#------------------------------------------------------------------------------
#$Date: 2025-10-14 05:32:25 +0300 (Tue, 14 Oct 2025) $
#$Revision: 302846 $
#$URL: file:///home/coder/svn-repositories/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.'
'Lehmkühler, Felix'
'Appel, Karen'
'Konôpková, 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  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  φ    -12.00  11.00   0.50    1.00   0.00   0.00   0.00    --    46
  2  φ    -12.00  11.00   0.50    1.00   0.00   0.00   0.00    --    46
  3  φ    -12.00  11.00   0.50    1.00   0.00   0.00   0.00    --    46
  4  φ    -12.00  11.00   0.50    1.00   0.00   0.00   0.00    --    46
  5  φ    -12.00  11.00   0.50    1.00   0.00   0.00   0.00    --    46
  6  φ    -12.00  11.00   0.50    1.00   0.00   0.00   0.00    --    46
  7  φ    -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       'φ 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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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 > 2σ(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
;
;
_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
