Photoexcited and ground-state diradical(oid) character in a triquino[3]radialene
Hillier, Bethany K.; de Clercq, Damon M.; Bortolussi, Stephen D. S.; Capomolla, Simona S.; Nielsen, Michael P.; Młodzikowska-Pieńko, Katarzyna; Gershoni-Poranne, Renana; Schmidt, Timothy W.; Peeks, Martin D.; Chemical Science 16 (2025) 11331–11338; doi:10.1039/D5SC01676B

data_1574695
_publ_section_title
;
 Photoexcited and ground-state diradical(oid) character in a
 triquino[3]radialene
;
_journal_issue                   25
_journal_name_full               'Chemical Science'
_journal_page_first              11331
_journal_page_last               11338
_journal_paper_doi               10.1039/D5SC01676B
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C45 H62 O3, C H2 Cl2'
_chemical_formula_sum            'C46 H64 Cl2 O3'
_chemical_formula_weight         735.87
_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
_audit_creation_date             2025-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-28 deposited with the CCDC.	2025-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.27(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.120(3)
_cell_length_b                   14.550(3)
_cell_length_c                   22.230(4)
_cell_measurement_reflns_used    2509
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      1.7
_cell_volume                     4209.5(15)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 13.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  'MX1 Beamline Australian Synchrotron'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            84330
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.280
_diffrn_reflns_theta_min         1.677
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         9873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0755P)^2^+4.0719P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9079
_reflns_number_total             9873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01676b2.cif
_cod_data_source_block           bkhtbucyclo
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' 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 1574695.cif.
;
_cod_database_code               1574695
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.990
_diffrn_measurement_detector_type 'Dectris Eiger2 9M'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H46A,H46B} of C46, {H48A,H48B} of C48, {H47A,H47B} of C47
 At 1.5 times of:
  All C(H,H,H) groups, {H29A,H29B} of C29, All O(H) groups
2. Others
 Fixed Sof: Cl2(0.333333) Cl3(0.333333) C46(0.333333) H46A(0.333333)
 H46B(0.333333) Cl4(0.333333) C47(0.333333) H47A(0.333333) H47B(0.333333)
 C48(0.333333) H48A(0.333333) H48B(0.333333)
3.a Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B)
3.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C33(H33), C3(H3A), C19(H19), C5(H5), C23(H23)
3.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C30(H30A,H30B,
 H30C), C45(H45A,H45B,H45C), C40(H40A,H40B,H40C), C14(H14A,H14B,H14C), C44(H44A,
 H44B,H44C), C43(H43A,H43B,H43C), C41(H41A,H41B,H41C), C26(H26A,H26B,H26C),
 C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C10(H10A,H10B,H10C), C25(H25A,H25B,
 H25C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O2(H2)
;
_shelx_res_checksum              30939
_olex2_submission_special_instructions 'No special instructions were received'