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_4130473
_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 H216 Mo12 N48 O48 Zn8, 16(C F3 S O3), 9(H2 O)'
_chemical_formula_sum            'C328 H234 F48 Mo12 N48 O105 S16 Zn8'
_chemical_formula_weight         9626.82
_space_group_crystal_system      cubic
_space_group_IT_number           209
_space_group_name_Hall           'F 4 2 3'
_space_group_name_H-M_alt        'F 4 3 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.9008(15)
_cell_length_b                   40.9008(15)
_cell_length_c                   40.9008(15)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.621
_cell_measurement_theta_min      4.317
_cell_volume                     68422(4)
_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-2014/7 (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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.1628
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            84020
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        20.343
_diffrn_reflns_theta_max         20.343
_diffrn_reflns_theta_min         0.836
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.5101
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    0.935
_exptl_crystal_description       block
_exptl_crystal_F_000             19240
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.4(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3089
_refine_ls_number_restraints     310
_refine_ls_restrained_S_all      1.331
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.1358
_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^)+(0.2000P)^2^+300.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3741
_refine_ls_wR_factor_ref         0.3893
_reflns_Friedel_coverage         0.660
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2235
_reflns_number_total             3089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03858_si_002.cif
_cod_data_source_block           wjr71b
_cod_original_cell_volume        68422(8)
_cod_database_code               4130473
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.994
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              7075
_shelx_hkl_checksum              22653