A Chiral 60-Metal Sodalite Cage Featuring 24 Vertex-Sharing [Er4(μ3-OH)4] Cubanes
Xiang-Jian Kong; Yinglan Wu; La-Sheng Long; Lan-Sun Zheng; Zhiping Zheng; Journal of the American Chemical Society 131 (2009) 6918–6919; doi:10.1021/ja901214d

data_4104412
_publ_section_title
;
 A Chiral 60-Metal Sodalite Cage Featuring 24 Vertex-Sharing
 [Er4(\m3-OH)4] Cubanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6918
_journal_page_last               6919
_journal_paper_doi               10.1021/ja901214d
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration am
_chemical_formula_sum            'C144 H484 Br12 Cl18 Er60 N34 O354'
_chemical_formula_weight         19990.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 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                   29.2379(3)
_cell_length_b                   43.3554(6)
_cell_length_c                   46.0899(5)
_cell_measurement_reflns_used    38112
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.2155
_cell_measurement_theta_min      3.1639
_cell_volume                     58424.5(12)
_computing_cell_refinement       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Oxford Gemini S Ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1122
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            71573
_diffrn_reflns_theta_full        62.29
_diffrn_reflns_theta_max         62.29
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    17.682
_exptl_absorpt_correction_T_max  0.2708
_exptl_absorpt_correction_T_min  0.1767
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             36896
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.664
_refine_diff_density_min         -6.571
_refine_diff_density_rms         0.370
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2126
_refine_ls_number_reflns         40667
_refine_ls_number_restraints     715
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.1042
_refine_ls_shift/su_max          0.158
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+7488.7417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2441
_refine_ls_wR_factor_ref         0.2529
_reflns_number_gt                33231
_reflns_number_total             40667
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901214d_si_003.cif
_cod_data_source_block           Er60-D
_cod_database_code               4104412
_platon_er60-d_details
;
SQUEEZE removed 12 disordered Br-, 18 ClO4- disordered anions and 
40 disordered water molecules per formula unit. This valueis 
calculated based upon elemental analysis data.
;