#------------------------------------------------------------------------------
#$Date: 2024-11-29 05:01:49 +0200 (Fri, 29 Nov 2024) $
#$Revision: 296163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/33/1573357.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1573357
loop_
_publ_author_name
'Gajda, Roman'
'Sławiński, Wojciech'
'Poręba, Tomasz'
'Parafiniuk, Jan'
'Mezouar, Mohamed'
'Dera, Przemysław'
'Woźniak, Krzysztof'
_publ_section_title
;
 Incommensurately modulated structure of
 Zn₄Si₂O₇(OH)₂·H₂O
 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            'O10 Si2 Zn4'
_chemical_formula_weight         477.66
_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'
_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                   8.2501(2)
_cell_length_b                   10.694(3)
_cell_length_c                   5.06794(16)
_cell_measurement.pressure       1920000
_cell_measurement_reflns_used    1616
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.3090
_cell_measurement_theta_min      1.5470
_cell_volume                     447.13(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.419
_diffrn_measured_fraction_theta_max 0.289
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  φ     50.00 130.00   0.50    1.00  90.00   0.00   0.00    --   160
  2  φ     50.00 130.00   0.50    2.00  90.00   0.00   0.00    --   160
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0016223000
_diffrn_orient_matrix_UB_12      -0.0331074000
_diffrn_orient_matrix_UB_13      0.0014800000
_diffrn_orient_matrix_UB_21      0.0406878000
_diffrn_orient_matrix_UB_22      0.0014028000
_diffrn_orient_matrix_UB_23      0.0221385000
_diffrn_orient_matrix_UB_31      -0.0136101000
_diffrn_orient_matrix_UB_32      0.0002691000
_diffrn_orient_matrix_UB_33      0.0662603000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.35424
_diffrn_reflns_av_R_equivalents  0.1231
_diffrn_reflns_av_unetI/netI     0.0951
_diffrn_reflns_Laue_measured_fraction_full 0.419
_diffrn_reflns_Laue_measured_fraction_max 0.289
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2462
_diffrn_reflns_point_group_measured_fraction_full 0.348
_diffrn_reflns_point_group_measured_fraction_max 0.255
_diffrn_reflns_theta_full        12.271
_diffrn_reflns_theta_max         23.559
_diffrn_reflns_theta_min         2.351
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.548
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.488
_refine_diff_density_min         -2.185
_refine_diff_density_rms         0.452
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.6(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         737
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0990
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2505
_refine_ls_wR_factor_ref         0.2519
_reflns_Friedel_coverage         0.660
_reflns_Friedel_fraction_full    0.259
_reflns_Friedel_fraction_max     0.217
_reflns_number_gt                678
_reflns_number_total             737
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fc5081.cif
_cod_data_source_block           1_92GPa_Imm2_DESY_crystal_3
_cod_original_cell_volume        447.12(12)
_cod_database_code               1573357
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Zn4Si2O10H4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
;
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 12.042
_oxdiff_exptl_absorpt_empirical_full_min 0.380
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, z'
'-x, y, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.70714(8) 0.3407(2) 0.53930(2) 0.0159(10) Uani 1 1 d . . . . .
Si1 Si 0.500000 0.3550(6) 0.0309(11) 0.013(2) Uani 1 2 d S T P . .
O1 O 0.6617(8) 0.2936(18) -0.0964(16) 0.017(5) Uani 1 1 d . . . . .
O2 O 0.500000 0.3370(16) 0.3462(18) 0.015(7) Uani 1 2 d S T P . .
O3 O 0.8141(14) 0.500000 0.500(4) 0.033(11) Uani 1 2 d S T P . .
O4 O 0.500000 0.500000 -0.060(3) 0.047(18) Uani 1 4 d S T P . .
O5 O 0.000000 0.500000 0.028(13) 0.063(10) Uiso 1 4 d S . P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0003 0.0013 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0175 0.0165 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2130 0.4015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O1 104.7(3) 6_655 1_556 ?
O1 Zn1 O2 107.1(5) 6_655 . ?
O1 Zn1 O2 107.3(3) 1_556 . ?
O1 Zn1 O3 111.4(5) 6_655 . ?
O3 Zn1 O1 114.5(8) . 1_556 ?
O3 Zn1 O2 111.3(7) . . ?
O1 Si1 O1 110.8(11) 4_655 . ?
O1 Si1 O4 105.9(8) 4_655 . ?
O1 Si1 O4 105.9(8) . . ?
O2 Si1 O1 110.3(5) . . ?
O2 Si1 O1 110.3(5) . 4_655 ?
O2 Si1 O4 113.4(9) . . ?
Zn1 O1 Zn1 115.0(5) 6_654 1_554 ?
Si1 O1 Zn1 115.5(7) . 1_554 ?
Si1 O1 Zn1 128.5(7) . 6_654 ?
Zn1 O2 Zn1 120.4(5) 4_655 . ?
Si1 O2 Zn1 119.4(3) . . ?
Si1 O2 Zn1 119.4(3) . 4_655 ?
Zn1 O3 Zn1 124.0(6) . 3_565 ?
Si1 O4 Si1 147.0(12) 2_665 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 1.926(14) 6_655 ?
Zn1 O1 1.950(9) 1_556 ?
Zn1 O2 1.970(5) . ?
Zn1 O3 1.929(6) . ?
Si1 O1 1.620(9) . ?
Si1 O1 1.620(9) 4_655 ?
Si1 O2 1.609(12) . ?
Si1 O4 1.618(8) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Si1 O1 Zn1 -96.4(7) 4_655 . . 6_654 ?
O1 Si1 O1 Zn1 71.5(16) 4_655 . . 1_554 ?
O1 Si1 O2 Zn1 33.9(13) . . . . ?
O1 Si1 O2 Zn1 156.6(11) 4_655 . . . ?
O1 Si1 O2 Zn1 -33.9(13) 4_655 . . 4_655 ?
O1 Si1 O2 Zn1 -156.6(11) . . . 4_655 ?
O1 Si1 O4 Si1 -121.1(5) . . . 2_665 ?
O1 Si1 O4 Si1 121.1(5) 4_655 . . 2_665 ?
O2 Si1 O1 Zn1 -166.0(9) . . . 1_554 ?
O2 Si1 O1 Zn1 26.0(14) . . . 6_654 ?
O2 Si1 O4 Si1 0.000(4) . . . 2_665 ?
O4 Si1 O1 Zn1 -42.9(11) . . . 1_554 ?
O4 Si1 O1 Zn1 149.1(11) . . . 6_654 ?
O4 Si1 O2 Zn1 84.7(9) . . . 4_655 ?
O4 Si1 O2 Zn1 -84.7(9) . . . . ?
