Phenyltin-Substituted 9-Tungstogermanate and Comparison with Its Tungstosilicate Analogue
Santiago Reinoso; Michael H. Dickman; Antonia Praetorius; Luis Fernando Piedra-Garza; Ulrich Kortz; Inorganic Chemistry 47 (2008) 8798–8806; doi:10.1021/ic800852d

data_4305934
_publ_contact_author_address
;
School of Engineering and Science,
Jacobs University Bremen,
P.O. Box 750 561,
28725 Bremen, Germany
;
_publ_contact_author_email       u.kortz@jacobs-university.de
_publ_contact_author_fax         '+49-421-200 3229'
_publ_contact_author_name        'Ulrich Kortz'
_publ_section_title
;
Phenyltin-Substituted 9-Tungstogermanate and Comparison with Its
Tungstosilicate Analogue
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8798
_journal_page_last               8806
_journal_paper_doi               10.1021/ic800852d
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C18 H36 Cs3 Na O46 Si Sn3 W9'
_chemical_formula_weight         3449.00
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   16.75840(10)
_cell_length_b                   16.75840(10)
_cell_length_c                   33.6877(5)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.91
_cell_measurement_theta_min      3.03
_cell_volume                     8193.46(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      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0717
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            116640
_diffrn_reflns_theta_full        31.62
_diffrn_reflns_theta_max         31.62
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    22.322
_exptl_absorpt_correction_T_max  0.1021
_exptl_absorpt_correction_T_min  0.0900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.194
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedron
_exptl_crystal_F_000             9108
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.558
_refine_diff_density_min         -3.683
_refine_diff_density_rms         0.350
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         6099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+300.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                4981
_reflns_number_total             6099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800852d_si_001_4.cif
_cod_data_source_block           CsNa-2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        8193.45(14)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4305934