Chain-Reaction Anion Exchange between Metal-Organic Cages
Shucong Ma; Maarten M. J. Smulders; Yana R. Hristova; Jack K. Clegg; Tanya K. Ronson; Salvatore Zarra; Jonathan R. Nitschke; Journal of the American Chemical Society 135 (2013) 5678–5684; doi:10.1021/ja311882h

data_4119580
_publ_section_title
;
 Chain-Reaction Anion Exchange between Metal-Organic Cages
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5678
_journal_page_last               5684
_journal_paper_doi               10.1021/ja311882h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
'C192 H156 N24 O12 Fe4, 8(B F4), 3.5(C2 H3 N)'
_chemical_formula_sum            'C199 H166.5 B8 F32 Fe4 N27.5 O12'
_chemical_formula_weight         4052.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.369(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.191(11)
_cell_length_b                   39.825(15)
_cell_length_c                   20.852(8)
_cell_measurement_reflns_used    31058
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1.2
_cell_volume                     22441(15)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_molecular_graphics
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999) 
;
_computing_publication_material  'enCIFer 1.1 (CCDC, 2005)'
_computing_structure_refinement  'SHELXH-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Rigaku Saturn 724+ detector on Crystal Logic diffractometer'
_diffrn_measurement_method       '\w  scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            118110
_diffrn_reflns_theta_full        20.15
_diffrn_reflns_theta_max         20.15
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       blade
_exptl_crystal_F_000             8324
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.001
_platon_squeeze_details
;
electrons included as missing tetrafluoroborate anions.
;
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.487
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2045
_refine_ls_number_reflns         23420
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.487
_refine_ls_R_factor_all          0.1613
_refine_ls_R_factor_gt           0.1310
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3031
_refine_ls_wR_factor_ref         0.3206
_reflns_number_gt                16737
_reflns_number_total             23420
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja311882h_si_002_1.cif
_cod_data_source_block           squeezed
_cod_original_cell_volume        22442(15)
_cod_original_formula_sum        'C199 H166.50 B8 F32 Fe4 N27.50 O12'
_cod_database_code               4119580