#------------------------------------------------------------------------------
#$Date: 2024-11-29 05:01:49 +0200 (Fri, 29 Nov 2024) $
#$Revision: 296163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/33/1573352.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_1573352
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           34
_space_group_name_Hall           'P 2 -2n'
_space_group_name_H-M_alt        'P n n 2'
_atom_sites_solution_primary     dual
_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                   8.1701(4)
_cell_length_b                   10.6651(3)
_cell_length_c                   5.05540(10)
_cell_measurement.pressure       3260000
_cell_measurement_reflns_used    2670
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.8490
_cell_measurement_theta_min      2.2130
_cell_volume                     440.50(3)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.687
_diffrn_measured_fraction_theta_max 0.448
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.35424
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.687
_diffrn_reflns_Laue_measured_fraction_max 0.448
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4747
_diffrn_reflns_point_group_measured_fraction_full 0.608
_diffrn_reflns_point_group_measured_fraction_max 0.378
_diffrn_reflns_theta_full        12.271
_diffrn_reflns_theta_max         22.851
_diffrn_reflns_theta_min         2.273
_diffrn_source                   synchrotron
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98470
_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    3.601
_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         0.736
_refine_diff_density_min         -1.592
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details
;
 Flack x determined using 633 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1836
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0279
_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)+(0.0503P)²+0.0842P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.579
_reflns_Friedel_fraction_full    0.507
_reflns_Friedel_fraction_max     0.297
_reflns_number_gt                1764
_reflns_number_total             1836
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fc5081.cif
_cod_data_source_block           3_26GPa_Pnn2_DESY_crystal_1
_cod_database_code               1573352
_shelx_shelxl_version_number     2018/3
_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.
;
_cell_oxdiff_length_a            10.6641(16)
_cell_oxdiff_length_b            8.1721(16)
_cell_oxdiff_length_c            5.05464(19)
_cell_oxdiff_angle_alpha         90.010(8)
_cell_oxdiff_angle_beta          90.023(7)
_cell_oxdiff_angle_gamma         89.982(14)
_cell_oxdiff_volume              440.50(12)
_cell_oxdiff_measurement_reflns_used 2670
_oxdiff_exptl_absorpt_empirical_full_min 0.940
_oxdiff_exptl_absorpt_empirical_full_max 1.114
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'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 0.22853(5) 0.15013(3) 0.61516(7) 0.01228(7) Uani 1 1 d . . . . .
Zn2 Zn 0.31113(5) 0.33485(3) 0.11940(6) 0.01266(7) Uani 1 1 d . . . . .
Si1 Si 0.51794(9) 0.35575(6) 0.6084(2) 0.00874(12) Uani 1 1 d . . . . .
O1 O 0.3641(4) 0.2836(3) 0.4790(4) 0.0192(5) Uani 1 1 d . . . . .
O2 O 0.6902(4) 0.3089(2) 0.4852(4) 0.0162(4) Uani 1 1 d . . . . .
O3 O 0.5187(4) 0.3407(2) 0.9255(5) 0.0134(4) Uani 1 1 d . . . . .
O4 O 0.1832(4) 0.4840(2) 0.0734(8) 0.0246(7) Uani 1 1 d . . . . .
O5 O 0.500000 0.500000 0.5099(7) 0.0168(6) Uani 1 2 d S T P . .
O6 O 0.000000 0.500000 -0.404(2) 0.078(4) Uani 1 2 d S T 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 O2 105.61(10) . 3_455 ?
O1 Zn1 O3 106.84(12) . 3_454 ?
O2 Zn1 O3 108.50(11) 3_455 3_454 ?
O4 Zn1 O1 115.14(15) 4_545 . ?
O4 Zn1 O2 111.87(14) 4_545 3_455 ?
O4 Zn1 O3 108.60(13) 4_545 3_454 ?
O1 Zn2 O3 106.48(12) . 1_554 ?
O2 Zn2 O1 102.57(9) 3_454 . ?
O2 Zn2 O3 106.86(11) 3_454 1_554 ?
O4 Zn2 O1 117.85(16) . . ?
O4 Zn2 O2 109.53(14) . 3_454 ?
O4 Zn2 O3 112.62(13) . 1_554 ?
O1 Si1 O2 112.00(17) . . ?
O1 Si1 O5 104.91(13) . . ?
O2 Si1 O5 104.67(12) . . ?
O3 Si1 O1 111.05(14) . . ?
O3 Si1 O2 110.41(14) . . ?
O3 Si1 O5 113.57(16) . . ?
Zn1 O1 Zn2 114.33(12) . . ?
Si1 O1 Zn1 130.89(14) . . ?
Si1 O1 Zn2 114.73(12) . . ?
Zn2 O2 Zn1 115.50(11) 3 3_554 ?
Si1 O2 Zn1 116.13(13) . 3_554 ?
Si1 O2 Zn2 123.42(14) . 3 ?
Zn2 O3 Zn1 120.79(12) 1_556 3 ?
Si1 O3 Zn1 118.92(17) . 3 ?
Si1 O3 Zn2 119.84(16) . 1_556 ?
Zn2 O4 Zn1 123.09(18) . 4_554 ?
Si1 O5 Si1 144.3(2) 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 1.931(2) . ?
Zn1 O2 1.946(2) 3_455 ?
Zn1 O3 1.967(3) 3_454 ?
Zn1 O4 1.925(3) 4_545 ?
Zn2 O1 1.947(2) . ?
Zn2 O2 1.946(2) 3_454 ?
Zn2 O3 1.960(3) 1_554 ?
Zn2 O4 1.917(3) . ?
Si1 O1 1.612(3) . ?
Si1 O2 1.618(3) . ?
Si1 O3 1.611(3) . ?
Si1 O5 1.6236(13) . ?
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 O2 Zn1 67.23(19) . . . 3_554 ?
O1 Si1 O2 Zn2 -86.7(2) . . . 3 ?
O1 Si1 O3 Zn1 152.92(16) . . . 3 ?
O1 Si1 O3 Zn2 -34.7(2) . . . 1_556 ?
O1 Si1 O5 Si1 121.79(12) . . . 2_665 ?
O2 Si1 O1 Zn1 103.5(3) . . . . ?
O2 Si1 O1 Zn2 -73.7(2) . . . . ?
O2 Si1 O3 Zn1 28.07(19) . . . 3 ?
O2 Si1 O3 Zn2 -159.54(15) . . . 1_556 ?
O2 Si1 O5 Si1 -120.15(12) . . . 2_665 ?
O3 Si1 O1 Zn1 -20.5(3) . . . . ?
O3 Si1 O1 Zn2 162.32(16) . . . . ?
O3 Si1 O2 Zn1 -168.46(15) . . . 3_554 ?
O3 Si1 O2 Zn2 37.6(2) . . . 3 ?
O3 Si1 O5 Si1 0.35(12) . . . 2_665 ?
O5 Si1 O1 Zn1 -143.6(2) . . . . ?
O5 Si1 O1 Zn2 39.2(2) . . . . ?
O5 Si1 O2 Zn1 -45.9(2) . . . 3_554 ?
O5 Si1 O2 Zn2 160.21(19) . . . 3 ?
O5 Si1 O3 Zn1 -89.13(14) . . . 3 ?
O5 Si1 O3 Zn2 83.26(14) . . . 1_556 ?
