The influence of molecular conformation on the photophysics of organic room temperature phosphorescent luminophores
Huang, Rongjuan; Ward, Jonathan S.; Kukhta, Nadzeya A.; Avó, João; Gibson, Jamie; Penfold, Thomas; Lima, João C.; Batsanov, Andrei S.; Berberan-Santos, Mário N.; Bryce, Martin R.; Dias, Fernando B.; Journal of Materials Chemistry C 6 (2018) 9238–; doi:10.1039/C8TC02987C

data_7237441
_publ_section_title
;
 The influence of molecular conformation on the photophysics of organic
 room temperature phosphorescent luminophores
;
_journal_issue                   34
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              9238
_journal_paper_doi               10.1039/C8TC02987C
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C38 H26 N2 S3, C H Cl3'
_chemical_formula_sum            'C39 H27 Cl3 N2 S3'
_chemical_formula_weight         726.15
_chemical_name_systematic
'2,8-bis(1-methyl-10H-phenothiazin-10-yl)dibenzo[b,d]thiophene, chloroform solvate'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-10-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-29 deposited with the CCDC.
2018-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                93.7823(19)
_cell_angle_beta                 97.0827(19)
_cell_angle_gamma                93.6859(17)
_cell_formula_units_Z            4
_cell_length_a                   11.0581(4)
_cell_length_b                   15.5487(6)
_cell_length_c                   20.2305(8)
_cell_measurement_reflns_used    5831
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      50.18
_cell_measurement_theta_min      3.48
_cell_volume                     3435.1(2)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2016/6 multi-CPU (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.916
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34432
_diffrn_reflns_point_group_measured_fraction_full 0.916
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        58.978
_diffrn_reflns_theta_max         58.978
_diffrn_reflns_theta_min         2.207
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.367
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker, 2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0495 before and 0.0387 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0850 before and 0.0438 after correction.
 The Ratio of minimum to maximum transmission is 0.82.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 34432 reflections, Rint = 0.0575
 (14176 with I > 3sig(I), Rint = 0.0333)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, hexane'
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         21960
_refine_ls_number_restraints     825
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0790
_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^)+(0.0630P)^2^+8.4890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13875
_reflns_number_total             21960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8tc02987c2.cif
_cod_data_source_block           DPTZ-Me-DBT_17srv241
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7237441
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.519
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6744(11)
 0.3256(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Cl3B-C2SB \\sim Cl4B-C2SB \\sim Cl5B-C2SB \\sim Cl3A-C2SA \\sim Cl4A-C2SA
\\sim Cl5A-C2SA
 with sigma of 0.02
 C38A-C30 \\sim C38B-C36 \\sim C37A-C18 \\sim C37B-C24
 with sigma of 0.007
4. Rigid body (RIGU) restrains
 S3', N2', C25', C26', C27', C28', C29', C30'
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cl3B)=Sof(Cl4B)=Sof(Cl5B)=Sof(C2SB)=Sof(H2SB)=1-FVAR(1)
 Sof(Cl3A)=Sof(Cl4A)=Sof(Cl5A)=Sof(C2SA)=Sof(H2SA)=FVAR(1)
 Fixed Sof: H18(0.3) H24(0.7) H30(0.3) H36(0.7) C37A(0.7) H37A(0.7) H37B(0.7)
 H37C(0.7) C38A(0.7) H38A(0.7) H38B(0.7) H38C(0.7) C37B(0.3) H37D(0.3)
 H37E(0.3) H37F(0.3) C38B(0.3) H38D(0.3) H38E(0.3) H38F(0.3)
6.a Riding coordinates:
 C30(H30), C36(H36)
6.b Rotating group:
 C38A(H38A,H38B,H38C), C38B(H38D,H38E,H38F)
6.c Ternary CH refined with riding coordinates:
 C1S(H1S), C2SB(H2SB), C2SA(H2SA)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C15(H15), C16(H16),
 C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28),
  C29(H29), C33(H33), C34(H34), C35(H35), C2'(H2'), C3'(H3'), C5'(H5'),
 C8'(H8'), C10'(H10'), C11'(H11'), C15'(H15'), C16'(H16'), C17'(H17'),
 C21'(H21'), C22'(H22'), C23'(H23'), C24'(H24'), C27'(H27'), C28'(H28'),
 C29'(H29'), C33'(H33'), C34'(H34'), C35'(H35'), C36'(H36')
6.e Idealised Me refined as rotating group:
 C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F), C37'(H37G,H37H,H37I), C38'(H38G,
 H38H,H38I)
;
_shelx_res_checksum              22869
_shelx_hkl_checksum              65734
_olex2_submission_special_instructions 'No special instructions were received'
_twin_special_details
; Twin law: rotation by 180\% about reciprocal axis  (0 1 0)*  
and real axis  [0.098  1.000  0.056]. Deconvoluted using programs RLATT and CELL_NOW 2008/4, 
scaled using TWINABS 2012/1. 
12562 data (   4679 unique ) involve domain  1 only,  mean I/sigma  10.7
12523 data (   4687 unique ) involve domain  2 only,  mean I/sigma   6.4
 9478 data (   4190 unique ) involve   2 domains,     mean I/sigma   8.9
34472 total and  13552 unique reflections left after |I-<I>|/su test. 
28582 Corrected reflections written to HKLF5 format file.
;