Examination of photoinduced radicals in two crystal forms of triphenylamine bis-urea macrocycles
Islam, Md Faizul; Wijesekera, Gamage Isuri P.; Sindt, Ammon J.; Smith, Mark D.; Shimizu, Linda S.; CrystEngComm 26 (2024) 6025–6033; doi:10.1039/D4CE00839A

data_7249422
_publ_section_title
;
 Examination of photoinduced radicals in two crystal forms of
 triphenylamine bis-urea macrocycles
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6025
_journal_page_last               6033
_journal_paper_doi               10.1039/D4CE00839A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C42 H36 Br2 N6 O2, 0.716(C2 H6 O S)'
_chemical_formula_sum            'C43.43 H40.29 Br2 N6 O2.72 S0.71'
_chemical_formula_weight         872.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2024-03-31 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.584(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.878(2)
_cell_length_b                   4.6413(6)
_cell_length_c                   26.735(3)
_cell_measurement_reflns_used    8762
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.271
_cell_measurement_theta_min      2.602
_cell_volume                     1942.7(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker APEX3 v2019.1-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 PHOTON-II
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            26749
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.374
_diffrn_reflns_theta_min         1.847
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.173
_exptl_absorpt_correction_T_max  0.5624
_exptl_absorpt_correction_T_min  0.4717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0854 before and 0.0590 after correction.
The Ratio of minimum to maximum transmission is 0.8387.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       needle
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.456
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3961
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0667
_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^)+(0.0001P)^2^+7.7180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3335
_reflns_number_total             3961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00839a2.cif
_cod_data_source_block           mfi_brmc_tegme
_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/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7249420--7249422.cif.
;
_cod_original_cell_volume        1942.8(4)
_cod_database_code               7249422
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.751
_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, All N(H) groups
2. Restrained distances
 S1S-O1S
 1.5 with sigma of 0.015
 S1S-C1S = S1S-C2S
 1.775 with sigma of 0.02
 S2S-O2S
 1.5 with sigma of 0.015
 S2S-C3S = S2S-C4S
 1.775 with sigma of 0.02
 N1-H1 = N2-H2
 0.85 with sigma of 0.02
 O1S-C1S = O1S-C2S
 2.623 with sigma of 0.04
 C1S-C2S
 2.66 with sigma of 0.04
 O2S-C3S = O2S-C4S
 2.623 with sigma of 0.04
 C3S-C4S
 2.66 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(C2S) = Uiso(O2S)
4. Others
 Sof(S1S)=Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(H2SA)=
 Sof(H2SB)=Sof(H2SC)=FVAR(1)
 Sof(S2S)=Sof(O2S)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=Sof(C4S)=Sof(H4SA)=
 Sof(H4SB)=Sof(H4SC)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20)
5.c Idealised Me refined with riding coordinates:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB,
 H4SC)
;
_shelx_res_checksum              55794
_shelx_hkl_checksum              855
_olex2_submission_special_instructions 'No special instructions were received'