Synthesis of fused chalcogenophenocarbazoles: towards dual emission resulting from hybridized local and charge-transfer states
Petrenko, Alla; Bezvikonnyi, Oleksandr; Volyniuk, Dmytro; Danyliv, Yan; Simokaitiene, Jurate; Belyakov, Sergey; Grazulevicius, Juozas Vidas; Arsenyan, Pavel; New Journal of Chemistry 44 (2020) 3903–3911; doi:10.1039/C9NJ06211D

data_7059310
_publ_section_title
;
 Synthesis of fused chalcogenophenocarbazoles: towards dual emission
 resulting from hybridized local and charge-transfer states
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3903
_journal_page_last               3911
_journal_paper_doi               10.1039/C9NJ06211D
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C32 H43 N Se2 Si'
_chemical_formula_sum            'C32 H43 N Se2 Si'
_chemical_formula_weight         627.68
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-01-18
_audit_creation_method
;
Olex2 1.2-ac4
(compiled 2018.05.17 svn.r3504 for Rigaku Oxford Diffraction, GUI svn.r5492)
;
_audit_update_record
;
2019-01-23 deposited with the CCDC.	2020-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.393(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8872(10)
_cell_length_b                   5.8066(2)
_cell_length_c                   26.9647(16)
_cell_measurement_reflns_used    11403
_cell_measurement_temperature    140.0(1)
_cell_measurement_theta_max      32.1310
_cell_measurement_theta_min      3.1140
_cell_volume                     3029.1(3)
_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      140.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.879
_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     -1.00  84.00   0.50   18.00    --   11.72  48.00  16.00  170
  2  \w    -11.00  15.00   0.50   18.00    --   11.72  77.00   0.00   52
  3  \w     -2.00  38.00   0.50   18.00    --   11.72  77.00-150.00   80
  4  \w    -61.00  19.00   0.50   18.00    --   11.72 -48.00-131.00  160
  5  \w    -12.00  14.00   0.50   18.00    --  -12.34 -99.00-120.00   52
  6  \w    -36.00   6.00   0.50   18.00    --  -12.34 -77.00-150.00   84
  7  \w    -77.00 -44.00   0.50   18.00    --  -12.34 -38.00-180.00   66
  8  \w     -4.00  21.00   0.50   18.00    --  -12.34 -99.00  60.00   50
  9  \w    -16.00   9.00   0.50   18.00    --  -12.34 -99.00 120.00   50
 10  \w    -16.00   9.00   0.50   18.00    --  -12.34 -99.00 150.00   50
 11  \w     42.00  78.00   0.50   18.00    --   11.72 178.00 150.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0310085000
_diffrn_orient_matrix_UB_12      -0.0390913000
_diffrn_orient_matrix_UB_13      -0.0165275000
_diffrn_orient_matrix_UB_21      -0.0195798000
_diffrn_orient_matrix_UB_22      0.0612708000
_diffrn_orient_matrix_UB_23      0.0145564000
_diffrn_orient_matrix_UB_31      -0.0001512000
_diffrn_orient_matrix_UB_32      0.0982566000
_diffrn_orient_matrix_UB_33      -0.0156560000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            47064
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.466
_diffrn_reflns_theta_min         1.445
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.502
_exptl_absorpt_correction_T_max  0.98902
_exptl_absorpt_correction_T_min  0.79149
_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            Yellow
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       'Needle '
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         10395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+2.4018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7358
_reflns_number_total             10395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj06211d2.cif
_cod_data_source_block           a184
_cod_depositor_comments
;Adding full bibliography for 7059310.cif.

 Adding full bibliography for 7059310.cif.
;
_cod_database_code               7059310
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C128 H172 N4 Se8 Si4 '
_chemical_oxdiff_usercomment     'A-184 (from Pavel)'
_diffrn_oxdiff_digest_frames
;
01fc99894846fed616d83f2be9ee496ddd000251564
;
_diffrn_oxdiff_digest_hkl
;
01613891ce5f5cb3f0fefa6bc19f6177490b0b
;
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,
 H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C23(H23A,H23B),
 C24(H24A,H24B)
2.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11)
;
_shelx_res_checksum              90565
_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 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.501