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_1567354
_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             2022-03-16
_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                   6.1737(5)
_cell_length_b                   6.1737(5)
_cell_length_c                   5.6843(3)
_cell_measurement_reflns_used    1312
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.7120
_cell_measurement_theta_min      3.6700
_cell_volume                     216.65(3)
_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                 '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_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -37.00  59.00   1.00   35.00    --  -25.00 -19.00-180.00   96
  2  \w    -63.00  26.00   1.00   35.00    --  -25.00  67.00 -23.00   89
  3  \w    -52.00 -21.00   1.00   35.00    --  -25.00 -38.00  30.00   31
  4  \w    -62.00  37.00   1.00   35.00    --  -25.00  39.00 167.00   99
  5  \w      8.00  51.00   1.00   35.00    --  -25.00-135.00-123.00   43
  6  \w    -37.00  29.00   1.00   35.00    --  -25.00 -39.00-167.00   66
  7  \w    -21.00  20.00   1.00   35.00    --  -25.00 -81.00-151.00   41
  8  \w      8.00  51.00   1.00   35.00    --  -25.00-135.00  57.00   43
  9  \w    -41.00  55.00   1.00   35.00    --  -25.00 -26.00   8.00   96
 10  \w     21.00 101.00   1.00   35.00    --   25.16-135.00-123.00   80
 11  \w    -34.00  57.00   1.00   35.00    --   25.16 -26.00-171.00   91
 12  \w     -8.00  79.00   1.00   35.00    --   25.16 -97.00  35.00   87
 13  \w    -20.00  21.00   1.00   35.00    --   25.16  81.00 151.00   41
 14  \w   -115.00 -87.00   1.00   35.00    --  -25.00-160.00  90.00   28
 15  \w    -73.00 -40.00   1.00   35.00    --  -25.00  38.00-120.00   33
 16  \w    -73.00 -40.00   1.00   35.00    --  -25.00  38.00  60.00   33
 17  \w    -14.00  29.00   1.00   35.00    --  -25.00 -97.00  35.00   43
 18  \w     -5.00   7.00   1.00   35.00    --  -25.00-114.00-135.00   12
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0592310000
_diffrn_orient_matrix_UB_12      0.0662281000
_diffrn_orient_matrix_UB_13      -0.0193139000
_diffrn_orient_matrix_UB_21      -0.0437671000
_diffrn_orient_matrix_UB_22      0.0184545000
_diffrn_orient_matrix_UB_23      -0.0838208000
_diffrn_orient_matrix_UB_31      -0.0527781000
_diffrn_orient_matrix_UB_32      0.0590096000
_diffrn_orient_matrix_UB_33      0.0478433000
_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_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       disc
_exptl_crystal_F_000             100.058
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.2649
_refine_diff_density_min         -0.2772
_refine_diff_density_rms         0.0698
_refine_ls_d_res_high            0.6231
_refine_ls_d_res_low             4.3655
_refine_ls_goodness_of_fit_ref   1.1553
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     22
_refine_ls_number_reflns         238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1553
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+0.0138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0751
_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_IAM
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_database_code               1567354
_chemical_oxdiff_formula         H2O
_olex2_refinement_description
;
1. Others
 Fixed Sof: H1a(0.5) H2(0.25) H1b(0.25) H1c(0.25)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.858