Tetrahedral metal-organic cages with cube-like cavities for selective encapsulation of fullerene guests and their spin-crossover properties.
Han, Wang-Kang; Zhang, Hai-Xia; Wang, Yong; Liu, Wei; Yan, Xiaodong; Li, Tao; Gu, Zhi-Guo; Chemical communications (Cambridge, England) 54 (2018) 12646–12649; doi:10.1039/c8cc06652c

data_7122447
_publ_section_title
;
 Tetrahedral metal-organic cages with cube-like cavities for selective
 encapsulation of fullerene guests and their spin-crossover properties.
;
_journal_issue                   89
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12646
_journal_page_last               12649
_journal_paper_doi               10.1039/c8cc06652c
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_formula_moiety
'C276 H252 Fe4 N36 O12, 7(C F3 O3 S) [+ anion] [+ solvent]'
_chemical_formula_sum            'C283 H252 F21 Fe4 N36 O33 S7'
_chemical_formula_weight         5532.01
_space_group_crystal_system      trigonal
_space_group_IT_number           145
_space_group_name_Hall           'P 32'
_space_group_name_H-M_alt        'P 32'
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-07 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.7520(11)
_cell_length_b                   23.7520(11)
_cell_length_c                   49.776(5)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.09
_cell_measurement_theta_min      2.33
_cell_volume                     24319(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            111340
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        22.123
_diffrn_reflns_theta_max         22.123
_diffrn_reflns_theta_min         0.990
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       block
_exptl_crystal_F_000             8613
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 9107 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.053(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     3751
_refine_ls_number_reflns         39566
_refine_ls_number_restraints     5722
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1204P)^2^+7.5784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2439
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                25052
_reflns_number_total             39566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06652c2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7122446--7122447.cif.'
_cod_database_code               7122447
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.879
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              54023
_shelx_fab_checksum              67931