Incommensurately modulated structure of Zn<sub>4</sub>Si<sub>2</sub>O<sub>7</sub>(OH)<sub>2</sub>·H<sub>2</sub>O at high pressure.
Gajda, Roman; Sławiński, Wojciech; Poręba, Tomasz; Parafiniuk, Jan; Mezouar, Mohamed; Dera, Przemysław; Woźniak, Krzysztof; IUCrJ 12 (2025) –; doi:10.1107/S2052252524011060

data_1573350
_publ_section_title
;
 Incommensurately modulated structure of
 Zn<sub>4</sub>Si<sub>2</sub>O<sub>7</sub>(OH)<sub>2</sub>&#xb7;H<sub>2</sub>O
 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     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                   8.1572(3)
_cell_length_b                   10.640(3)
_cell_length_c                   5.04990(10)
_cell_measurement.pressure       3110000
_cell_measurement_reflns_used    2573
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.5440
_cell_measurement_theta_min      2.2300
_cell_volume                     438.29(12)
_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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.369
_diffrn_measured_fraction_theta_max 0.242
_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  0.0380
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.369
_diffrn_reflns_Laue_measured_fraction_max 0.242
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4480
_diffrn_reflns_point_group_measured_fraction_full 0.368
_diffrn_reflns_point_group_measured_fraction_max 0.240
_diffrn_reflns_theta_full        12.271
_diffrn_reflns_theta_max         22.871
_diffrn_reflns_theta_min         2.225
_diffrn_source                   synchrotron
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.619
_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         0.576
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.08(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1164
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0387
_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/[\s^2^(Fo^2^)+(0.0700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.368
_reflns_Friedel_fraction_max     0.237
_reflns_number_gt                1064
_reflns_number_total             1164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fc5081.cif
_cod_data_source_block           3_11GPa_Pnn2_DESY_crystal_2
_cod_original_cell_volume        438.31(11)
_cod_database_code               1573350
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_length_a            10.6441(16)
_cell_oxdiff_length_b            8.1564(2)
_cell_oxdiff_length_c            5.04856(10)
_cell_oxdiff_angle_alpha         89.979(2)
_cell_oxdiff_angle_beta          89.998(5)
_cell_oxdiff_angle_gamma         90.007(5)
_cell_oxdiff_volume              438.30(7)
_cell_oxdiff_measurement_reflns_used 2573
_oxdiff_exptl_absorpt_empirical_full_min 0.719
_oxdiff_exptl_absorpt_empirical_full_max 2.283
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'