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#$Date: 2022-07-23 07:17:47 +0300 (Sat, 23 Jul 2022) $
#$Revision: 276901 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/73/1567353.cif $
#------------------------------------------------------------------------------
#
# 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_1567353
loop_
_publ_author_name
'Chodkiewicz, Michal L.'
'Gajda, Roman'
'Lavina, Barbara'
'Tkachev, Sergey'
'Prakapenka, Vitali B.'
'Dera, Przemyslaw'
'Wozniak, Krzysztof'
_publ_section_title
;
 Accurate crystal structure of ice VI from X-ray diffraction with
 Hirshfeld atom refinement
;
_journal_issue                   5
_journal_name_full               IUCrJ
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052252522006662
_journal_volume                  9
_journal_year                    2022
_chemical_formula_moiety         'H2 O'
_chemical_formula_sum            'H2 O'
_chemical_formula_weight         18.015
_space_group_crystal_system      tetragonal
_space_group_IT_number           137
_space_group_name_Hall           '-P 4ac 2a'
_space_group_name_H-M_alt        'P 42/n m c :2'
_symmetry_Int_Tables_number      137
_audit_creation_date             2022-01-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            10
_cell_length_a                   6.1737(5)
_cell_length_b                   6.1737(5)
_cell_length_c                   5.6843(3)
_cell_measurement_reflns_used    1312
_cell_measurement_temperature    293(3)
_cell_measurement_theta_max      23.7120
_cell_measurement_theta_min      3.6700
_cell_volume                     216.65(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0128
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9426
_diffrn_measured_fraction_theta_max 0.8782
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.9426
_diffrn_reflns_Laue_measured_fraction_max 0.8782
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3861
_diffrn_reflns_point_group_measured_fraction_full 0.9426
_diffrn_reflns_point_group_measured_fraction_max 0.8782
_diffrn_reflns_theta_full        19.6651
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         3.68
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    0.090
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       disc
_exptl_crystal_F_000             100.055
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.2625
_refine_diff_density_min         -0.2668
_refine_diff_density_rms         0.0680
_refine_ls_d_res_high            0.6231
_refine_ls_d_res_low             4.3655
_refine_ls_goodness_of_fit_ref   1.1654
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     36
_refine_ls_number_reflns         238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1654
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0249P)²+0.0125P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0588
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                175
_reflns_number_total             238
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            lt5051.cif
_cod_data_source_block           H2O_D2O_home_HAR
_cod_original_cell_volume        216.66(3)
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_database_code               1567353
_olex2_refinement_description
;
1. Others
 Fixed Sof: D1A(0.5) D1B(0.25) D2(0.25) D1C(0.25)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y+1/2,x,z+1/2
3 y,-x+1/2,z+1/2
4 x+1/2,-y,-z
5 -x,y+1/2,-z
6 -x+1/2,-y+1/2,z
7 y+1/2,x+1/2,-z+1/2
8 -y,-x,-z+1/2
9 -x,-y,-z
10 y-1/2,-x,-z-1/2
11 -y,x-1/2,-z-1/2
12 -x-1/2,y,z
13 x,-y-1/2,z
14 x-1/2,y-1/2,-z
15 -y-1/2,-x-1/2,z-1/2
16 y,x,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_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
O1 O 0.52984(16) 0.75 0.12913(17) 0.0379(4) Uani 1.000000 2 S T P
O2 O 0.25 0.75 -0.25 0.0403(5) Uani 1.000000 8 S T P
D1A H 0.460(4) 0.628(5) 0.215(5) 0.057(8) Uani 0.500000 1 . . .
D1B H 0.687(7) 0.75 0.127(5) 0.070(15) Uani 0.500000 2 S T P
D2 H 0.136(8) 0.75 -0.144(8) 0.073(13) Uani 0.500000 2 S T P
D1C H 0.470(7) 0.75 -0.013(8) 0.070(15) Uani 0.500000 2 S T P
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.00627 0.00358 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
D1A O1 D1A 98(3) 13_575 . ?
D1B O1 D1A 116.0(17) . . ?
D1B O1 D1A 116.0(17) . 13_575 ?
D1C O1 D1A 105(2) . . ?
D1C O1 D1A 105(2) . 13_575 ?
D1C O1 D1B 114(3) . . ?
D2 O2 D2 115(3) . 7_454 ?
D2 O2 D2 115(3) 8_664 6_565 ?
D2 O2 D2 115(3) 8_664 . ?
D2 O2 D2 99(6) 6_565 . ?
D2 O2 D2 99(6) 8_664 7_454 ?
D2 O2 D2 115(3) 6_565 7_454 ?
D1A D1A O1 166.5(11) 8_665 . ?
D1B D1B O1 179.3(18) 6_665 . ?
D1C D2 O2 171(7) 6_565 7_454 ?
D2 D1C O1 164(6) 6_565 . ?
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
O1 D1A 1.00(3) . ?
O1 D1A 1.00(3) 13_575 ?
O1 D1B 0.97(4) . ?
O1 D1C 0.89(5) . ?
O2 D2 0.93(5) 6_565 ?
O2 D2 0.93(5) 8_664 ?
O2 D2 0.93(5) 7_454 ?
O2 D2 0.93(5) . ?
D1A D1A 0.86(6) 8_665 ?
D1B D1B 0.78(9) 6_665 ?
D2 D1C 0.99(8) 6_565 ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 D1A D1A O1 -20(30) . . 8_665 8_665 ?
O1 D1A D1A O1 -20(30) 10_566 8_665 . . ?
