First hydrothermally synthesized polar lithium niobium 1M mica germanate–silicate KNb (Li0.9Nb0.02□ 0.08)2[(Ge0.4Si0.6)4O10]O2 with disorder and isomorphism, and topology symmetry analysis of the polytype family
Belokoneva, Elena L.; van Dinteren-Tovstopyat, Sofiya V.; Volkov, Anatoly S.; Dimitrova, Olga V.; Vigasina, Marina F.; Stefanovich, Sergey Yu.; Simonov, Sergey V.; Ksenofontov, Dmitry A.; New Journal of Chemistry 49 (2025) 19955–19962; doi:10.1039/D5NJ02691A

data_7064109
_publ_section_title
;
 First hydrothermally synthesized polar lithium niobium 1M mica
 germanate--silicate KNb (Li0.9Nb0.02\\square 0.08)2[(Ge0.4Si0.6)4O10]O2
 with disorder and isomorphism, and topology symmetry analysis of the
 polytype family
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19955
_journal_page_last               19962
_journal_paper_doi               10.1039/D5NJ02691A
_journal_volume                  49
_journal_year                    2025
_chemical_compound_source        no
_chemical_formula_moiety         KNb(Li0.9Nb0.02o0.08)2[(Ge0.4Si0.6)4O10]O2
_chemical_formula_sum            'Ge1.6 K Li1.8 Nb1.04 O12 Si2.4'
_chemical_formula_weight         523.78
_chemical_melting_point          ?
_chemical_name_common            silicate-germanate
_chemical_name_systematic        'potassium lithium niobium silicate-germanate'
_chemical_properties_physical    Hygroscopic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2025-06-10 deposited with the CCDC.	2025-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.852(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.3102(4)
_cell_length_b                   9.1761(6)
_cell_length_c                   10.1904(6)
_cell_measurement_reflns_used    861
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.308
_cell_measurement_theta_min      4.04
_cell_volume                     489.22(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    WINATOM
_computing_publication_material  none
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'XCalibur S'
_diffrn_measurement_method       w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0841
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2073
_diffrn_reflns_theta_full        30.60
_diffrn_reflns_theta_max         30.60
_diffrn_reflns_theta_min         4.06
_exptl_absorpt_coefficient_mu    6.882
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic plate'
_exptl_crystal_F_000             496
_exptl_crystal_preparation       'Luminescent,nonlinear optical'
_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_size_max          0.054
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.244
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1137
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                1030
_reflns_number_total             1137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5nj02691a4.cif
_cod_data_source_block           8803-6l
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'none' was changed to '?'
-- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7064109.cif.
;
_cod_original_cell_volume        489.23(6)
_cod_original_sg_symbol_Hall     C2y
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'Ge1.60 K Li1.80 Nb1.04 O12 Si2.40'
_cod_database_code               7064109