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_4107819
_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 K18 O185 Si3 W30 Zr6'
_chemical_formula_weight         9935.88
_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                 93.5730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   52.1923(14)
_cell_length_b                   17.6634(4)
_cell_length_c                   36.4505(8)
_cell_measurement_reflns_used    8651
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.86
_cell_measurement_theta_min      2.72
_cell_volume                     33538.2(14)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.2016
_diffrn_reflns_av_sigmaI/netI    0.0824
_diffrn_reflns_limit_h_max       58
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            423603
_diffrn_reflns_theta_full        23.75
_diffrn_reflns_theta_max         23.75
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    21.438
_exptl_absorpt_correction_T_max  0.2962
_exptl_absorpt_correction_T_min  0.0822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    3.936
_exptl_crystal_description       platelet
_exptl_crystal_F_000             35584
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.303
_refine_diff_density_min         -2.225
_refine_diff_density_rms         0.473
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1106
_refine_ls_number_reflns         25307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0749
_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^)+(0.1110P)^2^+5000.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2253
_reflns_number_gt                16229
_reflns_number_total             25307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja801424q-file002_1.cif
_cod_data_source_block           c2c
_cod_database_code               4107819