#------------------------------------------------------------------------------
#$Date: 2012-09-11 12:26:43 +0300 (Tue, 11 Sep 2012) $
#$Revision: 66590 $
#$URL: file:///home/coder/svn-repositories/cod/hkl/2/30/03/2300369.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_2300369_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            'Ge0.83 O2 Si0.17'
_chemical_formula_weight         96.83
_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_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                   4.9707(3)
_cell_length_b                   4.9707(3)
_cell_length_c                   5.5873(3)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      32.275
_cell_measurement_theta_min      3.6334
_cell_volume                     119.555(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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0113
_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       -7
_diffrn_reflns_number            2176
_diffrn_reflns_theta_full        32.38
_diffrn_reflns_theta_max         32.38
_diffrn_reflns_theta_min         4.74
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    15.590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46056
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro_Software_system,_Version_1.171.32.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    4.035
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ?
_exptl_crystal_F_000             135
_exptl_crystal_size_max          0.1754
_exptl_crystal_size_mid          0.1616
_exptl_crystal_size_min          0.1028
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), 94 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_coef       0.031(3)
_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   1.220
_refine_ls_hydrogen_treatment    .
_refine_ls_matrix_type           full
_refine_ls_number_parameters     16
_refine_ls_number_reflns         279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0101
_refine_ls_R_factor_gt           0.0100
_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^)+(0.0064P)^2^+0.0732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0236
_refine_ls_wR_factor_ref         0.0236
_reflns_d_resolution_high        0.6636
_reflns_number_gt                277
_reflns_number_total             279
_reflns_threshold_expression     >2\s(I)
_[local]_cod_data_source_file    ce5127Ge0.8257Si0.1743O2sup3.hkl
_[local]_cod_data_source_block   Ge0.8257Si0.1743O2
_[local]_cod_cif_authors_sg_H-M  P_31_2_1
#BEGIN Tags that were not found in dictionaries:
_shelx_title                     ' R3-amb-abs in P3(1)21'
_shelx_refln_list_code           4
_shelx_f_calc_maximum            71.28
_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 0.54634(6) 0.0000 0.3333 0.00800(8) Uani 0.83 2 d SP . .
Si1 Si 0.54634(6) 0.0000 0.3333 0.00800(8) Uani 0.17 2 d SP . .
O O 0.5998(3) 0.7041(3) 0.2382(2) 0.0145(2) 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 0.00867(11) 0.00796(14) 0.00714(11) -0.00057(10) -0.00029(5) 0.00398(7)
Si1 0.00867(11) 0.00796(14) 0.00714(11) -0.00057(10) -0.00029(5) 0.00398(7)
O 0.0180(6) 0.0147(6) 0.0133(5) -0.0047(4) -0.0030(5) 0.0101(6)
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 108.08(9) 5_665 1_545 ?
O Ge1 O 112.57(7) 5_665 6_655 ?
O Ge1 O 106.91(3) 1_545 6_655 ?
O Ge1 O 106.91(3) 5_665 2_655 ?
O Ge1 O 112.57(7) 1_545 2_655 ?
O Ge1 O 109.87(9) 6_655 2_655 ?
Si1 O Si1 132.49(9) 1_565 3_664 ?
Ge1 O Si1 132.49(9) 1_565 3_664 ?
Si1 O Ge1 132.49(9) 1_565 3_664 ?
Ge1 O Ge1 132.49(9) 1_565 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 1.7053(15) 5_665 ?
Ge1 O 1.7053(15) 1_545 ?
Ge1 O 1.7158(12) 6_655 ?
Ge1 O 1.7158(12) 2_655 ?
O Si1 1.7053(15) 1_565 ?
O Ge1 1.7053(15) 1_565 ?
O Si1 1.7158(12) 3_664 ?
O Ge1 1.7158(12) 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 0 769.29 771.69 7.95 o
1 1 0 1125.94 1111.72 3.57 o
-1 2 0 1315.73 1316.48 20.62 o
0 2 0 2906.08 2868.90 18.28 o
1 2 0 286.85 276.17 2.35 o
2 2 0 869.35 841.28 10.10 o
-1 3 0 304.64 300.15 4.01 o
0 3 0 0.57 2.42 0.42 o
1 3 0 1551.30 1529.72 8.49 o
2 3 0 219.30 218.13 2.62 o
3 3 0 1033.24 1022.05 9.19 o
-2 4 0 859.07 847.03 8.33 o
-1 4 0 1531.39 1535.46 17.11 o
0 4 0 368.99 370.75 3.19 o
1 4 0 308.78 311.90 4.22 o
2 4 0 224.87 227.16 4.01 o
3 4 0 33.51 33.60 2.35 o
-2 5 0 211.82 208.59 2.99 o
-1 5 0 324.58 317.04 3.74 o
0 5 0 25.59 28.35 1.38 o
1 5 0 514.95 515.48 5.69 o
2 5 0 110.93 108.91 6.66 o
-3 6 0 1049.04 1078.13 11.67 o
-2 6 0 233.37 235.51 4.08 o
-1 6 0 494.73 480.88 4.73 o
0 6 0 7.18 6.49 1.86 o
-3 7 0 27.87 27.05 2.31 o
-2 7 0 97.61 98.50 4.28 o
-1 1 1 1500.94 1528.59 10.29 o
0 1 1 5080.94 5086.28 11.65 o
1 1 1 861.98 825.62 6.99 o
-3 2 1 2011.41 1978.46 8.81 o
-2 2 1 46.36 35.82 0.76 o
-1 2 1 962.59 938.30 5.69 o
0 2 1 281.83 288.02 3.26 o
1 2 1 738.45 748.99 4.32 o
2 2 1 660.94 642.75 7.77 o
-5 3 1 117.79 114.37 1.84 o
-4 3 1 209.52 209.32 3.61 o
-3 3 1 8.47 9.05 0.63 o
-2 3 1 2037.07 2035.61 9.10 o
-1 3 1 747.82 770.02 4.61 o
0 3 1 3816.80 3743.95 22.23 o
1 3 1 228.67 230.54 2.77 o
2 3 1 1124.49 1104.70 7.28 o
3 3 1 27.06 28.34 1.81 o
-7 4 1 207.32 202.54 4.62 o
-6 4 1 557.99 563.10 6.52 o
-5 4 1 573.69 568.20 4.09 o
-4 4 1 1128.47 1114.42 9.12 o
-3 4 1 206.99 208.75 1.79 o
-2 4 1 600.11 594.25 7.12 o
-1 4 1 211.08 211.40 2.18 o
0 4 1 101.34 104.09 1.59 o
1 4 1 195.75 201.23 2.71 o
2 4 1 191.87 188.23 3.32 o
3 4 1 275.46 273.84 9.87 o
-7 5 1 76.57 73.98 6.75 o
-6 5 1 161.12 161.90 2.81 o
-5 5 1 100.38 101.59 2.07 o
-4 5 1 560.03 560.32 4.00 o
-3 5 1 112.27 113.95 2.28 o
-2 5 1 1163.31 1136.45 17.73 o
-1 5 1 224.35 232.66 2.74 o
0 5 1 560.42 564.15 9.56 o
1 5 1 71.66 71.28 2.44 o
2 5 1 266.58 260.05 12.81 o
-6 6 1 559.08 552.58 9.58 o
-5 6 1 169.48 170.19 4.23 o
-4 6 1 541.07 545.21 7.36 o
-3 6 1 24.80 27.39 1.89 o
-2 6 1 209.31 210.45 3.31 o
-1 6 1 71.73 70.54 2.24 o
0 6 1 5.37 4.78 1.67 o
-5 7 1 72.09 76.83 5.28 o
-4 7 1 200.07 192.68 5.43 o
-3 7 1 277.92 282.85 4.91 o
-2 7 1 265.72 258.61 6.32 o
-1 1 2 2733.45 2774.00 12.96 o
0 1 2 26.23 13.43 0.56 o
1 1 2 1442.37 1467.84 6.69 o
-3 2 2 194.71 185.58 2.26 o
-2 2 2 805.20 822.15 6.09 o
-1 2 2 1470.25 1499.03 9.74 o
0 2 2 841.39 859.70 9.35 o
1 2 2 2341.29 2360.74 18.00 o
2 2 2 283.74 285.00 2.57 o
-5 3 2 714.42 721.69 6.72 o
-4 3 2 245.04 243.11 2.24 o
-3 3 2 2636.74 2621.95 18.37 o
-2 3 2 214.30 216.85 3.24 o
-1 3 2 2271.77 2254.30 17.18 o
0 3 2 98.97 98.77 1.58 o
1 3 2 792.18 790.48 4.73 o
2 3 2 60.45 63.92 1.77 o
3 3 2 0.67 0.85 1.51 o
-6 4 2 107.21 107.02 2.37 o
-5 4 2 244.65 244.30 2.88 o
-4 4 2 89.36 91.09 2.39 o
-3 4 2 246.82 247.19 2.38 o
-2 4 2 272.78 276.59 2.92 o
-1 4 2 771.57 768.19 8.01 o
0 4 2 794.59 786.11 9.34 o
1 4 2 343.25 358.17 5.45 o
2 4 2 484.77 473.38 6.79 o
3 4 2 130.75 119.18 8.72 o
-6 5 2 112.55 117.06 2.55 o
-5 5 2 975.44 991.23 6.09 o
-4 5 2 263.56 268.35 3.88 o
-3 5 2 709.42 710.40 7.12 o
-2 5 2 61.76 65.54 1.87 o
-1 5 2 363.62 364.88 6.16 o
0 5 2 8.87 10.84 1.28 o
1 5 2 122.45 119.80 3.68 o
-6 6 2 13.74 12.65 2.73 o
-5 6 2 122.57 122.51 3.42 o
-4 6 2 92.44 91.66 3.06 o
-3 6 2 3.28 3.97 1.91 o
-2 6 2 519.05 524.24 10.47 o
-1 6 2 121.33 125.68 3.00 o
0 6 2 529.83 538.83 8.31 o
-4 7 2 261.03 274.95 11.12 o
-3 7 2 126.29 126.94 4.58 o
-2 7 2 141.11 136.91 9.38 o
0 0 3 2965.67 2931.88 14.97 o
-1 1 3 100.11 96.80 1.90 o
0 1 3 598.50 610.19 2.54 o
1 1 3 829.21 830.50 11.33 o
-3 2 3 845.42 840.22 6.09 o
-2 2 3 2933.18 3002.83 15.87 o
-1 2 3 805.38 811.62 5.94 o
0 2 3 1472.76 1471.74 5.44 o
1 2 3 167.70 170.84 2.04 o
2 2 3 734.44 730.61 4.88 o
-5 3 3 23.73 24.85 1.32 o
-4 3 3 764.07 762.05 7.36 o
-3 3 3 53.47 56.70 1.12 o
-2 3 3 861.11 864.14 8.34 o
-1 3 3 142.62 145.50 1.90 o
0 3 3 2.80 5.29 1.02 o
1 3 3 846.75 854.66 10.98 o
2 3 3 109.85 111.31 3.17 o
3 3 3 610.85 597.33 5.78 o
-6 4 3 82.40 78.97 2.26 o
-5 4 3 219.75 219.80 3.04 o
-4 4 3 759.57 775.94 9.32 o
-3 4 3 816.05 836.99 9.96 o
-2 4 3 734.95 731.70 6.90 o
-1 4 3 805.66 815.60 7.58 o
0 4 3 236.62 245.26 2.77 o
1 4 3 462.46 457.19 4.69 o
2 4 3 85.30 82.66 2.61 o
-6 5 3 365.09 361.67 4.45 o
-5 5 3 54.22 53.10 2.28 o
-4 5 3 221.19 234.41 4.05 o
-3 5 3 17.49 18.02 1.59 o
-2 5 3 120.23 114.72 2.52 o
-1 5 3 459.57 448.44 8.47 o
0 5 3 61.86 63.29 2.29 o
1 5 3 465.90 479.52 6.48 o
-5 6 3 384.94 386.74 5.65 o
-4 6 3 79.09 78.09 2.99 o
-3 6 3 605.41 596.28 6.80 o
-2 6 3 84.86 88.94 2.82 o
-1 6 3 453.35 462.43 9.45 o
0 6 3 85.09 79.29 7.45 o
-1 1 4 1452.36 1489.96 6.96 o
0 1 4 1510.66 1507.12 6.43 o
1 1 4 880.32 865.08 6.78 o
-3 2 4 981.97 1005.57 8.88 o
-2 2 4 234.68 231.64 2.15 o
-1 2 4 845.64 834.36 8.36 o
0 2 4 9.70 11.91 0.71 o
1 2 4 145.18 147.18 1.84 o
2 2 4 427.16 419.68 4.10 o
-5 3 4 143.99 148.33 2.47 o
-4 3 4 260.49 256.72 2.89 o
-3 3 4 11.52 14.10 1.00 o
-2 3 4 1017.24 1013.68 5.18 o
-1 3 4 128.82 130.56 2.36 o
0 3 4 996.44 1019.26 9.94 o
1 3 4 112.67 119.36 2.09 o
2 3 4 898.64 889.67 6.62 o
3 3 4 55.17 52.88 2.55 o
-6 4 4 320.07 316.29 4.55 o
-5 4 4 437.30 439.61 7.94 o
-4 4 4 412.71 425.09 4.31 o
-3 4 4 277.03 279.92 3.76 o
-2 4 4 449.84 450.90 4.77 o
-1 4 4 118.14 117.97 2.46 o
0 4 4 178.05 185.24 3.06 o
1 4 4 146.71 142.11 4.22 o
2 4 4 163.51 160.74 3.64 o
-6 5 4 17.78 23.41 3.73 o
-5 5 4 40.43 45.36 2.52 o
-4 5 4 429.82 431.68 5.47 o
-3 5 4 145.32 146.44 3.85 o
-2 5 4 890.73 875.45 8.38 o
-1 5 4 126.56 131.86 3.00 o
0 5 4 507.73 517.48 5.51 o
1 5 4 54.42 49.85 5.71 o
-4 6 4 295.86 292.70 6.04 o
-3 6 4 53.19 52.47 2.74 o
-2 6 4 167.29 163.52 4.46 o
-1 6 4 44.91 46.16 4.57 o
-1 1 5 923.60 926.25 6.49 o
0 1 5 578.38 575.09 3.20 o
1 1 5 741.50 733.93 7.03 o
-3 2 5 46.72 47.47 1.35 o
-2 2 5 51.69 51.87 1.33 o
-1 2 5 704.76 713.36 6.99 o
0 2 5 372.42 377.49 2.95 o
1 2 5 840.08 840.61 5.96 o
2 2 5 282.89 287.03 3.93 o
-5 3 5 600.83 587.13 5.61 o
-4 3 5 97.28 95.37 2.18 o
-3 3 5 645.00 662.97 6.45 o
-2 3 5 37.84 40.90 1.27 o
-1 3 5 844.32 865.89 11.97 o
0 3 5 36.55 38.82 1.47 o
1 3 5 375.14 364.96 4.58 o
2 3 5 80.47 77.09 2.54 o
-5 4 5 139.86 138.22 3.36 o
-4 4 5 136.80 137.75 2.83 o
-3 4 5 104.44 105.34 2.40 o
-2 4 5 314.35 319.39 4.95 o
-1 4 5 383.71 386.80 6.41 o
0 4 5 286.66 290.36 4.05 o
1 4 5 300.01 295.86 5.60 o
-5 5 5 522.13 514.61 15.99 o
-4 5 5 117.91 119.71 3.34 o
-3 5 5 578.07 582.55 5.53 o
-2 5 5 84.94 85.11 2.67 o
-1 5 5 301.39 308.40 4.45 o
0 5 5 3.22 11.20 5.03 o
0 0 6 711.57 721.99 8.73 o
-1 1 6 121.33 117.89 2.08 o
0 1 6 66.19 67.83 1.72 o
1 1 6 393.56 383.61 3.86 o
-3 2 6 170.31 168.87 3.73 o
-2 2 6 713.67 724.16 7.02 o
-1 2 6 354.59 354.20 4.22 o
0 2 6 932.29 927.91 7.47 o
1 2 6 269.64 261.84 4.27 o
2 2 6 358.49 359.53 4.78 o
-5 3 6 12.19 12.42 3.38 o
-4 3 6 321.06 305.53 4.01 o
-3 3 6 11.86 13.06 1.32 o
-2 3 6 161.21 161.44 3.77 o
-1 3 6 270.80 266.61 3.29 o
0 3 6 21.68 23.98 1.62 o
1 3 6 283.44 281.58 4.81 o
2 3 6 8.10 8.91 4.54 o
-4 4 6 220.47 222.82 5.09 o
-3 4 6 313.73 322.48 4.25 o
-2 4 6 362.47 368.65 6.27 o
-1 4 6 302.76 308.85 5.13 o
0 4 6 311.48 312.07 6.79 o
-3 5 6 16.34 19.60 2.91 o
-2 5 6 9.27 9.44 3.73 o
-1 1 7 109.18 110.71 2.35 o
0 1 7 461.46 452.92 5.10 o
1 1 7 352.38 348.24 4.42 o
-3 2 7 469.16 463.21 5.39 o
-2 2 7 189.98 185.24 2.98 o
-1 2 7 339.25 335.39 3.79 o
0 2 7 66.70 63.79 2.46 o
1 2 7 25.27 28.04 2.08 o
-3 3 7 28.15 29.10 2.26 o
-2 3 7 456.09 445.66 4.63 o
-1 3 7 27.25 27.64 2.10 o
0 3 7 408.86 400.52 7.23 o
-3 4 7 241.30 267.91 11.10 o
-2 4 7 105.52 103.12 7.75 o
-1 1 8 398.54 403.04 8.84 o
0 1 8 242.70 238.62 5.81 o
1 1 8 144.72 134.24 7.86 o
-2 2 8 11.62 11.92 4.79 o
-1 2 8 146.30 132.12 7.87 o