data_Coesite-IV_35.9GPa _publ_requested_journal 'Nature (London)' _publ_contact_author_name 'Elena Bykova' _publ_contact_author_address ;P02.2 Extreme Conditions Beamline, Deutsches Elektronen-Synchrotron Notkestra\&se 85, Hamburg, D-22607 Germany ; _publ_contact_author_email elena.bykova@desy.de _publ_contact_author_phone 49(0)4089985674 loop_ _publ_author_name _publ_author_address 'Bykova, E.' ;P02.2 Extreme Conditions Beamline, Deutsches Elektronen-Synchrotron Notkestra\&se 85, Hamburg, D-22607 Germany ; '\ 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_structure_solution 'SHELXS-2013/1 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1586P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 452 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.2280 _refine_ls_wR_factor_gt 0.2083 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.343(2) 0.6470(19) 0.4574(5) 0.0108(11) Uiso 1 1 d . . . . . O1 O 0.328(5) 0.840(4) 0.5202(12) 0.011(3) Uiso 1 1 d . . . . . Si2 Si 0.1921(19) 0.5167(19) 0.9919(5) 0.0113(12) Uiso 1 1 d . . . . . O2 O 0.470(5) 0.791(4) 0.2580(13) 0.009(2) Uiso 1 1 d . . . . . Si3 Si 0.1029(19) 0.3115(18) 0.6505(5) 0.0093(11) Uiso 1 1 d . . . . . O3 O 0.149(5) 0.680(4) 0.3230(12) 0.008(3) Uiso 1 1 d . . . . . Si4 Si 0.496(2) 0.330(2) 0.2676(5) 0.0121(12) Uiso 1 1 d . . . . . O4 O 0.174(5) 0.517(4) 0.6127(13) 0.010(2) Uiso 1 1 d . . . . . Si5 Si 0.349(2) 0.1278(18) 0.9200(5) 0.0099(11) Uiso 1 1 d . . . . . O5 O 0.450(5) 0.429(5) 0.4144(13) 0.010(2) Uiso 1 1 d . . . . . Si6 Si 0.199(2) 0.0597(19) 0.4397(5) 0.0094(12) Uiso 1 1 d . . . . . O6 O 0.097(4) 0.745(4) 0.0412(12) 0.008(2) Uiso 1 1 d . . . . . Si7 Si 0.039(2) 0.8616(18) 0.8375(5) 0.0102(11) Uiso 1 1 d . . . . . O7 O 0.363(4) 0.514(4) 0.1269(12) 0.008(2) Uiso 1 1 d . . . . . Si8 Si 0.2806(19) 0.7717(18) 0.1392(5) 0.0091(12) Uiso 1 1 d . . . . . O8 O 0.039(5) 0.382(5) 0.1363(13) 0.014(3) Uiso 1 1 d . . . . . O9 O 0.176(5) 0.020(4) 0.1006(13) 0.010(3) Uiso 1 1 d . . . . . O10 O 0.366(6) 0.138(6) 0.2878(14) 0.013(3) Uiso 1 1 d . . . . . O11 O 0.164(5) 0.266(4) 0.4901(13) 0.012(3) Uiso 1 1 d . . . . . O12 O 0.179(5) 0.101(4) 0.7975(12) 0.008(2) Uiso 1 1 d . . . . . O13 O 0.274(5) 0.354(4) 0.9001(13) 0.008(2) Uiso 1 1 d . . . . . O14 O 0.287(5) 0.721(4) 0.8186(13) 0.011(3) Uiso 1 1 d . . . . . O15 O 0.000(5) 0.957(4) 0.6403(13) 0.010(3) Uiso 1 1 d . . . . . O16 O 0.435(4) 0.866(4) 0.9701(11) 0.007(3) Uiso 1 1 d . . . . . _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Si1 O1 1.60(3) . ? Si1 O4 1.71(3) . ? Si1 O5 1.73(2) . ? Si1 O3 1.75(3) . ? Si1 O5 1.76(3) 2_666 ? Si1 O2 1.84(3) . ? Si1 Si8 2.656(7) . ? Si1 Si1 2.698(11) 2_666 ? Si1 Si4 2.766(17) 2_666 ? O1 Si6 1.620(14) 1_565 ? O1 Si4 2.182(15) 2_666 ? Si2 O13 1.61(2) . ? Si2 O8 1.61(4) 1_556 ? Si2 O7 1.69(3) 1_556 ? Si2 O14 1.79(3) . ? Si2 O6 1.81(2) 1_556 ? Si2 O8 1.90(3) 2_566 ? Si2 Si7 2.465(9) . ? Si2 Si2 2.53(3) 2_567 ? Si2 Si8 2.65(2) 1_556 ? O2 Si8 1.73(3) . ? O2 Si5 1.81(3) 2_666 ? Si3 O4 1.47(4) . ? Si3 O11 1.532(14) . ? Si3 O3 1.63(3) 2_566 ? Si3 O12 1.647(16) . ? Si3 Si5 2.821(10) . ? O3 Si3 1.63(3) 2_566 ? O3 Si8 1.68(2) . ? Si4 O14 1.59(2) 2_666 ? Si4 O10 1.61(5) . ? Si4 O5 1.63(2) . ? Si4 O7 1.670(11) . ? Si4 O1 2.182(15) 2_666 ? Si4 Si1 2.765(17) 2_666 ? Si4 Si6 2.79(3) . ? Si5 O13 1.55(2) . ? Si5 O12 1.68(4) . ? Si5 O16 1.76(2) 1_545 ? Si5 O16 1.79(3) 2_667 ? Si5 O2 1.81(3) 2_666 ? Si5 O9 1.82(3) 1_556 ? Si5 Si8 2.54(2) 2_666 ? Si5 Si8 2.605(17) 1_546 ? Si5 Si5 2.659(12) 2_657 ? O5 Si1 1.76(3) 2_666 ? Si6 O15 1.57(4) 2_566 ? Si6 O10 1.60(3) . ? Si6 O1 1.620(14) 1_545 ? Si6 O11 1.62(3) . ? Si6 O15 2.03(3) 1_545 ? Si6 Si6 2.80(3) 2_556 ? O6 Si8 1.60(3) . ? O6 Si7 1.735(11) 1_554 ? O6 Si2 1.81(2) 1_554 ? Si7 O15 1.647(11) . ? Si7 O9 1.681(15) 2_566 ? Si7 O6 1.735(11) 1_556 ? Si7 O8 1.76(5) 2_566 ? Si7 O14 1.814(18) . ? Si7 O12 1.89(5) 1_565 ? O7 Si2 1.69(3) 1_554 ? O7 Si8 1.85(3) . ? Si8 O16 1.67(2) 1_554 ? Si8 O9 1.72(2) 1_565 ? Si8 Si5 2.54(2) 2_666 ? Si8 Si5 2.605(17) 1_564 ? Si8 Si2 2.65(2) 1_554 ? O8 Si2 1.61(4) 1_554 ? O8 Si7 1.76(5) 2_566 ? O8 Si2 1.90(3) 2_566 ? O9 Si7 1.681(15) 2_566 ? O9 Si8 1.72(2) 1_545 ? O9 Si5 1.82(3) 1_554 ? O12 Si7 1.89(5) 1_545 ? O14 Si4 1.59(2) 2_666 ? O15 Si6 1.57(4) 2_566 ? O15 Si6 2.03(3) 1_565 ? O16 Si8 1.67(2) 1_556 ? O16 Si5 1.76(2) 1_565 ? O16 Si5 1.79(3) 2_667 ? 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 O1 Si1 O4 93.2(15) . . ? O1 Si1 O5 158.6(18) . . ? O4 Si1 O5 94.4(16) . . ? O1 Si1 O3 109.7(11) . . ? O4 Si1 O3 87.5(14) . . ? O5 Si1 O3 90.5(13) . . ? O1 Si1 O5 80.9(14) . 2_666 ? O4 Si1 O5 92.0(13) . 2_666 ? O5 Si1 O5 79.0(17) . 2_666 ? O3 Si1 O5 169.4(14) . 2_666 ? O1 Si1 O2 92.2(14) . . ? O4 Si1 O2 165.5(15) . . ? O5 Si1 O2 85.3(11) . . ? O3 Si1 O2 78.1(13) . . ? O5 Si1 O2 102.1(15) 2_666 . ? O1 Si1 Si8 110.2(6) . . ? O4 Si1 Si8 125.2(13) . . ? O5 Si1 Si8 81.3(5) . . ? O3 Si1 Si8 38.4(9) . . ? O5 Si1 Si8 139.0(9) 2_666 . ? O2 Si1 Si8 40.5(11) . . ? O1 Si1 Si1 119.7(13) . 2_666 ? O4 Si1 Si1 94.2(7) . 2_666 ? O5 Si1 Si1 39.8(10) . 2_666 ? O3 Si1 Si1 130.4(11) . 2_666 ? O5 Si1 Si1 39.1(9) 2_666 2_666 ? O2 Si1 Si1 94.8(7) . 2_666 ? Si8 Si1 Si1 113.2(3) . 2_666 ? O1 Si1 Si4 52.0(6) . 2_666 ? O4 Si1 Si4 77.8(11) . 2_666 ? O5 Si1 Si4 110.5(8) . 2_666 ? O3 Si1 Si4 154.9(5) . 2_666 ? O5 Si1 Si4 33.9(6) 2_666 2_666 ? O2 Si1 Si4 115.9(14) . 2_666 ? Si8 Si1 Si4 154.4(9) . 2_666 ? Si1 Si1 Si4 71.5(4) 2_666 2_666 ? Si1 O1 Si6 126.0(15) . 1_565 ? Si1 O1 Si4 92.6(8) . 2_666 ? Si6 O1 Si4 141.1(16) 1_565 2_666 ? O13 Si2 O8 100.7(18) . 1_556 ? O13 Si2 O7 110.0(11) . 1_556 ? O8 Si2 O7 92.0(15) 1_556 1_556 ? O13 Si2 O14 90.1(12) . . ? O8 Si2 O14 161.3(8) 1_556 . ? O7 Si2 O14 98.6(17) 1_556 . ? O13 Si2 O6 165.1(7) . 1_556 ? O8 Si2 O6 90.4(13) 1_556 1_556 ? O7 Si2 O6 79.1(11) 1_556 1_556 ? O14 Si2 O6 76.7(10) . 1_556 ? O13 Si2 O8 93.4(12) . 2_566 ? O8 Si2 O8 88.0(9) 1_556 2_566 ? O7 Si2 O8 156.1(12) 1_556 2_566 ? O14 Si2 O8 76.1(14) . 2_566 ? O6 Si2 O8 77.0(12) 1_556 2_566 ? O13 Si2 Si7 120.8(5) . . ? O8 Si2 Si7 114.2(6) 1_556 . ? O7 Si2 Si7 114.6(12) 1_556 . ? O14 Si2 Si7 47.2(6) . . ? O6 Si2 Si7 44.7(4) 1_556 . ? O8 Si2 Si7 45.2(13) 2_566 . ? O13 Si2 Si2 99.4(17) . 2_567 ? O8 Si2 Si2 48.5(9) 1_556 2_567 ? O7 Si2 Si2 135.0(8) 1_556 2_567 ? O14 Si2 Si2 115.0(9) . 2_567 ? O6 Si2 Si2 80.5(12) 1_556 2_567 ? O8 Si2 Si2 39.5(11) 2_566 2_567 ? Si7 Si2 Si2 74.5(5) . 2_567 ? O13 Si2 Si8 148.3(15) . 1_556 ? O8 Si2 Si8 98.0(12) 1_556 1_556 ? O7 Si2 Si8 43.7(8) 1_556 1_556 ? O14 Si2 Si8 79.6(11) . 1_556 ? O6 Si2 Si8 36.3(10) 1_556 1_556 ? O8 Si2 Si8 112.6(10) 2_566 1_556 ? Si7 Si2 Si8 72.8(5) . 1_556 ? Si2 Si2 Si8 112.2(4) 2_567 1_556 ? Si8 O2 Si5 91.7(7) . 2_666 ? Si8 O2 Si1 96(2) . . ? Si5 O2 Si1 163.8(7) 2_666 . ? O4 Si3 O11 102.4(16) . . ? O4 Si3 O3 110.5(13) . 2_566 ? O11 Si3 O3 107.1(16) . 2_566 ? O4 Si3 O12 126.7(19) . . ? O11 Si3 O12 105.2(10) . . ? O3 Si3 O12 103.6(16) 2_566 . ? O4 Si3 Si5 94.3(10) . . ? O11 Si3 Si5 119.2(6) . . ? O3 Si3 Si5 120.6(5) 2_566 . ? O12 Si3 Si5 32.4(15) . . ? Si3 O3 Si8 124.1(9) 2_566 . ? Si3 O3 Si1 132.6(8) 2_566 . ? Si8 O3 Si1 101.3(18) . . ? O14 Si4 O10 104.2(17) 2_666 . ? O14 Si4 O5 128(2) 2_666 . ? O10 Si4 O5 115.2(17) . . ? O14 Si4 O7 108.1(9) 2_666 . ? O10 Si4 O7 99.8(18) . . ? O5 Si4 O7 96.9(8) . . ? O14 Si4 O1 78.4(7) 2_666 2_666 ? O10 Si4 O1 93.0(12) . 2_666 ? O5 Si4 O1 68.1(7) . 2_666 ? O7 Si4 O1 163.6(16) . 2_666 ? O14 Si4 Si1 95.4(11) 2_666 2_666 ? O10 Si4 Si1 118.5(6) . 2_666 ? O5 Si4 Si1 37.0(8) . 2_666 ? O7 Si4 Si1 128.3(12) . 2_666 ? O1 Si4 Si1 35.4(8) 2_666 2_666 ? O14 Si4 Si6 128.3(15) 2_666 . ? O10 Si4 Si6 29.5(6) . . ? O5 Si4 Si6 85.7(15) . . ? O7 Si4 Si6 103.5(15) . . ? O1 Si4 Si6 82.6(11) 2_666 . ? Si1 Si4 Si6 95.9(5) 2_666 . ? Si3 O4 Si1 129.7(12) . . ? O13 Si5 O12 95.2(13) . . ? O13 Si5 O16 172.5(7) . 1_545 ? O12 Si5 O16 90.2(14) . 1_545 ? O13 Si5 O16 92.1(15) . 2_667 ? O12 Si5 O16 169.4(6) . 2_667 ? O16 Si5 O16 83.2(18) 1_545 2_667 ? O13 Si5 O2 91.0(13) . 2_666 ? O12 Si5 O2 88.6(13) . 2_666 ? O16 Si5 O2 94.2(9) 1_545 2_666 ? O16 Si5 O2 83.6(13) 2_667 2_666 ? O13 Si5 O9 94.6(11) . 1_556 ? O12 Si5 O9 90.8(15) . 1_556 ? O16 Si5 O9 80.2(10) 1_545 1_556 ? O16 Si5 O9 96.2(11) 2_667 1_556 ? O2 Si5 O9 174.4(11) 2_666 1_556 ? O13 Si5 Si8 89.3(15) . 2_666 ? O12 Si5 Si8 131.5(9) . 2_666 ? O16 Si5 Si8 90.9(12) 1_545 2_666 ? O16 Si5 Si8 40.8(8) 2_667 2_666 ? O2 Si5 Si8 43.0(10) 2_666 2_666 ? O9 Si5 Si8 137.0(10) 1_556 2_666 ? O13 Si5 Si8 135.2(8) . 1_546 ? O12 Si5 Si8 91.9(13) . 1_546 ? O16 Si5 Si8 39.3(7) 1_545 1_546 ? O16 Si5 Si8 88.2(10) 2_667 1_546 ? O2 Si5 Si8 133.5(7) 2_666 1_546 ? O9 Si5 Si8 41.0(6) 1_556 1_546 ? Si8 Si5 Si8 117.8(4) 2_666 1_546 ? O13 Si5 Si5 133.0(15) . 2_657 ? O12 Si5 Si5 131.7(11) . 2_657 ? O16 Si5 Si5 42.0(11) 1_545 2_657 ? O16 Si5 Si5 41.1(9) 2_667 2_657 ? O2 Si5 Si5 88.5(7) 2_666 2_657 ? O9 Si5 Si5 87.7(6) 1_556 2_657 ? Si8 Si5 Si5 60.0(6) 2_666 2_657 ? Si8 Si5 Si5 57.8(5) 1_546 2_657 ? O13 Si5 Si3 67.6(9) . . ? O12 Si5 Si3 31.7(10) . . ? O16 Si5 Si3 119.0(11) 1_545 . ? O16 Si5 Si3 149.5(12) 2_667 . ? O2 Si5 Si3 74.6(7) 2_666 . ? O9 Si5 Si3 107.5(9) 1_556 . ? Si8 Si5 Si3 113.4(5) 2_666 . ? Si8 Si5 Si3 122.2(8) 1_546 . ? Si5 Si5 Si3 154.4(4) 2_657 . ? Si4 O5 Si1 143.2(7) . . ? Si4 O5 Si1 109.1(9) . 2_666 ? Si1 O5 Si1 101.0(17) . 2_666 ? O15 Si6 O10 104.6(15) 2_566 . ? O15 Si6 O1 113.5(18) 2_566 1_545 ? O10 Si6 O1 94.0(11) . 1_545 ? O15 Si6 O11 107.7(13) 2_566 . ? O10 Si6 O11 98(2) . . ? O1 Si6 O11 132.1(12) 1_545 . ? O15 Si6 O15 78.4(8) 2_566 1_545 ? O10 Si6 O15 176.9(15) . 1_545 ? O1 Si6 O15 84.0(10) 1_545 1_545 ? O11 Si6 O15 81.3(14) . 1_545 ? O15 Si6 Si4 121.9(10) 2_566 . ? O10 Si6 Si4 29.6(16) . . ? O1 Si6 Si4 105.2(14) 1_545 . ? O11 Si6 Si4 70.4(14) . . ? O15 Si6 Si4 148.9(13) 1_545 . ? O15 Si6 Si6 45.2(8) 2_566 2_556 ? O10 Si6 Si6 149.8(15) . 2_556 ? O1 Si6 Si6 98.5(15) 1_545 2_556 ? O11 Si6 Si6 93.5(13) . 2_556 ? O15 Si6 Si6 33.2(9) 1_545 2_556 ? Si4 Si6 Si6 156.3(4) . 2_556 ? Si8 O6 Si7 131(2) . 1_554 ? Si8 O6 Si2 101.8(9) . 1_554 ? Si7 O6 Si2 88.1(9) 1_554 1_554 ? O15 Si7 O9 95.4(7) . 2_566 ? O15 Si7 O6 175.0(7) . 1_556 ? O9 Si7 O6 89.4(6) 2_566 1_556 ? O15 Si7 O8 94.8(17) . 2_566 ? O9 Si7 O8 102.4(17) 2_566 2_566 ? O6 Si7 O8 82.7(15) 1_556 2_566 ? O15 Si7 O14 97.4(7) . . ? O9 Si7 O14 167.0(8) 2_566 . ? O6 Si7 O14 77.9(6) 1_556 . ? O8 Si7 O14 79.0(15) 2_566 . ? O15 Si7 O12 84.8(17) . 1_565 ? O9 Si7 O12 89.5(15) 2_566 1_565 ? O6 Si7 O12 96.6(16) 1_556 1_565 ? O8 Si7 O12 168.1(10) 2_566 1_565 ? O14 Si7 O12 89.2(16) . 1_565 ? O15 Si7 Si2 128.1(9) . . ? O9 Si7 Si2 125.2(9) 2_566 . ? O6 Si7 Si2 47.2(8) 1_556 . ? O8 Si7 Si2 50.0(8) 2_566 . ? O14 Si7 Si2 46.4(9) . . ? O12 Si7 Si2 121.8(10) 1_565 . ? Si4 O7 Si2 135(2) . 1_554 ? Si4 O7 Si8 124.3(15) . . ? Si2 O7 Si8 96.9(7) 1_554 . ? O6 Si8 O16 94.2(13) . 1_554 ? O6 Si8 O3 93.0(14) . . ? O16 Si8 O3 172.8(16) 1_554 . ? O6 Si8 O9 86.0(13) . 1_565 ? O16 Si8 O9 85.9(11) 1_554 1_565 ? O3 Si8 O9 94.7(9) . 1_565 ? O6 Si8 O2 175.9(13) . . ? O16 Si8 O2 89.8(14) 1_554 . ? O3 Si8 O2 83.0(14) . . ? O9 Si8 O2 95.0(14) 1_565 . ? O6 Si8 O7 80.3(13) . . ? O16 Si8 O7 87.2(11) 1_554 . ? O3 Si8 O7 93.9(12) . . ? O9 Si8 O7 164.2(10) 1_565 . ? O2 Si8 O7 99.2(12) . . ? O6 Si8 Si5 138.6(7) . 2_666 ? O16 Si8 Si5 44.7(10) 1_554 2_666 ? O3 Si8 Si5 128.1(12) . 2_666 ? O9 Si8 Si5 93.8(14) 1_565 2_666 ? O2 Si8 Si5 45.3(9) . 2_666 ? O7 Si8 Si5 91.3(12) . 2_666 ? O6 Si8 Si5 91.6(11) . 1_564 ? O16 Si8 Si5 41.9(7) 1_554 1_564 ? O3 Si8 Si5 138.0(8) . 1_564 ? O9 Si8 Si5 44.0(9) 1_565 1_564 ? O2 Si8 Si5 91.9(12) . 1_564 ? O7 Si8 Si5 128.0(7) . 1_564 ? Si5 Si8 Si5 62.2(4) 2_666 1_564 ? O6 Si8 Si2 41.9(6) . 1_554 ? O16 Si8 Si2 84.1(12) 1_554 1_554 ? O3 Si8 Si2 101.3(14) . 1_554 ? O9 Si8 Si2 125.6(10) 1_565 1_554 ? O2 Si8 Si2 138.1(6) . 1_554 ? O7 Si8 Si2 39.3(9) . 1_554 ? Si5 Si8 Si2 114.3(4) 2_666 1_554 ? Si5 Si8 Si2 109.7(4) 1_564 1_554 ? O6 Si8 Si1 132.3(11) . . ? O16 Si8 Si1 132.6(12) 1_554 . ? O3 Si8 Si1 40.3(11) . . ? O9 Si8 Si1 103.2(6) 1_565 . ? O2 Si8 Si1 43.6(10) . . ? O7 Si8 Si1 91.9(4) . . ? Si5 Si8 Si1 88.0(5) 2_666 . ? Si5 Si8 Si1 127.4(8) 1_564 . ? Si2 Si8 Si1 122.3(6) 1_554 . ? Si2 O8 Si7 127.9(11) 1_554 2_566 ? Si2 O8 Si2 92.0(9) 1_554 2_566 ? Si7 O8 Si2 84.8(19) 2_566 2_566 ? Si7 O9 Si8 137(2) 2_566 1_545 ? Si7 O9 Si5 126.9(12) 2_566 1_554 ? Si8 O9 Si5 95.0(7) 1_545 1_554 ? Si6 O10 Si4 120.8(17) . . ? Si3 O11 Si6 134.9(19) . . ? Si3 O12 Si5 116(2) . . ? Si3 O12 Si7 118(2) . 1_545 ? Si5 O12 Si7 124.9(9) . 1_545 ? Si5 O13 Si2 146.3(9) . . ? Si4 O14 Si2 116.0(10) 2_666 . ? Si4 O14 Si7 156.7(13) 2_666 . ? Si2 O14 Si7 86.4(13) . . ? Si6 O15 Si7 126(2) 2_566 . ? Si6 O15 Si6 101.6(8) 2_566 1_565 ? Si7 O15 Si6 131(2) . 1_565 ? Si8 O16 Si5 98.8(6) 1_556 1_565 ? Si8 O16 Si5 94.5(7) 1_556 2_667 ? Si5 O16 Si5 96.8(18) 1_565 2_667 ? _refine_diff_density_max 0.700 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.170 _shelx_res_file ; C:\XCALIB~1\HASYLA~1\COESIT~1\p03_cal\struct\tmp\SOL_FI~1\dom3_cal.res created by SHELXL-2014/7 REM P-1 (#2 in standard setting) TITL dom3_cal in P-1 CELL 0.29004 6.5242 6.9419 8.6742 70.068 84.053 83.629 ZERR 16.0000 0.0088 0.0094 0.0047 0.080 0.070 0.111 LATT 1 SFAC O SI DISP Si 0.00816 0.01070 28.03 DISP O -0.00101 0.00082 6.64 UNIT 32 16 MERG 2 SHEL 99999.00 0.75 FMAP 2 GRID PLAN 20 TEMP 23 SIZE 0.02 0.02 0.005 EQIV $1 1-X,1-Y,1-Z EQIV $2 -X,1-Y,2-Z EQIV $3 -X,1-Y,1-Z EQIV $4 X,Y-1,Z OMIT -4 3 0 OMIT -2 3 5 L.S. 10 ACTA 21 WGHT 0.158600 FVAR 8.03106 SI1 2 0.342689 0.646952 0.457412 11.00000 0.01080 O1 1 0.327898 0.840344 0.520176 11.00000 0.01052 SI2 2 0.192130 0.516745 0.991884 11.00000 0.01126 O2 1 0.470403 0.790678 0.258000 11.00000 0.00921 SI3 2 0.102909 0.311456 0.650500 11.00000 0.00931 O3 1 0.148889 0.679978 0.323017 11.00000 0.00837 SI4 2 0.495920 0.329740 0.267553 11.00000 0.01209 O4 1 0.174251 0.516803 0.612740 11.00000 0.00963 SI5 2 0.348878 0.127753 0.920021 11.00000 0.00989 O5 1 0.449703 0.429252 0.414434 11.00000 0.00990 SI6 2 0.199017 0.059673 0.439691 11.00000 0.00944 O6 1 0.096566 0.745109 0.041239 11.00000 0.00761 SI7 2 0.039344 0.861581 0.837542 11.00000 0.01025 O7 1 0.362777 0.513935 0.126892 11.00000 0.00763 SI8 2 0.280640 0.771736 0.139198 11.00000 0.00914 O8 1 0.039489 0.381952 0.136350 11.00000 0.01434 O9 1 0.176167 0.020115 0.100601 11.00000 0.00995 O10 1 0.366408 0.137526 0.287777 11.00000 0.01263 O11 1 0.163610 0.266101 0.490144 11.00000 0.01190 O12 1 0.178797 0.100547 0.797547 11.00000 0.00777 O13 1 0.273806 0.354156 0.900116 11.00000 0.00836 O14 1 0.286583 0.720681 0.818551 11.00000 0.01081 O15 1 -0.000160 0.957164 0.640345 11.00000 0.00985 O16 1 0.435276 0.865587 0.970057 11.00000 0.00664 HKLF 4 REM dom3_cal in P-1 REM R1 = 0.0811 for 332 Fo > 4sig(Fo) and 0.1086 for all 452 data REM 97 parameters refined using 0 restraints END WGHT 0.1586 0.0000 REM Highest difference peak 0.700, deepest hole -0.597, 1-sigma level 0.170 Q1 1 0.5589 0.4854 0.3565 11.00000 0.05 0.70 Q2 1 0.5867 0.5290 0.3480 11.00000 0.05 0.70 Q3 1 -0.1321 0.8480 0.6990 11.00000 0.05 0.64 Q4 1 0.2155 0.4836 0.9440 11.00000 0.05 0.57 Q5 1 0.0907 0.2602 0.6108 11.00000 0.05 0.54 Q6 1 0.2817 0.6548 0.4974 11.00000 0.05 0.53 Q7 1 0.3715 0.1052 0.8829 11.00000 0.05 0.52 Q8 1 0.4114 0.1327 0.8771 11.00000 0.05 0.51 Q9 1 0.4933 0.2691 0.2586 11.00000 0.05 0.50 Q10 1 0.2846 0.2935 0.7113 11.00000 0.05 0.49 Q11 1 0.4524 0.8511 0.4226 11.00000 0.05 0.49 Q12 1 0.2128 0.8061 0.2960 11.00000 0.05 0.48 Q13 1 0.1324 0.4189 0.5489 11.00000 0.05 0.48 Q14 1 0.5386 0.3126 0.2412 11.00000 0.05 0.48 Q15 1 0.2491 0.2623 0.8583 11.00000 0.05 0.47 Q16 1 0.2786 0.3226 0.8428 11.00000 0.05 0.46 Q17 1 0.1313 0.8986 0.8030 11.00000 0.05 0.46 Q18 1 0.3208 0.3753 0.8206 11.00000 0.05 0.46 Q19 1 0.3162 0.3309 0.7019 11.00000 0.05 0.46 Q20 1 0.4656 0.5434 0.0635 11.00000 0.05 0.45 ; _shelx_res_checksum 40826 _shelx_hkl_file ; 0 0 3 37662.9 1646.74 1 0 0 -3 34813.5 1680.18 1 0 0 4 26333.1 1913.87 1 0 0 -4 25331.0 1775.95 1 0 0 5 17378.1 2197.97 1 0 0 -5 17028.3 1821.86 1 0 0 -6 14620.0 1961.60 1 0 0 6 17229.4 2589.19 1 0 0 7 53056.2 3947.01 1 0 0 -7 50366.6 3183.43 1 0 0 8 7629.19 2888.19 1 0 0 -8 4438.62 2098.69 1 0 0 9 1712.94 2961.14 1 0 0 -9-508.566 2537.08 1 0 0 10 16229.7 3973.62 1 0 0 -10 19681.0 3247.43 1 0 0 -11 31006.1 3867.38 1 0 0 11 32033.7 5223.23 1 0 1 -10 24855.6 3657.26 1 0 -1 10 20336.6 4499.62 1 0 -1 9 15736.4 3855.66 1 0 1 -9 9969.23 2794.63 1 0 -1 8-336.321 2580.99 1 0 1 -8 3401.51 2149.75 1 0 -1 7 11158.2 2564.15 1 0 1 -7 10127.0 2416.54 1 0 1 -6 16140.6 2283.80 1 0 -1 6 15378.6 2453.24 1 0 1 -5 1856.37 1541.53 1 0 -1 5 1700.03 1784.26 1 0 1 -4 72274.8 3097.30 1 0 -1 4 70391.5 3156.72 1 0 1 -3 207328. 4268.95 1 0 -1 3 206203. 4352.02 1 0 -1 -3 2864.70 746.838 1 0 1 3 1654.60 1019.57 1 0 1 4 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22037.7 2884.77 1 -2 2 -6 223480. 6705.18 1 2 -2 6 216607. 7318.39 1 2 -2 7 22026.1 3570.81 1 -2 2 -7 22816.6 3160.66 1 2 -2 8 22769.7 4022.48 1 -2 2 -8 26069.8 3511.50 1 2 -2 9-2725.59 3834.75 1 -2 2 -9 8.94145 3000.38 1 2 -2 10 10950.2 5052.49 1 -2 1 10 2346.05 3238.15 1 -2 1 9 5970.78 2697.77 1 -2 1 8 1357.66 2007.56 1 -2 1 7-1351.53 1817.47 1 -2 1 6 283866. 5881.29 1 -2 1 5 255949. 4630.96 1 -2 1 4 3214.08 975.434 1 -2 1 -1 435.464 930.571 1 2 -1 2 338628. 6377.46 1 -2 1 -2 325876. 5689.71 1 2 -1 3 217597. 5438.95 1 -2 1 -3 207820. 5241.08 1 2 -1 4 6806.58 1741.26 1 -2 1 -4 5238.48 1808.98 1 -2 1 -5 11171.9 1840.02 1 2 -1 5 11349.3 2096.33 1 2 -1 6 76050.9 4322.47 1 -2 1 -6 87634.2 4104.18 1 -2 1 -7 9546.33 2439.62 1 2 -1 7 8862.56 2653.18 1 2 -1 8 181561. 7153.34 1 -2 1 -8 187490. 7289.44 1 -2 1 -9 10992.8 3055.26 1 2 -1 9 14747.2 3590.31 1 2 -1 10 5254.42 3708.20 1 -2 1 -10 7150.64 3174.01 1 -2 0 10 25914.6 3802.90 1 -2 0 9 152950. 6355.22 1 -2 0 8 3275.48 2470.14 1 -2 0 7 6490.39 2365.26 1 -2 0 6 4251.99 1863.76 1 -2 0 -3 14866.6 2288.52 1 2 0 4 52075.2 4036.17 1 -2 0 -4 48320.3 3015.61 1 -2 0 -5 45570.8 3260.34 1 2 0 5 39877.3 4118.03 1 -2 0 -6 5338.95 2269.04 1 2 0 6 1654.21 2734.34 1 -2 0 -7-2732.51 2932.67 1 2 0 7-9707.81 4023.96 1 -2 0 -8 32639.6 3647.27 1 2 0 8 23512.8 4071.77 1 2 0 9 3311.17 4062.32 1 -2 0 -9 3751.62 2582.16 1 -2 0 -10 27266.0 3862.21 1 2 0 10 14368.7 5022.50 1 -2 0 -11 13478.4 4481.18 1 2 0 11 185.965 5024.44 1 -2 -1 -6 121451. 6001.30 1 -2 -1 -7 5264.32 2204.07 1 -2 -1 -8 1096.17 2778.52 1 2 1 8-2013.91 4380.84 1 2 1 9 72485.0 7357.52 1 -2 -1 -9 77591.0 5305.47 1 2 1 10 18208.8 6085.73 1 -2 -1 -10 27911.8 4238.60 1 2 1 11 6693.94 6026.08 1 -2 -1 -11 3987.84 3034.37 1 -2 -2 -9 15544.6 3333.58 1 -2 -2 -10 2852.04 3177.89 1 -2 -2 -11 21865.9 4215.71 1 3 -7 -9 9171.51 1591.49 1 3 -7 -8 6234.77 1214.15 1 3 -6 -10 8814.18 1809.98 1 3 -6 -9 2628.67 1282.84 1 3 -6 -8 9404.83 1200.28 1 3 -6 -7 12100.8 1125.01 1 3 -6 -1 2863.33 1545.46 1 3 -6 0 3528.12 1801.36 1 3 -6 1 6863.76 2257.68 1 3 -6 2 6400.14 2602.81 1 3 -6 3 110816. 5277.39 1 3 -6 4 32649.7 3532.78 1 3 -6 5 5501.12 3257.00 1 3 -5 -10 6741.37 1712.37 1 3 -5 -9 3123.11 1362.67 1 3 -5 -8 25861.7 1600.00 1 3 -5 -7 26823.2 1286.12 1 3 -5 -3 7788.82 842.594 1 3 -5 -2 6632.14 1176.42 1 3 -5 -1 7059.33 1394.69 1 3 -5 0 43809.4 2611.72 1 3 -5 1 2654.35 1702.31 1 3 -5 2 8159.19 1965.65 1 3 -5 3 9066.28 2186.64 1 3 -5 4 15641.9 2927.57 1 -3 5 -5 81629.3 5033.18 1 3 -5 5 88682.4 5058.35 1 -3 5 -6 46990.7 4471.84 1 3 -5 6 46828.1 5079.40 1 3 -5 7-8247.26 4429.49 1 3 -4 -11 7680.63 1726.77 1 3 -4 -10 41103.3 2570.54 1 -3 4 10 55350.8 5168.26 1 3 -4 -9-749.199 1441.83 1 3 -4 -2 102709. 2538.60 1 3 -4 -1 938.688 1181.95 1 3 -4 0 193722. 4385.84 1 -3 4 -1 2009.33 1408.67 1 3 -4 1 806.820 1617.13 1 -3 4 -2 181105. 5087.63 1 3 -4 2 183283. 5554.02 1 -3 4 -3 22626.8 2486.64 1 3 -4 3 20169.4 2960.42 1 -3 4 -4 4049.35 2192.57 1 3 -4 4 2797.61 2831.71 1 3 -4 5 66622.7 4744.97 1 -3 4 -5 77373.3 4198.39 1 3 -4 6 17069.5 3849.24 1 -3 4 -6 24684.4 3798.68 1 3 -4 7 34107.2 4663.01 1 -3 4 -7 36895.1 3886.33 1 3 -4 8 12085.5 4896.14 1 -3 3 10 11710.7 2693.09 1 -3 3 9 2044.80 2238.72 1 -3 3 8 218.785 1921.28 1 -3 3 7-1203.52 1564.20 1 -3 3 6 13941.4 1852.86 1 -3 3 5 224312. 3320.06 1 -3 3 1-288.700 779.442 1 -3 3 0 118102. 2985.99 1 3 -3 0 117188. 3021.76 1 -3 3 -1 5537.90 1392.09 1 3 -3 1 5296.13 1508.11 1 -3 3 -2 9140.50 1700.68 1 3 -3 2 8840.82 1958.47 1 3 -3 3 3175.49 2223.48 1 -3 3 -3-541.420 1772.71 1 -3 3 -4 56019.0 3654.69 1 3 -3 4 65542.3 4458.67 1 -3 3 -5 2532.20 2156.71 1 3 -3 5 6442.54 2745.68 1 3 -3 6-1888.28 3135.46 1 -3 3 -6 1166.51 2633.75 1 3 -3 7 12263.0 4056.16 1 -3 3 -7-2156.89 2668.86 1 3 -3 8 292.070 3961.17 1 -3 3 -8 496.355 2882.82 1 3 -3 9-2941.14 3692.34 1 -3 2 10 39283.9 4049.77 1 -3 2 9 13845.1 2953.32 1 -3 2 8-247.976 1848.75 1 -3 2 7 89059.2 3382.47 1 -3 2 6 4831.94 1607.95 1 -3 2 5 570245. 6005.16 1 -3 2 0 165635. 3414.48 1 3 -2 1-477.665 1909.82 1 -3 2 -1 872.911 1227.56 1 3 -2 2 155831. 5066.98 1 -3 2 -2 167863. 4586.22 1 3 -2 3 25117.9 2941.78 1 -3 2 -3 27055.8 2650.60 1 3 -2 4 14961.9 3214.73 1 -3 2 -4 15201.7 1870.63 1 3 -2 5 312.945 2192.19 1 -3 2 -5 4236.79 2005.88 1 -3 2 -6 55070.1 3928.68 1 3 -2 6 51071.5 4109.78 1 -3 2 -7 12907.4 3037.06 1 3 -2 7 10117.0 2801.37 1 -3 2 -8 12803.8 3226.51 1 3 -2 8 13693.5 3592.53 1 3 -2 9-1649.24 3509.86 1 -3 2 -9 440.090 3025.34 1 -3 1 10 1415.49 2610.50 1 -3 1 9 14567.7 2841.95 1 -3 1 8 13408.7 2659.58 1 -3 1 7 31568.4 2761.99 1 -3 1 -2 3769.50 2084.05 1 -3 1 -3 157931. 4765.95 1 3 -1 4 68053.8 5096.58 1 -3 1 -4 86421.5 4228.03 1 3 -1 5 42112.3 4674.35 1 -3 1 -5 48467.7 3709.13 1 3 -1 6 67591.3 5536.42 1 -3 1 -6 83228.7 4926.17 1 3 -1 7 385.920 3628.94 1 -3 1 -7 4096.76 2746.94 1 3 -1 8 94445.1 6859.38 1 -3 1 -8 116445. 5815.34 1 -3 1 -9 25764.4 3674.01 1 3 -1 9 16449.3 5056.19 1 -3 1 -10 17931.2 4070.83 1 3 -1 10 6106.73 5142.19 1 -3 0 -5 223821. 7722.43 1 -3 0 -6 13309.0 2602.93 1 -3 0 -7-3558.01 3106.05 1 3 0 7-4393.81 4478.81 1 -3 0 -8 18803.1 3651.89 1 3 0 8 11658.7 4769.97 1 3 0 9-5209.12 5064.67 1 -3 0 -9-770.557 3586.73 1 3 0 10 21408.1 6767.32 1 -3 0 -10 15469.8 3944.47 1 -3 -1 -8 13540.9 3526.23 1 -3 -1 -9 27232.4 4345.19 1 -3 -1 -10 11125.3 3828.50 1 -3 -1 -11 1412.25 3944.26 1 4 -7 -4 3118.00 879.735 1 4 -7 -3 1873.28 1192.22 1 4 -7 -2 1229.00 1447.89 1 4 -7 -1 58396.2 2977.72 1 4 -7 0 2381.13 1833.59 1 4 -7 1 40847.1 3186.29 1 4 -7 2 3841.84 2573.22 1 4 -7 3-3193.19 2273.43 1 4 -6 -3-1269.24 1073.85 1 4 -6 -2 45721.0 2453.65 1 4 -6 -1 22702.2 2287.22 1 4 -6 0 42962.8 2973.38 1 4 -6 1-301.502 2220.77 1 4 -6 2 44146.1 3854.27 1 4 -6 3 38092.5 4018.42 1 4 -6 4 29390.8 3955.65 1 4 -5 -2 1253.32 1354.68 1 4 -5 -1 24933.5 2012.53 1 4 -5 0 4145.40 1807.15 1 -4 5 -1 35832.4 2839.87 1 4 -5 1 43974.7 3079.37 1 4 -5 2 17465.4 2622.12 1 -4 5 -2 15622.4 2362.29 1 4 -5 3 2012.18 2523.13 1 -4 5 -3-512.098 2239.56 1 4 -5 4-3026.23 3186.78 1 -4 5 -4-2292.32 2464.71 1 4 -5 5 11875.5 3562.48 1 -4 5 -5 10989.7 3224.71 1 4 -5 6 84498.7 5794.99 1 -4 4 9 15865.6 3125.64 1 -4 4 8 7355.37 2352.38 1 -4 4 1 49017.5 2074.97 1 4 -4 0 983.431 1982.43 1 -4 4 0-119.948 1344.99 1 -4 4 -1 24650.8 2122.47 1 4 -4 1 23138.1 2432.34 1 -4 4 -2 118451. 4193.13 1 4 -4 2 114754. 4444.97 1 -4 4 -3 7529.39 2039.08 1 4 -4 3 7793.42 2291.30 1 -4 4 -4 16591.0 2560.46 1 4 -4 4 19631.8 2982.07 1 -4 4 -5-1563.44 2475.34 1 4 -4 5-1527.22 2765.33 1 -4 4 -6 2407.78 3032.14 1 4 -4 6 2047.63 3086.75 1 4 -4 7 1347.16 3445.17 1 -4 3 9 38299.6 3220.25 1 -4 3 8 24709.7 2736.22 1 -4 3 7 3622.85 1523.02 1 -4 3 6 10505.2 1229.30 1 -4 3 5 10172.0 948.350 1 -4 3 2 243.062 794.782 1 -4 3 1 40370.0 2128.08 1 -4 3 0 56279.4 3534.35 1 -4 3 -1 345984. 6552.61 1 4 -3 2-1042.89 2649.16 1 -4 3 -2 1407.41 1756.08 1 4 -3 3 49385.1 4111.63 1 -4 3 -3 48249.7 3139.33 1 -4 3 -4 1221.93 1962.68 1 4 -3 4 3777.55 2963.28 1 -4 3 -5 54771.5 3855.88 1 4 -3 5 57751.5 5004.71 1 -4 3 -6 16107.3 3154.29 1 4 -3 6 10444.0 3378.21 1 -4 3 -7 6005.23 3372.83 1 4 -3 7 6706.03 3758.08 1 4 -3 8 30692.7 5050.51 1 -4 3 -8 21328.0 3394.63 1 -4 2 9 37871.3 3148.83 1 -4 2 8 12522.9 2285.55 1 -4 2 7 20270.6 2200.27 1 -4 2 -1 228315. 6002.95 1 -4 2 -2 411662. 7388.93 1 -4 2 -3 429566. 8567.83 1 -4 2 -4 9948.69 2571.70 1 4 -2 4 6138.69 3887.44 1 -4 2 -5-1762.72 2827.22 1 4 -2 5 1979.91 3781.04 1 4 -2 6 7967.65 4044.12 1 -4 2 -6 8652.83 2877.92 1 4 -2 7 52694.6 5637.15 1 -4 2 -7 82336.4 5118.85 1 -4 2 -8 21311.9 3517.26 1 4 -2 8 10281.3 4407.42 1 4 -2 9 5684.79 4936.40 1 -4 1 -4 52807.9 4306.58 1 -4 1 -5 24992.2 3007.93 1 -4 1 -6-1417.80 2920.82 1 -4 1 -7 457.690 3055.17 1 4 -1 7 1585.13 4704.05 1 4 -1 8-2619.50 5497.85 1 -4 1 -8 5221.47 3696.16 1 4 -1 9 19158.6 6760.53 1 -4 1 -9 39824.5 4929.03 1 -4 0 -8 5271.84 3642.70 1 -4 0 -9 79586.7 6346.75 1 -4 0 -10 34442.1 5222.64 1 5 -7 -3 11727.7 1930.65 1 5 -7 -2-19.9902 1597.22 1 5 -7 -1 151.019 2096.23 1 5 -7 0 5920.74 2322.61 1 5 -7 1 27377.7 3432.87 1 5 -6 -1 6131.83 2364.03 1 5 -6 0 8577.42 2515.51 1 5 -6 1 178337. 5364.26 1 -5 6 -2 57130.8 4036.64 1 5 -6 2 59762.9 4030.44 1 5 -6 3 7302.37 3176.24 1 -5 5 1 558.820 1451.29 1 5 -5 0 4783.63 2783.83 1 -5 5 0 1202.10 1622.92 1 -5 5 -1 5001.93 1923.86 1 5 -5 1 2133.36 2675.63 1 -5 5 -2 46145.3 3281.01 1 5 -5 2 45563.4 3991.14 1 -5 5 -3 52870.1 3712.16 1 5 -5 3 55705.1 4335.05 1 -5 5 -4 11654.7 3208.36 1 5 -5 4 6479.78 3184.25 1 5 -5 5 32771.3 4255.80 1 -5 4 8 102750. 3471.13 1 -5 4 7 2578.54 1185.34 1 -5 4 2 29643.7 1616.15 1 -5 4 1 1134.52 1261.94 1 -5 4 0 8883.87 1794.57 1 -5 4 -1 11096.3 2186.46 1 -5 4 -2 6813.73 2383.69 1 5 -4 2 1714.01 3263.28 1 -5 4 -3 136833. 5112.02 1 5 -4 3 98713.3 6386.21 1 -5 4 -4 40611.2 3799.47 1 5 -4 4 28377.8 4231.93 1 -5 4 -5 9804.57 3041.85 1 5 -4 5 7550.89 4019.01 1 5 -4 6-5804.03 4453.09 1 -5 3 8 41550.4 2614.12 1 -5 3 7 3275.10 1568.31 1 -5 3 1 57402.2 3330.06 1 -5 3 0 37227.5 2445.43 1 -5 3 -1 31723.2 2852.20 1 -5 3 -2 1920.33 2234.74 1 -5 3 -3 2195.31 2558.76 1 5 -3 4 12560.8 4081.81 1 -5 3 -4 20229.8 3478.35 1 5 -3 5 17395.2 4866.07 1 -5 3 -5 27959.4 3527.45 1 5 -3 6 13981.1 4673.63 1 -5 3 -6 21813.2 3311.45 1 -5 3 -7 14725.4 3955.62 1 5 -3 7 6371.02 5611.82 1 -5 2 -3 12439.0 2840.36 1 -5 2 -4 2074.56 2470.77 1 -5 2 -5 37719.5 4142.14 1 -5 2 -6 2534.59 3995.86 1 5 -2 7 23117.4 7127.25 1 -5 2 -7 20525.8 4886.16 1 5 -2 8 110829. 9284.99 1 -5 2 -8 109624. 7022.19 1 -5 1 -7 4844.71 3852.74 1 -5 1 -8 790.799 3540.51 1 6 -6 1 3979.30 3736.30 1 6 -6 2 6837.45 3726.30 1 -6 5 3 56653.5 1852.52 1 -6 5 2-73.6874 1301.50 1 -6 5 1 18829.5 2004.32 1 -6 5 0-609.942 2093.31 1 -6 5 -1-2435.93 2388.12 1 -6 5 -2 14298.8 2870.07 1 6 -5 3-1377.75 4367.29 1 6 -5 4 42900.9 6708.18 1 -6 4 6 2802.02 739.487 1 -6 4 3 325.230 1037.51 1 -6 4 2 38771.1 2370.45 1 -6 4 1 7188.95 1969.68 1 -6 4 0 2225.67 2154.01 1 -6 4 -1 2499.36 2444.34 1 -6 4 -2-4274.36 2581.66 1 -6 4 -3 2042.83 2378.10 1 -6 4 -4 17478.0 3151.45 1 6 -4 5 43231.6 6880.47 1 -6 3 -1 157764. 5918.44 1 -6 3 -2 22890.2 3259.21 1 -6 3 -3 30684.4 3676.28 1 -6 3 -4 40574.6 4258.40 1 -6 3 -5 9305.47 3596.00 1 -6 2 -6 5748.43 3847.47 1 -6 2 -7 14910.0 3889.88 1 -7 4 1 6871.84 2150.71 1 -7 4 0 26285.5 3139.07 1 -7 4 -1 16155.8 3207.38 1 0 0 0 0.00 0.00 0 TITL dom3_cal in P-1 REM P-1 (#2 in standard setting) CELL 0.29004 6.524164 6.941940 8.674242 70.0684 84.0531 83.6287 ZERR 16.00 0.008780 0.009440 0.004666 0.0800 0.0702 0.1110 LATT 1 SFAC O Si UNIT 32.00 16.00 TREF HKLF 4 END ; _shelx_hkl_checksum 88690 # start Validation Reply Form _vrf_ATOM007_Coesite-IV_35.9GPa ; PROBLEM: _atom_site_aniso_label is missing RESPONSE: Due to incompleteness of the dataset thermal parameters were refined in isotropic approximation. ; _vrf_PLAT029_Coesite-IV_35.9GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.255 Why? RESPONSE: The dataset was incomplete since the data were collected in a diamond anvil cell metallic body of which shadows more than 60% of the reflections. ; _vrf_PLAT088_Coesite-IV_35.9GPa ; PROBLEM: Poor Data / Parameter Ratio .................... 4.66 Note RESPONSE: Poor data/parameter ratio is due to low symmetry of the structure (P-1), big amount of the parameters to refine (23 atoms) and incompleteness of the dataset (measurement in a diamond anvil cell). ; _vrf_PLAT910_Coesite-IV_35.9GPa ; PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 32 Note RESPONSE: Certain part of the reflections is missing due to geometry of the experiment. The metallic body of the diamond anvil cell absorbs more than 60% of the reflections. ; _vrf_PLAT911_Coesite-IV_35.9GPa ; PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 937 Report RESPONSE: Certain part of the reflections is missing due to geometry of the experiment. The metallic body of the diamond anvil cell absorbs more than 60% of the reflections. ; # end Validation Reply Form