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_7719405
_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 Fe I4 N4 O2, N O3'
_chemical_formula_sum            'C21 H22 Fe I4 N5 O5'
_chemical_formula_weight         987.88
_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             2025-06-04
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-04 deposited with the CCDC.	2025-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.6990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.16520(10)
_cell_length_b                   14.32910(10)
_cell_length_c                   23.63980(10)
_cell_measurement_reflns_used    161128
_cell_measurement_temperature    105.3(8)
_cell_measurement_theta_max      29.3290
_cell_measurement_theta_min      1.6480
_cell_volume                     5539.27(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_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      105.3(8)
_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 0.963
_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    -43.00  14.00   0.30    4.00    --  -10.68  74.00 143.00  190
  2  \w    -36.00  21.00   0.30    4.00    --  -10.68 -74.00  15.00  190
  3  \w    -36.00  42.00   0.30    4.00    --   10.99 -74.00  15.00  260
  4  \w    -42.00  21.00   0.30    4.00    --  -10.68 -77.00-180.00  210
  5  \w    -86.00 -43.10   0.30    4.00    --  -10.68 153.00-175.78  143
  6  \w    -69.00 -30.00   0.30    4.00    --  -10.68 128.00  15.59  130
  7  \w    -62.00  37.90   0.30    4.00    --   10.99 -57.00 -90.00  333
  8  \w    -62.00  40.00   0.30    4.00    --   10.99 -64.00 113.19  340
  9  \w     16.00  79.00   0.30    4.00    --   10.99-145.00-122.77  210
 10  \w    -13.00  83.90   0.30    4.00    --   10.99  37.00  90.00  323
 11  \w    -13.00  83.90   0.30    4.00    --   10.99  37.00   0.00  323
 12  \w    -17.00  82.90   0.30    4.00    --   10.99  57.00-180.00  333
 13  \w    -15.00  30.00   0.30    4.00    --  -10.68 -99.00 150.00  150
 14  \w    -84.00 -42.00   0.30    4.00    --  -10.68 151.00  87.97  140
 15  \w    -69.00 -30.00   0.30    4.00    --  -10.68 128.00 111.91  130
 16  \w    -88.00 -45.10   0.30    4.00    --  -10.68 156.00 123.71  143
 17  \w    -82.00 -39.10   0.30    4.00    --  -10.68 148.00 -36.54  143
 18  \w    -68.00 -29.00   0.30    4.00    --  -10.68 127.00  85.00  130
 19  \w    -86.00 -43.10   0.30    4.00    --  -10.68 153.00-117.56  143
 20  \w    -69.00 -30.00   0.30    4.00    --  -10.68 128.00 -66.70  130
 21  \w      7.00  67.00   0.30    4.00    --   10.99-126.00  12.81  200
 22  \w    -63.00  33.90   0.30    4.00    --   10.99 -37.00   0.00  323
 23  \w    -24.00  48.00   0.30    4.00    --   10.99 -91.00  60.55  240
 24  \w    -88.00 -45.10   0.30    4.00    --  -10.68 156.00 159.99  143
 25  \w    -15.00  30.00   0.30    4.00    --  -10.68 -99.00-150.00  150
 26  \w    -15.00  13.20   0.30    4.00    --  -10.68 -99.00 -60.00   94
 27  \w    -82.00 -39.10   0.30    4.00    --  -10.68 148.00  29.87  143
;
_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      -0.0388839000
_diffrn_orient_matrix_UB_12      -0.0007904000
_diffrn_orient_matrix_UB_13      0.0047165000
_diffrn_orient_matrix_UB_21      0.0153406000
_diffrn_orient_matrix_UB_22      0.0286186000
_diffrn_orient_matrix_UB_23      0.0254502000
_diffrn_orient_matrix_UB_31      -0.0116111000
_diffrn_orient_matrix_UB_32      0.0403771000
_diffrn_orient_matrix_UB_33      -0.0179369000
_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  0.0270
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            254145
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.483
_diffrn_reflns_theta_min         1.684
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.044
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.451
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
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 brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.369
_exptl_crystal_description       block
_exptl_crystal_F_000             3688
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         14828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0156
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0093P)^2^+6.3615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0329
_refine_ls_wR_factor_ref         0.0339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13793
_reflns_number_total             14828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01833a2.cif
_cod_data_source_block           1-9b_mor1744
_cod_depositor_comments
'Adding full bibliography for 7719387--7719420.cif.'
_cod_database_code               7719405
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C42 H44 N10 O10 Fe2 I8'
_chemical_oxdiff_usercomment     'Eoin, EP34'
_shelx_estimated_absorpt_t_max   0.518
_shelx_estimated_absorpt_t_min   0.365
_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:
 C29(H29A,H29B), C35(H35A,H35B), C14(H14A,H14B), C8(H8A,H8B), C34(H34A,H34B),
 C13(H13A,H13B), C30(H30A,H30B), C33(H33A,H33B), C11(H11A,H11B), C9(H9A,H9B),
 C12(H12A,H12B), C32(H32A,H32B), C10(H10A,H10B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C36(H36), C26(H26), C28(H28), C7(H7A), C24(H24), C40(H40),
  C5(H5), C19(H19), C3(H3A), C38(H38)
;
_shelx_res_checksum              23117
_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 1.155
_oxdiff_exptl_absorpt_empirical_full_min 0.861