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_7237437
_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'
_chemical_formula_sum            'C38 H26 N2 S3'
_chemical_formula_weight         606.79
_chemical_melting_point          509(1)
_chemical_name_systematic
2,8-bis(1-methyl-10H-phenothiazin-10-yl)dibenzo[b,d]thiophene
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-10-11
_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                90
_cell_angle_beta                 101.501(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7234(4)
_cell_length_b                   14.3733(4)
_cell_length_c                   18.1421(6)
_cell_measurement_reflns_used    4566
_cell_measurement_temperature    120
_cell_measurement_theta_max      73.95
_cell_measurement_theta_min      3.95
_cell_volume                     2995.63(17)
_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
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       \w-scan
_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  0.0844
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25201
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.955
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.496
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS-2016/2 (Krause et al., 2015) was used for absorption correction. 
 wR2(int) was 0.0749 before and 0.0564 after correction. 
 The Ratio of minimum to maximum transmission is 0.8329. 
 The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       trapetzoid
_exptl_crystal_F_000             1264
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, hexane'
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.00043(6)
_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   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         5016
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0210P)^2^+3.5050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3425
_reflns_number_total             5016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8tc02987c2.cif
_cod_data_source_block           DPTZ-Me-DBT_17srv251
_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               7237437
_shelx_shelxl_version_number     2016/6
_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. Restrained distances
 C18A-C13A \\sim C18B-C13B
 with sigma of 0.02
 C18A-C17A \\sim C18B-C17B
 with sigma of 0.02
 S2B-C14B \\sim S2A-C14A
 with sigma of 0.02
 S2B-C20B \\sim S2A-C20A
 with sigma of 0.02
 N1B-C19B \\sim N1B-C19A
 with sigma of 0.02
 N1B-C13A \\sim N1B-C13B
 with sigma of 0.02
 N1A-C19A \\sim N1A-C13A \\sim N1B-C19B \\sim N1B-C13B
 with sigma of 0.02
 N1A-C4 \\sim N1B-C4
 with sigma of 0.02
 C37A-C18A \\sim C37B-C18B
 with sigma of 0.02
 C17A-C16A \\sim C17B-C16B
 with sigma of 0.02
 C16B-C15B \\sim C16A-C15A
 with sigma of 0.02
 C15A-C14A \\sim C15B-C14B
 with sigma of 0.02
 C14B-C13B \\sim C14A-C13A
 with sigma of 0.02
 C20B-C19B \\sim C20A-C19A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1B) = Uanis(N1A)
4. Rigid body (RIGU) restrains
 S2A, C19A, C20A, C21A, C22A, C23A, C24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S2B)=Sof(N1B)=Sof(C13B)=Sof(C14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16B)=
 Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(C19B)=Sof(C20B)=Sof(C21B)=Sof(H21B)=
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24B)=Sof(C37B)=
 Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(S2A)=Sof(N1A)=Sof(C13A)=Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=
 Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(C19A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C37A)=
 Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
 Fixed Sof: H30(0.4) H36(0.6) C38A(0.6) H38A(0.6) H38B(0.6) H38C(0.6)
 C38B(0.4) H38D(0.4) H38E(0.4) H38F(0.4)
6.a Riding coordinates:
 C30(H30), C36(H36), C37A(H37A,H37B,H37C), C37B(H37D,H37E,H37F), C38A(H38A,
 H38B,H38C), C38B(H38D,H38E,H38F)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C15A(H15A), C16A(H16A),
 C17A(H17A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C15B(H15B),
 C16B(H16B), C17B(H17B), C21B(H21B), C22B(H22B), C23B(H23B), C24B(H24B),
 C27(H27), C28(H28), C29(H29), C33(H33), C34(H34), C35(H35)
6.c Fitted hexagon refined as free rotating group:
 C19B(C20B,C21B,C22B,C23B,C24B)
;
_shelx_res_checksum              61394
_shelx_hkl_checksum              30789
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'