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_7717555
_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, 2(C2 H3 N), B F4'
_chemical_formula_sum            'C36 H28 B F4 Fe N6 O4'
_chemical_formula_weight         751.30
_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             2024-06-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-11-16 deposited with the CCDC.	2024-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                109.640(6)
_cell_angle_beta                 105.304(6)
_cell_angle_gamma                92.463(6)
_cell_formula_units_Z            2
_cell_length_a                   9.761(2)
_cell_length_b                   11.913(3)
_cell_length_c                   15.666(4)
_cell_measurement_reflns_used    5462
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.71
_cell_volume                     1637.4(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_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  0.1017
_diffrn_reflns_av_unetI/netI     0.0971
_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       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21657
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.182
_diffrn_reflns_theta_max         25.182
_diffrn_reflns_theta_min         1.882
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.899
_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    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             770
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         5809
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0727
_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^)+(0.1040P)^2^+1.1823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4067
_reflns_number_total             5809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02736a2.cif
_cod_data_source_block           1_150K
_cod_depositor_comments
'Adding full bibliography for 7717555--7717562.cif.'
_cod_original_cell_volume        1637.4(6)
_cod_database_code               7717555
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.901
_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
 F005-B1 \\sim F0-B1
 with sigma of 0.02
 F00P-B1 \\sim F00Q-B1
 with sigma of 0.02
 F00A-B1 \\sim F00B-B1
 with sigma of 0.02
 F00F-B1 \\sim F00G-B1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F00P) \\sim Ueq, Uanis(F00F) \\sim Ueq, Uanis(F00A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(F00G) \\sim Ueq, Uanis(F00B) \\sim Ueq, Uanis(F0) \\sim Ueq, Uanis(F00Q)
\\sim Ueq, Uanis(F00P) \\sim Ueq, Uanis(F00F) \\sim Ueq, Uanis(F00A) \\sim Ueq,
Uanis(F005) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F0)=Sof(F00B)=Sof(F00G)=Sof(F00Q)=1-FVAR(1)
 Sof(F00A)=Sof(F00F)=Sof(F00P)=Sof(F005)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
  C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25),
 C26(H26), C28(H28), C29(H29), C30(H30)
5.b Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
5.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4)
;
_shelx_res_checksum              97157
_shelx_hkl_checksum              45579
_olex2_submission_special_instructions 'No special instructions were received'