A Cyanide-Bridged Magnetically Switchable Cage with Encapsulated Water Molecules.
Wei, Rong-Jia; Shiga, Takuya; Newton, Graham N.; Robinson, David; Takeda, Sadamu; Oshio, Hiroki; Inorganic chemistry 55 (2016) 12114–12117; doi:10.1021/acs.inorgchem.6b02306

data_4349288
_publ_section_title
;
 A Cyanide-Bridged Magnetically Switchable Cage with Encapsulated Water
 Molecules.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12114
_journal_page_last               12117
_journal_paper_doi               10.1021/acs.inorgchem.6b02306
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration syn
_chemical_formula_sum            'C160 H188 B4 Br4 Co5 D8 Fe4 N44 O20'
_chemical_formula_weight         3944.59
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.432(4)
_cell_length_b                   24.169(4)
_cell_length_c                   35.472(6)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.86
_cell_measurement_theta_min      2.30
_cell_volume                     18374(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0961
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            192814
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    1.687
_exptl_absorpt_correction_T_max  0.9356
_exptl_absorpt_correction_T_min  0.8232
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8092
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
The unit cell volume comprises a large region of solvent molecules outside the Co5Fe4 cage and only six acetone molecules can be modeled as discrete atomic sites, while the rest of them (approximately 31.6 % of the unit cell volume) are disordered. SQUEEZE program in the PLATON suite was employed to calculate the contribution to the diffraction from the solvent region. SQUEEZE estimated a total count of 1370.7 electrons per unit cell which were assigned to be ten acetone and two D2O molecules per cage.
;
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.062(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1797
_refine_ls_number_reflns         36123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+19.7327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                29472
_reflns_number_total             36123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02306_si_002.cif
_cod_data_source_block           D2O
_cod_original_cell_volume        18374(5)
_cod_database_code               4349288