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_7135727
_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         'C32 H22 Ga N4 O2, C N Se, C H2 Cl2'
_chemical_formula_sum            'C34 H24 Cl2 Ga N5 O2 Se'
_chemical_formula_weight         754.189
_chemical_name_systematic        Ga(qsal)2NCSe
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2025-11-05
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-11-05 deposited with the CCDC.	2026-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                91.819(9)
_cell_angle_beta                 99.672(9)
_cell_angle_gamma                108.052(11)
_cell_formula_units_Z            2
_cell_length_a                   10.3788(12)
_cell_length_b                   11.6467(15)
_cell_length_c                   13.5263(13)
_cell_measurement_reflns_used    4713
_cell_measurement_temperature    130
_cell_measurement_theta_max      28.7350
_cell_measurement_theta_min      1.9390
_cell_volume                     1526.3(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.9928
_diffrn_measured_fraction_theta_max 0.9904
_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    -74.00  -7.00   0.50   29.39    --   20.00  54.00  30.00  134
  2  \w     12.00  38.00   0.50   29.39    --   20.00  54.00  30.00   52
  3  \w     73.00 110.00   0.50   29.39    --   20.00  54.00  30.00   74
  4  \w    -70.00 -15.00   0.50   29.39    --   20.00  54.00 150.00  110
  5  \w    -13.00  14.00   0.50   29.39    --   20.00  54.00 150.00   54
  6  \w     49.00 108.00   0.50   29.39    --   20.00  54.00 150.00  118
  7  \w    -71.00 -25.00   0.50   29.39    --   20.00  54.00 -30.00   92
  8  \w    -10.00  60.00   0.50   29.39    --   20.00  54.00 -30.00  140
  9  \w    -72.00 -32.00   0.50   29.39    --   20.00  54.00  90.00   80
 10  \w    -17.00  88.00   0.50   29.39    --   20.00  54.00  90.00  210
 11  \w    -63.00  93.00   0.50   29.39    --   20.00  54.00-180.00  312
 12  \w    -66.00  51.00   0.50   29.39    --   20.00  54.00-150.00  234
 13  \w    -73.00 -20.00   0.50   29.39    --   20.00  54.00 -60.00  106
 14  \w     30.00  59.00   0.50   29.39    --   20.00  54.00 -60.00   58
 15  \w     85.00 110.00   0.50   29.39    --   20.00  54.00 -60.00   50
 16  \w    -60.00 -35.00   0.50   29.39    --   20.00  54.00  60.00   50
 17  \w     68.00  93.00   0.50   29.39    --   20.00  54.00  60.00   50
 18  \w    -70.00  16.00   0.50   29.39    --   20.00  54.00-103.42  172
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0082264000
_diffrn_orient_matrix_UB_12      0.0040971000
_diffrn_orient_matrix_UB_13      0.0532561000
_diffrn_orient_matrix_UB_21      -0.0580704000
_diffrn_orient_matrix_UB_22      0.0204836000
_diffrn_orient_matrix_UB_23      -0.0031496000
_diffrn_orient_matrix_UB_31      -0.0437534000
_diffrn_orient_matrix_UB_32      -0.0608247000
_diffrn_orient_matrix_UB_33      -0.0025229000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1188
_diffrn_reflns_av_unetI/netI     0.1081
_diffrn_reflns_Laue_measured_fraction_full 0.9928
_diffrn_reflns_Laue_measured_fraction_max 0.9904
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21898
_diffrn_reflns_point_group_measured_fraction_full 0.9928
_diffrn_reflns_point_group_measured_fraction_max 0.9904
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50433
_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    1.641
_exptl_crystal_description       plate
_exptl_crystal_F_000             757.533
_refine_diff_density_max         1.9197
_refine_diff_density_min         -2.0352
_refine_diff_density_rms         0.2721
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             9.6936
_refine_ls_goodness_of_fit_ref   1.0464
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    47
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0464
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1897
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4077
_reflns_number_total             6175
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5cc06360d2.cif
_cod_data_source_block           Ga(qsal)2NCSeCH2Cl2
_cod_depositor_comments
'Adding full bibliography for 7135726--7135727.cif.'
_cod_database_code               7135727
_chemical_oxdiff_formula         'Ga C N O Se H Cl'
_chemical_oxdiff_usercomment     130K
_diffrn_oxdiff_ac4_digest_frames
;
01de14b7daed29c659da2e12622a71f5a102096b0e1
;
_diffrn_oxdiff_ac4_digest_hkl
;
01c0361deaff402de6e8610aea976d565294be
;
_reflns_odcompleteness_completeness 99.04
_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:
 C00D(H00D), C00E(H00E), C00F(H00F), C00J(H00J), C00K(H00K), C00M(H00M),
 C00R(H00R), C00T(H00T), C00U(H00U), C00V(H00V), C00X(H00X), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C011(H011), C012(H012), C013(H013), C014(H014),
 C015(H015), C016(H016), C017(H017), C018(H018)
;
_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 2.532
_oxdiff_exptl_absorpt_empirical_full_min 0.336