Accurate crystal structure of ice VI from X-ray diffraction with Hirshfeld atom refinement
Chodkiewicz, Michal L.; Gajda, Roman; Lavina, Barbara; Tkachev, Sergey; Prakapenka, Vitali B.; Dera, Przemyslaw; Wozniak, Krzysztof; IUCrJ 9 (2022) –; doi:10.1107/S2052252522006662

data_1567350
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            10
_cell_length_a                   6.1711(3)
_cell_length_b                   6.1711(3)
_cell_length_c                   5.6747(5)
_cell_measurement_reflns_used    594
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.2430
_cell_measurement_theta_min      2.3260
_cell_volume                     216.11(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.9669
_diffrn_measured_fraction_theta_max 0.7640
_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     40.00 141.00   1.00    8.00  90.00   0.00   0.00    --   101
  2  \f    220.00 321.00   1.00    8.00  90.00   0.00   0.00    --   101
;
_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      0.0398331000
_diffrn_orient_matrix_UB_12      0.0681823000
_diffrn_orient_matrix_UB_13      0.0191399000
_diffrn_orient_matrix_UB_21      -0.0705867000
_diffrn_orient_matrix_UB_22      0.0390939000
_diffrn_orient_matrix_UB_23      0.0091277000
_diffrn_orient_matrix_UB_31      -0.0014347000
_diffrn_orient_matrix_UB_32      -0.0195093000
_diffrn_orient_matrix_UB_33      0.0855992000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.50014
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_Laue_measured_fraction_full 0.9669
_diffrn_reflns_Laue_measured_fraction_max 0.7640
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            1022
_diffrn_reflns_point_group_measured_fraction_full 0.9669
_diffrn_reflns_point_group_measured_fraction_max 0.7640
_diffrn_reflns_theta_full        17.4626
_diffrn_reflns_theta_max         22.95
_diffrn_reflns_theta_min         3.29
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       disc
_exptl_crystal_F_000             100.044
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.8179
_refine_diff_density_min         -0.5335
_refine_diff_density_rms         0.2228
_refine_ls_d_res_high            0.6414
_refine_ls_d_res_low             4.3636
_refine_ls_goodness_of_fit_ref   0.9361
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     22
_refine_ls_number_reflns         191
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.9174
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0776
_refine_ls_shift/su_max          0.0018
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1575P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              0
_reflns_limit_k_max              5
_reflns_limit_k_min              0
_reflns_limit_l_max              7
_reflns_limit_l_min              0
_reflns_number_gt                178
_reflns_number_total             191
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            lt5051.cif
_cod_data_source_block           D2O_DESY_IAM
_cod_original_cell_volume        216.11(3)
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_database_code               1567350
_chemical_oxdiff_formula         H2O
_olex2_refinement_description
;
1. Restrained distances
 O1-H1a
 0.952 with sigma of 0.02
 O1-H1b
 0.952 with sigma of 0.02
 O1-H1c
 0.952 with sigma of 0.02
 O2-H2
 0.952 with sigma of 0.02
 H1a-H1b
 1.5 with sigma of 0.04
 H1b-H1a
 1.5 with sigma of 0.04
 H1b-H1c
 1.5 with sigma of 0.04
2. Others
 Fixed Sof: H1a(0.5) H1b(0.25) H2(0.25) H1c(0.25)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.422
_oxdiff_exptl_absorpt_empirical_full_min 0.681