Ultrastrong Alkali-Resisting Lanthanide-Zeolites Assembled by [Ln60] Nanocages.
Dong, Jie; Cui, Ping; Shi, Peng-Fei; Cheng, Peng; Zhao, Bin; Journal of the American Chemical Society 137 (2015) 15988–15991; doi:10.1021/jacs.5b10000

data_4124804
_publ_section_title
;
 Ultrastrong Alkali-Resisting Lanthanide-Zeolites Assembled by [Ln60]
 Nanocages.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15988
_journal_page_last               15991
_journal_paper_doi               10.1021/jacs.5b10000
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         '0.13(C8 H48 Gd24 O72), 0.99(H O)'
_chemical_formula_sum            'C H6.99 Gd3 O9.99'
_chemical_formula_weight         650.65
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_Hall           'I 4 2 3'
_space_group_name_H-M_alt        'I 4 3 2'
_symmetry_space_group_name_Hall  'I 4 2 3'
_symmetry_space_group_name_H-M   'I 4 3 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6606(4)
_cell_length_b                   12.6606(4)
_cell_length_c                   12.6606(4)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.22
_cell_volume                     2029.38(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0107
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14242
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         3.22
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.411
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0977 before and 0.0754 after correction.
The Ratio of minimum to maximum transmission is 0.8529.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    4.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2279
_refine_diff_density_max         2.098
_refine_diff_density_min         -2.436
_refine_diff_density_rms         0.311
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.5(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     26
_refine_ls_number_reflns         308
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0260P)^2^+217.9960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                294
_reflns_number_total             308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b10000_si_003.cif
_cod_data_source_block           Gd5M
_cod_database_code               4124804
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
2. Restrained distances
 H-O
 0.85 with sigma of 0.02
 H1-O1
 0.85 with sigma of 0.02
 H-H1
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Gd2) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of
0.0005
Uanis(O) \\sim Ueq, Uanis(O0AA) \\sim Ueq, Uanis(C) \\sim Ueq: with sigma of
0.0005 and sigma for terminal atoms of 0.0005
Uanis(O) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.05
4. Others
 Fixed Sof: O1(0.165) H1(0.165)
5.a Riding coordinates:
 O(H), O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'