Self-contained photo-acid generators with high quantum yields triggered by photo-cyclization
Xu, Zixuan; Wang, Zhaoyu; Zhang, Yanyun; Yao, Xiaokang; Ding, Meijuan; Shi, Huifang; An, Zhongfu; Chemical Communications  (2022) –; doi:10.1039/D2CC04941D

data_7131003
_publ_section_title
;
 Self-contained photo-acid generators with high quantum yields triggered
 by photo-cyclization
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04941D
_journal_year                    2022
_chemical_formula_moiety         'C17 H10 F N O S'
_chemical_formula_sum            'C17 H10 F N O S'
_chemical_formula_weight         295.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-08-22
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-23 deposited with the CCDC.	2022-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.087(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9441(17)
_cell_length_b                   5.3279(5)
_cell_length_c                   13.3123(10)
_cell_measurement_reflns_used    1169
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.1000
_cell_measurement_theta_min      2.2890
_cell_volume                     1330.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -12.00  30.50   0.50   20.00    --   20.00  54.00  30.00   85
  2  \w    -73.00 -48.00   0.50   20.00    --   20.00  54.00 120.00   50
  3  \w    -43.00  40.00   0.50   20.00    --   20.00  54.00 120.00  166
  4  \w     49.00  75.00   0.50   20.00    --   20.00  54.00 120.00   52
  5  \w    -72.00 -47.00   0.50   20.00    --   20.00  54.00 -30.00   50
  6  \w     -7.00 105.00   0.50   20.00    --   20.00  54.00 -30.00  224
  7  \w    -14.00  37.00   0.50   20.00    --   20.00  54.00  60.00  102
  8  \w     80.00 105.00   0.50   20.00    --   20.00  54.00  60.00   50
  9  \w    -66.00 -40.00   0.50   20.00    --   20.00  54.00  30.00   52
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0169588000
_diffrn_orient_matrix_UB_12      0.0012039000
_diffrn_orient_matrix_UB_13      -0.0509970000
_diffrn_orient_matrix_UB_21      -0.0335885000
_diffrn_orient_matrix_UB_22      -0.0162031000
_diffrn_orient_matrix_UB_23      0.0169210000
_diffrn_orient_matrix_UB_31      -0.0039448000
_diffrn_orient_matrix_UB_32      0.1321400000
_diffrn_orient_matrix_UB_33      0.0025800000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4869
_diffrn_reflns_point_group_measured_fraction_full 0.856
_diffrn_reflns_point_group_measured_fraction_max 0.764
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.253
_diffrn_reflns_theta_min         2.482
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 550 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.15(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3037
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0454P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.455
_reflns_Friedel_fraction_full    0.679
_reflns_Friedel_fraction_max     0.531
_reflns_number_gt                2036
_reflns_number_total             3037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04941d2.cif
_cod_data_source_block           zyy
_cod_database_code               7131003
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C13(H13), C5(H5), C12(H12), C11(H11), C4(H4), C3(H3), C10(H10),
 C19(H19), C20(H20)
;
_shelx_res_checksum              65810
_shelx_hkl_checksum              97235
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.808