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_1576072
_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             2022-10-19
_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                 106.6610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1400(2)
_cell_length_b                   16.0326(2)
_cell_length_c                   10.65500(10)
_cell_measurement_reflns_used    15285
_cell_measurement_temperature    93
_cell_measurement_theta_max      71.1550
_cell_measurement_theta_min      3.8320
_cell_volume                     2805.06(6)
_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      93
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -47.00  83.00   0.50    0.05    --    0.00  77.00 150.00  260
  2  \w    -19.00  83.00   0.50    0.05    --    0.00  19.00   0.00  204
  3  \w    -47.00  83.00   0.50    0.05    --    0.00  77.00-150.00  260
  4  \w   -101.00 -42.00   0.50    0.05    --    0.00-178.00 -90.00  118
  5  \w   -101.00 -42.00   0.50    0.05    --    0.00-178.00  90.00  118
  6  \w    -18.00  58.00   0.50    0.05    --    0.00 -99.00 -30.00  152
  7  \w     35.00  82.00   0.50    0.05    --    0.00-157.00  -8.00   94
  8  \w    -40.00  23.00   0.50    0.06    --   55.18 -19.00-150.00  126
  9  \w    -40.00  23.00   0.50    0.06    --   55.18 -19.00 -60.00  126
 10  \w     26.00  59.00   0.50    0.06    --  110.35 -50.00 -30.00   66
 11  \w     20.00 108.00   0.50    0.06    --  110.35-111.00 -30.00  176
 12  \w     34.00 134.00   0.50    0.06    --  110.35-157.00  -8.00  200
 13  \w     15.00 105.00   0.50    0.06    --  110.35 -91.00 -30.00  180
 14  \w     20.00 108.00   0.50    0.06    --  110.35-111.00  60.00  176
 15  \w     13.00 109.00   0.50    0.06    --   55.18-118.00 146.00  192
 16  \w     22.00 110.00   0.50    0.06    --  110.35-118.00 146.00  176
 17  \w   -142.00 -74.00   0.50    0.06    --  -55.18-125.00-120.00  136
 18  \w   -160.00 -52.00   0.50    0.06    -- -102.00-157.00  -8.00  216
 19  \w   -151.00 -52.00   0.50    0.06    --  -55.18-157.00  -8.00  198
 20  \w   -142.00 -74.00   0.50    0.06    --  -55.18-125.00  30.00  136
 21  \w   -143.00 -80.00   0.50    0.06    --  -55.18-118.00 146.00  126
 22  \w   -149.00 -87.00   0.50    0.06    --  -55.18 -99.00  60.00  124
 23  \w    -19.00  27.00   0.50    0.06    --  -55.18  19.00 120.00   92
 24  \w    -74.00 -19.00   0.50    0.06    -- -102.00  63.00  90.00  110
 25  \w    -74.00 -19.00   0.50    0.06    -- -102.00  63.00  60.00  110
 26  \w    -54.00 -19.00   0.50    0.06    -- -102.00  50.00  30.00   70
 27  \w    -54.00 -19.00   0.50    0.06    -- -102.00  50.00   0.00   70
 28  \w    -54.00 -19.00   0.50    0.06    -- -102.00  50.00 -90.00   70
 29  \w    -54.00 -19.00   0.50    0.06    -- -102.00  50.00-120.00   70
 30  \w    -54.00 -19.00   0.50    0.06    -- -102.00  50.00-180.00   70
 31  \w    -19.00  27.00   0.50    0.06    --  -55.18  19.00-150.00   92
 32  \w    -19.00  27.00   0.50    0.06    --  -55.18  19.00-120.00   92
 33  \w    -19.00  27.00   0.50    0.06    --  -55.18  19.00 -60.00   92
 34  \w    -38.00  27.00   0.50    0.06    --  -55.18  37.00 150.00  130
 35  \w   -175.00 -55.00   0.50    0.06    -- -102.00 -77.00  60.00  240
 36  \w   -109.00 -19.00   0.50    0.06    -- -102.00 118.00-127.00  180
 37  \w   -108.00 -19.00   0.50    0.06    -- -102.00 111.00  30.00  178
 38  \w      8.00 138.00   0.50    0.06    --   55.18  77.00 120.00  260
 39  \w      8.00 138.00   0.50    0.06    --   55.18  77.00 -30.00  260
 40  \w      8.00 138.00   0.50    0.06    --   55.18  77.00  60.00  260
 41  \w     70.00 178.00   0.50    0.06    --  110.35  63.00  30.00  216
 42  \w      8.00 138.00   0.50    0.06    --   55.18  77.00 -90.00  260
 43  \w      8.00 138.00   0.50    0.06    --   55.18  77.00-150.00  260
 44  \w     14.00 107.00   0.50    0.06    --   55.18  57.00-150.00  186
 45  \w     64.00 178.00   0.50    0.06    --  110.35  77.00-180.00  228
 46  \w     87.00 178.00   0.50    0.06    --  110.35 111.00   0.00  182
 47  \w     47.00 146.00   0.50    0.06    --  110.35 178.00  90.00  198
 48  \w     47.00 146.00   0.50    0.06    --  110.35 178.00 -60.00  198
 49  \w     47.00 146.00   0.50    0.06    --  110.35 178.00 -30.00  198
 50  \w     47.00 146.00   0.50    0.06    --  110.35 178.00 -60.00  198
 51  \w     47.00 146.00   0.50    0.06    --  110.35 178.00 -90.00  198
 52  \w     47.00 146.00   0.50    0.06    --  110.35 178.00-180.00  198
 53  \w     57.00 161.00   0.50    0.06    --  110.35 157.00  27.00  208
 54  \w     58.00 137.00   0.50    0.06    --   55.18 157.00  27.00  158
 55  \w     83.00 178.00   0.50    0.06    --  110.35 118.00-127.00  190
 56  \w     79.00 138.00   0.50    0.06    --   55.18 125.00 120.00  118
 57  \w     79.00 138.00   0.50    0.06    --   55.18 125.00 150.00  118
 58  \w     87.00 178.00   0.50    0.06    --  110.35 111.00  90.00  182
 59  \w     87.00 178.00   0.50    0.06    --  110.35 111.00 -90.00  182
 60  \w     84.00 137.00   0.50    0.06    --   55.18 118.00-127.00  106
 61  \w   -100.00 -40.00   0.50    0.05    --    0.00 178.00-150.00  120
 62  \w    -91.00 -31.00   0.50    0.05    --    0.00 157.00  27.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0156074000
_diffrn_orient_matrix_UB_12      -0.0938804000
_diffrn_orient_matrix_UB_13      0.0267579000
_diffrn_orient_matrix_UB_21      -0.0924815000
_diffrn_orient_matrix_UB_22      -0.0160952000
_diffrn_orient_matrix_UB_23      -0.0421057000
_diffrn_orient_matrix_UB_31      0.0017607000
_diffrn_orient_matrix_UB_32      -0.0128823000
_diffrn_orient_matrix_UB_33      -0.1424226000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25481
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.259
_diffrn_reflns_theta_min         3.853
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_exptl_absorpt_coefficient_mu    5.302
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.741
_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 red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         2712
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0340P)^2^+2.6010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2625
_reflns_number_total             2712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04311e2.cif
_cod_data_source_block           Fecdpp_93K
_cod_depositor_comments
'Adding full bibliography for 1576072--1576077.cif.'
_cod_database_code               1576072
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H18 O4 N10 Fe B2 F8'
_shelx_estimated_absorpt_t_max   0.676
_shelx_estimated_absorpt_t_min   0.363
_olex2_refinement_description
;
1. Restrained distances
 O1-H1
 0.82 with sigma of 0.02
 O2-H2
 0.82 with sigma of 0.02
2. Others
 Fixed Sof: H1(0.5) H2(0.5)
3.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              9677
_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 3.669
_oxdiff_exptl_absorpt_empirical_full_min 0.695