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_7719390
_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 Br4 Fe N4 O2, Cl O4'
_chemical_formula_sum            'C21 H22 Br4 Cl Fe N4 O6'
_chemical_formula_weight         837.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-17
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.06 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-06-04 deposited with the CCDC.	2025-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.135(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2501(2)
_cell_length_b                   17.1644(3)
_cell_length_c                   16.7990(3)
_cell_measurement_reflns_used    28696
_cell_measurement_temperature    105(7)
_cell_measurement_theta_max      29.4190
_cell_measurement_theta_min      2.3600
_cell_volume                     2625.60(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (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_environment      N~2~
_diffrn_ambient_temperature      105(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3196
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.937
_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     -7.00  55.00   0.50   10.00    --    9.99-109.00  77.00  124
  2  \w    -41.00  21.00   0.50   10.00    --   -9.60  77.00   0.00  124
  3  \w    -15.00  30.00   0.50   10.00    --   -9.60 -99.00 -90.00   90
  4  \w    -15.00  50.00   0.50   10.00    --    9.99 -99.00 -30.00  130
  5  \w    -12.00  83.00   0.50   10.00    --    9.99  37.00 150.00  190
  6  \w    -12.00  83.00   0.50   10.00    --    9.99  37.00  30.00  190
  7  \w    -42.00  41.00   0.50   10.00    --    9.99 -77.00-150.00  166
  8  \w    -41.00  21.00   0.50   10.00    --   -9.60  77.00 120.00  124
  9  \w    -60.00   5.00   0.50   10.00    --    9.99 -57.00  90.00  130
 10  \w    -12.00  83.00   0.50   10.00    --    9.99  37.00 -90.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0523643000
_diffrn_orient_matrix_UB_12      0.0237192000
_diffrn_orient_matrix_UB_13      -0.0146499000
_diffrn_orient_matrix_UB_21      0.0237031000
_diffrn_orient_matrix_UB_22      -0.0326398000
_diffrn_orient_matrix_UB_23      -0.0202078000
_diffrn_orient_matrix_UB_31      -0.0525413000
_diffrn_orient_matrix_UB_32      0.0089369000
_diffrn_orient_matrix_UB_33      -0.0348918000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57367
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.550
_diffrn_reflns_theta_min         1.710
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.809
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.354
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (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            'dark black'
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0211
_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^)+(0.0135P)^2^+2.5934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6316
_reflns_number_total             6892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01833a2.cif
_cod_data_source_block           1-8a_mor1755
_cod_depositor_comments
'Adding full bibliography for 7719387--7719420.cif.'
_cod_database_code               7719390
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C21 H22 N4 O6 Cl Fe Br4'
_chemical_oxdiff_usercomment     'Eoin, EP52_1'
_shelx_estimated_absorpt_t_max   0.420
_shelx_estimated_absorpt_t_min   0.286
_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:
 C9(H9A,H9B), C13(H13A,H13B), C8(H8A,H8B), C14(H14A,H14B), C10(H10A,H10B),
 C12(H12A,H12B), C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C15(H15), C19(H19), C7(H7), C17(H17)
;
_shelx_res_checksum              5493
_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 1.324
_oxdiff_exptl_absorpt_empirical_full_min 0.843