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_7719395
_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 H24 Fe I2 N4 O2, Cl O4'
_chemical_formula_sum            'C21 H24 Cl Fe I2 N4 O6'
_chemical_formula_weight         773.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-04 deposited with the CCDC.	2025-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.856(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7520(4)
_cell_length_b                   20.1215(6)
_cell_length_c                   9.8930(3)
_cell_measurement_reflns_used    9289
_cell_measurement_temperature    100.00(14)
_cell_measurement_theta_max      29.1210
_cell_measurement_theta_min      2.0290
_cell_volume                     2493.01(13)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(14)
_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 0.920
_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 44.00 69.00 0.50 12.00 -- 10.07 174.00 -94.00 50
 2 \w 40.00 65.00 0.50 12.00 -- 10.07-174.00-104.00 50
 3 \w 5.00 57.00 0.50 12.00 -- 10.07-113.00 34.00 104
 4 \w -6.00 21.00 0.50 12.00 -- -9.60 -99.00-150.00 54
 5 \w 2.00 62.00 0.50 12.00 -- -9.60 37.00-180.00 120
 6 \w -40.00 -4.00 0.50 12.00 -- -9.60 77.00-120.00 72
 7 \w -83.00 13.00 0.50 12.00 -- -9.60 -37.00 60.00 192
 8 \w -42.00 19.00 0.50 12.00 -- -9.60 -77.00-150.00 122
 9 \w -32.00 -5.00 0.50 12.00 -- -9.60 37.00-180.00 54
 10 \w -63.00 -8.00 0.50 12.00 -- 10.07 -37.00 0.00 110
 11 \w 10.00 47.00 0.50 12.00 -- 10.07 -99.00 -90.00 74
 12 \w -1.00 31.00 0.50 12.00 -- 10.07 -37.00 0.00 64
;
_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      -0.0509621000
_diffrn_orient_matrix_UB_12      0.0055788000
_diffrn_orient_matrix_UB_13      -0.0415601000
_diffrn_orient_matrix_UB_21      0.0121978000
_diffrn_orient_matrix_UB_22      0.0342429000
_diffrn_orient_matrix_UB_23      -0.0040747000
_diffrn_orient_matrix_UB_31      0.0215059000
_diffrn_orient_matrix_UB_32      -0.0061944000
_diffrn_orient_matrix_UB_33      -0.0598951000
_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  0.0310
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19515
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.532
_diffrn_reflns_theta_min         1.915
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.234
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.573
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_description       plate
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3211
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0144P)^2^+4.7855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2748
_reflns_number_total             3211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01833a2.cif
_cod_data_source_block           1-5_mor1761
_cod_depositor_comments
'Adding full bibliography for 7719387--7719420.cif.'
_cod_database_code               7719395
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C21 H22 N4 O6 Cl Fe I2'
_chemical_oxdiff_usercomment     'Eoin, EP49_1'
_shelx_estimated_absorpt_t_max   0.901
_shelx_estimated_absorpt_t_min   0.544
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C11-C10
 1.51 with sigma of 0.02
 C11-C12
 1.51 with sigma of 0.02
 H12B-C12
 0.99 with sigma of 0.001
 H12A-C12
 0.99 with sigma of 0.001
 C10-N2
 1.49 with sigma of 0.02
 H12A-H12B
 1.598 with sigma of 0.001
 N2-H2
 1 with sigma of 0.02
3. Others
 Fixed Sof: C11(0.5) H11A(0.5) H11B(0.5) C10(0.5) H10A(0.5) H10B(0.5) C12(0.5)
 H12A(0.5) H12B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C2(H2A), C7(H7)
;
_shelx_res_checksum              64751
_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 1.331
_oxdiff_exptl_absorpt_empirical_full_min 0.846