#------------------------------------------------------------------------------ #$Date: 2025-10-14 03:32:25 +0100 (Tue, 14 Oct 2025) $ #$Revision: 302846 $ #$URL: svn://www.crystallography.net/cod/cif/3/00/06/3000611.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_3000611 loop_ _publ_author_name 'Lee, Yun-Hee' 'Kim, Jin Kyun' 'Kim, Yong-Jae' 'Kim, Minju' 'Cho, Yong Chan' 'Husband, Rachel J.' 'Strohm, Cornelius' 'Ehrenreich-Petersen, Emma' 'Glazyrin, Konstantin' 'Laurus, Torsten' 'Graafsma, Heinz' 'Bauer, Robert P. C.' 'Lehmk\"uhler, Felix' 'Appel, Karen' 'Kon\^opkov\'a, Zuzana' 'Tang, Minxue' 'Dwivedi, Anand Prashant' 'Sztuck-Dambietz, Jolanta' 'Randolph, Lisa' 'Buakor, Khachiwan' 'Humphries, Oliver' 'Baehtz, Carsten' 'Eklund, Tobias' 'Mohrbach, Lisa Katharina' 'Mondal, Anshuman' 'Marquardt, Hauke' 'O Bannon, Earl Francis' 'Amann-Winkel, Katrin' 'Yoo, Choong-Shik' 'Zastrau, Ulf' 'Liermann, Hanns-Peter' 'Nada, Hiroki' 'Lee, Geun Woo' _publ_section_title ; Multiple freezing--melting pathways of high-density ice through ice XXI phase at room temperature ; _journal_name_full 'Nature Materials' _journal_page_first 1 _journal_paper_doi 10.1038/s41563-025-02364-x _journal_year 2025 _chemical_formula_moiety O _chemical_formula_sum 'H2 O' _chemical_formula_weight 18.02 _chemical_name_common Water _chemical_name_systematic Oxidane _space_group_crystal_system tetragonal _space_group_IT_number 122 _space_group_name_Hall 'I -4 2bw' _space_group_name_H-M_alt 'I -4 2 d' _atom_sites_solution_hydrogens . _atom_sites_solution_primary dual _audit_creation_date 2025-04-29 _audit_creation_method ; Olex2 1.5 (compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 152 _cell_length_a 20.1966(16) _cell_length_b 20.1966(16) _cell_length_c 7.8912(6) _cell_measurement_reflns_used 427 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 10.3010 _cell_measurement_theta_min 1.6190 _cell_volume 3218.8(4) _computing_cell_refinement 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 5.0000 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \f -12.00 11.00 0.50 1.00 0.00 0.00 0.00 -- 46 2 \f -12.00 11.00 0.50 1.00 0.00 0.00 0.00 -- 46 3 \f -12.00 11.00 0.50 1.00 0.00 0.00 0.00 -- 46 4 \f -12.00 11.00 0.50 1.00 0.00 0.00 0.00 -- 46 5 \f -12.00 11.00 0.50 1.00 0.00 0.00 0.00 -- 46 6 \f -12.00 11.00 0.50 1.00 0.00 0.00 0.00 -- 46 7 \f -12.00 11.00 0.50 1.00 0.00 0.00 0.00 -- 46 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'esperanto-CrysAlisPro-abstract goniometer imported esperanto images' _diffrn_measurement_method '\f scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0009532000 _diffrn_orient_matrix_UB_12 0.0142782000 _diffrn_orient_matrix_UB_13 -0.0004853000 _diffrn_orient_matrix_UB_21 0.0065430000 _diffrn_orient_matrix_UB_22 -0.0006126000 _diffrn_orient_matrix_UB_23 -0.0326696000 _diffrn_orient_matrix_UB_31 -0.0127475000 _diffrn_orient_matrix_UB_32 0.0007295000 _diffrn_orient_matrix_UB_33 -0.0168161000 _diffrn_radiation_monochromator synchrotron _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.2896 _diffrn_reflns_av_R_equivalents 0.2217 _diffrn_reflns_av_unetI/netI 0.0956 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 4726 _diffrn_reflns_point_group_measured_fraction_full 0.967 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 8.306 _diffrn_reflns_theta_max 8.306 _diffrn_reflns_theta_min 1.620 _diffrn_source synchrotron _exptl_absorpt_coefficient_mu 0.039 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.413 _exptl_crystal_description prismatic _exptl_crystal_F_000 1216 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.323 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.086 _refine_ls_abs_structure_details ; Flack x determined using 152 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.328 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 39 _refine_ls_number_reflns 819 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.328 _refine_ls_R_factor_all 0.1275 _refine_ls_R_factor_gt 0.0941 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2678 _refine_ls_wR_factor_ref 0.3422 _reflns_Friedel_coverage 0.685 _reflns_Friedel_fraction_full 0.943 _reflns_Friedel_fraction_max 0.943 _reflns_number_gt 608 _reflns_number_total 819 _reflns_threshold_expression 'I > 2\s(I)' _journal_article_reference https://doi.org/10.1038/s41563-025-02364-x _cod_data_source_file iceXXI_KRISS.cif _cod_data_source_block iceXXI_KRISS _cod_depositor_comments 'Releasing structure 3000611 into public domain as published material.' _cod_original_cell_volume 3218.8(6) _cod_original_formula_sum H2O _cod_database_code 3000611 _shelx_shelxl_version_number 2019/3 _chemical_oxdiff_formula O0 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _cell_oxdiff_angle_alpha 90.03(3) _cell_oxdiff_angle_beta 90.007(5) _cell_oxdiff_angle_gamma 90.07(2) _cell_oxdiff_length_a 20.1670(14) _cell_oxdiff_length_b 20.252(18) _cell_oxdiff_length_c 7.8814(5) _cell_oxdiff_measurement_reflns_used 432 _cell_oxdiff_volume 3219(3) _diffrn_orient_matrix_axis[1] matrixX _diffrn_orient_matrix_axis[2] matrixY _diffrn_orient_matrix_axis[3] matrixZ _olex2_refinement_description ; ; _shelx_res_file ; TITL merge_250429_a.res in I-42d merge_250429.res created by SHELXL-2019/3 at 15:19:18 on 29-Apr-2025 REM Old TITL merge_250429_a.res in I-42d REM SHELXT solution in I-42d: R1 0.250, Rweak 0.015, Alpha 0.003 REM 0.061 for 24 systematic absences, Orientation as input REM Flack x = -9.990 ( 9.990 ) from 219 Parsons' quotients REM Formula found by SHELXT: O CELL 0.2896 20.1966 20.1966 7.8912 90 90 90 ZERR 192 0.0016 0.0016 0.0006 0 0 0 LATT -2 SYMM -X,-Y,+Z SYMM +Y,-X,-Z SYMM -Y,+X,-Z SYMM 0.5-X,+Y,0.75-Z SYMM 0.5+X,-Y,0.75-Z SYMM 0.5-Y,-X,0.75+Z SYMM 0.5+Y,+X,0.75+Z SFAC O DISP O -0.001 0.0008 6.4585 UNIT 192 L.S. 10 0 0 PLAN 50 CONF list 4 MORE -1 fmap 2 53 acta OMIT -11 14 3 OMIT -10 10 4 OMIT -7 7 2 OMIT -7 7 6 OMIT -6 6 4 OMIT -6 7 5 OMIT -5 5 6 OMIT -4 13 3 OMIT -4 14 4 OMIT -4 15 5 OMIT 2 12 0 OMIT 4 15 3 OMIT 4 16 4 OMIT 5 5 6 OMIT 6 10 4 OMIT 6 11 5 OMIT 7 11 6 OMIT 8 14 4 OMIT 10 11 3 REM REM REM WGHT 0.200000 FVAR 0.39163 O1 1 0.000000 0.500000 0.507251 10.50000 0.06584 O2 1 0.897983 0.614097 0.000619 11.00000 0.06519 O3 1 0.823608 0.917279 0.856241 11.00000 0.06561 O4 1 0.561127 0.678237 0.145706 11.00000 0.06516 O5 1 0.767784 0.575390 0.037910 11.00000 0.06071 O6 1 0.956616 0.735946 0.958449 11.00000 0.06713 O7 1 0.888071 0.535712 0.698309 11.00000 0.06341 O8 1 0.020485 0.387939 0.298506 11.00000 0.06882 O9 1 0.692818 0.688158 0.043729 11.00000 0.07734 O10 1 0.825744 0.783762 0.963033 11.00000 0.07592 HKLF 4 REM merge_250429_a.res in I-42d REM wR2 = 0.3422, GooF = S = 1.328, Restrained GooF = 1.328 for all data REM R1 = 0.0941 for 608 Fo > 4sig(Fo) and 0.1275 for all 819 data REM 39 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.323, deepest hole -0.365, 1-sigma level 0.086 Q1 1 0.9005 0.5772 0.8399 11.00000 0.05 0.32 Q2 1 0.7813 0.6709 1.0118 11.00000 0.05 0.30 Q3 1 0.9780 0.7987 0.9537 11.00000 0.05 0.30 Q4 1 0.7500 0.5565 0.8750 10.50000 0.05 0.29 Q5 1 0.9142 0.5143 0.5113 11.00000 0.05 0.28 Q6 1 0.9196 0.6788 0.8408 11.00000 0.05 0.28 Q7 1 0.9264 0.6013 1.1451 11.00000 0.05 0.27 Q8 1 1.0199 0.4244 0.5088 11.00000 0.05 0.27 Q9 1 0.9832 0.6783 1.1028 11.00000 0.05 0.26 Q10 1 0.7453 0.6337 1.1232 11.00000 0.05 0.25 Q11 1 0.6947 0.7244 1.2308 11.00000 0.05 0.25 Q12 1 0.7027 0.7631 1.0479 11.00000 0.05 0.24 Q13 1 0.7151 0.7389 1.1726 11.00000 0.05 0.24 Q14 1 1.0000 0.5000 0.7500 10.25000 0.05 0.23 Q15 1 0.9663 0.5425 0.7077 11.00000 0.05 0.23 Q16 1 1.0319 0.4183 0.4905 11.00000 0.05 0.23 Q17 1 0.5176 0.6956 1.0625 11.00000 0.05 0.23 Q18 1 0.6395 0.6781 1.1471 11.00000 0.05 0.23 Q19 1 0.9508 0.7500 1.1250 10.50000 0.05 0.22 Q20 1 0.9361 0.7500 1.1250 10.50000 0.05 0.22 Q21 1 0.8232 0.9205 0.6671 11.00000 0.05 0.22 Q22 1 0.9624 0.6409 0.9925 11.00000 0.05 0.21 Q23 1 0.7320 0.6379 0.9196 11.00000 0.05 0.21 Q24 1 0.5807 0.7500 1.1250 10.50000 0.05 0.21 Q25 1 0.9767 0.3413 0.2389 11.00000 0.05 0.21 Q26 1 1.0815 0.4203 0.2039 11.00000 0.05 0.20 Q27 1 1.0564 0.3452 0.4116 11.00000 0.05 0.20 Q28 1 0.9386 0.5379 0.5506 11.00000 0.05 0.20 Q29 1 0.9000 0.6996 0.8834 11.00000 0.05 0.20 Q30 1 0.7216 0.5192 1.0885 11.00000 0.05 0.20 Q31 1 0.8173 0.8832 0.9020 11.00000 0.05 0.19 Q32 1 0.9526 0.5838 1.1021 11.00000 0.05 0.19 Q33 1 1.0582 0.4452 0.4104 11.00000 0.05 0.19 Q34 1 0.4784 0.6792 1.1574 11.00000 0.05 0.18 Q35 1 0.9018 0.7629 0.9635 11.00000 0.05 0.18 Q36 1 0.5946 0.7135 1.0882 11.00000 0.05 0.18 Q37 1 1.0433 0.5624 0.4250 11.00000 0.05 0.18 Q38 1 0.8319 0.7808 1.0985 11.00000 0.05 0.18 Q39 1 1.0584 0.5267 0.6048 11.00000 0.05 0.18 Q40 1 0.6010 0.6933 1.3404 11.00000 0.05 0.18 Q41 1 1.0000 0.5000 0.2500 10.25000 0.05 0.18 Q42 1 0.8778 0.8560 0.9511 11.00000 0.05 0.18 Q43 1 0.8021 0.6000 1.0571 11.00000 0.05 0.18 Q44 1 0.7500 0.9130 0.8750 10.50000 0.05 0.18 Q45 1 1.0473 0.3605 0.4089 11.00000 0.05 0.18 Q46 1 0.8168 0.7638 1.0671 11.00000 0.05 0.18 Q47 1 0.8270 0.9170 1.0503 11.00000 0.05 0.18 Q48 1 0.7500 0.7153 0.8750 10.50000 0.05 0.18 Q49 1 0.6265 0.6591 1.0789 11.00000 0.05 0.17 Q50 1 0.7610 0.5025 1.0216 11.00000 0.05 0.17 ; _shelx_res_checksum 13496 _shelx_hkl_file ; 0 0 -2 0.12 2.45 0 0 -2 0.88 2.75 0 0 2 0.84 1.51 0 0 -2 -0.71 1.83 0 0 2 -0.38 2.73 0 0 2 -0.08 1.55 0 0 -4 2610.99 33.69 0 0 4 2537.65 31.92 0 0 -4 2605.29 32.36 0 0 -6 -4.86 7.47 0 0 6 0.69 7.11 0 0 -6 0.08 5.65 0 0 -6 5.58 9.75 0 0 6 -3.40 6.60 -1 0 -3 31.64 5.13 1 0 3 26.29 6.30 0 -1 3 22.85 6.31 0 -1 3 29.32 3.79 -1 0 -3 33.60 3.86 1 0 -3 27.41 5.36 1 0 -3 41.49 5.15 0 1 3 33.51 3.99 0 1 -3 32.23 3.97 -1 0 -3 43.48 6.03 0 -1 -3 29.89 5.86 -1 0 3 29.05 3.73 0 1 3 34.00 4.13 1 0 -3 31.37 4.21 0 -1 3 24.07 5.08 1 0 3 42.48 3.39 -1 0 3 31.62 4.05 1 0 3 31.41 4.07 1 0 3 24.85 3.52 0 1 -3 34.11 4.30 0 -1 -5 0.28 5.75 0 -1 5 2.28 2.80 0 1 -5 0.65 5.07 0 -1 5 1.23 4.83 0 -1 5 3.33 6.86 1 0 5 -0.11 9.20 -1 0 5 1.33 5.22 0 1 -5 3.12 5.13 1 0 5 0.27 5.50 0 1 5 -0.57 5.55 -1 0 -5 1.72 5.16 0 1 -5 -1.04 9.67 1 0 -5 3.29 6.08 0 -1 -5 1.80 8.31 1 0 -5 3.10 5.69 1 0 -5 -0.71 7.55 1 0 5 0.25 5.11 -1 0 5 3.95 5.63 0 -1 -5 3.08 2.88 -1 0 -5 1.83 4.61 -1 0 -5 3.84 7.17 1 0 5 1.42 3.17 0 1 5 0.54 4.57 0 -1 5 2.58 8.74 -1 0 7 9.95 8.03 0 -1 7 -0.27 6.98 0 -1 -7 4.67 11.64 -1 0 7 2.00 7.33 1 0 7 -6.76 8.90 0 1 -7 4.96 7.74 0 1 7 2.83 6.85 0 1 -7 3.22 7.62 1 0 7 4.74 7.01 1 0 7 3.03 13.18 1 0 7 4.71 8.71 -1 0 -7 0.88 6.89 1 0 -7 6.01 8.36 1 0 -7 0.24 10.63 0 1 7 4.04 6.82 0 -1 7 2.85 9.21 -1 1 6 111.49 10.56 1 -1 6 99.43 14.63 -1 1 6 105.44 10.06 1 1 -6 151.10 13.98 1 -1 6 106.76 10.11 1 1 -6 104.68 10.47 -1 -1 -6 139.22 8.61 1 -1 6 114.28 7.06 -1 -1 -6 109.06 14.76 1 -1 4 -1.25 4.23 -1 -1 -4 -0.75 3.04 1 -1 4 -1.10 2.53 1 -1 4 1.21 6.48 1 1 -4 -1.89 4.42 -1 1 4 1.11 4.14 1 1 -4 1.23 4.56 -1 1 4 1.41 6.14 1 -1 4 0.79 7.07 1 1 -4 -1.96 4.62 -1 -1 -4 1.79 7.14 -1 -1 -2 8.02 3.82 1 1 -2 10.05 2.01 1 1 -2 9.10 2.27 -1 1 2 13.34 2.41 1 -1 2 9.49 4.40 -1 1 -2 11.93 2.10 -1 1 -2 8.80 3.95 1 1 2 9.80 3.87 -1 1 -2 11.59 2.49 -1 -1 4 1.78 5.90 -1 1 -4 -0.55 4.03 -1 -1 4 -1.78 5.11 1 -1 -4 -0.10 1.34 -1 -1 4 -0.74 4.18 1 1 4 0.87 6.82 -1 1 -4 1.79 3.94 1 1 4 -0.74 4.20 1 -1 -4 -0.61 3.68 1 -1 -4 1.16 5.32 -1 1 -6 120.63 10.88 1 1 6 114.57 10.16 1 -1 -6 119.58 11.19 1 -1 -6 142.95 6.70 -1 1 -6 168.80 15.82 -1 -1 6 111.88 10.13 1 1 6 124.28 10.17 1 -1 -6 -1.06 1.80 -1 -1 6 1.77 7.53 1 -1 -6 77.36 12.46 2 0 2 44.47 2.99 2 0 -2 51.21 3.93 -2 0 2 33.43 2.76 2 0 2 48.96 3.28 2 0 -2 37.92 3.56 -2 0 2 37.80 3.46 0 -2 2 30.16 5.29 -2 0 -2 39.74 2.88 -2 0 -2 64.15 5.67 2 0 2 38.17 4.35 0 2 -2 28.06 5.04 2 0 2 39.85 3.97 2 0 2 28.86 4.72 0 2 -4 10.00 4.61 0 2 -4 13.70 4.12 -2 0 4 10.38 4.80 -2 0 -4 10.43 5.21 2 0 4 13.32 4.71 2 0 4 10.54 7.75 2 0 4 13.82 4.23 2 0 -4 9.58 4.15 2 0 -4 10.06 5.61 2 0 4 16.88 3.95 2 0 -4 14.17 1.56 0 2 4 2.02 2.86 0 -2 4 10.02 5.86 0 -2 -4 -3.15 5.36 2 0 4 1.19 6.21 2 0 -4 15.21 5.24 0 2 4 -0.06 2.89 -2 0 -4 9.23 5.19 0 -2 -4 15.10 1.44 -2 0 4 14.43 4.24 -2 0 -4 11.67 3.83 2 0 -6 1389.11 29.97 2 0 -6 1326.00 29.22 2 0 6 -2.16 9.02 0 2 -6 1482.16 32.68 0 2 6 73.86 12.13 -2 0 6 1531.94 32.11 -2 0 6 1436.85 30.70 0 -2 6 1652.16 20.46 0 2 -6 1363.91 30.62 0 -2 -6 1199.60 36.28 0 -2 -6 1697.37 23.81 -2 0 -6 1515.50 30.77 2 0 6 1472.70 29.10 0 -2 6 7.94 10.85 2 0 6 1277.66 38.43 0 2 6 1492.67 30.59 2 0 6 1424.73 31.82 2 0 -6 1049.18 29.74 -2 0 -6 1455.68 32.36 -2 0 -6 1367.70 28.30 2 0 6 1449.78 23.79 0 -2 6 1186.31 33.88 2 -1 7 87.17 7.78 2 1 -7 108.56 11.83 1 -2 7 -0.61 11.84 1 -2 7 118.35 7.68 -2 1 7 102.67 11.11 2 1 -7 119.96 11.92 -1 -2 -7 94.25 15.98 1 2 -7 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-18 1 2.95 6.02 -18 3 -1 37.64 4.20 -18 3 -1 33.31 6.20 18 3 1 0.06 4.10 -18 3 -1 1.47 4.62 18 3 1 40.78 9.51 -18 -3 3 -0.01 1.52 -18 3 -3 65.91 11.70 18 3 3 -4.84 9.44 3 18 3 -1.87 4.85 18 3 3 44.62 10.65 18 4 -2 -0.48 7.06 18 4 -2 -0.45 4.01 -18 4 2 -0.89 4.59 -4 18 2 -0.66 4.95 -18 -4 -2 1.25 3.38 4 -18 2 -3.07 5.66 -18 4 0 1.07 3.70 4 -18 0 44.74 9.93 -4 18 0 52.87 11.42 -18 4 0 0.19 3.42 -4 -18 0 3.73 5.71 18 4 0 44.40 9.89 -18 4 -2 -0.04 2.04 18 4 2 3.54 8.37 18 4 2 -1.91 5.91 18 4 2 1.97 3.73 -18 4 -2 -0.36 5.25 4 18 2 0.48 5.89 -18 4 -2 4.22 7.41 18 5 -1 34.42 9.82 -18 -5 -1 48.17 12.53 -5 -18 -1 44.70 8.26 5 -18 1 40.60 10.15 -5 18 1 38.00 8.94 18 5 1 50.42 11.22 18 5 1 1.77 6.87 -18 5 -1 -0.86 5.35 -18 5 -1 -0.54 3.64 -18 -5 1 48.52 11.91 -18 -6 -2 7.61 9.64 18 6 -2 -0.47 4.87 -18 6 2 1.32 3.08 -6 18 2 -1.43 5.39 6 -18 2 -2.53 6.62 -18 -6 0 0.74 8.86 18 6 0 2.57 8.73 18 6 0 1.13 8.42 -18 6 0 -1.43 3.86 6 -18 0 -2.84 9.89 -6 -18 0 -0.85 5.47 -6 18 0 0.49 9.76 -18 -6 2 9.05 9.77 -18 -6 2 0.10 1.97 18 6 2 5.88 10.16 18 6 2 -5.21 12.38 -18 6 -2 5.12 7.72 -18 -7 -1 2.96 8.82 18 7 -1 12.06 10.02 -7 -18 -1 9.47 5.98 7 -18 1 7.17 9.31 -7 18 1 -3.38 8.43 -18 -7 1 -0.43 1.72 -18 -7 1 13.38 8.54 18 7 1 3.70 12.51 -18 -7 1 -0.08 5.91 -18 7 -1 5.59 6.36 -18 -8 0 0.18 1.45 -18 -8 0 10.97 8.99 18 8 0 4.95 12.67 -18 -8 0 -1.66 5.38 8 -18 0 15.43 12.23 -18 8 0 -0.64 4.80 -8 18 0 6.03 8.37 -8 -18 0 -2.72 4.71 19 0 -1 -1.68 4.50 19 0 1 -0.14 5.50 19 0 -1 0.78 5.20 0 -19 -1 1.08 10.08 -19 0 -1 1.75 3.95 0 -19 1 0.21 6.05 19 -1 2 0.75 4.14 19 1 -2 -0.21 4.64 19 1 -2 -2.68 6.15 -1 19 2 0.84 6.75 -19 -1 -2 -0.24 4.62 19 1 0 -0.70 5.26 19 1 0 2.70 4.43 1 -19 0 7.93 8.25 -1 -19 0 5.25 7.53 19 1 0 2.65 4.17 19 1 2 0.25 5.36 19 1 2 -2.44 6.36 1 19 2 1.41 6.57 -19 1 -2 0.18 5.27 19 2 -1 -1.97 6.37 -19 2 1 2.49 4.92 19 2 -1 2.64 3.21 -2 -19 -1 1.72 8.12 19 2 -1 0.24 4.70 2 -19 1 2.23 6.22 -2 19 1 6.01 7.84 19 2 1 -0.74 6.74 -19 2 -1 4.06 5.19 2 -19 -1 5.11 8.91 19 2 1 2.62 5.15 -19 2 -1 2.51 4.89 -2 -19 1 2.22 5.44 19 2 1 0.97 3.17 -19 3 2 56.29 7.62 19 3 -2 4.15 7.11 19 3 -2 2.07 5.37 19 3 -2 0.26 2.25 -19 -3 -2 63.40 5.82 -3 19 2 0.81 6.00 3 -19 2 -1.05 5.48 19 3 0 1.16 3.42 19 3 0 -1.35 7.64 -19 3 0 16.48 4.58 19 3 0 -1.64 5.18 -19 3 0 10.87 5.06 3 -19 0 18.37 8.88 -3 -19 0 15.41 7.19 19 3 2 -2.71 9.07 -19 3 -2 67.14 10.53 19 3 2 -1.65 8.55 3 19 2 53.37 7.70 -19 3 -2 61.48 8.79 19 4 -1 22.87 8.18 -19 4 1 -1.33 4.45 -4 -19 -1 18.55 8.30 -19 4 1 1.67 2.78 4 -19 1 15.56 8.25 -4 19 1 18.66 7.91 -19 4 -1 -1.13 3.28 19 4 1 -0.58 3.51 -19 4 -1 -1.32 4.26 -19 4 -1 -0.48 5.19 -19 -5 0 5.53 11.47 19 5 0 10.52 9.55 5 -19 0 4.13 10.02 -19 5 0 -0.40 2.85 -5 -19 0 -1.84 5.80 -5 19 0 15.96 10.55 -19 -6 -1 13.46 11.36 19 6 -1 -0.83 6.26 -19 6 1 0.67 2.69 -6 -19 -1 6.04 6.62 6 -19 1 6.58 8.51 -6 19 1 5.56 8.01 -19 -6 1 10.28 10.25 19 6 1 10.08 8.85 19 6 1 1.63 8.97 -19 6 -1 -2.04 5.94 20 0 0 55.20 6.51 0 -20 0 64.84 9.98 20 2 0 -0.25 6.72 -20 2 0 0.19 3.78 20 2 0 -0.85 4.43 20 2 0 0.05 4.40 2 -20 0 2.19 8.65 -2 -20 0 1.03 7.35 0 0 0 0.00 0.00 TITL merge_250429 in I-42d REM I-42d (#122 in standard setting) CELL 0.28960 20.196624 20.196624 7.891245 90.0000 90.0000 90.0000 ZERR 176.00 0.001619 0.001619 0.000551 0.0000 0.0000 0.0000 LATT -2 SYMM -x,-y, z SYMM y,-x,-z SYMM -y, x,-z SYMM -x+1/2, y,-z+3/4 SYMM x+1/2,-y,-z+3/4 SYMM -y+1/2,-x, z+3/4 SYMM y+1/2, x, z+3/4 SFAC O UNIT 176.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 58692 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.751 _oxdiff_exptl_absorpt_empirical_full_min 0.112 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' 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 O1 O 0.000000 0.500000 0.5073(16) 0.066(3) Uiso 1 2 d S . P . . O2 O 0.8980(3) 0.6141(4) 0.0006(9) 0.065(3) Uiso 1 1 d . . . . . O3 O 0.8236(4) 0.9173(4) 0.8562(10) 0.066(3) Uiso 1 1 d . . . . . O4 O 0.5611(3) 0.6782(4) 0.1457(10) 0.065(3) Uiso 1 1 d . . . . . O5 O 0.7678(3) 0.5754(3) 0.0379(9) 0.061(3) Uiso 1 1 d . . . . . O6 O 0.9566(4) 0.7359(4) 0.9584(9) 0.067(3) Uiso 1 1 d . . . . . O7 O 0.8881(3) 0.5357(4) 0.6983(9) 0.063(3) Uiso 1 1 d . . . . . O8 O 0.0205(4) 0.3879(4) 0.2985(10) 0.069(3) Uiso 1 1 d . . . . . O9 O 0.6928(4) 0.6882(4) 0.0437(9) 0.077(3) Uiso 1 1 d . . . . . O10 O 0.8257(4) 0.7838(4) 0.9630(9) 0.076(3) Uiso 1 1 d . . . . . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O -0.0010 0.0008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H 'not located in XRD' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _axis.id _axis.type _axis.equipment _axis.parity _axis.depends_on _axis.zero _axis.vector[1] _axis.vector[2] _axis.vector[3] source . source . . . 1.00000000 0.00000000 0.00000000 omega rotation goniometer -1 . 0.00000000 0.00000000 0.00000000 1.00000000 kappa rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000 0.64278761 phi rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000 theta rotation goniometer -1 . -0.19277000 0.00000000 0.00000000 1.00000000 matrixX general general . phi . 1.00000000 0.00000000 0.00000000 matrixY general general . phi . 0.00000000 1.00000000 0.00000000 matrixZ general general . phi . 0.00000000 0.00000000 1.00000000 dacX translation general . phi . 0.00000000 1.00000000 0.00000000 dacY translation general . phi . -1.00000000 0.00000000 0.00000000 dacZ translation general . phi . 0.00000000 0.00000000 1.00000000