Electron transfer coupled spin transition in cyano-bridged mixed-valence {FeIII2FeII2} molecular squares.
Jia, Shuwen; Shang, Mengjia; Jin, Sai; Zhu, Xinrui; Cai, Yuanyuan; Li, Dongfeng; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2807–2814; doi:10.1039/d3dt03208f

data_7714970
_publ_section_title
;
 Electron transfer coupled spin transition in cyano-bridged mixed-valence
 {FeIII2FeII2} molecular squares.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2807
_journal_page_last               2814
_journal_paper_doi               10.1039/d3dt03208f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C96 H88 B2 Fe4 N26, 2(Cl O4)'
_chemical_formula_sum            'C96 H88 B2 Cl2 Fe4 N26 O8'
_chemical_formula_weight         2049.84
_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             2023-12-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-28 deposited with the CCDC.	2024-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                111.570(3)
_cell_angle_beta                 93.521(4)
_cell_angle_gamma                106.655(3)
_cell_formula_units_Z            1
_cell_length_a                   11.0057(9)
_cell_length_b                   15.8520(14)
_cell_length_c                   17.6035(16)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    165
_cell_measurement_theta_max      57.05
_cell_measurement_theta_min      2.39
_cell_volume                     2687.9(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      165.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39555
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        51.243
_diffrn_reflns_theta_max         51.243
_diffrn_reflns_theta_min         2.390
_diffrn_source_current           3.57
_diffrn_source_power             0.2497215
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.576
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.3838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1626 before and 0.0951 after correction.
The Ratio of minimum to maximum transmission is 0.5109.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         8821
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0867P)^2^+2.3497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7563
_reflns_number_total             8821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03208f2.cif
_cod_data_source_block           1-8CH3OH-165K
_cod_depositor_comments
'Adding full bibliography for 7714965--7714970.cif.'
_cod_database_code               7714970
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.694
_shelx_estimated_absorpt_t_min   0.634
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 O1-O2 = O1-O3 = O1-O4 = O2-O3 = O2-O4 = O3-O4
 2.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C53) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C55) \\sim Ueq,
Uanis(C58) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C49) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H19C)=Sof(H19D)=Sof(C54)=Sof(C53)=Sof(H53)=Sof(C52)=Sof(C51)=Sof(H51)=
 Sof(C50)=Sof(H50)=Sof(C49)=Sof(H49)=Sof(C58)=Sof(H58)=Sof(C57)=Sof(C56)=
 Sof(H56)=Sof(C55)=Sof(H55)=1-FVAR(1)
 Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=
 Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=
 Sof(C28)=Sof(C29)=Sof(H29)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 B1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C19(H19C,H19D), C30(H30A,H30B), C31(H31A,
 H31B), C37(H37A,H37B), C38(H38A,H38B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C32(H32), C33(H33), C34(H34), C35(H35),
  C40(H40), C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48),
 C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C53(H53),
  C51(H51), C50(H50), C49(H49), C58(H58), C56(H56), C55(H55)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11776
_shelx_fab_checksum              82497
_platon_squeeze_special_details
;
A solvent mask was calculated and 146 electrons were 
found in a volume of 552\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
8[CH3OH], 2[] per Formula Unit 
which account for 144 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'