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_1576075
_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 N10 O4 Zn, 2(B F4)'
_chemical_formula_sum            'C24 H18 B2 F8 N10 O4 Zn'
_chemical_formula_weight         749.47
_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                 104.5040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9573(2)
_cell_length_b                   16.5167(2)
_cell_length_c                   10.50670(10)
_cell_measurement_reflns_used    16446
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      71.1760
_cell_measurement_theta_min      3.7760
_cell_volume                     2848.92(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(2)
_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 0.988
_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    -95.00 -34.00   0.50    0.05    --    0.00 163.00 137.00  122
  2  \w   -100.00 -40.00   0.50    0.05    --    0.00 178.00   0.00  120
  3  \w    -47.00  83.00   0.50    0.05    --    0.00  77.00 -60.00  260
  4  \w    -47.00  83.00   0.50    0.05    --    0.00  77.00-120.00  260
  5  \w    -67.00  -7.00   0.50    0.05    --    0.00 116.00 -10.00  120
  6  \w    -19.00  83.00   0.50    0.05    --    0.00  19.00 -60.00  204
  7  \w    -54.00 -19.00   0.50    0.09    -- -102.00  50.00 150.00   70
  8  \w    -54.00 -19.00   0.50    0.09    -- -102.00  50.00 120.00   70
  9  \w    -19.00  27.00   0.50    0.09    --  -55.18  19.00   0.00   92
 10  \w    -19.00  27.00   0.50    0.09    --  -55.18  19.00 -30.00   92
 11  \w    -19.00  27.00   0.50    0.09    --  -55.18  19.00 -60.00   92
 12  \w    -19.00  27.00   0.50    0.09    --  -55.18  19.00 -90.00   92
 13  \w    -54.00 -19.00   0.50    0.09    -- -102.00  50.00-180.00   70
 14  \w    -19.00  27.00   0.50    0.09    --  -55.18  19.00-120.00   92
 15  \w      3.00  42.00   0.50    0.09    --   55.18  87.00 -30.28   78
 16  \w     47.00 146.00   0.50    0.09    --  110.35 178.00-120.00  198
 17  \w     47.00 146.00   0.50    0.09    --  110.35 178.00 -90.00  198
 18  \w     79.00 138.00   0.50    0.09    --   55.18 125.00-150.00  118
 19  \w     84.00 178.00   0.50    0.09    --  110.35 116.00 -10.00  188
 20  \w     85.00 137.00   0.50    0.09    --   55.18 116.00 -10.00  104
 21  \w     79.00 138.00   0.50    0.09    --   55.18 125.00  60.00  118
 22  \w     55.00 137.00   0.50    0.09    --   55.18 163.00 137.00  164
 23  \w     54.00 156.00   0.50    0.09    --  110.35 163.00 137.00  204
 24  \w     87.00 178.00   0.50    0.09    --  110.35 111.00  60.00  182
 25  \w     87.00 178.00   0.50    0.09    --  110.35 111.00  90.00  182
 26  \w      0.00  33.00   0.50    0.09    --   55.18  94.00 145.68   66
 27  \w      0.00  33.00   0.50    0.09    --   55.18  93.00  71.34   66
 28  \w      2.00  42.00   0.50    0.09    --   55.18  89.00  15.04   80
 29  \w      0.00  33.00   0.50    0.09    --   55.18  94.00-129.39   66
 30  \w     42.00 178.00   0.50    0.09    --  110.35  37.00-120.00  272
 31  \w     14.00 138.00   0.50    0.09    --   55.18  57.00   0.00  248
 32  \w     64.00 178.00   0.50    0.09    --  110.35  77.00   0.00  228
 33  \w     64.00 178.00   0.50    0.09    --  110.35  77.00  60.00  228
 34  \w      8.00 138.00   0.50    0.09    --   55.18  77.00 120.00  260
 35  \w    -95.00  23.00   0.50    0.05    --    0.00 -19.00  60.00  236
 36  \w    -40.00  23.00   0.50    0.09    --   55.18 -19.00  60.00  126
 37  \w     26.00  78.00   0.50    0.09    --  110.35 -63.00-120.00  104
 38  \w    -34.00  43.00   0.50    0.09    --   55.18 -37.00 120.00  154
 39  \w     26.00  59.00   0.50    0.09    --  110.35 -50.00  90.00   66
 40  \w     26.00  78.00   0.50    0.09    --  110.35 -63.00 150.00  104
 41  \w     15.00 105.00   0.50    0.09    --  110.35 -91.00  90.00  180
 42  \w     37.00 138.00   0.50    0.09    --  110.35-163.00 111.00  202
 43  \w     21.00 109.00   0.50    0.09    --  110.35-116.00 -99.00  176
 44  \w     20.00 108.00   0.50    0.09    --  110.35-111.00 -30.00  176
 45  \w     20.00 108.00   0.50    0.09    --  110.35-111.00  30.00  176
 46  \w     20.00 108.00   0.50    0.09    --  110.35-111.00   0.00  176
 47  \w     12.00 109.00   0.50    0.09    --   55.18-116.00 -99.00  194
 48  \w     20.00 108.00   0.50    0.09    --  110.35-111.00-180.00  176
 49  \w   -101.00 -42.00   0.50    0.05    --    0.00-178.00-120.00  118
 50  \w    -97.00 -50.00   0.50    0.05    --    0.00-163.00 111.00   94
 51  \w   -175.00 -56.00   0.50    0.09    -- -102.00 -76.00 174.32  238
 52  \w   -175.00 -58.00   0.50    0.09    -- -102.00 -71.00  75.51  234
 53  \w   -155.00 -49.00   0.50    0.09    -- -102.00-163.00 111.00  212
 54  \w   -175.00 -82.00   0.50    0.09    -- -102.00-111.00 150.00  186
 55  \w   -153.00 -49.00   0.50    0.09    --  -55.18-163.00 111.00  208
 56  \w   -143.00 -81.00   0.50    0.09    --  -55.18-116.00 -99.00  124
 57  \w   -175.00 -80.00   0.50    0.09    -- -102.00 -91.00-150.00  190
 58  \w   -175.00 -80.00   0.50    0.09    -- -102.00-116.00 -99.00  190
 59  \w   -149.00 -87.00   0.50    0.09    --  -55.18 -99.00-180.00  124
 60  \w   -138.00 -15.00   0.50    0.09    --  -55.18 -57.00-150.00  246
 61  \w   -108.00  -7.00   0.50    0.09    --  -55.18 116.00 -10.00  202
 62  \w   -108.00 -19.00   0.50    0.09    -- -102.00 116.00 -10.00  178
 63  \w   -137.00 -33.00   0.50    0.09    -- -102.00 163.00 137.00  208
;
_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      -0.0065244000
_diffrn_orient_matrix_UB_12      0.0526323000
_diffrn_orient_matrix_UB_13      -0.1232659000
_diffrn_orient_matrix_UB_21      0.0129701000
_diffrn_orient_matrix_UB_22      -0.0756549000
_diffrn_orient_matrix_UB_23      -0.0779860000
_diffrn_orient_matrix_UB_31      -0.0927275000
_diffrn_orient_matrix_UB_32      -0.0144109000
_diffrn_orient_matrix_UB_33      -0.0405121000
_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  0.0659
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25098
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.456
_diffrn_reflns_theta_min         3.796
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.172
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.820
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2752
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0503
_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^)+(0.1060P)^2^+2.1186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2548
_reflns_number_total             2752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04311e2.cif
_cod_data_source_block           Zncdpp_shell
_cod_depositor_comments
'Adding full bibliography for 1576072--1576077.cif.'
_cod_database_code               1576075
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H18 O4 N10 Zn B2 F8'
_shelx_estimated_absorpt_t_max   0.765
_shelx_estimated_absorpt_t_min   0.635
_olex2_refinement_description
;
1. Restrained distances
 H2-O2
 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              27514
_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 5.463
_oxdiff_exptl_absorpt_empirical_full_min 0.456