#------------------------------------------------------------------------------ #$Date: 2024-12-24 05:00:08 +0200 (Tue, 24 Dec 2024) $ #$Revision: 296959 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/35/1573529.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1573529 loop_ _publ_author_name 'Tajiri, Hiroo' 'Kohara, Shinji' 'Kimura, Koji' 'Halubai, Sekhar' 'Morimoto, Haruto' 'Happo, Naohisa' 'Stellhorn, Jens R.' 'Onodera, Yohei' 'Qiao, Xvsheng' 'Urushihara, Daisuke' 'Hu, Peidong' 'Wakihara, Toru' 'Kinoshita, Toyohiko' 'Hayashi, Koichi' _publ_section_title ; Diffractometer for element-specific analysis on local structures using a combination of X-ray fluorescence holography and anomalous X-ray scattering. ; _journal_issue 1 _journal_name_full 'Journal of synchrotron radiation' _journal_page_first 125 _journal_page_last 132 _journal_paper_doi 10.1107/S1600577524011366 _journal_volume 32 _journal_year 2025 _chemical_formula_sum 'Al2 Ca H6 O13 Si3' _chemical_formula_weight 392.3 _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 9 _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _cell_angle_alpha 90 _cell_angle_beta 108.8570(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.52520(10) _cell_length_b 18.9769(3) _cell_length_c 9.7779(2) _cell_measurement_temperature 293 _cell_volume 1145.79(3) _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker CCD' _diffrn_measurement_method 'Bruker CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_unetI/netI 0.0241 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 66889 _diffrn_reflns_theta_full 45.3 _diffrn_reflns_theta_max 45.3 _diffrn_reflns_theta_min 2.15 _exptl_absorpt_coefficient_mu 1.084 _exptl_crystal_density_diffrn 2.2744 _exptl_crystal_F_000 792 _refine_diff_density_max 0.74 _refine_diff_density_min -0.70 _refine_ls_abs_structure_details ' 2451 of Friedel pairs used in the refinement' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_extinction_coef 5000(300) _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_goodness_of_fit_gt 1.95 _refine_ls_goodness_of_fit_ref 2.26 _refine_ls_hydrogen_treatment refall _refine_ls_number_constraints 8 _refine_ls_number_parameters 190 _refine_ls_number_reflns 4918 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0240 _refine_ls_shift/su_max 0.0282 _refine_ls_shift/su_mean 0.0023 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details w=1/(\s^2^(I)+0.0004I^2^) _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.0730 _reflns_number_gt 4761 _reflns_number_total 4918 _reflns_threshold_expression I>3\s(I) _cod_data_source_file ok5128.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_formula_sum 'Al2 Ca1 H6 O13 Si3' _cod_database_code 1573529 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 x,-y,z+1/2 3 x+1/2,y+1/2,z 4 x+1/2,-y+1/2,z+1/2 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca 0.10920(9) 0.393259(18) 0.44799(6) Uani 0.01279(9) 4 1 d . . . Al1 Al 0.92202(10) 0.46661(3) 0.06623(7) Uani 0.00754(12) 4 1 d . . . Al2 Al 0.33439(11) 0.21209(3) 0.40026(7) Uani 0.00771(12) 4 1 d . . . Si1 Si 0.5 0.37938(2) 0 Uani 0.00788(11) 4 1 d . . . Si2 Si 0.20879(10) 0.33259(2) 0.16895(6) Uani 0.00732(11) 4 1 d . . . Si3 Si 0.52980(10) 0.08182(2) 0.29989(6) Uani 0.00746(11) 4 1 d . . . O1 O 0.4952(2) 0.02117(7) 0.40923(14) Uani 0.0125(3) 4 1 d . . . O2 O 0.4955(2) 0.04953(6) 0.14160(13) Uani 0.0101(3) 4 1 d . . . O3 O 0.3623(2) 0.14568(7) 0.28522(15) Uani 0.0138(3) 4 1 d . . . O4 O 0.1264(2) 0.18708(7) 0.46554(16) Uani 0.0138(4) 4 1 d . . . O5 O 0.2731(2) 0.29604(7) 0.32592(14) Uani 0.0111(3) 4 1 d . . . O6 O 0.0812(2) 0.28149(7) 0.03937(15) Uani 0.0135(3) 4 1 d . . . O7 O 0.4325(2) 0.36014(7) 0.14335(14) Uani 0.0126(3) 4 1 d . . . O8 O 0.0677(2) 0.40120(7) 0.18449(14) Uani 0.0120(3) 4 1 d . . . O9 O 0.7804(2) 0.10844(7) 0.36576(15) Uani 0.0140(3) 4 1 d . . . O10 O 0.6478(2) 0.44930(7) 0.03223(15) Uani 0.0133(3) 4 1 d . . . O11 O 0.9674(3) 0.07623(10) 0.0598(3) Uani 0.0360(6) 4 1 d . . . O12 O 0.7048(3) 0.19534(9) 0.12548(18) Uani 0.0276(5) 4 1 d . . . O13 O 0.7826(3) 0.33045(12) 0.3917(2) Uani 0.0323(6) 4 1 d . . . H1 H 1.078(4) 0.1030(14) 0.130(3) Uiso 0.0432 4 1 d . . . H2 H 1.036(4) 0.0324(9) 0.052(4) Uiso 0.0432 4 1 d . . . H3 H 0.662(5) 0.2433(5) 0.100(3) Uiso 0.0332 4 1 d . . . H4 H 0.768(6) 0.1958(14) 0.2288(5) Uiso 0.0332 4 1 d . . . H5 H 0.664(3) 0.3523(18) 0.319(3) Uiso 0.0388 4 1 d . . . H6 H 0.722(5) 0.3161(19) 0.465(3) Uiso 0.0388 4 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 Ca1 Ca 0.01464(13) 0.01219(13) 0.01241(13) 0.00067(11) 0.00558(10) -0.00066(10) Al1 Al 0.00812(19) 0.00653(19) 0.00843(19) 0.00009(15) 0.00328(15) -0.00020(15) Al2 Al 0.00784(18) 0.00670(19) 0.00862(19) 0.00057(15) 0.00269(15) 0.00064(15) Si1 Si 0.00678(16) 0.00797(17) 0.00927(17) 0.00032(13) 0.00313(13) 0.00026(13) Si2 Si 0.00740(17) 0.00697(16) 0.00750(17) 0.00075(13) 0.00226(13) 0.00075(13) Si3 Si 0.00879(17) 0.00732(17) 0.00642(17) 0.00014(13) 0.00266(13) -0.00079(13) O1 O 0.0192(5) 0.0104(5) 0.0103(5) 0.0010(4) 0.0082(4) 0.0016(4) O2 O 0.0141(5) 0.0083(5) 0.0083(4) -0.0020(4) 0.0043(4) -0.0011(4) O3 O 0.0145(5) 0.0118(5) 0.0144(5) 0.0044(4) 0.0037(4) -0.0039(4) O4 O 0.0143(5) 0.0111(5) 0.0198(6) -0.0035(4) 0.0107(5) -0.0008(4) O5 O 0.0153(5) 0.0091(5) 0.0091(5) 0.0015(4) 0.0041(4) 0.0023(4) O6 O 0.0130(5) 0.0136(5) 0.0113(5) -0.0008(4) 0.0003(4) -0.0027(4) O7 O 0.0107(5) 0.0180(6) 0.0097(5) -0.0033(4) 0.0042(4) 0.0005(4) O8 O 0.0139(5) 0.0096(5) 0.0129(5) 0.0041(4) 0.0049(4) 0.0018(4) O9 O 0.0094(5) 0.0185(6) 0.0115(5) -0.0027(4) 0.0000(4) -0.0011(4) O10 O 0.0104(5) 0.0111(5) 0.0189(6) -0.0023(4) 0.0052(4) -0.0005(4) O11 O 0.0176(7) 0.0249(8) 0.0594(13) 0.0058(6) 0.0038(8) -0.0078(8) O12 O 0.0489(11) 0.0147(7) 0.0178(7) -0.0039(6) 0.0088(7) 0.0011(5) O13 O 0.0168(7) 0.0471(11) 0.0279(8) -0.0086(7) -0.0001(6) 0.0085(7) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al 0.0645 0.0514 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Ca 0.2262 0.3064 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag ? ? ? ? ? ? ? ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ca1 Al1 . 2_465 3.2883(8) ? Ca1 Si2 . . 3.2153(9) ? Ca1 O11 . 4_455 2.3113(18) ? Ca1 O12 . 4_455 2.3511(17) ? Ca1 O13 . 1_455 2.3468(19) ? Si1 O4 . 4_554 1.6015(15) ? Si1 O7 . . 1.6404(15) ? Si1 O9 . 4_454 1.6166(12) ? Si1 O10 . . 1.6102(13) ? Si2 O5 . . 1.6113(14) ? Si2 O6 . . 1.5992(14) ? Si2 O7 . . 1.6442(16) ? Si2 O8 . . 1.6297(15) ? Si3 O1 . . 1.6355(15) ? Si3 O2 . . 1.6116(14) ? Si3 O3 . . 1.6072(15) ? Si3 O9 . . 1.6321(14) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O11 H1 O3 . . 1_655 0.96(2) 2.14(2) 3.092(2) 169(2) ? O11 H2 O10 . . 3_545 0.96(2) 1.77(2) 2.732(2) 176(2) ? O12 H3 O4 . . 4_554 0.960(13) 1.83(2) 2.678(2) 146(3) ? O12 H4 O9 . . . 0.960(6) 2.12(2) 2.781(2) 125(2) ? O13 H5 O7 . . . 0.96(2) 1.89(2) 2.801(2) 158(3) ? O13 H6 O6 . . 4_555 0.96(3) 2.29(3) 3.090(3) 140(3) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? 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 2 0 0 8198.89 8341.74 56.61 o -2 0 0 8360.81 8585.11 49.75 o 4 0 0 1144.82 1184.98 18.87 o -4 0 0 1229.00 1275.28 20.96 o 6 0 0 373.42 389.13 14.59 o -6 0 0 342.03 328.19 14.35 o 8 0 0 265.19 301.70 20.18 o -8 0 0 255.22 217.85 14.85 o 1 1 0 16646.00 -1.07 221.95 < 3 1 0 79.53 93.80 2.91 o -3 1 0 102.17 127.50 3.22 o 5 1 0 2490.84 2383.26 28.25 o -5 1 0 2629.38 2518.91 29.23 o 7 1 0 574.12 572.70 14.72 o -7 1 0 618.94 592.54 15.42 o 9 1 0 44.09 34.13 6.50 o -9 1 0 41.07 34.13 5.63 o 0 2 0 0.09 0.43 0.43 < 2 2 0 27564.00 29898.00 212.98 o -2 2 0 27668.80 30717.40 247.28 o 4 2 0 1922.39 1953.45 17.36 o -4 2 0 1900.63 1905.77 19.87 o 6 2 0 178.27 155.16 7.06 o -6 2 0 169.97 138.74 7.09 o 8 2 0 1039.78 1091.56 28.04 o -8 2 0 1032.14 1077.29 22.82 o 1 3 0 7753.02 8089.81 161.37 o -1 3 0 7629.44 7905.28 17.97 o 3 3 0 16235.70 17374.20 346.28 o -3 3 0 16124.80 17379.30 344.27 o 5 3 0 3268.64 3145.27 32.21 o -5 3 0 3315.15 3239.88 34.22 o 7 3 0 372.87 382.64 12.89 o -7 3 0 387.88 373.11 11.80 o 9 3 0 649.27 705.88 23.79 o -9 3 0 675.64 679.90 21.16 o 0 4 0 19997.90 21455.10 387.81 o 2 4 0 3415.19 2956.48 33.23 o -2 4 0 3456.53 2993.63 35.55 o 4 4 0 751.66 698.31 11.33 o -4 4 0 810.06 758.38 13.38 o 6 4 0 2.05 1.73 1.73 < -6 4 0 0.52 -1.73 1.30 < 8 4 0 669.70 678.62 20.68 o -8 4 0 643.21 651.40 18.09 o 1 5 0 6131.58 6437.56 22.59 o -1 5 0 5876.65 6108.17 34.39 o 3 5 0 11907.60 12183.80 60.75 o -3 5 0 12024.40 12240.00 66.91 o 5 5 0 5616.38 5523.68 45.23 o -5 5 0 5680.89 5704.62 47.02 o 7 5 0 84.36 71.73 5.66 o -7 5 0 69.25 53.15 5.23 o 9 5 0 165.53 139.58 13.04 o -9 5 0 145.28 119.28 10.03 o 0 6 0 274.14 257.59 5.41 o 2 6 0 14282.10 14544.60 60.89 o -2 6 0 14412.50 14606.10 79.21 o 4 6 0 5132.06 5095.09 44.19 o -4 6 0 5259.15 5318.17 44.24 o 6 6 0 287.04 314.70 8.83 o -6 6 0 264.35 269.76 9.04 o 8 6 0 275.08 281.38 12.06 o -8 6 0 254.75 245.51 13.01 o 1 7 0 4258.57 4219.13 34.52 o -1 7 0 4196.16 4148.57 41.59 o 3 7 0 2101.78 2135.53 18.14 o -3 7 0 2118.00 2189.83 25.41 o 5 7 0 2513.36 2555.96 24.04 o -5 7 0 2489.85 2547.42 32.74 o 7 7 0 193.84 182.82 8.71 o -7 7 0 197.42 175.90 10.05 o 9 7 0 405.51 402.06 17.31 o -9 7 0 399.48 386.07 18.67 o 0 8 0 2309.13 2667.26 14.24 o 2 8 0 3793.64 3848.14 26.55 o -2 8 0 3950.66 3987.70 38.97 o 4 8 0 384.89 395.34 8.96 o -4 8 0 405.32 397.91 12.61 o 6 8 0 345.67 347.18 10.36 o -6 8 0 351.95 351.49 12.97 o 8 8 0 398.07 410.28 14.61 o -8 8 0 392.76 435.79 17.01 o 1 9 0 4316.38 4725.10 25.34 o -1 9 0 4230.87 4694.45 20.40 o 3 9 0 6336.78 6415.43 40.96 o -3 9 0 6304.11 6462.04 57.22 o 5 9 0 7126.93 7172.94 51.48 o -5 9 0 7226.27 7386.43 66.60 o 7 9 0 2210.29 2283.62 31.14 o -7 9 0 2174.62 2236.93 38.08 o 9 9 0 808.96 853.12 28.64 o -9 9 0 808.16 895.95 27.83 o 0 10 0 6110.12 6029.81 59.03 o 2 10 0 3997.56 4177.28 23.95 o -2 10 0 3889.75 4088.25 41.64 o 4 10 0 6814.46 6689.23 57.32 o -4 10 0 7038.23 6796.83 71.17 o 6 10 0 412.03 399.52 12.22 o -6 10 0 400.77 380.93 15.27 o 8 10 0 222.99 213.51 12.58 o -8 10 0 225.90 186.28 13.98 o 1 11 0 5134.37 5151.26 44.84 o -1 11 0 5038.00 5019.32 45.05 o 3 11 0 856.70 808.29 14.20 o -3 11 0 888.35 817.74 19.04 o 5 11 0 636.08 660.21 12.65 o -5 11 0 639.43 679.67 18.66 o 7 11 0 302.64 297.40 12.14 o -7 11 0 299.23 298.70 13.84 o 9 11 0 153.80 110.63 10.94 o -9 11 0 141.37 123.59 12.58 o 0 12 0 4298.29 4426.77 37.42 o 2 12 0 2458.53 2484.14 23.68 o -2 12 0 2482.95 2557.96 31.98 o 4 12 0 897.77 846.46 16.33 o -4 12 0 893.33 844.73 20.05 o 6 12 0 1833.36 1890.17 30.29 o -6 12 0 1818.89 1828.66 38.03 o 8 12 0 154.69 129.64 9.60 o -8 12 0 148.84 125.75 10.88 o 1 13 0 153.03 126.21 5.79 o -1 13 0 132.76 102.44 6.20 o 3 13 0 1681.24 1665.01 21.17 o -3 13 0 1575.72 1560.04 28.01 o 5 13 0 4169.96 4246.80 39.71 o -5 13 0 4134.75 4246.68 53.47 o 7 13 0 1246.96 1259.58 30.17 o -7 13 0 1281.98 1308.86 30.44 o 0 14 0 1898.53 1891.49 26.64 o 2 14 0 3616.40 3531.27 35.10 o -2 14 0 3574.55 3549.15 40.74 o 4 14 0 1186.40 1203.10 17.89 o -4 14 0 1092.02 1123.22 24.75 o 6 14 0 1632.18 1665.74 29.40 o -6 14 0 1651.09 1686.91 35.08 o 8 14 0 196.88 158.17 13.53 o -8 14 0 168.60 145.64 11.75 o 1 15 0 6666.79 6541.41 60.52 o -1 15 0 6780.00 6689.31 59.55 o 3 15 0 35.85 42.77 3.43 o -3 15 0 31.65 36.29 4.31 o 5 15 0 1082.68 1102.61 20.94 o -5 15 0 1039.53 1050.32 25.86 o 7 15 0 953.68 1034.32 25.12 o -7 15 0 1003.62 1080.97 27.79 o 0 16 0 2956.13 2921.81 33.89 o 2 16 0 502.93 481.43 10.23 o -2 16 0 490.94 469.76 14.46 o 4 16 0 874.45 894.66 16.59 o -4 16 0 895.16 904.14 25.02 o 6 16 0 892.01 923.01 23.04 o -6 16 0 911.60 934.66 26.61 o 8 16 0 633.47 652.20 24.09 o -8 16 0 638.96 659.98 24.50 o 1 17 0 4746.75 4730.83 44.58 o -1 17 0 4651.47 4604.79 49.68 o 3 17 0 458.42 440.67 10.58 o -3 17 0 450.13 447.16 14.30 o 5 17 0 551.76 542.29 15.23 o -5 17 0 525.42 516.81 19.95 o 7 17 0 797.35 845.79 23.34 o -7 17 0 818.97 862.63 25.57 o 0 18 0 383.17 380.96 11.26 o 2 18 0 3732.96 3678.62 34.67 o -2 18 0 3631.12 3644.18 57.27 o 4 18 0 253.04 260.22 10.76 o -4 18 0 278.65 277.07 12.11 o 6 18 0 155.49 137.85 10.01 o -6 18 0 137.53 141.31 12.52 o 1 19 0 923.44 879.21 17.50 o -1 19 0 927.85 886.13 21.68 o 3 19 0 1132.65 1106.20 16.92 o -3 19 0 1084.72 1072.10 28.27 o 5 19 0 280.46 268.01 11.32 o -5 19 0 308.43 280.53 15.70 o 7 19 0 1714.06 1790.66 35.83 o -7 19 0 1706.77 1903.33 44.69 o 0 20 0 84.93 79.51 5.64 o 2 20 0 1351.48 1352.27 21.21 o -2 20 0 1293.61 1302.61 33.70 o 4 20 0 1887.18 1953.39 31.45 o -4 20 0 1892.15 1923.90 38.16 o 6 20 0 616.61 622.78 20.28 o -6 20 0 618.04 621.48 22.90 o 1 21 0 103.39 79.51 5.29 o -1 21 0 105.04 82.10 7.85 o 3 21 0 2033.31 2083.74 25.83 o -3 21 0 2052.17 2100.58 42.30 o 5 21 0 8.88 -1.30 3.03 < -5 21 0 6.87 -2.59 3.46 < 7 21 0 368.58 313.41 15.87 o -7 21 0 362.14 341.08 18.69 o 0 22 0 874.92 854.25 24.00 o 2 22 0 224.59 200.11 8.80 o -2 22 0 203.97 185.42 14.76 o 4 22 0 179.36 147.37 11.36 o -4 22 0 190.57 149.10 13.10 o 6 22 0 42.07 25.92 4.35 o -6 22 0 37.78 39.32 6.48 o 1 23 0 407.94 447.89 13.05 o -1 23 0 372.53 404.68 18.85 o 3 23 0 5.66 4.75 3.02 < -3 23 0 9.34 12.96 4.32 < 5 23 0 1072.02 1094.11 25.72 o -5 23 0 1057.79 1133.09 33.98 o 0 24 0 701.43 691.25 22.58 o 2 24 0 358.80 359.68 11.66 o -2 24 0 357.54 369.62 18.96 o 4 24 0 1793.90 1913.11 38.79 o -4 24 0 1772.01 1901.05 43.63 o 6 24 0 1303.59 1367.34 30.87 o -6 24 0 1313.37 1388.10 43.54 o 1 25 0 259.86 248.54 13.03 o -1 25 0 275.05 289.59 16.79 o 3 25 0 507.30 519.33 17.20 o -3 25 0 524.81 520.18 22.51 o 5 25 0 2.26 -4.32 3.89 < -5 25 0 3.54 -3.89 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-14 33.08 23.33 5.63 o -3 1 14 291.27 237.73 11.98 o 3 1 -14 273.99 227.79 19.60 o -1 1 14 511.00 547.88 19.19 o 1 1 -14 534.72 575.10 22.21 o 1 1 14 231.11 187.57 14.43 o -1 1 -14 220.49 201.41 12.62 o -6 2 14 41.61 25.92 5.64 o 6 2 -14 43.91 38.02 6.92 o -4 2 14 601.77 601.14 17.74 o 4 2 -14 603.80 628.81 26.66 o -2 2 14 66.66 59.63 6.50 o 2 2 -14 67.63 47.96 9.54 o 0 2 14 902.94 949.76 28.59 o 0 2 -14 917.08 999.07 27.80 o -7 3 14 149.29 104.14 10.51 o 7 3 -14 137.67 108.90 11.75 o -5 3 14 453.64 455.72 17.28 o 5 3 -14 470.00 472.14 20.31 o -3 3 14 246.53 211.79 11.42 o 3 3 -14 264.86 245.50 19.09 o -1 3 14 354.39 353.60 16.00 o 1 3 -14 336.02 376.09 18.82 o 1 3 14 1141.46 1274.74 34.24 o -1 3 -14 1132.59 1220.22 29.81 o -6 4 14 188.03 139.59 12.27 o 6 4 -14 169.54 131.38 12.22 o -4 4 14 534.64 552.19 18.46 o 4 4 -14 522.43 526.69 23.76 o -2 4 14 588.08 608.88 18.85 o 2 4 -14 566.69 607.61 25.70 o 0 4 14 1454.52 1571.75 36.83 o 0 4 -14 1497.19 1585.93 38.91 o -7 5 14 382.27 374.84 18.63 o 7 5 -14 419.31 401.18 21.28 o -5 5 14 1070.46 1046.47 26.23 o 5 5 -14 1039.20 1017.52 34.79 o -3 5 14 65.22 43.64 5.67 o 3 5 -14 49.43 33.70 6.94 o -1 5 14 640.52 619.31 20.07 o 1 5 -14 616.63 629.71 21.09 o 1 5 14 965.26 1041.16 31.37 o -1 5 -14 973.15 1059.32 28.16 o -6 6 14 12.92 -3.89 4.75 < 6 6 -14 8.57 9.07 5.62 < -4 6 14 1195.49 1242.32 26.70 o 4 6 -14 1153.30 1230.72 37.88 o -2 6 14 166.41 135.69 10.06 o 2 6 -14 148.61 127.49 13.45 o 0 6 14 309.41 299.12 17.34 o 0 6 -14 315.14 280.10 15.31 o -5 7 14 618.43 634.87 20.63 o 5 7 -14 606.94 621.91 24.55 o -3 7 14 1201.11 1219.90 27.92 o 3 7 -14 1196.14 1259.30 38.42 o -1 7 14 43.81 32.40 6.07 o 1 7 -14 43.15 36.29 5.63 o -6 8 14 93.39 76.92 10.41 o 6 8 -14 101.18 82.53 9.55 o -4 8 14 231.07 204.43 12.65 o 4 8 -14 236.59 200.11 17.41 o -2 8 14 31.57 18.15 5.20 o 2 8 -14 36.14 27.22 6.92 o 0 8 14 456.52 451.40 19.06 o 0 8 -14 475.19 495.92 19.75 o -5 9 14 762.38 748.82 23.48 o 5 9 -14 778.48 819.74 28.68 o -3 9 14 184.64 159.90 11.76 o 3 9 -14 158.32 136.57 13.03 o -1 9 14 479.99 472.14 19.08 o 1 9 -14 456.37 480.37 19.30 o -4 10 14 379.78 355.77 16.14 o 4 10 -14 353.37 286.62 19.73 o -2 10 14 11.05 -2.16 4.75 < 2 10 -14 10.39 -3.02 4.32 < -5 11 14 30.40 -4.75 5.63 < 5 11 -14 27.41 -0.86 5.20 < -3 11 14 212.63 163.80 12.29 o 3 11 -14 215.47 197.51 17.34 o -1 11 14 440.35 450.50 20.69 o 1 11 -14 431.10 496.77 18.14 o -4 12 14 394.16 392.11 17.31 o 4 12 -14 387.64 384.76 22.49 o -2 12 14 209.74 177.63 13.52 o 2 12 -14 207.50 145.21 15.73 o -3 13 14 5.66 -17.71 5.17 < 3 13 -14 6.38 -3.02 5.18 < -5 1 15 909.02 979.55 31.45 o 5 1 -15 877.11 942.83 34.58 o -3 1 15 47.00 35.00 7.36 o 3 1 -15 50.28 30.24 8.23 o -1 1 15 630.18 611.09 23.92 o 1 1 -15 618.65 631.43 28.04 o -4 2 15 38.19 16.85 7.36 < 4 2 -15 50.29 25.06 8.24 o -2 2 15 199.88 163.80 13.10 o 2 2 -15 208.80 178.49 18.67 o -5 3 15 22.98 4.75 5.63 < 5 3 -15 28.41 -0.43 6.49 < -3 3 15 418.58 412.86 16.90 o 3 3 -15 395.87 402.94 26.78 o -1 3 15 242.12 203.56 15.70 o 1 3 -15 222.72 213.08 14.73 o -4 4 15 8.01 -5.62 5.18 < 4 4 -15 8.95 -6.48 5.62 < -2 4 15 202.15 162.50 12.25 o 2 4 -15 192.10 169.85 18.21 o -5 5 15 45.12 31.54 6.50 o 5 5 -15 43.90 33.27 8.22 o -3 5 15 21.38 9.94 5.19 < 3 5 -15 18.03 4.32 5.62 < -1 5 15 291.15 263.67 17.83 o 1 5 -15 302.14 301.71 19.89 o -4 6 15 58.76 40.18 6.95 o 4 6 -15 61.72 61.35 9.94 o -2 6 15 71.06 47.53 6.96 o 2 6 -15 73.29 50.99 9.11 o -3 7 15 533.20 559.56 20.13 o 3 7 -15 542.07 580.30 26.59 o -4 8 15 549.60 593.32 24.81 o 4 8 -15 580.29 603.67 27.54 o loop_ _restr_angle_atom_site_label_1 _restr_angle_site_symmetry_1 _restr_angle_atom_site_label_2 _restr_angle_site_symmetry_2 _restr_angle_atom_site_label_3 _restr_angle_site_symmetry_3 _restr_angle_target _restr_angle_target_weight_param H5 . O13 . H6 . 104.5 0.01 H3 . O12 . H4 . 104.5 0.01 H1 . O11 . H2 . 104.5 0.01 loop_ _restr_distance_atom_site_label_1 _restr_distance_site_symmetry_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param O13 . H5 . 0.96 0.001 O13 . H6 . 0.96 0.001 O12 . H3 . 0.96 0.001 O12 . H4 . 0.96 0.001 O11 . H1 . 0.96 0.001 O11 . H2 . 0.96 0.001 loop_ _restr_equal_angle_atom_site_label_1 _restr_equal_angle_site_symmetry_1 _restr_equal_angle_atom_site_label_2 _restr_equal_angle_site_symmetry_2 _restr_equal_angle_atom_site_label_3 _restr_equal_angle_site_symmetry_3 _restr_equal_angle_class_class_id _restr_equal_angle_class_target_weight_param ? ? ? ? ? ? ? ? loop_ _restr_equal_distance_atom_site_label_1 _restr_equal_distance_site_symmetry_1 _restr_equal_distance_atom_site_label_2 _restr_equal_distance_site_symmetry_2 _restr_equal_distance_class_class_id _restr_equal_distance_class_target_weight_param ? ? ? ? ? ? loop_ _restr_equal_torsion_atom_site_label_1 _restr_equal_torsion_site_symmetry_1 _restr_equal_torsion_atom_site_label_2 _restr_equal_torsion_site_symmetry_2 _restr_equal_torsion_atom_site_label_3 _restr_equal_torsion_site_symmetry_3 _restr_equal_torsion_atom_site_label_4 _restr_equal_torsion_site_symmetry_4 _restr_equal_torsion_class_class_id _restr_equal_torsion_class_target_weight_param ? ? ? ? ? ? ? ? ? ? loop_ _restr_torsion_atom_site_label_1 _restr_torsion_site_symmetry_1 _restr_torsion_atom_site_label_2 _restr_torsion_site_symmetry_2 _restr_torsion_atom_site_label_3 _restr_torsion_site_symmetry_3 _restr_torsion_atom_site_label_4 _restr_torsion_site_symmetry_4 _restr_torsion_angle_target _restr_torsion_weight_param ? ? ? ? ? ? ? ? ? ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.99(2) 1 0 0 0 1 0 0 0 1 2 0.01(2) -1 0 0 0 -1 0 0 0 -1 loop_ _twin_refln_datum_id _twin_refln_individual_id _twin_refln_index_h _twin_refln_index_k _twin_refln_index_l _twin_refln_F_squared_calc _twin_refln_F_squared_meas _twin_refln_F_squared_sigma _twin_refln_include_status ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_adp_c_label _jana_atom_site_adp_c_type_symbol _jana_atom_site_adp_c_111 _jana_atom_site_adp_c_112 _jana_atom_site_adp_c_113 _jana_atom_site_adp_c_122 _jana_atom_site_adp_c_123 _jana_atom_site_adp_c_133 _jana_atom_site_adp_c_222 _jana_atom_site_adp_c_223 _jana_atom_site_adp_c_233 _jana_atom_site_adp_c_333 ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_adp_d_label _jana_atom_site_adp_d_type_symbol _jana_atom_site_adp_d_1111 _jana_atom_site_adp_d_1112 _jana_atom_site_adp_d_1113 _jana_atom_site_adp_d_1122 _jana_atom_site_adp_d_1123 _jana_atom_site_adp_d_1133 _jana_atom_site_adp_d_1222 _jana_atom_site_adp_d_1223 _jana_atom_site_adp_d_1233 _jana_atom_site_adp_d_1333 _jana_atom_site_adp_d_2222 _jana_atom_site_adp_d_2223 _jana_atom_site_adp_d_2233 _jana_atom_site_adp_d_2333 _jana_atom_site_adp_d_3333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_adp_e_label _jana_atom_site_adp_e_type_symbol _jana_atom_site_adp_e_11111 _jana_atom_site_adp_e_11112 _jana_atom_site_adp_e_11113 _jana_atom_site_adp_e_11122 _jana_atom_site_adp_e_11123 _jana_atom_site_adp_e_11133 _jana_atom_site_adp_e_11222 _jana_atom_site_adp_e_11223 _jana_atom_site_adp_e_11233 _jana_atom_site_adp_e_11333 _jana_atom_site_adp_e_12222 _jana_atom_site_adp_e_12223 _jana_atom_site_adp_e_12233 _jana_atom_site_adp_e_12333 _jana_atom_site_adp_e_13333 _jana_atom_site_adp_e_22222 _jana_atom_site_adp_e_22223 _jana_atom_site_adp_e_22233 _jana_atom_site_adp_e_22333 _jana_atom_site_adp_e_23333 _jana_atom_site_adp_e_33333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? loop_ _jana_atom_site_adp_f_label _jana_atom_site_adp_f_type_symbol _jana_atom_site_adp_f_111111 _jana_atom_site_adp_f_111112 _jana_atom_site_adp_f_111113 _jana_atom_site_adp_f_111122 _jana_atom_site_adp_f_111123 _jana_atom_site_adp_f_111133 _jana_atom_site_adp_f_111222 _jana_atom_site_adp_f_111223 _jana_atom_site_adp_f_111233 _jana_atom_site_adp_f_111333 _jana_atom_site_adp_f_112222 _jana_atom_site_adp_f_112223 _jana_atom_site_adp_f_112233 _jana_atom_site_adp_f_112333 _jana_atom_site_adp_f_113333 _jana_atom_site_adp_f_122222 _jana_atom_site_adp_f_122223 _jana_atom_site_adp_f_122233 _jana_atom_site_adp_f_122333 _jana_atom_site_adp_f_123333 _jana_atom_site_adp_f_133333 _jana_atom_site_adp_f_222222 _jana_atom_site_adp_f_222223 _jana_atom_site_adp_f_222233 _jana_atom_site_adp_f_222333 _jana_atom_site_adp_f_223333 _jana_atom_site_adp_f_233333 _jana_atom_site_adp_f_333333 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?