#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/71/2017124.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2017124
loop_
_publ_author_name
'Jennene Boukharrata, Nefla'
'Thomas, Philippe'
'Laval, Jean-Paul'
_publ_section_title
;
 GeTe₂O₆, a germanium tellurate(IV) with an open framework
;
_journal_coeditor_code           SQ3186
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i23
_journal_page_last               i26
_journal_paper_doi               10.1107/S0108270109010488
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'Ge Te2 O6'
_chemical_formula_moiety         'Ge O6 Te2'
_chemical_formula_sum            'Ge O6 Te2'
_chemical_formula_weight         423.79
_chemical_name_systematic
;
germanium tellurate(IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.66(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.2201(8)
_cell_length_b                   6.9730(13)
_cell_length_c                   7.3252(15)
_cell_measurement_reflns_used    2864
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      4.86
_cell_volume                     266.52(8)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg, 1992)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1998)'
_computing_data_reduction        'EvalCCD (Duisenberg et al.,  2003)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_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  0.1048
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5004
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         4.86
_exptl_absorpt_coefficient_mu    16.430
_exptl_absorpt_correction_T_max  0.9524
_exptl_absorpt_correction_T_min  0.7347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    5.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.018
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.003
_refine_diff_density_max         2.241
_refine_diff_density_min         -1.717
_refine_ls_extinction_coef       0.0024(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0161P)²+0.2280P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0545
_reflns_number_gt                551
_reflns_number_total             771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sq3186.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               2017124
_cod_database_fobs_code          2017124
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Te Te1 0.52166(8) 0.15761(7) 0.71712(7) 0.00782(16) Uani d . 1 . .
Ge Ge1 0.5000 0.5000 1.0000 0.0069(3) Uani d S 1 . .
O O1 0.3012(8) 0.1473(7) 0.5059(7) 0.0104(11) Uani d . 1 . .
O O2 0.8158(9) 0.2115(7) 0.5856(7) 0.0101(12) Uani d . 1 . .
O O3 0.4440(9) 0.4156(7) 0.7598(7) 0.0101(12) Uani d . 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Te1 0.0068(2) 0.0082(2) 0.0085(3) 0.0001(2) 0.00028(16) -0.0003(3)
Ge1 0.0053(5) 0.0075(6) 0.0078(6) 0.0004(5) 0.0008(4) 0.0000(5)
O1 0.008(2) 0.011(3) 0.012(3) -0.002(2) -0.002(2) -0.001(3)
O2 0.009(2) 0.007(3) 0.014(3) -0.003(2) 0.002(2) -0.003(2)
O3 0.012(3) 0.012(3) 0.007(3) 0.001(2) -0.002(2) -0.002(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Te1 O2 . . 94.5(2) ?
O3 Te1 O1 . . 92.5(2) ?
O2 Te1 O1 . . 94.3(2) ?
O3 Te1 O1 . 3_656 152.54(19) ?
O2 Te1 O1 . 3_656 64.59(17) ?
O1 Te1 O1 . 3_656 72.81(19) ?
O3 Te1 O1 . 4_666 62.00(16) ?
O2 Te1 O1 . 4_666 82.96(18) ?
O1 Te1 O1 . 4_666 153.87(8) ?
O1 Te1 O1 3_656 4_666 127.44(9) ?
O3 Te1 O3 . 2_546 110.80(9) ?
O2 Te1 O3 . 2_546 145.88(18) ?
O1 Te1 O3 . 2_546 63.11(17) ?
O1 Te1 O3 3_656 2_546 83.60(13) ?
O1 Te1 O3 4_666 2_546 128.74(14) ?
O3 Ge1 O3 . 3_667 180.000(2) ?
O3 Ge1 O1 . 2_556 92.4(2) ?
O3 Ge1 O1 3_667 2_556 87.6(2) ?
O3 Ge1 O1 . 4_666 87.6(2) ?
O3 Ge1 O1 3_667 4_666 92.4(2) ?
O1 Ge1 O1 2_556 4_666 180.0000(10) ?
O3 Ge1 O2 . 2_656 90.0(2) ?
O3 Ge1 O2 3_667 2_656 90.0(2) ?
O1 Ge1 O2 2_556 2_656 90.0(2) ?
O1 Ge1 O2 4_666 2_656 90.0(2) ?
O3 Ge1 O2 . 4_566 90.0(2) ?
O3 Ge1 O2 3_667 4_566 90.0(2) ?
O1 Ge1 O2 2_556 4_566 90.0(2) ?
O1 Ge1 O2 4_666 4_566 90.0(2) ?
O2 Ge1 O2 2_656 4_566 180.0000(10) ?
Ge1 O1 Te1 2_546 . 121.7(3) ?
Te1 O2 Ge1 . 2_646 116.7(2) ?
Ge1 O3 Te1 . . 115.5(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Te1 O3 . 1.873(5) y
Te1 O2 . 1.874(5) y
Te1 O1 . 1.903(5) y
Te1 O1 3_656 2.852(5) y
Te1 O1 4_666 2.877(5) y
Te1 O3 2_546 2.968(5) y
Ge1 O3 . 1.870(5) y
Ge1 O3 3_667 1.870(5) n
Ge1 O1 2_556 1.877(4) n
Ge1 O1 4_666 1.877(4) y
Ge1 O2 2_656 1.878(5) n
Ge1 O2 4_566 1.878(5) y
O1 Ge1 2_546 1.877(4) ?
O2 Ge1 2_646 1.878(5) ?
