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_3000591
_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         'Ca H O4 P'
_chemical_formula_sum            'Ca H O4 P'
_chemical_formula_weight         136.06
_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             2025-02-26
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                76.15
_cell_angle_beta                 83.82
_cell_angle_gamma                88.42
_cell_formula_units_Z            4
_cell_length_a                   6.618
_cell_length_b                   6.892
_cell_length_c                   6.980
_cell_measurement_reflns_used    4382
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.214090117250148
_cell_measurement_theta_min      2.9705078770521576
_cell_volume                     307.313
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1781
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14415
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         27.801
_diffrn_reflns_theta_min         2.977
_exptl_absorpt_coefficient_mu    2.292
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.940
_exptl_crystal_description       plate
_exptl_crystal_F_000             272
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0512P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1115
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1163
_reflns_number_total             1527
_reflns_threshold_expression     'I > 2\s(I)'
_journal_article_reference       uoaf059
_cod_data_source_file            monetite.cif
_cod_data_source_block           monetite
_cod_depositor_comments
'Releasing structure 3000591 into public domain as published material.'
_cod_original_cell_volume        307.3
_cod_database_code               3000591
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Others
 Fixed Sof: H2(0.5) H3(0.5)
2.a Idealised tetrahedral OH refined as rotating group:
 O8(H8), O2(H2), O3(H3)
;
_shelx_res_checksum              69309
_shelx_hkl_checksum              93087
_olex2_submission_special_instructions 'No special instructions were received'