Application of multiple small-wedge synchrotron crystallography for post-reaction structural characterization of a stimuli-responsive small-molecule crystal
Sasaki, Toshiyuki; Nakane, Takanori; Takimoto, Kazuyoshi; Ichiyanagi, Kouhei; Mori, Yuki; Baba, Seiki; Sakai, Naoki; Kurisu, Genji; Miyata, Mikiji; Uno, Takahiro; Itoh, Takahito; Bulletin of the Chemical Society of Japan 98 (2025) –; doi:10.1093/bulcsj/uoaf059

data_3000590
_publ_section_title
;
 Application of multiple small-wedge synchrotron crystallography for
 post-reaction structural characterization of a stimuli-responsive
 small-molecule crystal
;
_journal_name_full               'Bulletin of the Chemical Society of Japan'
_journal_paper_doi               10.1093/bulcsj/uoaf059
_journal_volume                  98
_journal_year                    2025
_chemical_formula_moiety         'C16 H16 O8'
_chemical_formula_sum            'C16 H16 O8'
_chemical_formula_weight         336.29
_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   difmap
_audit_creation_date             2025-06-02
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.633(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7562(16)
_cell_length_b                   6.8045(10)
_cell_length_c                   12.4297(19)
_cell_measurement_reflns_used    1370
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.78850802421852
_cell_measurement_theta_min      3.747674960567056
_cell_volume                     725.4(2)
_computing_cell_refinement
'dials.two_theta_refine (Waterman et al., 2016)'
_computing_data_collection
;
ZOO (Hirata et al., 2019)
BSS (Ueno et al., 2005)
SHIKA (Barty et al., 2014)
KUMA (Hirata et al., 2016)
;
_computing_data_reduction        'dials.scale (Beilsten-Edmands et al., 2020)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'EIGER2 16M XE'
_diffrn_measurement_method       'Multiple small-wedge'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.1363
_diffrn_reflns_av_unetI/netI     0.1008
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11763
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         27.815
_diffrn_reflns_theta_min         2.575
_exptl_absorpt_coefficient_mu    0.121
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             352
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         1788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0700
_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^)+(0.1083P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1805
_refine_ls_wR_factor_ref         0.1898
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1056
_reflns_number_total             1788
_reflns_threshold_expression     'I > 2\s(I)'
_journal_article_reference       uoaf059
_cod_data_source_file            SWSX-poly1.cif
_cod_data_source_block           poly-1-SWSX
_cod_depositor_comments
;The structure was re-refined with the inclusion of unit cell parameter
 ESDs.

 Releasing structure 3000590 into public domain as published material.
;
_cod_original_cell_volume        725.4
_cod_database_code               3000590
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
;
_shelx_res_checksum              58400
_shelx_hkl_checksum              1237
_olex2_submission_special_instructions 'No special instructions were received'