Angle-dependent spin crossover properties in polymorphic iron(II) complexes based on pyridine-triazole derivatives.
Cuza, Emmelyne; Delsuc, Nicolas; Marrot, Jerôme; Shepard, William; Policar, Clotilde; Serre, Christian; Tissot, Antoine; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6274–6280; doi:10.1039/d4dt03376k

data_7718288
_publ_section_title
;
 Angle-dependent spin crossover properties in polymorphic iron(II)
 complexes based on pyridine-triazole derivatives.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6274
_journal_page_last               6280
_journal_paper_doi               10.1039/d4dt03376k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C28 H30 Fe N12 O6 S2'
_chemical_formula_sum            'C28 H30 Fe N12 O6 S2'
_chemical_formula_weight         750.61
_chemical_name_systematic        ec103-b2-200K
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-10 deposited with the CCDC.	2025-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.732(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5277(8)
_cell_length_b                   14.6210(7)
_cell_length_c                   9.2130(6)
_cell_measurement_reflns_used    2628
_cell_measurement_temperature    200
_cell_measurement_theta_max      46.23
_cell_measurement_theta_min      2.93
_cell_volume                     1770.14(18)
_computing_cell_refinement       'CrystFEL (White, 2018)'
_computing_data_collection       MXCuBE
_computing_data_reduction        'CrystFEL (White, 2018)'
_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_temperature      200
_diffrn_detector                 'pixel array detector'
_diffrn_detector_area_resol_mean 0.075
_diffrn_detector_type            'DECTRIS EIGER-9M'
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       'omega rotation shutterless scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72932
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16974
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         25.994
_diffrn_reflns_theta_min         1.590
_diffrn_source                   'Synchrotron SOLEIL'
_diffrn_source_target            Mo
_diffrn_source_type              'U24 Undulator, PROXIMA-2 Beamline'
_exptl_absorpt_coefficient_mu    0.641
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       needle
_exptl_crystal_F_000             776
_exptl_crystal_preparation       'In fine glass tube'
_exptl_crystal_recrystallization_method 'MeOH H2O'
_exptl_crystal_size_max          0.0728
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.0256
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1341P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1583
_reflns_number_total             2920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03376k2.cif
_cod_data_source_block           ec103-b2-200k
_cod_depositor_comments
'Adding full bibliography for 7718287--7718289.cif.'
_cod_database_code               7718288
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.955
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 N6(H6), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              56425
_shelx_hkl_checksum              90844
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id ec103-b2-200K
_olex2_submission_special_instructions 'No special instructions were received'