6-Peroxo-6-Zirconium Crown and Its Hafnium Analogue Embedded in a Triangular Polyanion: [M6(O2)6(OH)6(γ-SiW10O36)3]18- (M = Zr, Hf)
Bassem S. Bassil; Sib Sankar Mal; Michael H. Dickman; Ulrich Kortz; Holger Oelrich; Lorenz Walder; Journal of the American Chemical Society 130 (2008) 6696–6697; doi:10.1021/ja801424q

data_4107820
_publ_section_title
;
 6-Peroxo-6-Zirconium Crown and Its Hafnium Analogue Embedded in a
 Triangular Polyanion: [M6(O2)6(OH)6(\g-SiW10O36)3]18- (M = Zr, Hf)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6696
_journal_page_last               6697
_journal_paper_doi               10.1021/ja801424q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'H124 Hf6 K18 O185 Si3 W30'
_chemical_formula_weight         10459.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.667(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   52.2945(17)
_cell_length_b                   17.6832(4)
_cell_length_c                   36.3549(9)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.34
_cell_measurement_theta_min      2.25
_cell_volume                     33549.8(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1751
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            344828
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    24.768
_exptl_absorpt_correction_T_max  0.5140
_exptl_absorpt_correction_T_min  0.1356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.142
_exptl_crystal_description       block
_exptl_crystal_F_000             37120
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.934
_refine_diff_density_min         -2.873
_refine_diff_density_rms         0.499
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1104
_refine_ls_number_reflns         28558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0820P)^2^+6500.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1998
_reflns_number_gt                18982
_reflns_number_total             28558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801424q-file002_2.cif
_cod_data_source_block           hfw
_cod_database_code               4107820