44 H42 N2 O4 S2'
_chemical_formula_sum            'C44 H42 N2 O4 S2'
_chemical_formula_weight         726.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-11-01 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                84.935(2)
_cell_angle_beta                 77.163(2)
_cell_angle_gamma                84.614(2)
_cell_formula_units_Z            1
_cell_length_a                   7.2994(2)
_cell_length_b                   9.0319(3)
_cell_length_c                   14.3088(3)
_cell_measurement_reflns_used    6185
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.6550
_cell_measurement_theta_min      4.9190
_cell_volume                     913.49(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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    -14.00  53.00   0.50    1.00    --    0.00  57.00  90.00  134
  2  \w     59.00  85.00   0.50    1.00    --    0.00  57.00  90.00   52
  3  \w    -36.00 -11.00   0.50    1.00    --  -98.80  72.00-150.00   50
  4  \w    -45.00 -10.00   0.50    1.00    --  -98.80  57.00-120.00   70
  5  \w    -90.00 -47.00   0.50    1.00    --  -98.80  57.00 120.00   86
  6  \w    -42.00  -9.00   0.50    1.00    --  -98.80  57.00 120.00   66
  7  \w   -103.00 -31.00   0.50    1.00    --  -98.80  19.00   0.00  144
  8  \w   -101.00 -75.00   0.50    1.00    --  -98.80  72.00 -30.00   52
  9  \w   -107.00 -36.00   0.50    1.00    --  -98.80  57.00  30.00  142
 10  \w   -106.00 -80.00   0.50    1.00    --  -98.80  72.00 150.00   52
 11  \w   -114.00 -29.00   0.50    1.00    --  -98.80  72.00 120.00  170
 12  \w   -112.00 -32.00   0.50    1.00    --  -98.80  72.00 -90.00  160
 13  \w   -114.00 -53.00   0.50    1.00    --  -98.80  72.00-150.00  122
 14  \w   -112.00 -21.00   0.50    1.00    --  -98.80  72.00  30.00  182
 15  \w   -109.00 -83.00   0.50    1.00    --  -98.80  57.00-120.00   52
 16  \w   -122.00 -92.00   0.50    1.00    --  -98.80 -38.00  30.00   60
 17  \w   -177.00-141.00   0.50    1.00    --  -98.80 -38.00  30.00   72
 18  \w   -188.00-106.00   0.50    1.00    --  -98.80 -38.00  60.00  164
 19  \w   -184.00 -99.00   0.50    1.00    --  -98.80 -19.00 -60.00  170
 20  \w   -188.00-119.00   0.50    1.00    --  -98.80 -19.00   0.00  138
 21  \w    -42.00  12.00   0.50    1.00    --    0.00 -72.00-120.00  108
 22  \w    -89.00 -64.00   0.50    1.00    --    0.00 -19.00-180.00   50
 23  \w    -86.00 -50.00   0.50    1.00    --    0.00 -72.00-120.00   72
 24  \w    -89.00 -19.00   0.50    1.00    --    0.00 -57.00   0.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1339336000
_diffrn_orient_matrix_UB_12      -0.0979186000
_diffrn_orient_matrix_UB_13      0.0534504000
_diffrn_orient_matrix_UB_21      0.1177288000
_diffrn_orient_matrix_UB_22      -0.0511317000
_diffrn_orient_matrix_UB_23      -0.0966173000
_diffrn_orient_matrix_UB_31      0.1238299000
_diffrn_orient_matrix_UB_32      0.1315004000
_diffrn_orient_matrix_UB_33      -0.0078103000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7076
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.072
_diffrn_reflns_theta_max         67.072
_diffrn_reflns_theta_min         4.930
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.695
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0081(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0637P)^2^+0.4352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3066
_reflns_number_total             3202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03833c3.cif
_cod_data_source_block           hyy-tbu-1
_cod_depositor_comments
'Adding full bibliography for 7121855--7121856.cif.'
_cod_database_code               7121855
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 97.98
_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:
 C005(H005), C009(H009), C00A(H00A), C00C(H00C), C00D(H00D), C00E(H00E),
 C00F(H00F), C00G(H00G), C00H(H00H), C00J(H00J), C00M(H00M), C00N(H00N)
2.b Idealised Me refined as rotating group:
 C00O(H00B,H00I,H00K), C00P(H00L,H00O,H00P), C00Q(H00Q,H00R,H00S)
;
_shelx_res_checksum              94521
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.749
_oxdiff_exptl_absorpt_empirical_full_min 0.485