#------------------------------------------------------------------------------
#$Date: 2024-11-29 05:01:49 +0200 (Fri, 29 Nov 2024) $
#$Revision: 296163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/33/1573364.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_1573364
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'
_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                   8.2502(2)
_cell_length_b                   10.685(3)
_cell_length_c                   5.06950(10)
_cell_measurement_pressure       2100000
_cell_measurement_reflns_used    1740
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.4290
_cell_measurement_theta_min      2.0880
_cell_volume                     446.89(13)
_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 0.854
_diffrn_measured_fraction_theta_max 0.543
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.2229
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.854
_diffrn_reflns_Laue_measured_fraction_max 0.543
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7661
_diffrn_reflns_point_group_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.476
_diffrn_reflns_theta_full        7.686
_diffrn_reflns_theta_max         20.425
_diffrn_reflns_theta_min         1.479
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.46
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25506
_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    3.580
_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         5.239
_refine_diff_density_min         -2.125
_refine_diff_density_rms         0.341
_refine_ls_abs_structure_details
;
 Flack x determined using 1045 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.52(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         3598
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0549
_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)+(0.1051P)²+0.1189P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1621
_reflns_Friedel_coverage         0.676
_reflns_Friedel_fraction_full    0.810
_reflns_Friedel_fraction_max     0.403
_reflns_number_gt                2878
_reflns_number_total             3598
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fc5081.cif
_cod_data_source_block           2_1GPa_Imm2_ESRF
_cod_original_cell_volume        446.89(11)
_cod_database_code               1573364
_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.
;
_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, -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 0.70747(3) 0.34134(2) 0.53930(7) 0.01366(6) Uani 1 1 d . . . . .
Si1 Si 0.500000 0.35513(7) 0.0316(2) 0.00972(10) Uani 1 2 d S T P . .
O1 O 0.6631(3) 0.2956(2) -0.0962(3) 0.0185(3) Uani 1 1 d . . . . .
O2 O 0.500000 0.3382(3) 0.3472(4) 0.0147(4) Uani 1 2 d S T P . .
O3 O 0.8128(5) 0.500000 0.4946(13) 0.0269(10) Uani 1 2 d S T P . .
O4 O 0.500000 0.500000 -0.0626(8) 0.0183(7) Uani 1 4 d S T P . .
O5 O 0.000000 0.500000 0.0109(19) 0.095(8) 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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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 104.52(6) 6_655 1_556 ?
O1 Zn1 O2 106.90(11) 6_655 . ?
O1 Zn1 O2 107.55(10) 1_556 . ?
O3 Zn1 O1 114.8(2) . 1_556 ?
O3 Zn1 O1 112.08(15) . 6_655 ?
O3 Zn1 O2 110.52(18) . . ?
O1 Si1 O1 112.0(2) . 4_655 ?
O2 Si1 O1 110.64(9) . . ?
O2 Si1 O1 110.64(9) . 4_655 ?
O2 Si1 O4 113.60(18) . . ?
O4 Si1 O1 104.89(11) . . ?
O4 Si1 O1 104.89(11) . 4_655 ?
Zn1 O1 Zn1 115.00(10) 6_654 1_554 ?
Si1 O1 Zn1 115.88(12) . 1_554 ?
Si1 O1 Zn1 127.69(11) . 6_654 ?
Zn1 O2 Zn1 120.69(11) . 4_655 ?
Si1 O2 Zn1 119.30(6) . . ?
Si1 O2 Zn1 119.30(6) . 4_655 ?
Zn1 O3 Zn1 124.2(2) 3_565 . ?
Si1 O4 Si1 145.7(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 1.937(2) 6_655 ?
Zn1 O1 1.9460(17) 1_556 ?
Zn1 O2 1.9697(11) . ?
Zn1 O3 1.918(2) . ?
Si1 O1 1.623(2) 4_655 ?
Si1 O1 1.623(2) . ?
Si1 O2 1.610(3) . ?
Si1 O4 1.6198(14) . ?
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 -95.76(18) 4_655 . . 6_654 ?
O1 Si1 O1 Zn1 69.8(2) 4_655 . . 1_554 ?
O1 Si1 O2 Zn1 -32.4(2) 4_655 . . 4_655 ?
O1 Si1 O2 Zn1 -157.14(17) . . . 4_655 ?
O1 Si1 O2 Zn1 157.14(17) 4_655 . . . ?
O1 Si1 O2 Zn1 32.4(2) . . . . ?
O1 Si1 O4 Si1 120.94(10) 4_655 . . 2_665 ?
O1 Si1 O4 Si1 -120.94(10) . . . 2_665 ?
O2 Si1 O1 Zn1 28.2(2) . . . 6_654 ?
O2 Si1 O1 Zn1 -166.26(15) . . . 1_554 ?
O2 Si1 O4 Si1 0.000(1) . . . 2_665 ?
O4 Si1 O1 Zn1 -43.4(2) . . . 1_554 ?
O4 Si1 O1 Zn1 151.0(2) . . . 6_654 ?
O4 Si1 O2 Zn1 -85.21(16) . . . . ?
O4 Si1 O2 Zn1 85.21(16) . . . 4_655 ?
