#------------------------------------------------------------------------------
#$Date: 2024-11-29 05:01:49 +0200 (Fri, 29 Nov 2024) $
#$Revision: 296163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/33/1573363.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_1573363
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            '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  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -32.00  32.00   0.50    0.50    --    0.00   0.00   0.00  128
  2  ω    -32.00  32.00   0.50    0.50    --    0.00   0.00   0.00  128
  3  ω    -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       'ω 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/[σ²(Fo²)+(0.1190P)²] where P=(Fo²+2Fc²)/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 > 2σ(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
_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.
;
_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
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 0.70587(3) 0.34002(2) 0.53933(8) 0.01247(6) Uani 1 1 d . . . . .
Si1 Si 0.500000 0.35451(7) 0.0314(2) 0.00890(9) Uani 1 2 d S T P . .
O1 O 0.6614(3) 0.29502(19) -0.0963(3) 0.0158(3) Uani 1 1 d . . . . .
O2 O 0.500000 0.3356(3) 0.3465(4) 0.0140(3) Uani 1 2 d S T P . .
O3 O 0.8081(5) 0.500000 0.4981(12) 0.0239(9) Uani 1 2 d S T P . .
O4 O 0.500000 0.500000 -0.0566(7) 0.0166(6) Uani 1 4 d S T P . .
O5 O 0.000000 0.500000 0.0111(18) 0.079(7) Uani 1 4 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
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0021 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si -0.0003 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.0822 0.1631 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_axis.id
_axis.system
_axis.type
_axis.equipment
_axis.parity
_axis.depends_on
_axis.zero
_axis.vector[1]
_axis.vector[2]
_axis.vector[3]
source abstract . source . . . 0.99995009 0.00000000 -0.00999115
omega abstract rotation goniometer -1 . 0.00000000 0.00000000 0.00000000
1.00000000
kappa abstract rotation goniometer -1 omega 0.00000000 -0.76604444 0.00000000
0.64278761
phi abstract rotation goniometer -1 kappa . 0.00000000 0.00000000 1.00000000
theta abstract rotation goniometer -1 . -0.78051000 0.00000000 0.00000000
1.00000000
matrixX abstract general general . phi . 1.00000000 0.00000000 0.00000000
matrixY abstract general general . phi . 0.00000000 1.00000000 0.00000000
matrixZ abstract general general . phi . 0.00000000 0.00000000 1.00000000
dacX abstract translation general . phi . 0.00000000 1.00000000 0.00000000
dacY abstract translation general . phi . -1.00000000 0.00000000 0.00000000
dacZ abstract translation general . phi . 0.00000000 0.00000000 1.00000000
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 105.16(6) 6_655 1_556 ?
O1 Zn1 O2 107.29(9) 6_655 . ?
O1 Zn1 O2 107.63(9) 1_556 . ?
O3 Zn1 O1 114.03(19) . 1_556 ?
O3 Zn1 O1 111.83(13) . 6_655 ?
O3 Zn1 O2 110.52(17) . . ?
O1 Si1 O1 111.72(17) . 3_655 ?
O2 Si1 O1 110.40(8) . . ?
O2 Si1 O1 110.41(8) . 3_655 ?
O2 Si1 O4 113.27(17) . . ?
O4 Si1 O1 105.45(10) . . ?
O4 Si1 O1 105.44(10) . 3_655 ?
Zn1 O1 Zn1 114.42(9) 6_654 1_554 ?
Si1 O1 Zn1 116.16(10) . 1_554 ?
Si1 O1 Zn1 128.23(10) . 6_654 ?
Zn1 O2 Zn1 120.24(10) . 3_655 ?
Si1 O2 Zn1 119.38(5) . . ?
Si1 O2 Zn1 119.38(5) . 3_655 ?
Zn1 O3 Zn1 125.8(2) . 4_565 ?
Si1 O4 Si1 147.9(3) . 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 1.9456(18) 6_655 ?
Zn1 O1 1.9535(16) 1_556 ?
Zn1 O2 1.9747(10) . ?
Zn1 O3 1.9238(18) . ?
Si1 O1 1.6222(19) 3_655 ?
Si1 O1 1.6222(19) . ?
Si1 O2 1.618(2) . ?
Si1 O4 1.6209(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 O1 Zn1 -97.17(16) 3_655 . . 6_654 ?
O1 Si1 O1 Zn1 69.59(18) 3_655 . . 1_554 ?
O1 Si1 O2 Zn1 -33.7(2) 3_655 . . 3_655 ?
O1 Si1 O2 Zn1 -157.70(14) . . . 3_655 ?
O1 Si1 O2 Zn1 157.70(14) 3_655 . . . ?
O1 Si1 O2 Zn1 33.7(2) . . . . ?
O1 Si1 O4 Si1 120.83(9) 3_655 . . 2_665 ?
O1 Si1 O4 Si1 -120.83(9) . . . 2_665 ?
O2 Si1 O1 Zn1 26.1(2) . . . 6_654 ?
O2 Si1 O1 Zn1 -167.14(13) . . . 1_554 ?
O2 Si1 O4 Si1 0.000(1) . . . 2_665 ?
O4 Si1 O1 Zn1 -44.46(18) . . . 1_554 ?
O4 Si1 O1 Zn1 148.78(18) . . . 6_654 ?
O4 Si1 O2 Zn1 -84.32(15) . . . . ?
O4 Si1 O2 Zn1 84.32(15) . . . 3_655 ?
