Guest-induced pore breathing controls the spin state in a cyanido-bridged framework.
Magott, Michał; Płonka, Klaudia; Sieklucka, Barbara; Dziedzic-Kocurek, Katarzyna; Kosaka, Wataru; Miyasaka, Hitoshi; Pinkowicz, Dawid; Chemical science 14 (2023) 9651–9663; doi:10.1039/d3sc03255h

data_1569689
_publ_section_title
;
 Guest-induced pore breathing controls the spin state in a cyanido-bridged
 framework.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              9651
_journal_page_last               9663
_journal_paper_doi               10.1039/d3sc03255h
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C56 H32 Fe2 N24 W'
_chemical_formula_sum            'C56 H32 Fe2 N24 W'
_chemical_formula_weight         1336.60
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-09-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-07 deposited with the CCDC.	2023-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8695(4)
_cell_length_b                   18.8695(4)
_cell_length_c                   15.4503(5)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.75
_cell_volume                     5501.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      80.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29032
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.274
_diffrn_reflns_theta_min         2.750
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.670
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0746 before and 0.0610 after correction.
The Ratio of minimum to maximum transmission is 0.7687.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             2648
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.737
_refine_diff_density_min         -2.457
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.473(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0209P)^2^+27.7101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0674
_reflns_Friedel_coverage         0.827
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3241
_reflns_number_total             3429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03255h2.cif
_cod_data_source_block           fe2wanh_80k_0m
_cod_depositor_comments
'Adding full bibliography for 1569688--1569691.cif.'
_cod_original_cell_volume        5501.2(3)
_cod_database_code               1569689
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.740
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.527(14)
 0.473(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C11(H11), C7(H7), C12(H12), C14(H14), C8(H8)
;
_shelx_res_checksum              48695
_olex2_submission_special_instructions 'No special instructions were received'