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_4314496
_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
;
 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            'H50 K12 O107 Si2 W22 Zr2'
_chemical_formula_weight         6514.8
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.355(6)
_cell_angle_beta                 87.259(7)
_cell_angle_gamma                63.100(5)
_cell_formula_units_Z            1
_cell_length_a                   11.5163(13)
_cell_length_b                   12.4128(13)
_cell_length_c                   21.326(3)
_cell_measurement_reflns_used    9298
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2678.9(6)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1140
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            214947
_diffrn_reflns_theta_full        32.42
_diffrn_reflns_theta_max         32.42
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    24.296
_exptl_absorpt_correction_T_max  0.0528
_exptl_absorpt_correction_T_min  0.0397
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    4.038
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2870
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_refine_diff_density_max         5.147
_refine_diff_density_min         -2.531
_refine_diff_density_rms         0.532
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         19033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0875P)^2^+46.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1620
_reflns_number_gt                14895
_reflns_number_total             19033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902203p_si_002_1.cif
_cod_data_source_block           zrw
_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_cell_volume        2678.9(5)
_cod_database_code               4314496