Two-step spin transition around room temperature in a Fe<sup>III</sup> complex.
Wu, Jianfeng; Li, Mengtao; Yang, Qianqian; Zhang, Baoliang; Tang, Jinkui; Dalton transactions (Cambridge, England : 2003) 54 (2025) 1231–1238; doi:10.1039/d4dt02736a

data_7717560
_publ_section_title
;
 Two-step spin transition around room temperature in a Fe<sup>III</sup>
 complex.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1231
_journal_page_last               1238
_journal_paper_doi               10.1039/d4dt02736a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C32 H22 Fe N4 O4, 1.716(C2 H3 N), B F4'
_chemical_formula_sum            'C35.43 H27.15 B F4 Fe N5.71 O4'
_chemical_formula_weight         739.61
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-11-21 deposited with the CCDC.	2024-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                71.31(2)
_cell_angle_beta                 72.147(14)
_cell_angle_gamma                88.655(14)
_cell_formula_units_Z            2
_cell_length_a                   9.786(6)
_cell_length_b                   12.619(7)
_cell_length_c                   15.625(11)
_cell_measurement_reflns_used    3015
_cell_measurement_temperature    360.00
_cell_measurement_theta_max      20.75
_cell_measurement_theta_min      2.22
_cell_volume                     1733.8(19)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      360.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1408
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28995
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.121
_diffrn_reflns_theta_max         25.121
_diffrn_reflns_theta_min         1.842
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'multi-scan was used for absorption correction. wR2(int) was 0.0979 before and 0.0508 after correction. The Ratio of minimum to maximum transmission is 0.8290. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             757
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         6108
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0721
_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^)+(0.1172P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.2245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3459
_reflns_number_total             6108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02736a2.cif
_cod_data_source_block           1_360K
_cod_depositor_comments
'Adding full bibliography for 7717555--7717562.cif.'
_cod_original_cell_volume        1733.7(19)
_cod_database_code               7717560
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.906
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 B2-F5 = B2-F6 = B2-F7 = B2-F8
 1.42 with sigma of 0.02
 F5A-F8A
 2.1 with sigma of 0.01
 B2-F5 \\sim B2-F6 \\sim B2-F7 \\sim B2-F8
 with sigma of 0.02
 F5-F6 \\sim F6-F7 \\sim F7-F8 \\sim F8-F5 \\sim F6-F8 \\sim F5-F7
 with sigma of 0.04
 B2-F6 \\sim B2-F6A
 with sigma of 0.02
 B2-F5 \\sim B2-F5A
 with sigma of 0.02
 B2-F8 \\sim B2-F8A
 with sigma of 0.02
 B2-F7 \\sim B2-F7A
 with sigma of 0.02
3. Rigid bond restraints
 F7A, B2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
B2 \\sim F5 \\sim F6 \\sim F7 \\sim F8: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N5) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F5A) \\sim Ueq, Uanis(B2) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F8A)
\\sim Ueq, Uanis(F6A) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(B2) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim
Ueq, Uanis(F8) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F7A) \\sim Ueq,
Uanis(F8A) \\sim Ueq, Uanis(F6A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 B2, F5, F6, F7, F8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(F5A)=Sof(F7A)=Sof(F8A)=Sof(F6A)=1-FVAR(1)
 Sof(F5)=Sof(F6)=Sof(F7)=Sof(F8)=FVAR(1)
 Fixed Sof: N5(0.8627) C33(0.8627) C34(0.8627) HV(0.8627) HW(0.8627)
 HX(0.8627) N6(0.8534) C35(0.8534) C36(0.8534) HY(0.8534) HZ(0.8534) H1(0.8534)
7.a Aromatic/amide H refined with riding coordinates:
 C1(HB), C2(HC), C3(HD), C7(HE), C8(HF), C9(HG), C10(HH), C14(HI), C15(HJ),
 C16(HK), C17(HL), C18(HM), C19(HN), C23(HO), C24(HP), C25(HQ), C26(HR),
 C28(HS), C29(HT), C30(HU)
7.b Idealised Me refined as rotating group:
 C34(HV,HW,HX), C36(HY,HZ,H1)
7.c Idealised tetrahedral OH refined as rotating group:
 O2(H), O4(HA)
;
_shelx_res_checksum              50973
_shelx_hkl_checksum              88195
_olex2_submission_special_instructions 'No special instructions were received'