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_7719417
_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 H22 Br2 Cl2 Fe N4 O2, N O3'
_chemical_formula_sum            'C21 H22 Br2 Cl2 Fe N5 O5'
_chemical_formula_weight         711.00
_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   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                94.852(3)
_cell_angle_beta                 99.286(2)
_cell_angle_gamma                92.082(4)
_cell_formula_units_Z            4
_cell_length_a                   10.1862(5)
_cell_length_b                   15.0379(6)
_cell_length_c                   16.9381(5)
_cell_measurement_reflns_used    17049
_cell_measurement_temperature    105(5)
_cell_measurement_theta_max      27.9720
_cell_measurement_theta_min      2.1760
_cell_volume                     2548.09(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.75a (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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      105(5)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.899
_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    -20.00  41.00   1.00   32.50    --   -9.98  44.00  12.00   61
  2  \w    -83.00  12.00   1.00   32.50    --   -9.98 -44.00-139.00   95
  3  \w    -15.00  10.00   1.00   32.50    --   -9.98 -99.00 150.00   25
  4  \w    -32.00  12.00   1.00   32.50    --   -9.98  77.00  60.00   44
  5  \w    -33.00  20.00   1.00   32.50    --   -9.98  77.00-150.00   53
  6  \w     -8.00  26.00   1.00   32.50    --   -9.98 -99.00 -30.00   34
  7  \w    -15.00  49.00   1.00   32.50    --   10.37 -99.00 150.00   64
  8  \w     19.00  83.00   1.00   32.50    --   10.37  44.00  12.00   64
  9  \w    -81.00  14.00   1.00   32.50    --   -9.98 -37.00  30.00   95
 10  \w    -84.00   9.00   1.00   32.50    --   -9.98 -37.00 120.00   93
 11  \w    -77.00 -48.00   1.00   32.50    --   -9.98 142.00 -39.93   29
 12  \w     14.00  76.00   1.00   32.50    --   10.37-140.00  -0.25   62
 13  \w    -29.00  48.00   1.00   32.50    --   10.37 -90.00-152.93   77
;
_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  0.0627
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57591
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_min         1.744
_exptl_absorpt_coefficient_mu    3.981
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.75a (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    1.853
_exptl_crystal_description       block
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         12353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0576
_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^)+10.3316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9451
_reflns_number_total             12353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01833a2.cif
_cod_data_source_block           2-6b_mor1861
_cod_depositor_comments
'Adding full bibliography for 7719387--7719420.cif.'
_cod_original_cell_volume        2548.07(17)
_cod_database_code               7719417
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         FeBrCNO
_chemical_oxdiff_usercomment     EoinPasquetti
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.622
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C6) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2)
Uanis(Cl1A) = Uanis(Cl1B)
3. Rigid body (RIGU) restrains
 Cl1A, Cl1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl1B)=1-FVAR(1)
 Sof(Cl1A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C35(H35A,H35B), C34(H34A,H34B), C33(H33A,H33B),
  C32(H32A,H32B), C31(H31A,H31B), C30(H30A,H30B), C29(H29A,H29B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C15(H15), C19(H19), C17(H17), C38(H38), C40(H40),
 C36(H36), C28(H28), C26(H26), C24(H24)
;
_shelx_res_checksum              83218
_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 1.650
_oxdiff_exptl_absorpt_empirical_full_min 0.551