Quantitative Evaluation of Intermolecular Interactions in Fe(III) Spin Crossover Systems via Metal Dilution
Miyake, Kanta; Zenno, Hikaru; Sekine, Yoshihiro; Kosaka, Wataru; Miyasaka, Hitoshi; Hayami, Shinya; Chemical Communications  (2026) –; doi:10.1039/D5CC06360D

data_7135726
_publ_section_title
;
 Quantitative evaluation of intermolecular interactions in Fe(III) spin
 crossover systems <i>via</i> metal dilution.
;
_journal_issue                   33
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8435
_journal_page_last               8438
_journal_paper_doi               10.1039/d5cc06360d
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C N Se, C32 H22 Al N4 O2, C H2 Cl2'
_chemical_formula_sum            'C34 H24 Al Cl2 N5 O2 Se'
_chemical_formula_weight         711.42
_chemical_name_systematic        Al(qsal)2NCSeCH2Cl2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-11-05 deposited with the CCDC.	2026-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                92.051(3)
_cell_angle_beta                 98.084(3)
_cell_angle_gamma                106.815(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0023(4)
_cell_length_b                   11.3429(5)
_cell_length_c                   13.8445(5)
_cell_measurement_reflns_used    6812
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      30.2100
_cell_measurement_theta_min      2.3050
_cell_volume                     1483.78(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_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    -73.00 -16.00   0.50    3.50    --   20.00  54.00-180.00  114
  2  \w    -12.00  47.00   0.50    3.50    --   20.00  54.00-180.00  118
  3  \w     59.00 110.00   0.50    3.50    --   20.00  54.00-180.00  102
  4  \w      7.00  50.50   0.50    3.50    --   20.00  54.00 -60.00   87
  5  \w     85.00 110.00   0.50    3.50    --   20.00  54.00 -60.00   50
  6  \w    -72.00 -15.00   0.50    3.50    --   20.00  54.00-121.00  114
  7  \w    -10.00  36.00   0.50    3.50    --   20.00  54.00-121.00   92
  8  \w    -72.00  26.00   0.50    3.50    --   20.00  54.00 120.00  196
  9  \w     37.00  66.00   0.50    3.50    --   20.00  54.00 120.00   58
 10  \w     69.00 105.50   0.50    3.50    --   20.00  54.00 120.00   73
 11  \w    -73.00  91.50   0.50    3.50    --   20.00  54.00 -30.00  329
 12  \w    -74.00  21.50   0.50    3.50    --   20.00  54.00  90.00  191
 13  \w     83.00 108.00   0.50    3.50    --   20.00  54.00  90.00   50
 14  \w    -61.00 -36.00   0.50    3.50    --   20.00  54.00-150.00   50
 15  \w     -1.00  24.00   0.50    3.50    --   20.00  54.00-150.00   50
 16  \w    -72.00 -45.00   0.50    3.50    --   20.00  54.00  30.00   54
 17  \w     71.00  97.00   0.50    3.50    --   20.00  54.00  30.00   52
 18  \w    -61.00  28.50   0.50    3.50    --   20.00  54.00 -90.00  179
 19  \w    -55.00 -30.00   0.50    3.50    --   20.00  54.00-120.00   50
 20  \w    -64.00   9.00   0.50    3.50    --   20.00  54.00  60.00  146
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0267766000
_diffrn_orient_matrix_UB_12      -0.0514602000
_diffrn_orient_matrix_UB_13      0.0028061000
_diffrn_orient_matrix_UB_21      -0.0096386000
_diffrn_orient_matrix_UB_22      -0.0076399000
_diffrn_orient_matrix_UB_23      -0.0518379000
_diffrn_orient_matrix_UB_31      0.0694140000
_diffrn_orient_matrix_UB_32      0.0398605000
_diffrn_orient_matrix_UB_33      0.0005753000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23056
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.305
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0447P)^2^+1.5816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4819
_reflns_number_total             6005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06360d2.cif
_cod_data_source_block           230107_al(qsal)2ncse
_cod_depositor_comments
'Adding full bibliography for 7135726--7135727.cif.'
_cod_database_code               7135726
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Al N C Se O H Cl'
_chemical_oxdiff_usercomment     '100 K'
_diffrn_oxdiff_ac4_digest_frames
;
01499970dcdffde529aa66b0b7d99e8a8f0215501be
;
_diffrn_oxdiff_ac4_digest_hkl
;
0157034827d547c34cef006b47ff8dd7a06be5
;
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C019(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00F(H00F), C00H(H00H), C00I(H00I), C00M(H00M), C00N(H00N),
 C00P(H00P), C00R(H00R), C00U(H00U), C00W(H00W), C00X(H00X), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C011(H011), C012(H012), C013(H013), C014(H014),
 C015(H015), C016(H016), C017(H017), C018(H018)
;
_shelx_res_checksum              96742
_shelx_hkl_checksum              79790
_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 1.690
_oxdiff_exptl_absorpt_empirical_full_min 0.652