Photoinduced radical formation in hydrogen-bonded organic frameworks.
Almuhana, Asia R. Y.; Orton, Georgia R. F.; Rosenberg, Callum; Champness, Neil R.; Chemical communications (Cambridge, England) 60 (2024) 452–455; doi:10.1039/d3cc05236b

data_7132442
_publ_section_title
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 Photoinduced radical formation in hydrogen-bonded organic frameworks.
;
_journal_issue                   4
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              452
_journal_page_last               455
_journal_paper_doi               10.1039/d3cc05236b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C30 H11 N2 O13, C4 H3 N O, 5(O), 2.5(C8 H12 N4), 17[H2O]'
_chemical_formula_sum            'C54 H78 N13 O36'
_chemical_formula_weight         1485.29
_chemical_name_systematic        HOF_C
_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
_audit_creation_date             2023-11-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-12-01 deposited with the CCDC.	2023-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                88.568(5)
_cell_angle_beta                 81.294(4)
_cell_angle_gamma                86.534(5)
_cell_formula_units_Z            2
_cell_length_a                   7.8430(4)
_cell_length_b                   19.3052(12)
_cell_length_c                   23.3588(7)
_cell_measurement_reflns_used    14538
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.208
_cell_measurement_theta_min      0.855
_cell_volume                     3489.2(3)
_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      293(2)
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_measured_fraction_theta_full 0.706
_diffrn_measured_fraction_theta_max 0.706
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1969
_diffrn_reflns_av_unetI/netI     0.6103
_diffrn_reflns_Laue_measured_fraction_full 0.706
_diffrn_reflns_Laue_measured_fraction_max 0.706
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14538
_diffrn_reflns_point_group_measured_fraction_full 0.706
_diffrn_reflns_point_group_measured_fraction_max 0.706
_diffrn_reflns_theta_full        24.208
_diffrn_reflns_theta_max         24.208
_diffrn_reflns_theta_min         0.855
_diffrn_source                   Synchrotron
_exptl_absorpt_coefficient_mu    0.112
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       needle
_exptl_crystal_F_000             1562
_exptl_crystal_preparation       'See experimental section'
_exptl_crystal_recrystallization_method 'See experimental section'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0069(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   0.802
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         8715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.3195
_refine_ls_R_factor_gt           0.1372
_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^)+(0.1312P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3187
_refine_ls_wR_factor_ref         0.3727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1488
_reflns_number_total             8715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05236b2.cif
_cod_data_source_block           83685377_shelxt
_cod_depositor_comments
'Adding full bibliography for 7132441--7132443.cif.'
_cod_database_code               7132442
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1.a Rotating group:
 N11(H11A), N9(H9A,H9B)
1.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C5(H5), C7(H7), C3(H3), C11(H11), C12(H12), C16(H16), C18(H18),
 C26(H26), C30(H30), C28(H28), C53(H53), C54(H54), C35(H35), C39(H39), C38(H38),
  C36(H36), C46(H46), C47(H47), C43(H43), C44(H44), C51(H51), C52(H52)
1.c Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C2,C3), C21(C10,C9,N1,C20,C19), C27(C26,C25,C30,C29,C28), C35(C34,
 C39,C38,C37,C36), C46(C47,C42,C43,C44,C45)
1.d X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B), N7(H7A,H7B), N8(H8A,H8B),
 N10(H10A,H10B), N12(H12A,H12B), N13(H13A,H13B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 335 electrons were 
found in a volume of 992\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
17[H2O] per Unit Cell 
which account for 340 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38251
_shelx_hkl_checksum              68575
_shelx_fab_checksum              52509
_olex2_submission_special_instructions 'No special instructions were received'