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_7719415
_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 H34 Fe N4 O4, N O3, C H4 O'
_chemical_formula_sum            'C26 H38 Fe N5 O8'
_chemical_formula_weight         604.46
_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
_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                 103.876(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1749(2)
_cell_length_b                   15.7744(3)
_cell_length_c                   15.1118(3)
_cell_measurement_reflns_used    20053
_cell_measurement_temperature    114(2)
_cell_measurement_theta_max      28.8360
_cell_measurement_theta_min      1.8820
_cell_volume                     2817.55(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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      114(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.945
_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     26.00  52.00   1.00   25.86    --   10.37-110.00 108.00   26
  2  \w      2.00  28.00   1.00   25.86    --   -9.98 -99.00 -60.00   26
  3  \w    -15.00  48.00   1.00   25.86    --   10.37 -99.00-120.00   63
  4  \w    -37.00  43.00   1.00   25.86    --   10.37 -77.00  30.00   80
  5  \w    -12.00  44.00   1.00   25.86    --   10.37 -99.00 -30.00   56
  6  \w    -27.00  23.00   1.00   25.86    --   -9.98 -77.00-180.00   50
  7  \w     33.00  69.00   1.00   25.86    --   10.37  57.00-150.00   36
  8  \w    -12.00  83.00   1.00   25.86    --   10.37  37.00  90.00   95
  9  \w    -13.00  82.00   1.00   25.86    --   10.37  37.00   0.00   95
 10  \w    -10.00  74.00   1.00   25.86    --   10.37  37.00-180.00   84
 11  \w     50.00  76.00   1.00   25.86    --   10.37-140.00 -39.40   26
 12  \w     22.00  87.00   1.00   25.86    --   10.37-155.00-170.01   65
;
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            55060
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.102
_diffrn_reflns_theta_min         1.723
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (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            'metallic dark black'
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+2.5005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5791
_reflns_number_total             7156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01833a2.cif
_cod_data_source_block           2-8_mor1874
_cod_depositor_comments
'Adding full bibliography for 7719387--7719420.cif.'
_cod_database_code               7719415
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C26MnN5O8
_chemical_oxdiff_usercomment     'EP175_1_Eoin Pasquetti_Morgan'
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.861
_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:
 C16(H16A,H16B), C15(H15A,H15B), C14(H14A,H14B), C13(H13A,H13B), C12(H12A,
 H12B), C11(H11A,H11B), C10(H10A,H10B), C24(H24A,H24B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C21(H21), C9(H9), C5(H5), C4(H4), C3(H3A), C17(H17)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C8(H8A,H8B,H8C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              77970
_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 1.852
_oxdiff_exptl_absorpt_empirical_full_min 0.497