Magnetic-dielectric switching with wide hysteresis in an Fe(II) spin-crossover compound.
Ying, Ting-Ting; Chen, Yan-Cong; Ruan, Ze-Yu; Ni, Zhao-Ping; Tong, Ming-Liang; Dalton transactions (Cambridge, England : 2003)  (2025) –; doi:10.1039/d5dt02447a

data_7719912
_publ_section_title
;
 Magnetic-dielectric switching with wide hysteresis in an Fe(II)
 spin-crossover compound.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d5dt02447a
_journal_year                    2025
_chemical_formula_moiety
'C22 H18 Fe N10, 2(C2 F6 N O4 S2), H2 O, C11 H9 N5'
_chemical_formula_sum            'C37 H29 F12 Fe N17 O9 S4'
_chemical_formula_weight         1267.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-04-22 deposited with the CCDC.	2025-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7958(2)
_cell_length_b                   23.0586(4)
_cell_length_c                   24.1745(5)
_cell_measurement_reflns_used    16059
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7140
_cell_measurement_theta_min      2.6460
_cell_volume                     4903.04(17)
_computing_cell_refinement       'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.142a 64-bit (release 17-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.137a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.955
_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   -162.00-114.00   0.50    0.14    --  -97.00-103.00  65.00   96
  2  \w   -150.00 -82.00   0.50    0.14    --  -97.00 -57.00  60.00  136
  3  \w    -93.00 -63.00   0.50    0.14    --  -97.00  99.00 -94.00   60
  4  \w    -59.00 -28.00   0.50    0.14    --  -97.00  99.00 -94.00   62
  5  \w    -78.00 -24.00   0.50    0.14    --  -97.00  77.00-120.00  108
  6  \w    -66.00 -33.00   0.50    0.14    --  -97.00  57.00-180.00   66
  7  \w    -68.00 -34.00   0.50    0.14    --  -97.00  57.00  30.00   68
  8  \w    -54.00 -25.00   0.50    0.14    --  -97.00  57.00  90.00   58
  9  \w    -11.00  28.00   0.50    0.05    --  -47.40  19.00   0.00   78
 10  \w    -16.00  15.00   0.50    0.05    --   47.40 -19.00 150.00   62
 11  \w     98.00 149.00   0.50    0.14    --  109.16  33.00  67.00  102
 12  \w     77.00 163.00   0.50    0.14    --  109.16 125.00  90.00  172
 13  \w    -27.00  24.00   0.50    0.05    --   47.40 -19.00 120.00  102
 14  \w    -28.00  14.00   0.50    0.05    --   47.40 -19.00  90.00   84
 15  \w     32.00  58.00   0.50    0.05    --   47.40-125.00-180.00   52
 16  \w      9.00  71.00   0.50    0.05    --   47.40-103.00  65.00  124
 17  \w     40.00 112.00   0.50    0.14    --  109.16-125.00   0.00  144
 18  \w     42.00 102.00   0.50    0.14    --  109.16 -99.00-180.00  120
 19  \w     36.00  61.00   0.50    0.14    --  109.16 -57.00-150.00   50
 20  \w     36.00  61.00   0.50    0.14    --  109.16 -57.00 -90.00   50
 21  \w     36.00  61.00   0.50    0.14    --  109.16 -57.00  90.00   50
;
_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      -0.0770591000
_diffrn_orient_matrix_UB_12      0.0277627000
_diffrn_orient_matrix_UB_13      -0.0507501000
_diffrn_orient_matrix_UB_21      0.1492874000
_diffrn_orient_matrix_UB_22      -0.0058263000
_diffrn_orient_matrix_UB_23      -0.0328714000
_diffrn_orient_matrix_UB_31      -0.0495935000
_diffrn_orient_matrix_UB_32      -0.0604908000
_diffrn_orient_matrix_UB_33      -0.0200946000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29243
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.317
_diffrn_reflns_theta_min         2.648
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.137a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.483
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.091
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Flack x determined using 3168 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_coef       0.00078(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         9740
_refine_ls_number_restraints     502
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0685
_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^)+(0.1065P)^2^+17.2094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.1868
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                8753
_reflns_number_total             9740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02447a2.cif
_cod_data_source_block           exp_2862_autored
_cod_database_code               7719912
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CHONFSFe
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.191
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 O(H,H) groups
2. Restrained distances
 C34A-F2A
 1.32 with sigma of 0.02
 C34A-S1A
 1.84 with sigma of 0.02
 C34A-F3A
 1.31 with sigma of 0.02
 O1A-S1A
 1.43 with sigma of 0.02
 O2A-S1A
 1.45 with sigma of 0.02
 C34A-F1A
 1.33 with sigma of 0.02
 C34B-F2B
 1.32 with sigma of 0.02
 C34B-F3B
 1.31 with sigma of 0.02
 C34B-F1B
 1.33 with sigma of 0.02
 C34B-S1B
 1.84 with sigma of 0.02
 O1B-S1B
 1.43 with sigma of 0.02
 O2B-S1B
 1.45 with sigma of 0.02
 C34A-O1A
 2.59 with sigma of 0.04
 C34A-O2A
 2.6 with sigma of 0.04
 O1A-O2A
 2.46 with sigma of 0.04
 C34B-O1B
 2.59 with sigma of 0.04
 C34B-O2B
 2.6 with sigma of 0.04
 O1B-O2B
 2.46 with sigma of 0.04
 S1A-N16 \\sim N16-S1B
 with sigma of 0.02
 O1A-S1A \\sim S1A-O2A
 with sigma of 0.02
 F1A-S1A \\sim S1A-F2A
 with sigma of 0.02
 F1A-S1A \\sim S1A-F3A
 with sigma of 0.02
 F2B-F1B \\sim F1B-F3B
 with sigma of 0.02
 F2B-F3B \\sim F3B-F1B
 with sigma of 0.02
 F2B-S1B \\sim F5-S2
 with sigma of 0.02
 F1B-S1B \\sim F6-S2
 with sigma of 0.02
 F1B-S1B \\sim S1B-F2B
 with sigma of 0.02
 F3A-F1A \\sim F1A-F2A
 with sigma of 0.02
 O1B-S1B \\sim S1B-O2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S1A \\sim S1B \\sim F1A \\sim F1B \\sim F2A \\sim F2B \\sim F3A \\sim F3B \\sim
O1A \\sim O1B \\sim O2A \\sim O2B \\sim C34A \\sim C34B: within 3A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(S1A) \\sim Ueq, Uanis(O2B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(S1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O1B)=Sof(O2B)=Sof(C34B)=1-FVAR(1)
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O1A)=Sof(O2A)=Sof(C34A)=FVAR(1)
5.a Free rotating group:
 O9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N10(H10), N5(H5), N1(H1), N11(H11A), N14(H14), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C11(H11), C10(H10A), C7(H7),
 C6(H6A), C5(H5A), C2(H2), C1(H1A), C23(H23), C24(H24), C27(H27), C28(H28),
 C29(H29), C32(H32), C33(H33)
;
_shelx_res_checksum              11241
_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 4.403
_oxdiff_exptl_absorpt_empirical_full_min 0.253