Syntheses, characterization and properties of two new dodeca-niobates presenting unprecedented features.
Zhang, Ting-Ting; Lin, Po-Han; Yu, Gui-Yang; Zhang, Xiao; Cui, Xiao-Bing; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6495–6503; doi:10.1039/d0dt00953a

data_7704152
_publ_section_title
;
 Syntheses, characterization and properties of two new dodeca-niobates
 presenting unprecedented features.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6495
_journal_page_last               6503
_journal_paper_doi               10.1039/d0dt00953a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'H39 K3 Nb14 O58 Si'
_chemical_formula_weight         2413.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_Hall           'I 2 2'
_space_group_name_H-M_alt        'I 2 2 2'
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-04-08 deposited with the CCDC.	2020-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8913(8)
_cell_length_b                   11.6608(8)
_cell_length_c                   19.6414(15)
_cell_measurement_reflns_used    1613
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      28.5030
_cell_measurement_theta_min      3.3120
_cell_volume                     2494.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3684
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.663
_diffrn_reflns_theta_min         3.295
_exptl_absorpt_coefficient_mu    3.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    3.213
_exptl_crystal_description       Block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.118
_refine_diff_density_min         -2.378
_refine_diff_density_rms         0.379
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.6(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2617
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0758
_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^)+(0.1161P)^2^+182.0236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2183
_refine_ls_wR_factor_ref         0.2290
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.877
_reflns_number_gt                2321
_reflns_number_total             2617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00953a2.cif
_cod_data_source_block           k1
_cod_depositor_comments
'Adding full bibliography for 7704152--7704153.cif.'
_cod_database_code               7704152
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              76237