Wrapping a single crystal spin-crossover complex with a single crystal non-spin-crossover complex to modulate the spin-transition temperature.
Fukui, Tomoya; Tsuchiya, Masahiro; Mita, Naoya; Fukushima, Takanori; Chemical science 16 (2025) 22387–22393; doi:10.1039/d5sc04311e

data_1576076
_publ_section_title
;
 Wrapping a single crystal spin-crossover complex with a single crystal
 non-spin-crossover complex to modulate the spin-transition temperature.
;
_journal_issue                   47
_journal_name_full               'Chemical science'
_journal_page_first              22387
_journal_page_last               22393
_journal_paper_doi               10.1039/d5sc04311e
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C24 H18 Fe N10 O4, 2(B F4)'
_chemical_formula_sum            'C24 H18 B2 F8 Fe N10 O4'
_chemical_formula_weight         739.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-20
_audit_creation_method
;
Olex2 1.5-ac5-023
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-12-06 deposited with the CCDC.	2025-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.984(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3355(3)
_cell_length_b                   16.5509(2)
_cell_length_c                   10.6777(2)
_cell_measurement_reflns_used    14813
_cell_measurement_temperature    393.15
_cell_measurement_theta_max      71.0140
_cell_measurement_theta_min      3.7500
_cell_volume                     2959.46(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-023 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      393.15
_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 0.992
_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    -98.00 -50.00   0.50    0.12    --    0.00-164.00  -2.00   96
  2  \w    -67.00  -7.00   0.50    0.12    --    0.00 116.00-125.00  120
  3  \w   -108.00  -7.00   0.50    0.48    --  -55.18 116.00-125.00  202
  4  \w   -154.00 -49.00   0.50    0.48    --  -55.18-164.00  -2.00  210
  5  \w   -143.00 -81.00   0.50    0.48    --  -55.18-116.00 145.00  124
  6  \w     54.00 137.00   0.50    0.48    --   55.18 164.00  21.00  166
  7  \w     85.00 137.00   0.50    0.48    --   55.18 116.00-125.00  104
  8  \w     12.00 109.00   0.50    0.48    --   55.18-116.00 145.00  194
  9  \w   -108.00 -19.00   0.50    0.48    -- -102.00 116.00-125.00  178
 10  \w   -154.00 -49.00   0.50    0.48    -- -102.00-164.00  -2.00  210
 11  \w   -175.00 -80.00   0.50    0.48    -- -102.00-116.00 145.00  190
 12  \w     53.00 155.00   0.50    0.48    --  110.35 164.00  21.00  204
 13  \w     21.00 109.00   0.50    0.48    --  110.35-116.00 145.00  176
 14  \w     38.00 138.00   0.50    0.48    --  110.35-164.00  -2.00  200
 15  \w     53.00 155.00   0.50    0.48    --  110.35 164.00  21.00  204
 16  \w    -19.00  83.00   0.50    0.12    --    0.00  19.00 -30.00  204
 17  \w    -18.00  58.00   0.50    0.12    --    0.00 -99.00 -30.00  152
 18  \w     13.00  67.00   0.50    0.12    --    0.00-116.00 145.00  108
 19  \w    -95.00 -34.00   0.50    0.12    --    0.00 164.00  21.00  122
 20  \w   -142.00 -74.00   0.50    0.48    --  -55.18-125.00 -90.00  136
 21  \w    -19.00  27.00   0.50    0.48    --  -55.18  19.00-120.00   92
 22  \w    -19.00  27.00   0.50    0.48    --  -55.18  19.00 120.00   92
 23  \w    -40.00  23.00   0.50    0.48    --   55.18 -19.00-150.00  126
 24  \w    -34.00  43.00   0.50    0.48    --   55.18 -37.00 150.00  154
 25  \w    -40.00  23.00   0.50    0.48    --   55.18 -19.00 -60.00  126
 26  \w     79.00 138.00   0.50    0.48    --   55.18 125.00  90.00  118
 27  \w     79.00 138.00   0.50    0.48    --   55.18 125.00 150.00  118
 28  \w     14.00 138.00   0.50    0.48    --   55.18  57.00 -60.00  248
 29  \w   -175.00 -55.00   0.50    0.48    -- -102.00 -77.00  60.00  240
 30  \w    -54.00 -19.00   0.50    0.48    -- -102.00  50.00 -90.00   70
 31  \w   -149.00 -19.00   0.50    0.48    -- -102.00  77.00   0.00  260
 32  \w    -54.00 -19.00   0.50    0.48    -- -102.00  50.00-180.00   70
 33  \w    -54.00 -19.00   0.50    0.48    -- -102.00  50.00  90.00   70
 34  \w   -137.00 -33.00   0.50    0.48    -- -102.00 164.00  21.00  208
 35  \w    -54.00 -19.00   0.50    0.48    -- -102.00  50.00  60.00   70
 36  \w    -54.00 -19.00   0.50    0.48    -- -102.00  50.00  30.00   70
 37  \w     20.00 108.00   0.50    0.48    --  110.35-111.00 -30.00  176
 38  \w     15.00 105.00   0.50    0.48    --  110.35 -91.00-180.00  180
 39  \w     65.00 178.00   0.50    0.48    --  110.35  50.00   0.00  226
 40  \w     11.00 178.00   0.50    0.48    --  110.35  12.00 120.00  334
 41  \w     26.00  78.00   0.50    0.48    --  110.35 -63.00 150.00  104
 42  \w     26.00  59.00   0.50    0.48    --  110.35 -50.00-150.00   66
 43  \w     20.00 108.00   0.50    0.48    --  110.35-111.00-150.00  176
 44  \w     87.00 178.00   0.50    0.48    --  110.35 111.00-180.00  182
 45  \w     26.00  78.00   0.50    0.48    --  110.35 -63.00  60.00  104
 46  \w     15.00 105.00   0.50    0.48    --  110.35 -91.00 -30.00  180
 47  \w     64.00 178.00   0.50    0.48    --  110.35  77.00 150.00  228
 48  \w     26.00  78.00   0.50    0.48    --  110.35 -63.00-180.00  104
 49  \w     26.00  78.00   0.50    0.48    --  110.35 -63.00 120.00  104
 50  \w     20.00 108.00   0.50    0.48    --  110.35-111.00  30.00  176
 51  \w    -47.00  83.00   0.50    0.12    --    0.00  77.00 -90.00  260
 52  \w    -47.00  83.00   0.50    0.12    --    0.00  77.00 150.00  260
 53  \w   -101.00 -42.00   0.50    0.12    --    0.00-178.00 150.00  118
 54  \w   -101.00 -42.00   0.50    0.12    --    0.00-178.00  60.00  118
 55  \w   -100.00 -40.00   0.50    0.12    --    0.00 178.00 -90.00  120
 56  \w      8.00 138.00   0.50    0.48    --   55.18  77.00  60.00  260
 57  \w      8.00 138.00   0.50    0.48    --   55.18  77.00-180.00  260
 58  \w      8.00 138.00   0.50    0.48    --   55.18  77.00-120.00  260
 59  \w     14.00 138.00   0.50    0.48    --   55.18  57.00 150.00  248
 60  \w      8.00  99.00   0.50    0.48    --   55.18  77.00   0.00  182
 61  \w      8.00 138.00   0.50    0.48    --   55.18  77.00 -30.00  260
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0151152000
_diffrn_orient_matrix_UB_12      -0.0906182000
_diffrn_orient_matrix_UB_13      -0.0293854000
_diffrn_orient_matrix_UB_21      0.0906861000
_diffrn_orient_matrix_UB_22      -0.0156073000
_diffrn_orient_matrix_UB_23      0.0387484000
_diffrn_orient_matrix_UB_31      -0.0029008000
_diffrn_orient_matrix_UB_32      -0.0145281000
_diffrn_orient_matrix_UB_33      0.1412065000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            26589
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.143
_diffrn_reflns_theta_min         3.755
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.026
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         2854
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0947P)^2^+4.6490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1614
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2787
_reflns_number_total             2854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04311e2.cif
_cod_data_source_block           Fecdpp_393K
_cod_depositor_comments
'Adding full bibliography for 1576072--1576077.cif.'
_cod_database_code               1576076
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H18 O4 N10 Fe B2 F8'
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.418
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.02
 O2-H2
 0.82 with sigma of 0.02
3. Others
 Fixed Sof: H1(0.5) H2(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3), C5(H5), C8(H8), C9(H9), C10(H10), C12(H12)
;
_shelx_res_checksum              23806
_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 3.151
_oxdiff_exptl_absorpt_empirical_full_min 0.622