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_7719416
_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         'C25 H32 Fe N6 O8, Cl O4'
_chemical_formula_sum            'C25 H32 Cl Fe N6 O12'
_chemical_formula_weight         699.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-03
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.06 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-06-26 deposited with the CCDC.	2025-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.3980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.48950(10)
_cell_length_b                   16.2317(2)
_cell_length_c                   17.00970(10)
_cell_measurement_reflns_used    25728
_cell_measurement_temperature    110(5)
_cell_measurement_theta_max      76.0550
_cell_measurement_theta_min      3.7330
_cell_volume                     2857.24(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110(5)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -71.00  31.00   1.00   10.11    --  -42.20  60.00 -56.00  102
  2  \w   -114.00 -13.00   1.00   10.11    --  -42.20 -60.00 163.00  101
  3  \w     40.00 141.00   1.00   13.41    --  112.00 -60.00 163.00  101
  4  \w     40.00 141.00   1.00   13.41    --  112.00 -60.00 163.00  101
  5  \w     83.00 178.00   1.00   13.41    --  112.00  60.00 -56.00   95
  6  \w     83.00 178.00   1.00   13.41    --  112.00  60.00 -56.00   95
  7  \w    -87.00  -6.00   1.00   10.11    --  -42.20 125.00  60.00   81
  8  \w    -30.00  71.00   1.00   10.11    --   42.20 -60.00 163.00  101
  9  \w     13.00 114.00   1.00   10.11    --   42.20  60.00 -56.00  101
 10  \w     27.00  96.00   1.00   10.11    --   42.20-125.00  90.00   69
 11  \w     27.00  96.00   1.00   10.11    --   42.20-125.00 -30.00   69
 12  \w     86.00 178.00   1.00   13.41    --  112.00  45.00-120.00   92
 13  \w     86.00 178.00   1.00   13.41    --  112.00  45.00-120.00   92
 14  \w     39.00 109.00   1.00   13.41    --  112.00-111.00  30.00   70
 15  \w     83.00 178.00   1.00   13.41    --  112.00  61.00 -30.00   95
 16  \w     83.00 178.00   1.00   13.41    --  112.00  61.00 -30.00   95
 17  \w     39.00 109.00   1.00   13.41    --  112.00-111.00 150.00   70
 18  \w     61.00 146.00   1.00   13.41    --  112.00 178.00   0.00   85
 19  \w    104.00 178.00   1.00   13.41    --  112.00 111.00-180.00   74
 20  \w     29.00 107.00   1.00   13.41    --  112.00 -94.00 150.00   78
 21  \w     86.00 178.00   1.00   13.41    --  112.00  45.00-150.00   92
 22  \w     39.00 109.00   1.00   13.41    --  112.00-111.00  60.00   70
 23  \w     39.00 109.00   1.00   13.41    --  112.00-111.00   0.00   70
 24  \w     86.00 178.00   1.00   13.41    --  112.00  45.00-150.00   92
 25  \w     83.00 178.00   1.00   13.41    --  112.00  61.00  30.00   95
 26  \w     83.00 178.00   1.00   13.41    --  112.00  61.00  30.00   95
 27  \w     39.00 109.00   1.00   13.41    --  112.00-111.00 -30.00   70
 28  \w     39.00 109.00   1.00   13.41    --  112.00-111.00 150.00   70
 29  \w   -114.00 -14.00   1.00   10.11    --  -42.20 -57.00  90.00  100
 30  \w   -114.00 -14.00   1.00   10.11    --  -42.20 -57.00 -90.00  100
 31  \w   -114.00 -14.00   1.00   10.11    --  -42.20 -57.00  60.00  100
 32  \w   -114.00 -14.00   1.00   10.11    --  -42.20 -57.00  30.00  100
 33  \w   -114.00 -14.00   1.00   10.11    --  -42.20 -57.00 -30.00  100
 34  \w   -114.00 -14.00   1.00   10.11    --  -42.20 -57.00-150.00  100
 35  \w    -32.00  67.00   1.00   10.11    --   42.20 -37.00   0.00   99
 36  \w     86.00 153.00   1.00   13.41    --  112.00  45.00-180.00   67
 37  \w     83.00 178.00   1.00   13.41    --  112.00  61.00   0.00   95
 38  \w     83.00 175.00   1.00   13.41    --  112.00  61.00 -90.00   92
;
_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  0.0765
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            56313
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.229
_diffrn_reflns_theta_min         3.789
_exptl_absorpt_coefficient_mu    5.767
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       plate
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0610P)^2^+1.6006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5393
_reflns_number_total             5958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01833a2.cif
_cod_data_source_block           2-9_mor1881
_cod_depositor_comments
'Adding full bibliography for 7719387--7719420.cif.'
_cod_database_code               7719416
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C25H32ClFeN6O12
_chemical_oxdiff_usercomment     EP139-1_Eoin_Morgan
_shelx_estimated_absorpt_t_max   0.724
_shelx_estimated_absorpt_t_min   0.245
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C24(H24A,H24B), C13(H13A,H13B), C10(H10A,H10B), C11(H11A,H11B),
 C14(H14A,H14B), C15(H15A,H15B), C12(H12A,H12B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C21(H21), C9(H9), C19(H19), C17(H17)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              15533
_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 3.193
_oxdiff_exptl_absorpt_empirical_full_min 0.590