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_1567351
_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             2021-12-08
_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                   6.1918(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_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 0.9180
_diffrn_measured_fraction_theta_max 0.8856
_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  0.0357
_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    0.089
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.367
_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         0.1508
_refine_diff_density_min         -0.1232
_refine_diff_density_rms         0.0352
_refine_ls_d_res_high            0.6249
_refine_ls_d_res_low             4.3783
_refine_ls_goodness_of_fit_ref   0.9287
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     36
_refine_ls_number_reflns         240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9287
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0152
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0220
_refine_ls_wR_factor_ref         0.0255
_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_HAR
_cod_original_cell_volume        218.79(2)
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_database_code               1567351
_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'