Incommensurately modulated structure of Zn<sub>4</sub>Si<sub>2</sub>O<sub>7</sub>(OH)<sub>2</sub>·H<sub>2</sub>O at high pressure.
Gajda, Roman; Sławiński, Wojciech; Poręba, Tomasz; Parafiniuk, Jan; Mezouar, Mohamed; Dera, Przemysław; Woźniak, Krzysztof; IUCrJ 12 (2025) –; doi:10.1107/S2052252524011060

data_1573363
_publ_section_title
;
 Incommensurately modulated structure of
 Zn<sub>4</sub>Si<sub>2</sub>O<sub>7</sub>(OH)<sub>2</sub>&#xb7;H<sub>2</sub>O
 at high pressure.
;
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524011060
_journal_volume                  12
_journal_year                    2025
_chemical_formula_moiety         'O9 Si2 Zn4, O'
_chemical_formula_sum            'H4 O10 Si2 Zn4'
_chemical_formula_weight         481.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           44
_space_group_name_Hall           'I 2 -2'
_space_group_name_H-M_alt        'I m m 2'
_atom_sites_solution_primary     direct
_audit_creation_date             2024-08-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.31709(17)
_cell_length_b                   10.706(3)
_cell_length_c                   5.09489(7)
_cell_measurement.pressure       1000000
_cell_measurement_reflns_used    1914
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.2840
_cell_measurement_theta_min      2.0740
_cell_volume                     453.66(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024) (IMPORT)'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.838
_diffrn_measured_fraction_theta_max 0.555
_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    -32.00  32.00   0.50    0.50    --    0.00   0.00   0.00  128
  2  \w    -32.00  32.00   0.50    0.50    --    0.00   0.00   0.00  128
  3  \w    -32.00  32.00   0.50    0.50    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0023661532
_diffrn_orient_matrix_UB_12      -0.0207096284
_diffrn_orient_matrix_UB_13      0.0011843905
_diffrn_orient_matrix_UB_21      0.0117847391
_diffrn_orient_matrix_UB_22      -0.0013168728
_diffrn_orient_matrix_UB_23      -0.0392108108
_diffrn_orient_matrix_UB_31      0.0239750428
_diffrn_orient_matrix_UB_32      -0.0014043438
_diffrn_orient_matrix_UB_33      0.0193987165
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.2229
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.838
_diffrn_reflns_Laue_measured_fraction_max 0.555
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7678
_diffrn_reflns_point_group_measured_fraction_full 0.783
_diffrn_reflns_point_group_measured_fraction_max 0.482
_diffrn_reflns_theta_full        7.686
_diffrn_reflns_theta_max         20.203
_diffrn_reflns_theta_min         1.470
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.526
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.191
_refine_diff_density_min         -3.355
_refine_diff_density_rms         0.389
_refine_ls_abs_structure_details
;
 Flack x determined using 1095 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.29(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         3585
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1190P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1687
_reflns_Friedel_coverage         0.657
_reflns_Friedel_fraction_full    0.712
_reflns_Friedel_fraction_max     0.401
_reflns_number_gt                2967
_reflns_number_total             3585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fc5081.cif
_cod_data_source_block           1_0GPa_Imm2_ESRF
_cod_original_cell_volume        453.66(12)
_cod_database_code               1573363
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Zn4Si2O10H4
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   1469
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.555
_oxdiff_exptl_absorpt_empirical_full_min 0.676