#------------------------------------------------------------------------------
#$Date: 2016-04-03 07:30:20 +0300 (Sun, 03 Apr 2016) $
#$Revision: 181326 $
#$URL: file:///home/coder/svn-repositories/cod/hkl/2/30/03/2300368.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_2300368_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            'Ge0.90 O2 Si0.10'
_chemical_formula_weight         99.94
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic        ?
_space_group_IT_number           154
_symmetry_cell_setting           ?
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_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                   4.97517(17)
_cell_length_b                   4.97517(17)
_cell_length_c                   5.60565(19)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.4279
_cell_measurement_theta_min      3.6246
_cell_volume                     120.163(7)
_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 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2860
_diffrn_reflns_theta_full        32.45
_diffrn_reflns_theta_max         32.45
_diffrn_reflns_theta_min         4.73
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    16.741
_exptl_absorpt_correction_T_max  0.365
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro_Software_system,_Version_1.171.32.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    4.143
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             138
_exptl_crystal_size_max          0.3806
_exptl_crystal_size_mid          0.1810
_exptl_crystal_size_min          0.0904
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), 91 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.07(4)
_refine_ls_extinction_coef       0.275(11)
_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   1.194
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           full
_refine_ls_number_parameters     16
_refine_ls_number_reflns         282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0130
_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^)+(0.0095P)^2^+0.1155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0297
_refine_ls_wR_factor_ref         0.0299
_reflns_d_resolution_high        0.6623
_reflns_number_gt                274
_reflns_number_total             282
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ce5127Ge0.8961Si0.1039O2sup4.hkl
_cod_data_source_block           Ge0.8961Si0.1039O2
_cod_original_sg_symbol_H-M      P_32_2_1
#BEGIN Tags that were not found in dictionaries:
_shelx_title                     ' cristal-abs in P3(2)21'
_shelx_refln_list_code           4
_shelx_f_calc_maximum            73.86
_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+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'
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 -0.45280(7) 0.0000 0.6667 0.00885(13) Uani 0.90 2 d SP . .
Si1 Si -0.45280(7) 0.0000 0.6667 0.00885(13) Uani 0.10 2 d SP . .
O O -0.3997(4) -0.2992(4) 0.7599(3) 0.0145(3) 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 0.00968(16) 0.00879(19) 0.00778(16) 0.00056(13) 0.00028(7) 0.00439(10)
Si1 0.00968(16) 0.00879(19) 0.00778(16) 0.00056(13) 0.00028(7) 0.00439(10)
O 0.0183(9) 0.0147(8) 0.0128(6) 0.0051(6) 0.0037(6) 0.0102(8)
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'
Si Si 0.0817 0.0704 '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 108.12(12) . 5_556 ?
O Ge1 O 106.63(4) . 6_456 ?
O Ge1 O 112.60(10) 5_556 6_456 ?
O Ge1 O 112.60(10) . 2_454 ?
O Ge1 O 106.63(4) 5_556 2_454 ?
O Ge1 O 110.34(12) 6_456 2_454 ?
Ge1 O Si1 131.54(11) . 3_445 ?
Ge1 O Ge1 131.54(11) . 3_445 ?
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 1.718(2) . ?
Ge1 O 1.718(2) 5_556 ?
Ge1 O 1.7226(15) 6_456 ?
Ge1 O 1.7226(15) 2_454 ?
O Si1 1.7226(15) 3_445 ?
O Ge1 1.7226(15) 3_445 ?
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 0 828.04 856.94 6.11 o
1 1 0 1230.65 1215.57 18.77 o
-1 2 0 1442.18 1528.01 13.86 o
0 2 0 3226.30 3200.46 26.54 o
1 2 0 329.65 317.97 4.57 o
2 2 0 882.19 838.35 12.93 o
-1 3 0 346.61 339.73 3.43 o
0 3 0 0.24 1.14 0.77 o
1 3 0 1650.05 1602.18 16.11 o
2 3 0 222.87 209.47 5.15 o
3 3 0 1092.13 1001.58 18.72 o
-2 4 0 876.06 908.71 11.13 o
-1 4 0 1631.56 1625.40 8.40 o
0 4 0 374.85 378.22 4.63 o
1 4 0 342.02 334.22 4.98 o
2 4 0 216.87 209.56 5.79 o
3 4 0 33.34 35.56 4.77 o
-2 5 0 215.12 218.38 3.61 o
-1 5 0 359.32 360.23 5.16 o
0 5 0 33.57 32.54 2.14 o
1 5 0 546.67 544.17 14.54 o
2 5 0 119.31 109.96 14.03 o
-3 6 0 1105.83 1132.05 24.32 o
-2 6 0 225.63 239.37 5.77 o
-1 6 0 523.03 517.77 7.51 o
0 6 0 5.67 2.20 3.21 o
-3 7 0 27.60 29.32 3.39 o
-2 7 0 103.77 109.97 5.39 o
-1 1 1 5455.45 5395.21 68.94 o
0 1 1 1575.93 1576.73 18.93 o
1 1 1 976.77 938.26 9.98 o
-3 2 1 758.68 764.85 6.77 o
-2 2 1 309.35 318.71 4.13 o
-1 2 1 1084.47 1078.12 10.70 o
0 2 1 73.71 56.06 1.07 o
1 2 1 2202.98 2156.63 15.92 o
2 2 1 711.53 685.84 6.67 o
-5 3 1 1183.07 1156.39 15.83 o
-4 3 1 233.77 235.51 3.98 o
-3 3 1 4112.47 4149.81 38.22 o
-2 3 1 769.82 776.77 8.64 o
-1 3 1 2227.77 2244.38 13.50 o
0 3 1 8.85 10.03 0.72 o
1 3 1 216.86 215.37 2.97 o
2 3 1 136.71 129.60 3.63 o
3 3 1 21.58 17.80 2.67 o
-7 4 1 283.40 260.62 8.47 o
-6 4 1 195.74 187.38 5.28 o
-5 4 1 215.59 210.91 4.30 o
-4 4 1 105.64 102.02 2.56 o
-3 4 1 217.77 216.84 3.46 o
-2 4 1 643.47 633.95 4.90 o
-1 4 1 213.55 214.63 3.12 o
0 4 1 1194.47 1193.53 7.79 o
1 4 1 582.60 583.90 9.07 o
2 4 1 609.65 601.03 11.59 o
3 4 1 201.18 185.98 6.93 o
-7 5 1 249.39 223.10 11.84 o
-6 5 1 80.39 71.73 4.04 o
-5 5 1 605.82 617.51 9.47 o
-4 5 1 249.87 249.74 4.87 o
-3 5 1 1228.33 1267.97 16.05 o
-2 5 1 131.10 133.12 3.48 o
-1 5 1 566.53 573.24 6.75 o
0 5 1 118.16 117.46 3.44 o
1 5 1 150.71 142.60 4.46 o
2 5 1 87.52 90.14 8.13 o
-6 6 1 2.66 7.55 3.58 o
-5 6 1 80.08 82.83 3.97 o
-4 6 1 212.29 209.25 5.24 o
-3 6 1 18.67 19.91 2.22 o
-2 6 1 588.24 600.76 8.77 o
-1 6 1 159.36 156.02 4.56 o
0 6 1 578.39 580.04 8.67 o
-5 7 1 250.46 267.90 11.02 o
-4 7 1 285.36 294.39 7.12 o
-3 7 1 194.33 197.34 6.53 o
-2 7 1 83.07 87.46 7.83 o
-1 1 2 36.11 19.13 0.66 o
0 1 2 3022.88 2882.92 22.99 o
1 1 2 1513.50 1553.42 12.32 o
-3 2 2 2556.67 2562.42 13.59 o
-2 2 2 900.77 941.75 5.92 o
-1 2 2 1545.28 1575.66 14.45 o
0 2 2 891.72 902.75 5.69 o
1 2 2 202.69 200.80 2.78 o
2 2 2 333.94 336.49 4.02 o
-5 3 2 73.31 76.49 3.15 o
-4 3 2 808.72 796.92 8.86 o
-3 3 2 83.42 86.06 1.69 o
-2 3 2 2475.30 2456.80 21.64 o
-1 3 2 221.29 224.21 2.43 o
0 3 2 2863.53 2862.59 27.25 o
1 3 2 253.26 251.63 3.41 o
2 3 2 767.85 763.24 8.86 o
3 3 2 0.43 6.42 2.74 o
-7 4 2 120.68 126.67 21.08 o
-6 4 2 501.28 506.59 8.45 o
-5 4 2 359.09 363.86 6.45 o
-4 4 2 852.89 878.68 9.11 o
-3 4 2 789.20 805.98 6.59 o
-2 4 2 320.58 326.47 3.86 o
-1 4 2 251.47 248.49 3.78 o
0 4 2 97.83 97.61 2.83 o
1 4 2 262.95 258.17 4.87 o
2 4 2 106.05 102.09 4.00 o
3 4 2 302.13 324.31 14.85 o
-6 5 2 121.64 119.71 4.39 o
-5 5 2 9.87 12.07 2.59 o
-4 5 2 380.96 392.80 5.69 o
-3 5 2 75.93 77.01 2.86 o
-2 5 2 761.53 782.40 8.50 o
-1 5 2 285.00 291.88 5.61 o
0 5 2 975.95 968.28 9.50 o
1 5 2 122.46 120.58 4.01 o
2 5 2 262.41 263.95 29.39 o
-6 6 2 564.73 586.14 13.69 o
-5 6 2 120.62 126.42 5.41 o
-4 6 2 537.88 545.16 9.73 o
-3 6 2 2.78 3.77 2.30 o
-2 6 2 92.49 88.14 3.59 o
-1 6 2 132.78 134.11 4.50 o
0 6 2 9.20 10.98 3.60 o
-4 7 2 116.15 132.82 14.11 o
-2 7 2 276.64 275.83 13.01 o
0 0 3 3383.31 3429.64 23.57 o
-1 1 3 635.71 649.97 4.38 o
0 1 3 120.16 119.31 1.59 o
1 1 3 908.54 916.27 6.91 o
-3 2 3 177.90 183.00 2.53 o
-2 2 3 1616.14 1597.39 9.09 o
-1 2 3 885.93 887.58 6.30 o
0 2 3 3095.27 3046.29 25.29 o
1 2 3 892.25 872.52 6.20 o
2 2 3 762.89 765.06 6.62 o
-5 3 3 128.48 124.23 4.24 o
-4 3 3 927.21 933.32 7.69 o
-3 3 3 3.08 3.85 1.16 o
-2 3 3 152.56 157.59 2.59 o
-1 3 3 908.65 914.78 8.08 o
0 3 3 46.42 47.01 1.68 o
1 3 3 848.53 846.83 6.99 o
2 3 3 24.34 22.17 2.23 o
3 3 3 647.83 645.57 11.68 o
-7 4 3 59.53 52.39 11.12 o
-6 4 3 85.50 79.02 4.49 o
-5 4 3 461.08 464.95 7.23 o
-4 4 3 226.01 229.21 4.79 o
-3 4 3 881.32 902.34 8.90 o
-2 4 3 761.84 775.11 6.39 o
-1 4 3 905.17 907.20 8.13 o
0 4 3 780.81 758.59 7.11 o
1 4 3 237.23 232.30 5.11 o
2 4 3 80.67 75.14 4.53 o
-6 5 3 492.53 511.86 10.66 o
-5 5 3 70.84 70.33 3.52 o
-4 5 3 458.64 460.53 9.25 o
-3 5 3 139.54 144.61 3.47 o
-2 5 3 17.44 15.38 2.06 o
-1 5 3 239.24 238.50 5.02 o
0 5 3 65.11 67.07 3.19 o
1 5 3 364.66 351.72 9.10 o
-5 6 3 475.92 499.41 9.25 o
-4 6 3 83.66 90.62 3.71 o
-3 6 3 642.82 670.82 10.59 o
-2 6 3 79.07 78.67 3.65 o
-1 6 3 388.85 378.34 7.44 o
-3 7 3 57.78 48.83 12.36 o
-1 1 4 1693.76 1688.44 7.82 o
0 1 4 1553.04 1543.12 9.50 o
1 1 4 933.91 939.44 5.87 o
-3 2 4 163.50 159.77 3.37 o
-2 2 4 11.12 13.86 1.02 o
-1 2 4 899.46 895.08 6.54 o
0 2 4 251.24 249.26 3.04 o
1 2 4 1041.55 1045.38 6.55 o
2 2 4 451.73 451.30 6.47 o
-5 3 4 921.75 937.84 12.71 o
-4 3 4 116.04 116.73 3.29 o
-3 3 4 1103.05 1131.99 9.87 o
-2 3 4 147.28 147.20 2.63 o
-1 3 4 1085.14 1115.52 8.08 o
0 3 4 10.35 9.42 1.49 o
1 3 4 258.75 265.53 4.29 o
2 3 4 156.73 157.81 4.94 o
3 3 4 50.13 51.83 4.53 o
-6 4 4 171.62 160.63 6.48 o
-5 4 4 167.47 170.67 5.10 o
-4 4 4 180.02 176.97 4.85 o
-3 4 4 123.03 125.65 3.04 o
-2 4 4 475.33 474.52 5.89 o
-1 4 4 275.00 278.67 4.72 o
0 4 4 477.01 472.40 6.26 o
1 4 4 440.42 427.16 7.06 o
2 4 4 339.92 326.72 8.08 o
-6 5 4 52.90 53.14 8.61 o
-5 5 4 516.65 533.31 8.77 o
-4 5 4 145.12 145.41 4.73 o
-3 5 4 913.97 944.54 11.06 o
-2 5 4 156.93 155.05 3.90 o
-1 5 4 433.14 426.49 6.74 o
0 5 4 48.05 53.41 4.13 o
1 5 4 18.41 37.78 8.46 o
-5 6 4 43.01 50.19 13.82 o
-4 6 4 175.27 174.71 5.83 o
-3 6 4 48.62 41.00 3.61 o
-2 6 4 313.93 312.28 8.22 o
-1 6 4 16.45 3.88 12.64 o
-1 1 5 584.08 583.63 5.61 o
0 1 5 1015.43 1024.91 9.40 o
1 1 5 785.36 781.23 6.42 o
-3 2 5 899.97 902.05 7.70 o
-2 2 5 417.47 419.12 5.41 o
-1 2 5 746.89 755.34 6.91 o
0 2 5 63.34 61.57 1.85 o
1 2 5 48.97 47.00 2.02 o
2 2 5 300.11 287.75 5.19 o
-5 3 5 84.16 82.52 3.41 o
-4 3 5 402.07 409.54 5.84 o
-3 3 5 35.88 33.66 1.91 o
-2 3 5 905.19 919.15 7.50 o
-1 3 5 39.96 38.48 1.81 o
0 3 5 700.46 710.97 7.24 o
1 3 5 101.67 100.36 3.49 o
2 3 5 606.96 613.95 9.64 o
3 3 5 21.36 33.08 14.56 o
-5 4 5 301.47 303.72 7.74 o
-4 4 5 328.54 328.66 6.71 o
-3 4 5 410.28 412.17 6.44 o
-2 4 5 334.66 335.45 5.40 o
-1 4 5 109.11 110.45 3.39 o
0 4 5 138.38 132.24 3.70 o
1 4 5 160.61 159.09 5.06 o
-5 5 5 2.84 1.35 5.59 o
-4 5 5 304.27 303.70 6.65 o
-3 5 5 88.63 86.71 4.04 o
-2 5 5 580.14 585.26 9.41 o
-1 5 5 135.44 130.80 4.24 o
0 5 5 529.87 498.37 18.33 o
0 0 6 760.54 771.77 12.76 o
-1 1 6 74.95 75.59 2.92 o
0 1 6 122.44 117.80 3.29 o
1 1 6 435.29 421.75 5.36 o
-3 2 6 276.60 259.78 4.78 o
-2 2 6 958.57 958.65 8.47 o
-1 2 6 390.51 385.11 5.48 o
0 2 6 764.17 770.92 7.76 o
1 2 6 190.97 192.66 4.09 o
2 2 6 373.94 368.60 5.83 o
-5 3 6 8.95 14.04 8.08 o
-4 3 6 307.17 305.82 7.57 o
-3 3 6 21.42 19.83 2.57 o
-2 3 6 277.41 279.93 4.58 o
-1 3 6 182.22 183.43 4.32 o
0 3 6 13.68 13.10 2.02 o
1 3 6 347.67 340.35 6.23 o
2 3 6 12.61 6.76 8.40 o
-4 4 6 309.85 302.71 7.57 o
-3 4 6 326.17 343.09 7.10 o
-2 4 6 376.74 378.37 7.54 o
-1 4 6 339.86 339.37 5.65 o
0 4 6 230.18 228.27 5.23 o
-3 5 6 10.31 17.76 9.52 o
-2 5 6 16.98 14.50 5.98 o
-1 1 7 494.77 470.13 8.46 o
0 1 7 125.34 120.37 3.76 o
1 1 7 372.09 377.03 6.23 o
-3 2 7 25.70 31.10 3.06 o
-2 2 7 68.71 67.23 3.57 o
-1 2 7 356.32 350.76 6.47 o
0 2 7 203.70 206.02 4.83 o
1 2 7 489.88 488.36 7.79 o
-4 3 7 58.46 58.25 11.73 o
-3 3 7 414.03 427.07 9.80 o
-2 3 7 26.86 24.82 3.30 o
-1 3 7 476.17 474.44 7.82 o
0 3 7 26.29 28.82 3.48 o
-3 4 7 62.68 64.30 10.48 o
-1 4 7 247.12 276.18 13.68 o
-1 1 8 262.12 260.39 9.68 o
0 1 8 417.32 404.89 12.01 o
-1 2 8 157.43 178.59 16.30 o