Macrocycle formation-mediated augmentation in reactive oxygen species production.
Liu, Ao; Xin, Youtao; Zhu, Yong-Kang; Jin, Yuan-Hang; Yang, Yue; Chen, Hongzhu; Li, Meng-Hao; Lou, Xin-Yue; Wang, Xin; Gao, Hui; Yang, Ying-Wei; Chemical science 16 (2025) 20968–20977; doi:10.1039/d5sc06637a

data_1575936
_publ_section_title
;
 Macrocycle formation-mediated augmentation in reactive oxygen species
 production.
;
_journal_issue                   44
_journal_name_full               'Chemical science'
_journal_page_first              20968
_journal_page_last               20977
_journal_paper_doi               10.1039/d5sc06637a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C82 H78 N4 O8 S2, 2(C4 H8 O2)'
_chemical_formula_sum            'C90 H98 N4 O12 S2'
_chemical_formula_weight         1491.84
_chemical_name_systematic        bth
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-02-07 deposited with the CCDC.	2025-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                75.4060(10)
_cell_angle_beta                 81.8190(10)
_cell_angle_gamma                69.7240(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4700(4)
_cell_length_b                   13.1031(4)
_cell_length_c                   21.8976(8)
_cell_measurement_reflns_used    6562
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.30
_cell_volume                     2462.06(16)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23558
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.597
_diffrn_reflns_theta_min         1.759
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6506
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1375 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.8726.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull yellowish yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_description       block
_exptl_crystal_F_000             794
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         11305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0778P)^2^+1.2828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7116
_reflns_number_total             11305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06637a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1575936--1575938.cif.'
_cod_database_code               1575936
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.989
_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
2.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C82(H82A,H82B), C60(H60A,H60B), C78(H78A,H78B), C80(H80A,
 H80B), C69(H69A,H69B), C87(H87A,H87B), C88(H88A,H88B), C90(H90A,H90B),
 C89(H89A,H89B)
2.b Aromatic/amide H refined with riding coordinates:
 C76(H76), C73(H73), C65(H65), C47(H47), C62(H62), C58(H58), C46(H46),
 C59(H59), C52(H52), C43(H43), C44(H44), C53(H53), C56(H56), C55(H55), C67(H67)
2.c Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C70(H70A,H70B,H70C), C68(H68A,H68B,
 H68C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              89297
_shelx_fab_checksum              19877
_olex2_submission_special_instructions 'No special instructions were received'