Peroxo-Zr/Hf-Containing Undecatungstosilicates and -Germanates
Sib Sankar Mal; Nadeen H. Nsouli; Mauro Carraro; Andrea Sartorel; Gianfranco Scorrano; Holger Oelrich; Lorenz Walder; Marcella Bonchio; Ulrich Kortz; Inorganic Chemistry 49 (2010) 7–9; doi:10.1021/ic902203p

data_4314498
_publ_contact_author_address
;
Jacobs University, School of Engineering and Science, 
P.O. Box 750 561, 28725 Bremen, Germany
;
_publ_contact_author_email       u.kortz@jacobs-university.de
_publ_contact_author_name        'Ulrich Kortz'
_publ_section_title
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 Peroxo-Zr/Hf-Containing Undecatungstosilicates and -Germanates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7
_journal_page_last               9
_journal_paper_doi               10.1021/ic902203p
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'H42 Hf2 K10.5 O103 Rb1.5 Si2 W22'
_chemical_formula_weight         6686.9
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.487(3)
_cell_angle_beta                 92.993(3)
_cell_angle_gamma                103.241(3)
_cell_formula_units_Z            1
_cell_length_a                   11.5111(6)
_cell_length_b                   12.5996(7)
_cell_length_c                   19.0734(9)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2687.1(2)
_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         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            157106
_diffrn_reflns_theta_full        28.07
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         3.86
_exptl_absorpt_coefficient_mu    26.571
_exptl_absorpt_correction_T_max  0.2405
_exptl_absorpt_correction_T_min  0.0501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    4.132
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2921
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.144
_refine_diff_density_min         -5.113
_refine_diff_density_rms         0.449
_refine_ls_extinction_coef       0.00057(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         12944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0790P)^2^+68.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                9957
_reflns_number_total             12944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902203p_si_002_3.cif
_cod_data_source_block           hfw
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'H42 Hf2 K10.50 O103 Rb1.50 Si2 W22'
_cod_database_code               4314498