Optical cavity enhancement of visible light-driven photochemical reaction in the crystalline state.
Sasaki, Ikuto; Takahashi, Kiyonori; Taemaitree, Farsai; Nakamura, Takayoshi; Hutchison, James A.; Uji-I, Hiroshi; Hirai, Kenji; Chemical communications (Cambridge, England) 61 (2025) 2766–2769; doi:10.1039/d4cc05598e

data_7134156
_publ_section_title
;
 Optical cavity enhancement of visible light-driven photochemical reaction
 in the crystalline state.
;
_journal_issue                   13
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2766
_journal_page_last               2769
_journal_paper_doi               10.1039/d4cc05598e
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C10 H11 N O4'
_chemical_formula_sum            'C10 H11 N O4'
_chemical_formula_weight         209.20
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-12 deposited with the CCDC.	2025-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.588(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.85270(10)
_cell_length_b                   15.8701(5)
_cell_length_c                   15.9967(6)
_cell_measurement_reflns_used    4868
_cell_measurement_temperature    93.9(7)
_cell_measurement_theta_max      30.2990
_cell_measurement_theta_min      2.5470
_cell_volume                     974.95(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_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_environment      N~2~
_diffrn_ambient_temperature      93.9(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.831
_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     -5.00  29.00   0.50   19.31    --   -5.79 -99.00  90.00   68
  2  \w    -64.00  22.00   0.50   19.31    --    6.10 -57.00 -60.00  172
  3  \w      4.00  72.00   0.50   19.31    --    6.10  57.00   0.00  136
  4  \w    -64.00  76.00   0.50   19.31    --    6.10   0.00  30.00  280
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0285755000
_diffrn_orient_matrix_UB_12      0.0430236000
_diffrn_orient_matrix_UB_13      -0.0104008000
_diffrn_orient_matrix_UB_21      -0.0119740000
_diffrn_orient_matrix_UB_22      -0.0104919000
_diffrn_orient_matrix_UB_23      -0.0432365000
_diffrn_orient_matrix_UB_31      -0.1820924000
_diffrn_orient_matrix_UB_32      -0.0060470000
_diffrn_orient_matrix_UB_33      0.0008702000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.767
_diffrn_reflns_theta_min         2.555
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0534P)^2^+0.3792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2122
_reflns_number_total             2546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05598e2.cif
_cod_data_source_block           exp_840_auto
_cod_depositor_comments          'Adding full bibliography for 7134156.cif.'
_cod_database_code               7134156
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H11NO4
_chemical_oxdiff_usercomment     94K
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.983
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C8(H8), C9(H9), C2(H2)
1.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              10745
_shelx_hkl_checksum              33987
_olex2_exptl_crystal_mounting_method 'MIteGen Micromount'
_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 1.387
_oxdiff_exptl_absorpt_empirical_full_min 0.773