Spin-state versatility in FeII4L<sub>6</sub> supramolecular cages with a pyridyl-hydrazone ligand scaffold modulated by solvents and counter anions.
Li, Weiyang; Li, Xiaochun; Robeyns, Koen; Wolff, Mariusz; Kfoury, Joseph; Oláh, Julianna; Herchel, Radovan; Demeshko, Serhiy; Meyer, Franc; Garcia, Yann; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1449–1459; doi:10.1039/d3dt02474a

data_7714372
_publ_section_title
;
 Spin-state versatility in FeII4L<sub>6</sub> supramolecular cages with a
 pyridyl-hydrazone ligand scaffold modulated by solvents and counter
 anions.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1449
_journal_page_last               1459
_journal_paper_doi               10.1039/d3dt02474a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'2(C156 H84 Fe4 N36 O24), 13(C F3 O3 S), 11(C2 H3 N) [+ solvent]'
_chemical_formula_sum            'C347 H201 F39 Fe8 N83 O87 S13'
_chemical_formula_weight         8529.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-06-19 deposited with the CCDC.	2023-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.3311(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.3061(4)
_cell_length_b                   22.1383(2)
_cell_length_c                   70.1304(9)
_cell_measurement_reflns_used    41314
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.6480
_cell_measurement_theta_min      2.8350
_cell_volume                     43483.4(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       MAR
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'MERCURY (Macrae et al., 2008)'
_computing_publication_material
;
'MERCURY (Macrae et al., 2008), Platon (Spek, 2009)'
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method
;
'90 images, \D\F 3.0\% '
'49 images, \D\F 3.0\% (2nd orientation)'
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -85
_diffrn_reflns_number            239369
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.697
_diffrn_reflns_theta_min         2.854
_diffrn_source                   'Incoatec microfocus source'
_exptl_absorpt_coefficient_mu    0.418
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       plate
_exptl_crystal_F_000             17308
_exptl_crystal_recrystallization_method
'slow diffusion of diethylether in an acetonitrile solution of the compound'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.469
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.490(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5206
_refine_ls_number_reflns         78695
_refine_ls_number_restraints     1859
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+137.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.1987
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.931
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                66104
_reflns_number_total             78695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02474a2.cif
_cod_data_source_block           yg_wl_cage8_NTf2100k_sad
_cod_depositor_comments
'Adding full bibliography for 7714371--7714372.cif.'
_cod_original_cell_volume        43483.4(10)
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               7714372
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              73533
_shelx_fab_checksum              7477