Subtle Ligand Modification Inverts Guest Binding Hierarchy in M(II)8L6 Supramolecular Cubes.
Ramsay, William J.; Rizzuto, Felix J.; Ronson, Tanya K.; Caprice, Kenji; Nitschke, Jonathan R.; Journal of the American Chemical Society 138 (2016) 7264–7267; doi:10.1021/jacs.6b03858

data_4130474
_publ_section_title
;
 Subtle Ligand Modification Inverts Guest Binding Hierarchy in M(II)8L6
 Supramolecular Cubes.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7264
_journal_page_last               7267
_journal_paper_doi               10.1021/jacs.6b03858
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
;        
 C312 H192 F24 Fe8 Mo12 N48 O48, 16(C F3 O3 S), 27(C2 H3 N), 
 0.5(C4 H10 O), 4(H2 O) 
;
_chemical_formula_sum            'C384 H286 F72 Fe8 Mo12 N75 O100.5 S32'
_chemical_formula_weight         11550.86
_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   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                72.136(3)
_cell_angle_beta                 72.820(2)
_cell_angle_gamma                66.502(2)
_cell_formula_units_Z            2
_cell_length_a                   28.1822(15)
_cell_length_b                   28.6098(15)
_cell_length_c                   38.033(2)
_cell_measurement_reflns_used    9727
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.552
_cell_measurement_theta_min      4.430
_cell_volume                     26235(2)
_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        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.975
_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     0.6889
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            373850
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        23.743
_diffrn_reflns_theta_max         23.928
_diffrn_reflns_theta_min         0.770
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             11582
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.450
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     6369
_refine_ls_number_reflns         87480
_refine_ls_number_restraints     11875
_refine_ls_restrained_S_all      1.449
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0958
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2894
_refine_ls_wR_factor_ref         0.3219
_reflns_Friedel_coverage         0.000
_reflns_number_gt                60781
_reflns_number_total             87480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03858_si_003.cif
_cod_data_source_block           wjr1167_sqd
_cod_original_formula_sum        'C384 H286 F72 Fe8 Mo12 N75 O100.50 S32'
_cod_database_code               4130474
_shelx_estimated_absorpt_t_min   0.770
_shelx_estimated_absorpt_t_max   0.906
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              11023
_shelx_hkl_checksum              61576