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_1567352
_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             2022-03-15
_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                   6.1918(4)
_cell_length_b                   6.1918(4)
_cell_length_c                   5.7067(4)
_cell_measurement_reflns_used    1022
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.5850
_cell_measurement_theta_min      3.6640
_cell_volume                     218.79(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 0.9180
_diffrn_measured_fraction_theta_max 0.8856
_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    -99.00 -22.00   1.00   60.00    --  -25.00 135.00 -57.00   77
  2  \w    -62.00  23.00   1.00   60.00    --  -25.00  39.00 167.00   85
  3  \w    -73.00 -46.00   1.00   60.00    --  -25.00  38.00   0.00   27
  4  \w    -43.00  15.00   1.00   60.00    --  -25.00  53.00 -17.00   58
  5  \w      4.00  29.00   1.00   60.00    --  -25.00 -39.00-167.00   25
  6  \w     -5.00  26.00   1.00   60.00    --  -25.00-114.00  45.00   31
  7  \w     -5.00  44.00   1.00   60.00    --  -25.00 -26.00   8.00   49
  8  \w    -38.00 -13.00   1.00   60.00    --  -25.00 -57.00  30.00   25
  9  \w    -98.00 -21.00   1.00   60.00    --  -25.00 135.00 123.00   77
 10  \w      8.00  35.00   1.00   60.00    --  -25.00-135.00-123.00   27
 11  \w    -37.00 -11.00   1.00   60.00    --  -25.00 -39.00-167.00   26
 12  \w    -16.00  10.00   1.00   60.00    --   25.16 -26.00   8.00   26
 13  \w    -23.00  14.00   1.00   60.00    --   25.16  97.00 -35.00   37
 14  \w      2.00  28.00   1.00   60.00    --   25.16  19.00-180.00   26
 15  \w    -39.00  -1.00   1.00   60.00    --   25.16  19.00-180.00   38
 16  \w      1.00  36.00   1.00   60.00    --   25.16  39.00 -12.00   35
;
_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      0.0592605000
_diffrn_orient_matrix_UB_12      0.0609523000
_diffrn_orient_matrix_UB_13      -0.0331758000
_diffrn_orient_matrix_UB_21      0.0536528000
_diffrn_orient_matrix_UB_22      -0.0666710000
_diffrn_orient_matrix_UB_23      -0.0314616000
_diffrn_orient_matrix_UB_31      -0.0421458000
_diffrn_orient_matrix_UB_32      0.0008159000
_diffrn_orient_matrix_UB_33      -0.0866928000
_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  0.0357
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.9180
_diffrn_reflns_Laue_measured_fraction_max 0.8856
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2579
_diffrn_reflns_point_group_measured_fraction_full 0.9180
_diffrn_reflns_point_group_measured_fraction_max 0.8856
_diffrn_reflns_theta_full        19.6651
_diffrn_reflns_theta_max         26.66
_diffrn_reflns_theta_min         3.67
_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_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80935
_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    1.367
_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         0.1583
_refine_diff_density_min         -0.1445
_refine_diff_density_rms         0.0351
_refine_ls_d_res_high            0.6249
_refine_ls_d_res_low             4.3783
_refine_ls_goodness_of_fit_ref   0.9349
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     22
_refine_ls_number_reflns         240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9349
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0159
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0231
_refine_ls_wR_factor_ref         0.0265
_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                182
_reflns_number_total             240
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            lt5051.cif
_cod_data_source_block           D2O_home_IAM
_cod_original_cell_volume        218.79(2)
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_database_code               1567352
_chemical_oxdiff_formula         H2O
_olex2_refinement_description
;
1. 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 1.246
_oxdiff_exptl_absorpt_empirical_full_min 0.877