Caging Peroxide: Anion-Templated Synthesis and Characterization of a Rare-Earth Cluster
William J. Gee; Jonathan G. MacLellan; Craig M. Forsyth; Boujemaa Moubaraki; Keith S. Murray; Philip C. Andrews; Peter C. Junk; Inorganic Chemistry 51 (2012) 8661–8663; doi:10.1021/ic301382r

data_4330121
_publ_section_title
;
 Caging Peroxide: Anion-Templated Synthesis and Characterization of a
 Rare-Earth Cluster
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8661
_journal_page_last               8663
_journal_paper_doi               10.1021/ic301382r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C60 H68 N9 Na3 O31 Tb3'
_chemical_formula_weight         1956.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
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_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   20.8027(8)
_cell_length_b                   20.8027(8)
_cell_length_c                   58.306(4)
_cell_measurement_reflns_used    4511
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23.72
_cell_measurement_theta_min      2.37
_cell_volume                     21851.6(19)
_computing_cell_refinement       'Bruker Apex2 v2.0'
_computing_data_collection       'Bruker Apex2 v2.0'
_computing_data_reduction        'Bruker Apex2 v2.0'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1430
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            59689
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.991
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       prism
_exptl_crystal_F_000             11604
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.049
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4284
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0344P)^2^+405.1425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                3633
_reflns_number_total             4284
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301382r_si_002.cif
_cod_data_source_block           wgetb2r
_cod_original_cell_volume        21852(2)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4330121