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_7246624
_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   geom
_audit_creation_date             2022-02-12
_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                 117.356(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0591(6)
_cell_length_b                   17.8559(4)
_cell_length_c                   18.1668(7)
_cell_measurement_reflns_used    13543
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      30.4490
_cell_measurement_theta_min      2.4550
_cell_volume                     4914.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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     28.00  68.00   0.50   21.64    --  -15.90  45.00  30.00   80
  2  \w    -99.00 -48.00   0.50   21.64    --  -15.90  45.00 150.00  102
  3  \w     46.00  73.00   0.50   21.64    --  -15.90  45.00 150.00   54
  4  \w   -105.00   6.00   0.50   21.64    --  -15.90  45.00  30.00  222
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23307
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.502
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.43a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic blackish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       prism
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         8807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0586P)^2^+8.5243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8057
_reflns_number_total             8807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp00527e2.cif
_cod_data_source_block           FePy3OMe_HFDF_123K_Xray
_cod_depositor_comments
'Adding full bibliography for 7246623--7246626.cif.'
_cod_original_cell_volume        4914.9(3)
_cod_database_code               7246624
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.870
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N7(H2), N4(H1), C18(H3), C19(H38), C1(H19), C4(H16), C26(H30), C20(H37),
 C22(H35), C21(H36), C15(H5A), C2(H18), C11(H14), C16(H4), C14(H6), C36(H21),
 C8(H11), C3(H17), C32(H25), C10(H13), C28(H32), C27(H31), C33(H24), C9(H12),
 C29(H33), C34(H23)
2.b Idealised Me refined as rotating group:
 C37(H8A,H8B,H8C), C38(H27A,H27B,H27C)
;
_shelx_res_checksum              24413
_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
;