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_7714371
_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
'C156 H84 Fe4 N36 O24, 8(Cl O4), 3(C2 H3 N) [+ solvent]'
_chemical_formula_sum            'C162 H93 Cl8 Fe4 N39 O56'
_chemical_formula_weight         3988.75
_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     'dual space'
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2023-06-19 deposited with the CCDC.	2023-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                75.558(6)
_cell_angle_beta                 78.046(7)
_cell_angle_gamma                89.230(7)
_cell_formula_units_Z            2
_cell_length_a                   16.7950(17)
_cell_length_b                   16.8250(12)
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_cell_measurement_reflns_used    5224
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.7860
_cell_measurement_theta_min      2.5340
_cell_volume                     8837.4(13)
_computing_cell_refinement
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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
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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      120(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method
;
'150 images, \D\F 1.2\% '
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_unetI/netI     0.1173
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34789
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        20.815
_diffrn_reflns_theta_max         20.815
_diffrn_reflns_theta_min         2.513
_diffrn_source                   'Incoatec microfocus source'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       plate
_exptl_crystal_F_000             4052
_exptl_crystal_recrystallization_method
'slow diffusion of diethylether in an acetonitrile solution of the compound'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.281
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2514
_refine_ls_number_reflns         17635
_refine_ls_number_restraints     673
_refine_ls_restrained_S_all      1.342
_refine_ls_R_factor_all          0.1683
_refine_ls_R_factor_gt           0.0951
_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^)+(0.0650P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2111
_refine_ls_wR_factor_ref         0.2372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9411
_reflns_number_total             17635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02474a2.cif
_cod_data_source_block           yg_wl_cage8_ml
_cod_depositor_comments
'Adding full bibliography for 7714371--7714372.cif.'
_cod_database_code               7714371
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.995
_shelx_res_checksum              91647
_shelx_fab_checksum              594