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_7719410
_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, N O3'
_chemical_formula_sum            'C21 H22 Br4 Fe N5 O5'
_chemical_formula_weight         799.92
_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   geom
_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                94.2540(10)
_cell_angle_beta                 99.193(2)
_cell_angle_gamma                91.315(3)
_cell_formula_units_Z            4
_cell_length_a                   10.2620(2)
_cell_length_b                   15.17560(10)
_cell_length_c                   17.0023(3)
_cell_measurement_reflns_used    29384
_cell_measurement_temperature    105(5)
_cell_measurement_theta_max      76.0850
_cell_measurement_theta_min      2.6150
_cell_volume                     2604.96(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.92a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.92a (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      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 0.999
_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   -113.00 -14.00   1.00    7.03    --  -42.08 -55.00 -59.00   99
  2  \w    -53.00 -25.00   1.00    7.03    --  -42.08  55.00  84.00   28
  3  \w     -4.00  21.00   1.00    7.03    --   42.08 -55.00 -59.00   25
  4  \w     16.00 114.00   1.00    7.03    --   42.08  55.00  84.00   98
  5  \w     67.00  94.00   1.00    8.12    --  112.00 -55.00 -59.00   27
  6  \w    111.00 137.00   1.00    8.12    --  112.00  55.00  84.00   26
  7  \w     30.00  94.00   1.00    7.03    --   42.08-125.00-180.00   64
  8  \w     35.00  95.00   1.00    7.03    --   42.08-125.00 -90.00   60
  9  \w    -32.00  66.00   1.00    7.03    --   42.08 -37.00 150.00   98
 10  \w     58.00 109.00   1.00    8.12    --  112.00-111.00 -60.00   51
 11  \w    107.00 178.00   1.00    8.12    --  112.00  77.00  30.00   71
 12  \w     49.00  74.00   1.00    8.12    --  112.00 -94.00 -30.00   25
 13  \w    135.00 164.00   1.00    8.12    --  112.00  77.00 -30.00   29
 14  \w     40.00 109.00   1.00    8.12    --  112.00-111.00-120.00   69
 15  \w    104.00 144.00   1.00    8.12    --  112.00 111.00-120.00   40
 16  \w     39.00 109.00   1.00    8.12    --  112.00-111.00  60.00   70
 17  \w     89.00 175.00   1.00    8.12    --  112.00  45.00 150.00   86
 18  \w     80.00 109.00   1.00    8.12    --  112.00-111.00 150.00   29
 19  \w     44.00  71.00   1.00    8.12    --  112.00 -61.00 150.00   27
 20  \w     94.00 120.00   1.00    8.12    --  112.00 -61.00 150.00   26
 21  \w     85.00 177.00   1.00    8.12    --  112.00  61.00  60.00   92
 22  \w     75.00 130.00   1.00    8.12    --  112.00 178.00  30.00   55
 23  \w     68.00 108.00   1.00    8.12    --  112.00-111.00  90.00   40
 24  \w     86.00 164.00   1.00    8.12    --  112.00  45.00-180.00   78
 25  \w     40.00 109.00   1.00    8.12    --  112.00-111.00  30.00   69
 26  \w     52.00  95.00   1.00    8.12    --  112.00-111.00-150.00   43
 27  \w     84.00 109.00   1.00    8.12    --  112.00  61.00 120.00   25
 28  \w    117.00 177.00   1.00    8.12    --  112.00  61.00 120.00   60
 29  \w     39.00  88.00   1.00    8.12    --  112.00-111.00 120.00   49
 30  \w     61.00  87.00   1.00    8.12    --  112.00-111.00 -90.00   26
 31  \w    136.00 178.00   1.00    8.12    --  112.00  77.00   0.00   42
 32  \w     43.00 109.00   1.00    8.12    --  112.00-111.00   0.00   66
 33  \w     38.00  64.00   1.00    8.12    --  112.00 -77.00 -90.00   26
 34  \w     85.00 114.00   1.00    8.12    --  112.00 -77.00 -90.00   29
 35  \w    108.00 141.00   1.00    8.12    --  112.00 111.00-180.00   33
 36  \w     36.00 107.00   1.00    8.12    --  112.00 -94.00 150.00   71
 37  \w    -30.00  -1.00   1.00    7.03    --   42.08 -55.00 -59.00   29
 38  \w    -49.00 -16.00   1.00    7.03    --  -42.08 -57.00  30.00   33
 39  \w   -107.00 -21.00   1.00    7.03    --  -42.08 -57.00  90.00   86
 40  \w    -49.00  -7.00   1.00    7.03    --  -42.08 125.00  30.00   42
 41  \w   -117.00 -18.00   1.00    7.03    --  -42.08 -37.00-150.00   99
 42  \w    -87.00 -52.00   1.00    7.03    --  -42.08 -57.00  30.00   35
 43  \w    -77.00 -14.00   1.00    7.03    --  -42.08 -57.00 150.00   63
 44  \w      7.00  32.00   1.00    7.03    --   42.08  84.00  71.78   25
 45  \w      9.00  34.00   1.00    7.03    --   42.08  78.00 162.01   25
 46  \w     17.00  59.00   1.00    7.03    --   42.08 -55.00 -59.00   42
 47  \w      8.00  34.00   1.00    7.03    --   42.08  83.00  -8.39   26
 48  \w      7.00  33.00   1.00    7.03    --   42.08  84.00-138.52   26
 49  \w      9.00  39.00   1.00    7.03    --   42.08  80.00 -58.19   30
 50  \w    137.00 167.00   1.00    8.12    --  112.00  61.00 -90.00   30
 51  \w     86.00 127.00   1.00    8.12    --  112.00  45.00   0.00   41
 52  \w     85.00 114.00   1.00    8.12    --  112.00  61.00 -90.00   29
 53  \w     86.00 171.00   1.00    8.12    --  112.00  51.00 -35.05   85
 54  \w     83.00 109.00   1.00    8.12    --  112.00  60.00  74.07   26
 55  \w     83.00 110.00   1.00    8.12    --  112.00  61.00 -30.00   27
 56  \w     83.00 149.00   1.00    8.12    --  112.00  61.00   0.00   66
 57  \w     83.00 109.00   1.00    8.12    --  112.00  61.00 150.00   26
 58  \w    108.00 134.00   1.00    8.12    --  112.00  70.00  95.96   26
 59  \w     83.00 161.00   1.00    8.12    --  112.00  61.00-120.00   78
 60  \w     81.00 107.00   1.00    8.12    --  112.00  70.00  95.96   26
 61  \w     81.00 136.00   1.00    8.12    --  112.00  69.00-110.80   55
 62  \w     84.00 110.00   1.00    8.12    --  112.00  56.00  49.66   26
 63  \w     83.00 109.00   1.00    8.12    --  112.00  61.00-180.00   26
 64  \w     83.00 110.00   1.00    8.12    --  112.00  61.00  90.00   27
 65  \w     86.00 139.00   1.00    8.12    --  112.00  45.00-120.00   53
 66  \w    140.00 176.00   1.00    8.12    --  112.00  61.00-150.00   36
 67  \w     84.00 111.00   1.00    8.12    --  112.00  54.00 179.05   27
 68  \w     82.00 108.00   1.00    8.12    --  112.00  64.00  77.82   26
 69  \w     83.00 133.00   1.00    8.12    --  112.00  61.00  30.00   50
 70  \w    112.00 138.00   1.00    8.12    --  112.00 -45.00  30.00   26
 71  \w     44.00  97.00   1.00    8.12    --  112.00 -45.00  30.00   53
 72  \w    152.00 178.00   1.00    8.12    --  112.00  67.00-175.45   26
 73  \w    139.00 165.00   1.00    8.12    --  112.00  64.00  77.82   26
 74  \w    135.00 167.00   1.00    8.12    --  112.00  45.00 -60.00   32
 75  \w     87.00 125.00   1.00    8.12    --  112.00  45.00 -60.00   38
 76  \w     85.00 111.00   1.00    8.12    --  112.00  51.00 -54.69   26
 77  \w     82.00 123.00   1.00    8.12    --  112.00  67.00-175.45   41
 78  \w     84.00 123.00   1.00    8.12    --  112.00  57.00  25.55   39
 79  \w    151.00 177.00   1.00    8.12    --  112.00  57.00  25.55   26
 80  \w     83.00 109.00   1.00    8.12    --  112.00  61.00 -60.00   26
 81  \w     83.00 125.00   1.00    8.12    --  112.00  61.00-150.00   42
;
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53824
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.064
_diffrn_reflns_theta_min         2.641
_exptl_absorpt_coefficient_mu    12.206
_exptl_absorpt_correction_T_max  0.673
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
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    2.040
_exptl_crystal_description       block
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0099P)^2^+11.9937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9435
_reflns_number_total             9895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01833a2.cif
_cod_data_source_block           2-5_mor1868
_cod_depositor_comments
'Adding full bibliography for 7719387--7719420.cif.'
_cod_database_code               7719410
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         Br8C42Fe2N10O10
_chemical_oxdiff_usercomment     EP172-1_EoinPasquetti_Morgangroup
_shelx_estimated_absorpt_t_max   0.482
_shelx_estimated_absorpt_t_min   0.194
_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:
 N3(H3A), N2(H2), N7(H7A), N6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,
 H14B), C8(H8A,H8B), C9(H9A,H9B), C32(H32A,H32B), C31(H31A,H31B), C30(H30A,
 H30B), C29(H29A,H29B), C35(H35A,H35B), C34(H34A,H34B), C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C19(H19), C17(H17), C15(H15), C24(H24), C26(H26),
 C28(H28), C40(H40), C38(H38), C36(H36)
;
_shelx_res_checksum              4744
_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 1.854
_oxdiff_exptl_absorpt_empirical_full_min 0.549