Observation of proton-transfer-coupled spin transition by single-crystal neutron-diffraction measurement.
Nakanishi, Takumi; Hori, Yuta; Shigeta, Yasuteru; Sato, Hiroyasu; Wu, Shu-Qi; Kiyanagi, Ryoji; Munakata, Koji; Ohhara, Takashi; Sato, Osamu; Physical chemistry chemical physics : PCCP 25 (2023) 12394–12400; doi:10.1039/d3cp00527e

data_7246626
_publ_section_title
;
 Observation of proton-transfer-coupled spin transition by single-crystal
 neutron-diffraction measurement.
;
_journal_issue                   17
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              12394
_journal_page_last               12400
_journal_paper_doi               10.1039/d3cp00527e
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C38 H32 Fe N8 O4, 2(C3 F6 N O4 S2)'
_chemical_formula_sum            'C44 H32 F12 Fe N10 O12 S4'
_chemical_formula_weight         1304.88
_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   difmap
_audit_creation_date             2022-05-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-23 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.147(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.090(3)
_cell_length_b                   17.886(2)
_cell_length_c                   18.179(3)
_cell_measurement_reflns_used    5745
_cell_measurement_temperature    130(1)
_cell_measurement_theta_max      83.3
_cell_measurement_theta_min      6.6
_cell_volume                     4944.7(14)
_computing_cell_refinement       'STARGazer (Ohhara, 2009)'
_computing_data_collection       'STARGazer (Ohhara, 2009)'
_computing_data_reduction        'STARGazer (Ohhara, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean '4 mm'
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device
'single-crystal diffractometer SENJU at the BL18 in the MLF of the J-PARC'
_diffrn_measurement_device_type
'time-of-flight Laue-type single crystal neutron diffractometer'
_diffrn_measurement_method       'time-of-flight Laue method'
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     1.000
_diffrn_reflns_av_R_equivalents  0.1917
_diffrn_reflns_av_unetI/netI     0.1602
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            64073
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        36.870
_diffrn_reflns_theta_max         50.805
_diffrn_reflns_theta_min         2.473
_exptl_absorpt_coefficient_mu    1.594
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          4.5
_exptl_crystal_size_mid          3.5
_exptl_crystal_size_min          3.5
_refine_diff_density_max         1.659
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         17488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0427P)^2^+29.8942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10845
_reflns_number_total             17488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp00527e2.cif
_cod_data_source_block           FePy3OMe_HFDF_130k_Neutron
_cod_depositor_comments
'Adding full bibliography for 7246623--7246626.cif.'
_cod_database_code               7246626
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
;
_shelx_res_checksum              85417
_olex2_submission_special_instructions 'No special instructions were received'