Dynamic spin reordering in a hybrid layered ferrimagnet with intercalated biferrocenium radicals.
Liu, Qingxin; Kosaka, Wataru; Miyasaka, Hitoshi; Chemical science 15 (2024) 19411–19419; doi:10.1039/d4sc04722b

data_1572977
_publ_section_title
;
 Dynamic spin reordering in a hybrid layered ferrimagnet with intercalated
 biferrocenium radicals.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              19411
_journal_page_last               19419
_journal_paper_doi               10.1039/d4sc04722b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C68 H10 F34 N4 O16 Ru4, 2(C10 H9 Fe)'
_chemical_formula_sum            'C88 H28 F34 Fe2 N4 O16 Ru4'
_chemical_formula_weight         2559.12
_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             2023-12-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-07-16 deposited with the CCDC.	2024-10-30 downloaded from the CCDC.
;
_cell_angle_alpha                76.436(2)
_cell_angle_beta                 71.465(2)
_cell_angle_gamma                89.910(2)
_cell_formula_units_Z            2
_cell_length_a                   15.6986(3)
_cell_length_b                   17.2101(3)
_cell_length_c                   17.6280(3)
_cell_measurement_reflns_used    22074
_cell_measurement_temperature    102.1
_cell_measurement_theta_max      29.6850
_cell_measurement_theta_min      1.5110
_cell_volume                     4375.87(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 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      102.1
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.838
_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    -66.00  53.00   0.50   20.00    --   15.95 -39.00  53.00  238
  2  \w    -22.00  90.00   0.50   20.00    --   15.95  39.00-152.00  224
  3  \w    -94.00 -44.00   0.50   20.00    --  -15.48 -77.00-120.00  100
  4  \w   -104.00 -51.00   0.50   20.00    --  -15.48-179.00 -60.00  106
  5  \w    -73.00 -48.00   0.50   20.00    --  -15.48 179.00  30.00   50
  6  \w    -21.00  18.00   0.50   20.00    --  -15.48 -77.00-120.00   78
  7  \w     58.00  84.00   0.50   20.00    --   15.95 179.00  30.00   52
  8  \w    -11.00  40.00   0.50   20.00    --   15.95 -99.00 -30.00  102
  9  \w    -18.00  82.00   0.50   20.00    --   15.95  77.00-120.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0461263000
_diffrn_orient_matrix_UB_12      0.0133998000
_diffrn_orient_matrix_UB_13      -0.0204858000
_diffrn_orient_matrix_UB_21      -0.0003991000
_diffrn_orient_matrix_UB_22      -0.0163159000
_diffrn_orient_matrix_UB_23      -0.0332987000
_diffrn_orient_matrix_UB_31      -0.0125533000
_diffrn_orient_matrix_UB_32      0.0369195000
_diffrn_orient_matrix_UB_33      -0.0197341000
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54325
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.722
_diffrn_reflns_theta_min         1.521
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.139
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       block
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.566
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         20837
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+2.8914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15955
_reflns_number_total             20837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04722b2.cif
_cod_data_source_block           Ru2356F4_TCNQF2_Bifc
_cod_depositor_comments
'Adding full bibliography for 1572977--1572978.cif.'
_cod_database_code               1572977
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N F Ru Fe'
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.895
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C63 \\sim F34: within 2A with sigma of 0.01 and sigma for terminal atoms of 3.8
within 2A
Uanis(F34) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C12(H12), C19(H19), C26(H26), C33(H33), C40(H40), C47(H47), C54(H54),
 C62(H62), C64(H64), C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75),
  C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82),
 C83(H83), C84(H84), C85(H85), C86(H86), C88(H88)
;
_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 4.371
_oxdiff_exptl_absorpt_empirical_full_min 0.276