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_7718287
_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
_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             2025-02-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-21 deposited with the CCDC.	2025-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.910(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.271(3)
_cell_length_b                   13.139(3)
_cell_length_c                   9.619(2)
_cell_measurement_reflns_used    3057
_cell_measurement_temperature    180.00
_cell_measurement_theta_max      23.05
_cell_measurement_theta_min      2.20
_cell_volume                     1652.2(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      180.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1771
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            31560
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.108
_diffrn_reflns_theta_max         25.108
_diffrn_reflns_theta_min         2.650
_diffrn_source                   microsource
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0998 before and 0.0805 after correction.
The Ratio of minimum to maximum transmission is 0.8129.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         2930
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.1309
_refine_ls_R_factor_gt           0.0937
_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^)+(0.0416P)^2^+6.6556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2102
_reflns_number_total             2930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03376k2.cif
_cod_data_source_block           ts6k_0ma_a3
_cod_depositor_comments
'Adding full bibliography for 7718287--7718289.cif.'
_cod_original_cell_volume        1652.3(6)
_cod_database_code               7718287
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.927
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16-C17A
 1.53 with sigma of 0.02
 C16-C17B
 -1.53 with sigma of 0.02
 C17A-C18A
 1.5 with sigma of 0.02
 C18A-O19A
 1.2 with sigma of 0.02
 C17B-C18B
 1.5 with sigma of 0.02
 C18B-O19B
 1.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17A) \\sim Ueq, Uanis(C17B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O19A) \\sim Ueq, Uanis(O19B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C18A) = Uanis(C18B)
Uanis(C17A) = Uanis(C17B)
4. Others
 Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=Sof(O19B)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(O19A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C16(H16A,H16B), C16(H16C,H16D), C17A(H17A,H17B), C17B(H17C,
 H17D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), N15(H15)
5.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              7750
_shelx_hkl_checksum              81779
_olex2_submission_special_instructions 'No special instructions were received'