Symmetric and asymmetric ligands for Fe<sup>III</sup> spin crossover - the influence of the <i>C</i><sub>2</sub> axis.
Kelly, Conor T.; Cuza, Emmelyne; Pasquetti, Eoin; Quinn, Niall; Griffin, Michael; Nockemann, Peter; Müller-Bunz, Helge; Bruno-Colmenarez, Julia; Felton, Solveig; Lada, Zoi G.; Morgan, Grace G.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14522–14532; doi:10.1039/d5dt01833a

data_7719411
_publ_section_title
;
 Symmetric and asymmetric ligands for Fe<sup>III</sup> spin crossover -
 the influence of the <i>C</i><sub>2</sub> axis.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14522
_journal_page_last               14532
_journal_paper_doi               10.1039/d5dt01833a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C21 H24 Cl2 Fe N4 O2, Cl O4'
_chemical_formula_sum            'C21 H24 Cl3 Fe N4 O6'
_chemical_formula_weight         590.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-23
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-06-26 deposited with the CCDC.	2025-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.3660(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.27495(6)
_cell_length_b                   20.54207(13)
_cell_length_c                   14.38040(9)
_cell_measurement_reflns_used    21921
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.6820
_cell_measurement_theta_min      4.2830
_cell_volume                     2443.75(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.143a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3218
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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   -115.00 -63.00   1.00    1.00    --  -42.23-147.00-166.00   52
  2  \w   -102.00 -16.00   1.00    1.00    --  -42.23 147.00-116.00   86
  3  \w    -87.00  -5.00   1.00    1.00    --  -42.23 124.00  77.00   82
  4  \w     26.00  96.00   1.00    1.00    --   42.23-124.00  -1.00   70
  5  \w     38.00 112.00   1.00    1.00    --   42.23-147.00-166.00   74
  6  \w     39.00 128.00   1.00    1.00    --  112.00-147.00-166.00   89
  7  \w     41.00 111.00   1.00    1.00    --  112.00-124.00  -1.00   70
  8  \w     98.00 178.00   1.00    1.00    --  112.00 124.00  77.00   80
  9  \w     85.00 168.00   1.00    1.00    --  112.00 147.00-116.00   83
 10  \w    -67.00  32.00   1.00    1.00    --  -42.23  37.00   0.00   99
 11  \w    -87.00  -6.00   1.00    1.00    --  -42.23 125.00 -60.00   81
 12  \w   -117.00 -18.00   1.00    1.00    --  -42.23 -37.00 150.00   99
 13  \w      8.00  42.00   1.00    1.00    --   42.23  82.00-109.18   34
 14  \w     18.00 117.00   1.00    1.00    --   42.23  37.00  90.00   99
 15  \w      9.00  42.00   1.00    1.00    --   42.23  79.00  42.30   33
 16  \w     39.00 109.00   1.00    1.00    --  112.00-111.00  60.00   70
 17  \w    104.00 178.00   1.00    1.00    --  112.00 111.00-120.00   74
 18  \w    103.00 178.00   1.00    1.00    --  112.00  77.00-150.00   75
 19  \w     39.00 109.00   1.00    1.00    --  112.00-111.00-150.00   70
 20  \w     39.00 109.00   1.00    1.00    --  112.00-111.00 120.00   70
 21  \w     39.00 109.00   1.00    1.00    --  112.00-111.00 -60.00   70
 22  \w     39.00 138.00   1.00    1.00    --  112.00 -45.00 -90.00   99
 23  \w     29.00 107.00   1.00    1.00    --  112.00 -94.00 -30.00   78
 24  \w     39.00 109.00   1.00    1.00    --  112.00-111.00-180.00   70
 25  \w     36.00 140.00   1.00    1.00    --  112.00 -30.00 120.00  104
 26  \w    104.00 178.00   1.00    1.00    --  112.00 111.00  60.00   74
 27  \w     40.00 141.00   1.00    1.00    --  112.00 -61.00 -30.00  101
 28  \w     39.00 109.00   1.00    1.00    --  112.00-111.00  90.00   70
 29  \w     39.00 109.00   1.00    1.00    --  112.00-111.00-120.00   70
 30  \w     86.00 178.00   1.00    1.00    --  112.00  45.00 -60.00   92
 31  \w     40.00 141.00   1.00    1.00    --  112.00 -61.00 150.00  101
 32  \w    103.00 178.00   1.00    1.00    --  112.00  77.00 150.00   75
 33  \w     83.00 178.00   1.00    1.00    --  112.00  61.00-120.00   95
 34  \w    103.00 178.00   1.00    1.00    --  112.00  77.00  30.00   75
 35  \w    103.00 178.00   1.00    1.00    --  112.00  77.00 -30.00   75
 36  \w   -114.00 -14.00   1.00    1.00    --  -42.23 -57.00 -90.00  100
 37  \w   -114.00 -14.00   1.00    1.00    --  -42.23 -57.00   0.00  100
 38  \w    -67.00  32.00   1.00    1.00    --  -42.23  37.00-120.00   99
 39  \w   -114.00 -14.00   1.00    1.00    --  -42.23 -57.00  90.00  100
 40  \w    -32.00  67.00   1.00    1.00    --   42.23 -37.00   0.00   99
 41  \w      9.00  42.00   1.00    1.00    --   42.23  80.00 -28.43   33
 42  \w      9.00  42.00   1.00    1.00    --   42.23  80.00 -58.77   33
 43  \w      8.00  42.00   1.00    1.00    --   42.23  82.00 167.84   34
 44  \w      8.00  34.00   1.00    1.00    --   42.23  83.00 138.88   26
 45  \w     86.00 176.00   1.00    1.00    --  112.00  45.00  60.00   90
 46  \w     83.00 178.00   1.00    1.00    --  112.00  61.00-180.00   95
 47  \w     83.00 178.00   1.00    1.00    --  112.00  61.00   0.00   95
 48  \w     84.00 178.00   1.00    1.00    --  112.00  30.00 120.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27823
_diffrn_reflns_point_group_measured_fraction_full 0.886
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.827
_diffrn_reflns_theta_min         3.753
_exptl_absorpt_coefficient_mu    8.371
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.143a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 1836 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4493
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0223
_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^)+(0.0368P)^2^+1.3558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0579
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_full    0.772
_reflns_Friedel_fraction_max     0.741
_reflns_number_gt                4455
_reflns_number_total             4493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01833a2.cif
_cod_data_source_block           2-2a_mor1936
_cod_depositor_comments
'Adding full bibliography for 7719387--7719420.cif.'
_cod_database_code               7719411
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         CNOClFe
_chemical_oxdiff_usercomment     'Conor, CK-557-1'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C8(H8A,H8B), C9(H9A,H9B), C13(H13A,H13B), C11(H11A,H11B),
 C12(H12A,H12B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C7(H7), C2(H2A), C19(H19), C20(H20), C15(H15), C3(H3A), C5(H5)
;
_shelx_res_checksum              84423
_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 2.102
_oxdiff_exptl_absorpt_empirical_full_min 0.684