#------------------------------------------------------------------------------
#$Date: 2024-11-29 05:01:49 +0200 (Fri, 29 Nov 2024) $
#$Revision: 296163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/33/1573354.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_1573354
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'
_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                   8.1412(9)
_cell_length_b                   10.6227(8)
_cell_length_c                   5.0448(2)
_cell_measurement.pressure       3500000
_cell_measurement_reflns_used    1048
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.4120
_cell_measurement_theta_min      2.2900
_cell_volume                     436.28(6)
_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_measured_fraction_theta_full 0.696
_diffrn_measured_fraction_theta_max 0.445
_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  0.0331
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.696
_diffrn_reflns_Laue_measured_fraction_max 0.445
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2456
_diffrn_reflns_point_group_measured_fraction_full 0.639
_diffrn_reflns_point_group_measured_fraction_max 0.379
_diffrn_reflns_theta_full        12.271
_diffrn_reflns_theta_max         22.910
_diffrn_reflns_theta_min         2.282
_diffrn_source                   synchrotron
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51895
_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    3.636
_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         0.981
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.264
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.11(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1841
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0449
_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)+(0.0699P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1162
_reflns_Friedel_coverage         0.595
_reflns_Friedel_fraction_full    0.565
_reflns_Friedel_fraction_max     0.303
_reflns_number_gt                1654
_reflns_number_total             1841
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fc5081.cif
_cod_data_source_block           3_50GPa_Pnn2_DESY_crystal_1
_cod_database_code               1573354
_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            10.620(3)
_cell_oxdiff_length_b            8.141(2)
_cell_oxdiff_length_c            5.0462(4)
_cell_oxdiff_angle_alpha         89.961(14)
_cell_oxdiff_angle_beta          89.972(12)
_cell_oxdiff_angle_gamma         90.04(2)
_cell_oxdiff_volume              436.28(19)
_cell_oxdiff_measurement_reflns_used 1048
_oxdiff_exptl_absorpt_empirical_full_min 0.484
_oxdiff_exptl_absorpt_empirical_full_max 1.631
_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 0.23556(8) 0.14699(5) 0.61429(13) 0.01130(12) Uani 1 1 d . . . . .
Zn2 Zn 0.31788(8) 0.33239(5) 0.12008(11) 0.01166(12) Uani 1 1 d . . . . .
Si1 Si 0.52395(16) 0.35601(11) 0.6073(4) 0.00775(19) Uani 1 1 d . . . . .
O4 O 0.1824(8) 0.4786(5) 0.0755(14) 0.0249(14) Uani 1 1 d . . . . .
O3 O 0.5245(6) 0.3414(4) 0.9250(7) 0.0129(7) Uani 1 1 d . . . . .
O2 O 0.6987(7) 0.3133(4) 0.4866(7) 0.0141(7) Uani 1 1 d . . . . .
O1 O 0.3729(7) 0.2800(5) 0.4790(7) 0.0180(9) Uani 1 1 d . . . . .
O5 O 0.500000 0.500000 0.5110(12) 0.0161(11) Uani 1 2 d S T P . .
O6 O 0.000000 0.500000 -0.396(4) 0.072(5) 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
O4 Zn1 O3 108.2(2) 4_545 3_454 ?
O4 Zn1 O2 110.7(3) 4_545 3_455 ?
O4 Zn1 O1 116.5(3) 4_545 . ?
O2 Zn1 O3 108.6(2) 3_455 3_454 ?
O1 Zn1 O3 106.8(2) . 3_454 ?
O1 Zn1 O2 105.78(17) . 3_455 ?
O4 Zn2 Si1 110.58(19) . . ?
O4 Zn2 O3 113.4(2) . 1_554 ?
O4 Zn2 O2 108.5(3) . 3_454 ?
O4 Zn2 O1 118.2(3) . . ?
O3 Zn2 Si1 85.79(13) 1_554 . ?
O2 Zn2 Si1 129.16(14) 3_454 . ?
O2 Zn2 O3 107.12(18) 3_454 1_554 ?
O2 Zn2 O1 102.08(17) 3_454 . ?
O1 Zn2 Si1 29.44(13) . . ?
O1 Zn2 O3 106.6(2) . 1_554 ?
O3 Si1 Zn2 144.36(19) . . ?
O3 Si1 O2 110.3(2) . . ?
O3 Si1 O1 110.8(2) . . ?
O3 Si1 O5 113.0(3) . . ?
O2 Si1 Zn2 99.29(18) . . ?
O2 Si1 O5 105.0(2) . . ?
O1 Si1 Zn2 36.53(14) . . ?
O1 Si1 O2 112.4(3) . . ?
O1 Si1 O5 105.2(2) . . ?
O5 Si1 Zn2 76.38(19) . . ?
Zn2 O4 Zn1 122.9(3) . 4_554 ?
Zn2 O3 Zn1 120.70(19) 1_556 3 ?
Si1 O3 Zn1 118.6(3) . 3 ?
Si1 O3 Zn2 120.3(3) . 1_556 ?
Zn2 O2 Zn1 115.4(2) 3 3_554 ?
Si1 O2 Zn1 116.0(2) . 3_554 ?
Si1 O2 Zn2 122.2(2) . 3 ?
Zn1 O1 Zn2 113.9(2) . . ?
Si1 O1 Zn1 132.0(2) . . ?
Si1 O1 Zn2 114.0(2) . . ?
Si1 O5 Si1 145.0(5) . 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 O4 1.919(5) 4_545 ?
Zn1 O3 1.970(5) 3_454 ?
Zn1 O2 1.948(4) 3_455 ?
Zn1 O1 1.927(4) . ?
Zn2 Si1 2.986(2) . ?
Zn2 O4 1.918(5) . ?
Zn2 O3 1.951(5) 1_554 ?
Zn2 O2 1.946(4) 3_454 ?
Zn2 O1 1.946(4) . ?
Si1 O3 1.610(5) . ?
Si1 O2 1.613(5) . ?
Si1 O1 1.607(5) . ?
Si1 O5 1.617(2) . ?
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
Zn2 Si1 O3 Zn1 170.90(9) . . . 3 ?
Zn2 Si1 O3 Zn2 -16.2(5) . . . 1_556 ?
Zn2 Si1 O2 Zn1 31.1(3) . . . 3_554 ?
Zn2 Si1 O2 Zn2 -119.6(3) . . . 3 ?
Zn2 Si1 O1 Zn1 -179.8(8) . . . . ?
Zn2 Si1 O5 Si1 144.24(5) . . . 2_665 ?
O3 Si1 O2 Zn1 -169.2(2) . . . 3_554 ?
O3 Si1 O2 Zn2 40.2(4) . . . 3 ?
O3 Si1 O1 Zn1 -18.4(6) . . . . ?
O3 Si1 O1 Zn2 161.5(3) . . . . ?
O3 Si1 O5 Si1 0.6(2) . . . 2_665 ?
O2 Si1 O3 Zn1 26.8(4) . . . 3 ?
O2 Si1 O3 Zn2 -160.2(3) . . . 1_556 ?
O2 Si1 O1 Zn1 105.5(5) . . . . ?
O2 Si1 O1 Zn2 -74.7(4) . . . . ?
O2 Si1 O5 Si1 -119.6(2) . . . 2_665 ?
O1 Si1 O3 Zn1 151.9(3) . . . 3 ?
O1 Si1 O3 Zn2 -35.1(4) . . . 1_556 ?
O1 Si1 O2 Zn1 66.7(3) . . . 3_554 ?
O1 Si1 O2 Zn2 -84.0(4) . . . 3 ?
O1 Si1 O5 Si1 121.5(2) . . . 2_665 ?
O5 Si1 O3 Zn1 -90.3(3) . . . 3 ?
O5 Si1 O3 Zn2 82.6(3) . . . 1_556 ?
O5 Si1 O2 Zn1 -47.2(4) . . . 3_554 ?
O5 Si1 O2 Zn2 162.2(3) . . . 3 ?
O5 Si1 O1 Zn1 -140.7(5) . . . . ?
O5 Si1 O1 Zn2 39.1(4) . . . . ?
