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_1576073
_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 Co N10 O4, 2(B F4)'
_chemical_formula_sum            'C24 H18 B2 Co F8 N10 O4'
_chemical_formula_weight         743.03
_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 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-12-06 deposited with the CCDC.	2025-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.6190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9753(2)
_cell_length_b                   16.4202(2)
_cell_length_c                   10.53040(10)
_cell_measurement_reflns_used    13472
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      71.0290
_cell_measurement_theta_min      5.1300
_cell_volume                     2840.19(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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93(2)
_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 0.992
_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     64.00 178.00   0.50    0.05    --  110.35  77.00 -90.00  228
  2  \w     64.00 178.00   0.50    0.05    --  110.35  77.00-120.00  228
  3  \w     64.00 178.00   0.50    0.05    --  110.35  77.00-150.00  228
  4  \w     64.00 178.00   0.50    0.05    --  110.35  77.00-180.00  228
  5  \w     70.00 178.00   0.50    0.05    --  110.35  63.00-180.00  216
  6  \w     70.00 178.00   0.50    0.05    --  110.35  63.00 -60.00  216
  7  \w     25.00 178.00   0.50    0.05    --  110.35  33.00 135.00  306
  8  \w    -31.00 138.00   0.50    0.05    --   55.18  33.00 135.00  338
  9  \w    -34.00  83.00   0.50    0.05    --    0.00  33.00 135.00  234
 10  \w    -91.00  38.00   0.50    0.05    --    0.00 -33.00 -23.00  258
 11  \w    -83.00  40.00   0.50    0.05    --    0.00 -57.00 -30.00  246
 12  \w    -94.00  47.00   0.50    0.05    --    0.00 -77.00-180.00  282
 13  \w     79.00 138.00   0.50    0.05    --   55.18 125.00-120.00  118
 14  \w     87.00 178.00   0.50    0.05    --  110.35 111.00  30.00  182
 15  \w     87.00 178.00   0.50    0.05    --  110.35 111.00   0.00  182
 16  \w     87.00 178.00   0.50    0.05    --  110.35 111.00-180.00  182
 17  \w     79.00 138.00   0.50    0.05    --   55.18 125.00  30.00  118
 18  \w     79.00 138.00   0.50    0.05    --   55.18 125.00   0.00  118
 19  \w     -1.00  28.00   0.50    0.05    --   55.18  96.00   6.14   58
 20  \w     -2.00  26.00   0.50    0.05    --   55.18  98.00  64.10   56
 21  \w     -2.00  26.00   0.50    0.05    --   55.18  98.00-149.71   56
 22  \w     -2.00  26.00   0.50    0.05    --   55.18  98.00 -70.04   56
 23  \w   -100.00 -40.00   0.50    0.05    --    0.00 178.00 -30.00  120
 24  \w      4.00  42.00   0.50    0.05    --   55.18  86.00  -4.93   76
 25  \w      2.00  42.00   0.50    0.05    --   55.18  90.00 151.76   80
 26  \w     15.00 105.00   0.50    0.05    --  110.35 -91.00  30.00  180
 27  \w     26.00  78.00   0.50    0.05    --  110.35 -63.00 150.00  104
 28  \w     26.00  78.00   0.50    0.05    --  110.35 -63.00 -90.00  104
 29  \w     26.00  78.00   0.50    0.05    --  110.35 -63.00-120.00  104
 30  \w     26.00  78.00   0.50    0.05    --  110.35 -63.00-180.00  104
 31  \w     26.00  59.00   0.50    0.05    --  110.35 -50.00 -60.00   66
 32  \w     26.00  59.00   0.50    0.05    --  110.35 -50.00  60.00   66
 33  \w     26.00  59.00   0.50    0.05    --  110.35 -50.00  90.00   66
 34  \w    -35.00  38.00   0.50    0.05    --   55.18 -33.00 -23.00  146
 35  \w   -101.00 -42.00   0.50    0.05    --    0.00-178.00 120.00  118
 36  \w   -101.00 -42.00   0.50    0.05    --    0.00-178.00-180.00  118
 37  \w    -19.00  27.00   0.50    0.05    --  -55.18  19.00-150.00   92
 38  \w   -108.00 -19.00   0.50    0.05    -- -102.00 111.00-180.00  178
 39  \w   -108.00 -19.00   0.50    0.05    -- -102.00 111.00 150.00  178
 40  \w   -175.00 -55.00   0.50    0.05    -- -102.00 -77.00 -90.00  240
 41  \w   -175.00 -55.00   0.50    0.05    -- -102.00 -77.00-121.56  240
 42  \w   -175.00 -55.00   0.50    0.05    -- -102.00 -77.00-150.00  240
 43  \w   -175.00 -55.00   0.50    0.05    -- -102.00 -77.00-180.00  240
 44  \w   -175.00 -57.00   0.50    0.05    -- -102.00 -73.00-172.11  236
 45  \w   -175.00 -57.00   0.50    0.05    -- -102.00 -74.00-140.06  236
 46  \w   -175.00 -55.00   0.50    0.05    -- -102.00 -77.00-120.00  240
 47  \w   -175.00 -56.00   0.50    0.05    -- -102.00 -75.00-109.25  238
 48  \w   -175.00 -35.00   0.50    0.05    -- -102.00 -37.00-150.00  280
 49  \w   -175.00 -56.00   0.50    0.05    -- -102.00 -76.00 -77.83  238
 50  \w   -175.00 -19.00   0.50    0.05    -- -102.00 -33.00 -23.00  312
 51  \w   -146.00  27.00   0.50    0.05    --  -55.18 -33.00 -23.00  346
 52  \w   -138.00 -15.00   0.50    0.05    --  -55.18 -57.00-120.00  246
 53  \w    -37.00  -4.00   0.50    0.05    --  -55.18 -84.00-135.94   66
 54  \w   -142.00 -74.00   0.50    0.05    --  -55.18-125.00  90.00  136
;
_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      -0.0202354000
_diffrn_orient_matrix_UB_12      -0.0220598000
_diffrn_orient_matrix_UB_13      0.1304212000
_diffrn_orient_matrix_UB_21      0.0871300000
_diffrn_orient_matrix_UB_22      -0.0326824000
_diffrn_orient_matrix_UB_23      0.0537142000
_diffrn_orient_matrix_UB_31      0.0282330000
_diffrn_orient_matrix_UB_32      0.0851160000
_diffrn_orient_matrix_UB_33      0.0544459000
_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  0.1055
_diffrn_reflns_av_unetI/netI     0.0380
_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       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25097
_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         71.253
_diffrn_reflns_theta_min         3.806
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_exptl_absorpt_coefficient_mu    5.715
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.744
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       block
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2748
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0968P)^2^+2.6170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2645
_reflns_number_total             2748
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04311e2.cif
_cod_data_source_block           Cocdpp_shell
_cod_depositor_comments
'Adding full bibliography for 1576072--1576077.cif.'
_cod_database_code               1576073
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C24 H18 O4 N10 Co B2 F8'
_shelx_estimated_absorpt_t_max   0.502
_shelx_estimated_absorpt_t_min   0.380
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 O2-H2
 0.82 with sigma of 0.02
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C5(H5), C8(H8), C9(H9), C10(H10), C12(H12)
;
_shelx_res_checksum              34582
_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 4.405
_oxdiff_exptl_absorpt_empirical_full_min 0.481