A spin crossover FeII4L6 cage based on pyridyl-hydrazone sites
Li, Weiyang; Liu, Cuilian; Kfoury, Joseph; Oláh, Julianna; Robeyns, Koen; Singleton, Michael L.; Demeshko, Serhiy; Meyer, Franc; Garcia, Yann; Chemical Communications  (2022) –; doi:10.1039/D2CC04476E

data_7130718
_publ_section_title
;
 A spin crossover FeII4L6 cage based on pyridyl-hydrazone sites
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04476E
_journal_year                    2022
_chemical_formula_moiety
'C156 H84 Fe4 N36 O24, 8(B F4), 3.64(C4 H8 O), C2 H3 N [+ solvent]'
_chemical_formula_sum            'C172.56 H116.12 B8 F32 Fe4 N37 O27.64'
_chemical_formula_weight         4067.97
_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-2018/3
_audit_update_record
;
2022-07-21 deposited with the CCDC.	2022-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                93.602(7)
_cell_angle_beta                 91.560(7)
_cell_angle_gamma                96.891(8)
_cell_formula_units_Z            4
_cell_length_a                   22.121(2)
_cell_length_b                   22.881(2)
_cell_length_c                   38.937(3)
_cell_measurement_reflns_used    4815
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.5530
_cell_measurement_theta_min      2.7270
_cell_volume                     19515(3)
_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
_computing_data_reduction
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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 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method
;
'120 images, \D\F 1.5\% '
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.1650
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            56550
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        19.027
_diffrn_reflns_theta_max         19.027
_diffrn_reflns_theta_min         2.815
_diffrn_source                   'Incoatec microfocus source'
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38256
_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            'dark pink - red'
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       plate
_exptl_crystal_F_000             8254
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'diffusion of diethylether in a acetonitrile solution'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.422
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5333
_refine_ls_number_reflns         29971
_refine_ls_number_restraints     16405
_refine_ls_restrained_S_all      1.234
_refine_ls_R_factor_all          0.2296
_refine_ls_R_factor_gt           0.1377
_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^)+(0.0800P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2880
_refine_ls_wR_factor_ref         0.3247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14820
_reflns_number_total             29971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04476e2.cif
_cod_data_source_block           yg_wl_grid1120k
_cod_database_code               7130718
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              78102
_shelx_hkl_checksum              46486
_shelx_fab_checksum              38904