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_1567356
_publ_section_title
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 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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            10
_cell_length_a                   6.1665(3)
_cell_length_b                   6.1665(3)
_cell_length_c                   5.6756(4)
_cell_measurement_reflns_used    1521
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.9150
_cell_measurement_theta_min      3.6650
_cell_volume                     215.82(2)
_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 0.9917
_diffrn_measured_fraction_theta_max 0.9522
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.9917
_diffrn_reflns_Laue_measured_fraction_max 0.9522
_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       -8
_diffrn_reflns_number            4280
_diffrn_reflns_point_group_measured_fraction_full 0.9917
_diffrn_reflns_point_group_measured_fraction_max 0.9522
_diffrn_reflns_theta_full        19.6651
_diffrn_reflns_theta_max         26.88
_diffrn_reflns_theta_min         3.69
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68491
_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    1.386
_exptl_crystal_description       disc
_exptl_crystal_F_000             100.051
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.1777
_refine_diff_density_min         -0.1583
_refine_diff_density_rms         0.0458
_refine_ls_d_res_high            0.6203
_refine_ls_d_res_low             4.3603
_refine_ls_goodness_of_fit_ref   1.0414
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     22
_refine_ls_number_reflns         259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0414
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.0003
_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^+0.0017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0261
_refine_ls_wR_factor_ref         0.0294
_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              8
_reflns_limit_l_min              0
_reflns_number_gt                198
_reflns_number_total             259
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            lt5051.cif
_cod_data_source_block           H2O_home_IAM
_cod_original_cell_volume        215.818(19)
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_database_code               1567356
_olex2_refinement_description
;
1. Others
 Fixed Sof: H1a(0.5) H1b(0.25) H2(0.25) H1c(0.25)
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