#------------------------------------------------------------------------------
#$Date: 2012-09-11 12:26:43 +0300 (Tue, 11 Sep 2012) $
#$Revision: 66590 $
#$URL: file:///home/coder/svn-repositories/cod/hkl/2/30/03/2300365.hkl $
#------------------------------------------------------------------------------
#
# 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_2300365_Fobs
loop_
_publ_author_name
'Lignie, Adrien'
'Granier, Dominique'
'Armand, Pascale'
'Haines, Julien'
'Papet, Philippe'
_publ_section_title
;
 Modulation of quartz-like GeO~2~ structure by Si substitution: an X-ray
 diffraction study of Ge~1{-~<i>x</i>}Si<i>~x~</i>O~2~ (0 {\/leq} <i>x</i>
 < 0.2) flux-grown single crystals
;
_journal_issue                   2
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              272
_journal_page_last               278
_journal_volume                  45
_journal_year                    2012
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ge O2'
_chemical_formula_weight         104.59
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic        ?
_space_group_IT_number           152
_symmetry_cell_setting           ?
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2011-10-20 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   4.9890(3)
_cell_length_b                   4.9890(3)
_cell_length_c                   5.6527(3)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      36.9864
_cell_measurement_theta_min      3.6007
_cell_volume                     121.847(12)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    ?
_computing_publication_material  ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    ?
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_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  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2023
_diffrn_reflns_theta_full        37.04
_diffrn_reflns_theta_max         37.04
_diffrn_reflns_theta_min         4.72
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    18.330
_exptl_absorpt_correction_T_max  0.360
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro_Software_system,_Version_1.171.32.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    4.276
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             144
_exptl_crystal_size_max          0.1173
_exptl_crystal_size_mid          0.0816
_exptl_crystal_size_min          0.0794
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), 151 Friedel pairs'
_refine_ls_abs_structure_Flack   0.09(2)
_refine_ls_extinction_coef       0.226(6)
_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   1.153
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           full
_refine_ls_number_parameters     16
_refine_ls_number_reflns         416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0091
_refine_ls_R_factor_gt           0.0088
_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/[\s^2^(Fo^2^)+(0.0085P)^2^+0.0233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0211
_refine_ls_wR_factor_ref         0.0211
_reflns_d_resolution_high        0.6233
_reflns_number_gt                410
_reflns_number_total             416
_reflns_threshold_expression     >2\s(I)
_[local]_cod_data_source_file    ce5127GeO2sup7.hkl
_[local]_cod_data_source_block   GeO2
_[local]_cod_cif_authors_sg_H-M  P_31_2_1
#BEGIN Tags that were not found in dictionaries:
_shelx_title                     ' GeO2 in P3(1)21'
_shelx_refln_list_code           4
_shelx_f_calc_maximum            38.87
_shelx_f_squared_multiplier      1.000
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.45124(3) 0.0000 0.3333 0.00686(5) Uani 1 2 d S . .
O O 0.3974(2) 0.3022(2) 0.24285(14) 0.01203(16) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.00766(7) 0.00644(8) 0.00609(6) 0.00039(6) 0.00019(3) 0.00322(4)
O 0.0172(4) 0.0121(4) 0.0105(3) 0.0047(3) 0.0045(3) 0.0101(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O Ge1 O 107.80(6) . 5 ?
O Ge1 O 106.31(2) . 6_655 ?
O Ge1 O 112.97(5) 5 6_655 ?
O Ge1 O 112.97(5) . 2_655 ?
O Ge1 O 106.31(2) 5 2_655 ?
O Ge1 O 110.58(6) 6_655 2_655 ?
Ge1 O Ge1 130.11(6) . 3_664 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 O 1.7357(10) . ?
Ge1 O 1.7357(10) 5 ?
Ge1 O 1.7432(8) 6_655 ?
Ge1 O 1.7432(8) 2_655 ?
O Ge1 1.7432(8) 3_664 ?
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_calc
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_observed_status
0 1 0 30.15 30.10 180.00 o
-1 2 0 39.44 39.53 192.22 o
0 2 0 61.44 61.40 0.00 o
-1 3 0 20.70 20.94 119.42 o
0 3 0 1.98 2.06 0.00 o
-2 4 0 31.30 31.29 6.14 o
-1 4 0 44.55 44.56 240.44 o
0 4 0 20.60 20.53 0.00 o
-2 5 0 15.85 16.01 84.39 o
-1 5 0 21.39 21.52 107.24 o
0 5 0 7.75 7.76 0.00 o
-3 6 0 37.61 37.60 238.41 o
-2 6 0 15.91 15.90 26.30 o
-1 6 0 26.88 26.77 245.87 o
0 6 0 2.32 1.91 0.00 o
-3 7 0 6.18 6.02 88.10 o
-2 7 0 12.99 12.93 31.80 o
-1 7 0 10.78 10.83 122.53 o
0 7 0 15.19 15.28 0.00 o
-4 8 0 8.86 8.93 73.12 o
-3 8 0 18.18 18.19 233.44 o
-2 8 0 7.01 6.94 105.17 o
-1 1 1 76.78 78.27 0.00 o
0 1 1 40.98 41.21 120.00 o
-2 2 1 19.26 19.18 180.00 o
-1 2 1 34.87 35.08 215.25 o
0 2 1 11.01 11.72 120.00 o
-3 3 1 69.84 69.63 0.00 o
-2 3 1 29.16 29.01 159.07 o
-1 3 1 51.68 51.42 359.01 o
0 3 1 3.86 3.65 300.00 o
-4 4 1 10.35 10.81 180.00 o
-3 4 1 16.01 15.95 203.53 o
-2 4 1 28.74 28.89 149.21 o
-1 4 1 15.84 15.73 239.49 o
0 4 1 38.65 38.40 120.00 o
-5 5 1 28.30 28.22 0.00 o
-4 5 1 18.00 17.77 202.38 o
-3 5 1 38.28 38.32 353.99 o
-2 5 1 14.01 13.95 236.12 o
-1 5 1 25.95 26.06 358.83 o
0 5 1 12.82 13.02 300.00 o
-6 6 1 1.31 0.74 180.00 o
-5 6 1 11.16 11.13 133.67 o
-4 6 1 15.94 15.99 118.72 o
-3 6 1 4.01 3.95 248.20 o
-2 6 1 28.54 28.66 126.33 o
-1 6 1 13.14 13.21 262.49 o
0 6 1 27.50 27.76 120.00 o
-7 7 1 11.41 11.41 0.00 o
-6 7 1 20.08 19.85 246.10 o
-5 7 1 17.11 17.28 3.98 o
-4 7 1 19.84 19.75 237.58 o
-3 7 1 15.28 15.47 1.89 o
-2 7 1 11.76 11.76 252.76 o
-1 7 1 9.12 9.00 334.52 o
0 7 1 2.77 2.81 300.00 o
-6 8 1 7.63 7.59 91.22 o
-5 8 1 4.45 4.64 101.05 o
-4 8 1 12.02 12.05 112.93 o
-3 8 1 5.16 5.16 349.69 o
-2 8 1 15.77 16.22 113.33 o
-1 1 2 5.94 6.96 0.00 o
0 1 2 59.87 59.82 240.00 o
-2 2 2 32.66 32.14 0.00 o
-1 2 2 41.38 41.32 107.14 o
0 2 2 32.66 32.73 60.00 o
-3 3 2 8.17 8.15 0.00 o
-2 3 2 54.71 54.82 247.20 o
-1 3 2 15.62 15.65 33.15 o
0 3 2 58.85 58.69 240.00 o
-4 4 2 33.15 32.94 0.00 o
-3 4 2 29.95 29.93 121.42 o
-2 4 2 21.29 21.19 16.91 o
-1 4 2 16.54 16.78 79.73 o
0 4 2 11.16 10.90 60.00 o
-5 5 2 4.04 3.86 180.00 o
-4 5 2 21.53 21.37 227.12 o
-3 5 2 11.07 11.02 107.85 o
-2 5 2 31.04 31.11 240.65 o
-1 5 2 19.25 19.17 90.03 o
0 5 2 34.35 34.18 240.00 o
-6 6 2 28.50 28.30 0.00 o
-5 6 2 12.25 12.22 151.92 o
-4 6 2 26.02 26.09 353.76 o
-3 6 2 1.60 1.18 5.23 o
-2 6 2 11.20 11.23 17.25 o
-1 6 2 13.47 13.53 3.30 o
0 6 2 1.94 2.03 60.00 o
-7 7 2 4.80 4.70 180.00 o
-6 7 2 9.34 9.29 204.89 o
-5 7 2 14.34 14.34 140.25 o
-4 7 2 11.85 11.77 242.55 o
-3 7 2 20.58 20.57 125.65 o
-2 7 2 18.24 18.30 238.91 o
-1 7 2 16.68 16.82 107.07 o
0 7 2 14.29 14.44 240.00 o
-5 8 2 4.22 4.10 221.45 o
-4 8 2 14.77 14.74 3.16 o
-3 8 2 6.67 6.64 303.23 o
0 0 3 65.22 64.47 0.00 o
-1 1 3 27.04 26.70 180.00 o
0 1 3 12.42 12.53 180.00 o
-2 2 3 43.74 43.80 0.00 o
-1 2 3 32.97 32.95 230.58 o
0 2 3 59.07 59.45 0.00 o
-3 3 3 1.98 1.78 180.00 o
-2 3 3 14.24 14.15 138.54 o
-1 3 3 32.39 32.32 120.43 o
0 3 3 6.15 6.07 180.00 o
-4 4 3 15.68 15.55 0.00 o
-3 4 3 34.43 34.34 245.80 o
-2 4 3 29.62 29.79 7.07 o
-1 4 3 33.69 33.80 230.26 o
0 4 3 30.15 30.07 0.00 o
-5 5 3 10.10 10.13 0.00 o
-4 5 3 23.40 23.37 113.50 o
-3 5 3 13.80 13.78 64.18 o
-2 5 3 5.25 5.12 100.02 o
-1 5 3 17.80 17.71 110.99 o
0 5 3 10.79 10.65 0.00 o
-6 6 3 8.72 8.55 0.00 o
-5 6 3 25.24 25.59 244.56 o
-4 6 3 10.58 10.39 37.27 o
-3 6 3 29.27 29.53 240.40 o
-2 6 3 9.78 9.70 31.25 o
-1 6 3 22.04 22.09 233.79 o
0 6 3 0.86 0.67 0.00 o
-6 7 3 13.10 13.29 118.67 o
-5 7 3 8.66 8.59 6.62 o
-4 7 3 8.78 8.75 77.61 o
-3 7 3 8.32 8.34 70.67 o
-2 7 3 12.58 12.45 22.59 o
-1 7 3 10.16 10.27 110.91 o
-4 8 3 9.34 8.78 92.04 o
-1 1 4 46.22 45.77 0.00 o
0 1 4 42.14 42.35 120.00 o
-2 2 4 4.66 3.88 180.00 o
-1 2 4 32.45 32.53 236.34 o
0 2 4 17.59 17.72 120.00 o
-3 3 4 38.04 37.88 0.00 o
-2 3 4 14.00 14.12 177.04 o
-1 3 4 36.06 35.90 354.33 o
0 3 4 3.15 2.81 120.00 o
-4 4 4 14.96 14.70 180.00 o
-3 4 4 12.21 12.06 186.86 o
-2 4 4 23.96 24.12 125.03 o
-1 4 4 17.63 17.39 230.56 o
0 4 4 26.51 26.35 120.00 o
-5 5 4 25.78 25.51 0.00 o
-4 5 4 15.15 15.22 235.56 o
-3 5 4 33.54 33.68 1.20 o
-2 5 4 14.38 14.48 233.29 o
-1 5 4 22.98 23.06 356.48 o
0 5 4 8.59 8.66 300.00 o
-6 6 4 3.87 3.62 180.00 o
-5 6 4 7.71 7.72 149.45 o
-4 6 4 15.22 15.14 123.65 o
-3 6 4 7.19 7.08 222.37 o
-2 6 4 21.27 21.27 128.86 o
-1 6 4 5.17 4.99 278.55 o
0 6 4 20.59 20.41 120.00 o
-6 7 4 14.71 14.78 241.66 o
-5 7 4 14.95 15.23 11.91 o
-4 7 4 14.85 15.00 227.71 o
-3 7 4 16.54 16.68 355.55 o
-2 7 4 9.89 9.93 238.52 o
-1 7 4 6.57 6.90 330.21 o
-1 1 5 25.27 25.31 0.00 o
0 1 5 35.61 35.61 240.00 o
-2 2 5 23.35 23.25 0.00 o
-1 2 5 30.29 30.28 118.98 o
0 2 5 9.68 9.58 60.00 o
-3 3 5 6.27 6.28 0.00 o
-2 3 5 33.94 33.59 239.52 o
-1 3 5 7.38 7.42 60.01 o
0 3 5 30.45 30.30 240.00 o
-4 4 5 22.27 21.99 0.00 o
-3 4 5 23.00 22.69 115.26 o
-2 4 5 19.95 20.05 358.42 o
-1 4 5 11.61 11.52 67.11 o
0 4 5 13.08 13.04 60.00 o
-5 5 5 2.33 2.07 180.00 o
-4 5 5 19.16 19.28 231.16 o
-3 5 5 10.98 10.87 106.35 o
-2 5 5 27.17 27.14 245.55 o
-1 5 5 14.98 15.05 119.45 o
0 5 5 26.19 26.27 240.00 o
-6 6 5 18.12 18.85 0.00 o
-5 6 5 5.30 5.28 174.90 o
-4 6 5 17.66 17.61 359.27 o
-3 6 5 4.88 4.78 88.38 o
-2 6 5 10.95 10.89 14.32 o
-1 6 5 9.12 8.94 14.33 o
0 6 5 5.21 4.80 60.00 o
-5 7 5 9.96 10.36 122.58 o
-4 7 5 12.80 12.69 232.91 o
-3 7 5 14.04 14.07 113.93 o
-2 7 5 15.31 14.85 248.76 o
0 0 6 30.46 30.70 0.00 o
-1 1 6 10.27 10.11 180.00 o
0 1 6 11.76 11.84 180.00 o
-2 2 6 33.78 33.85 0.00 o
-1 2 6 23.22 23.27 242.92 o
0 2 6 31.32 31.17 0.00 o
-3 3 6 4.95 4.86 180.00 o
-2 3 6 18.30 18.20 125.77 o
-1 3 6 16.01 15.96 128.79 o
0 3 6 4.52 4.24 180.00 o
-4 4 6 19.37 19.25 0.00 o
-3 4 6 20.94 20.91 233.75 o
-2 4 6 21.87 21.68 6.51 o
-1 4 6 21.81 21.73 240.68 o
0 4 6 17.15 17.25 0.00 o
-5 5 6 10.34 10.23 0.00 o
-4 5 6 14.38 14.52 117.86 o
-3 5 6 4.19 3.80 66.65 o
-2 5 6 4.78 4.68 57.80 o
-1 5 6 16.34 16.41 116.43 o
0 5 6 8.41 8.36 0.00 o
-5 6 6 17.53 17.39 233.87 o
-4 6 6 5.33 5.13 42.97 o
-3 6 6 18.75 18.80 241.13 o
-2 6 6 6.09 6.00 45.97 o
-1 6 6 17.70 17.61 236.46 o
-1 1 7 25.29 25.32 0.00 o
0 1 7 13.24 13.30 120.00 o
-2 2 7 9.42 9.34 180.00 o
-1 2 7 21.18 21.45 236.86 o
0 2 7 16.50 16.34 120.00 o
-3 3 7 23.16 23.02 0.00 o
-2 3 7 5.85 5.69 167.12 o
-1 3 7 25.11 24.99 3.65 o
0 3 7 5.50 5.37 120.00 o
-4 4 7 7.84 7.73 180.00 o
-3 4 7 8.56 8.52 190.18 o
-2 4 7 13.09 13.09 116.66 o
-1 4 7 17.59 17.70 237.49 o
0 4 7 16.53 16.43 120.00 o
-5 5 7 20.93 21.14 0.00 o
-4 5 7 11.92 11.89 232.95 o
-3 5 7 18.59 18.67 5.39 o
-2 5 7 8.23 8.31 230.59 o
-1 5 7 13.59 13.47 348.92 o
0 5 7 1.27 1.18 300.00 o
-1 1 8 18.45 18.67 0.00 o
0 1 8 23.27 23.29 240.00 o
-2 2 8 7.43 7.54 0.00 o
-1 2 8 14.73 14.73 112.83 o
0 2 8 3.42 3.36 60.00 o
-3 3 8 0.29 0.11 180.00 o
-2 3 8 18.54 18.71 234.09 o
-1 3 8 8.82 8.90 46.40 o
0 3 8 22.09 22.01 240.00 o
-4 4 8 15.86 16.26 0.00 o
-3 4 8 8.07 7.98 114.48 o
-2 4 8 13.78 13.58 13.09 o
-1 4 8 6.23 6.08 73.77 o
0 4 8 7.26 6.80 60.00 o
0 0 9 24.73 25.14 0.00 o
-1 1 9 5.26 5.18 180.00 o
0 1 9 8.54 8.47 180.00 o
-2 2 9 19.66 20.21 0.00 o
-1 2 9 11.27 11.25 219.31 o
0 2 9 16.21 16.29 0.00 o