#------------------------------------------------------------------------------
#$Date: 2024-11-29 05:01:49 +0200 (Fri, 29 Nov 2024) $
#$Revision: 296163 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/33/1573353.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_1573353
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'
_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                   8.2334(7)
_cell_length_b                   10.717(6)
_cell_length_c                   5.0641(3)
_cell_measurement.pressure       2490000
_cell_measurement_reflns_used    511
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.3660
_cell_measurement_theta_min      2.2170
_cell_volume                     446.8(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    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.381
_diffrn_measured_fraction_theta_max 0.250
_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  0.0619
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.381
_diffrn_reflns_Laue_measured_fraction_max 0.250
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1340
_diffrn_reflns_point_group_measured_fraction_full 0.378
_diffrn_reflns_point_group_measured_fraction_max 0.240
_diffrn_reflns_theta_full        12.271
_diffrn_reflns_theta_max         23.325
_diffrn_reflns_theta_min         2.217
_diffrn_source                   synchrotron
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33622
_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    3.550
_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         1.010
_refine_diff_density_min         -1.594
_refine_diff_density_rms         0.222
_refine_ls_abs_structure_details
;
 Flack x determined using 192 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         677
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0503
_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)+(0.0911P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    0.376
_reflns_Friedel_fraction_max     0.229
_reflns_number_gt                528
_reflns_number_total             677
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fc5081.cif
_cod_data_source_block           2_49GPa_Imm2_DESY_crystal_2
_cod_database_code               1573353
_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            5.0674(3)
_cell_oxdiff_length_b            10.702(7)
_cell_oxdiff_length_c            8.2392(5)
_cell_oxdiff_angle_alpha         89.996(17)
_cell_oxdiff_angle_beta          89.966(6)
_cell_oxdiff_angle_gamma         90.002(16)
_cell_oxdiff_volume              446.8(3)
_cell_oxdiff_measurement_reflns_used 511
_oxdiff_exptl_absorpt_empirical_full_min 0.501
_oxdiff_exptl_absorpt_empirical_full_max 1.824
_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, 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 0.70766(10) 0.3412(2) 0.5392(3) 0.0204(8) Uani 1 1 d . . . . .
Si1 Si 0.500000 0.3558(8) 0.0314(13) 0.018(2) Uani 1 2 d S T P . .
O1 O 0.6631(10) 0.295(2) -0.0970(15) 0.023(5) Uani 1 1 d . . . . .
O2 O 0.500000 0.3407(19) 0.3481(16) 0.0107(12) Uiso 1 2 d S . P . .
O3 O 0.814(2) 0.500000 0.497(3) 0.041(18) Uani 1 2 d S T P . .
O4 O 0.500000 0.500000 -0.063(3) 0.07(3) Uani 1 4 d S T P . .
O5 O 0.000000 0.500000 0.014(6) 0.13(4) 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
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 104.4(3) 6_655 1_556 ?
O1 Zn1 O2 107.5(6) 6_655 . ?
O1 Zn1 O2 107.6(4) 1_556 . ?
O3 Zn1 O1 114.7(7) . 1_556 ?
O3 Zn1 O1 112.1(6) . 6_655 ?
O3 Zn1 O2 110.1(8) . . ?
O1 Si1 O1 111.1(11) 3_655 . ?
O2 Si1 O1 110.9(5) . 3_655 ?
O2 Si1 O1 110.9(5) . . ?
O2 Si1 O4 112.9(10) . . ?
O4 Si1 O1 105.4(7) . 3_655 ?
O4 Si1 O1 105.4(7) . . ?
Zn1 O1 Zn1 115.3(6) 6_654 1_554 ?
Si1 O1 Zn1 115.5(8) . 1_554 ?
Si1 O1 Zn1 127.9(7) . 6_654 ?
Zn1 O2 Zn1 121.0(4) 3_655 . ?
Si1 O2 Zn1 119.3(2) . 3_655 ?
Si1 O2 Zn1 119.3(2) . . ?
Zn1 O3 Zn1 124.1(9) . 4_565 ?
Si1 O4 Si1 145.6(11) 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 1.932(17) 6_655 ?
Zn1 O1 1.943(9) 1_556 ?
Zn1 O2 1.965(4) . ?
Zn1 O3 1.926(8) . ?
Si1 O1 1.629(12) . ?
Si1 O1 1.629(12) 3_655 ?
Si1 O2 1.612(11) . ?
Si1 O4 1.618(9) . ?
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 -95.7(8) 3_655 . . 6_654 ?
O1 Si1 O1 Zn1 70.9(17) 3_655 . . 1_554 ?
O1 Si1 O2 Zn1 31.5(16) . . . . ?
O1 Si1 O2 Zn1 155.4(11) 3_655 . . . ?
O1 Si1 O2 Zn1 -155.4(11) . . . 3_655 ?
O1 Si1 O2 Zn1 -31.5(16) 3_655 . . 3_655 ?
O1 Si1 O4 Si1 -121.2(5) . . . 2_665 ?
O1 Si1 O4 Si1 121.2(5) 3_655 . . 2_665 ?
O2 Si1 O1 Zn1 28.1(16) . . . 6_654 ?
O2 Si1 O1 Zn1 -165.2(9) . . . 1_554 ?
O2 Si1 O4 Si1 0.000(4) . . . 2_665 ?
O4 Si1 O1 Zn1 -42.7(12) . . . 1_554 ?
O4 Si1 O1 Zn1 150.7(10) . . . 6_654 ?
O4 Si1 O2 Zn1 86.6(11) . . . 3_655 ?
O4 Si1 O2 Zn1 -86.6(11) . . . . ?
