data_Berezanskite _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common Berezanskite _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'K Li3 O30 Si12 Ti2' _chemical_formula_weight 728.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O2-' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 '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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system hexagonal _space_group_IT_number 192 _space_group_name_H-M_alt 'P 6/m c c' _space_group_name_Hall '-P 6 2c' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z' 'y, -x+y, z' 'x-y, x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 9.898(4) _cell_length_b 9.898(4) _cell_length_c 14.276(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1211.2(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3868 _cell_measurement_theta_min 4 _cell_measurement_theta_max 55 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn ? _exptl_crystal_F_000 699 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 13 microns _exptl_crystal_size_mid 9 _exptl_crystal_size_min 6 _exptl_absorpt_coefficient_mu 1.429 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source Rotating-anode generator _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9718 _diffrn_reflns_av_unetI/netI 0.0213 _diffrn_reflns_av_R_equivalents 0.0905 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.376 _diffrn_reflns_theta_max 27.508 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 497 _reflns_number_gt 392 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+2.2780P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 497 _refine_ls_number_parameters 44 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0456 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 A Ti 0.3333 0.6667 0.2500 0.0044(3) Uani 1.000(4) 6 d S T . . . C K 0.0000 0.0000 0.2500 0.0220(6) Uani 1.037(8) 12 d S T . . . T1 Si 0.12243(7) 0.36149(7) 0.10896(4) 0.00600(16) Uani 1 1 d . . . . . T2 Li 0.0000 0.5000 0.2500 0.014(2) Uani 1.00(3) 4 d S T . . . O1 O2- 0.1378(3) 0.4075(3) 0.0000 0.0150(5) Uani 1 2 d S T P . . O2 O2- 0.22666(19) 0.28152(19) 0.13283(11) 0.0125(4) Uani 1 1 d . . . . . O3 O2- 0.16679(16) 0.50872(17) 0.17421(10) 0.0081(3) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 A 0.0038(3) 0.0038(3) 0.0055(4) 0.000 0.000 0.00190(16) C 0.0218(7) 0.0218(7) 0.0226(11) 0.000 0.000 0.0109(4) T1 0.0060(3) 0.0065(3) 0.0056(3) -0.0006(2) -0.0003(2) 0.0032(2) T2 0.008(4) 0.013(3) 0.020(4) 0.000 0.000 0.004(2) O1 0.0214(13) 0.0162(12) 0.0061(10) 0.000 0.000 0.0084(11) O2 0.0111(8) 0.0135(8) 0.0162(8) -0.0013(7) -0.0025(7) 0.0087(7) O3 0.0062(7) 0.0074(7) 0.0096(7) -0.0026(6) -0.0010(6) 0.0026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 A O3 1.9378(15) 12_565 ? A O3 1.9378(15) 3_565 ? A O3 1.9378(15) 10_665 ? A O3 1.9378(15) 2_665 ? A O3 1.9378(15) 11 ? A O3 1.9378(15) . ? A T2 2.8573(12) . ? A T2 2.8573(12) 3_565 ? A T2 2.8573(12) 2_665 ? C O2 3.0569(19) 7 ? C O2 3.0569(19) 4 ? C O2 3.0569(19) 11 ? C O2 3.0569(19) 2 ? C O2 3.0569(19) 12 ? C O2 3.0569(19) 3 ? C O2 3.0569(19) 10 ? C O2 3.0569(19) 9 ? C O2 3.0569(19) 8 ? C O2 3.0569(19) 6 ? C O2 3.0569(19) 5 ? C O2 3.0569(19) . ? T1 O3 1.5951(16) . ? T1 O1 1.6066(10) . ? T1 O2 1.6197(17) . ? T1 O2 1.6231(17) 6 ? T1 T2 3.0106(10) . ? T2 O3 1.9393(15) 12_565 ? T2 O3 1.9393(15) 4_565 ? T2 O3 1.9393(15) 9 ? T2 O3 1.9393(15) . ? T2 A 2.8573(12) 4_565 ? T2 T1 3.0105(10) 12_565 ? T2 T1 3.0105(10) 4_565 ? T2 T1 3.0105(10) 9 ? O1 T1 1.6067(10) 16 ? O2 T1 1.6231(17) 5 ? 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 O3 A O3 91.36(9) 12_565 3_565 ? O3 A O3 91.85(6) 12_565 10_665 ? O3 A O3 85.09(9) 3_565 10_665 ? O3 A O3 175.64(9) 12_565 2_665 ? O3 A O3 91.85(6) 3_565 2_665 ? O3 A O3 91.36(9) 10_665 2_665 ? O3 A O3 91.85(6) 12_565 11 ? O3 A O3 175.64(9) 3_565 11 ? O3 A O3 91.85(6) 10_665 11 ? O3 A O3 85.09(9) 2_665 11 ? O3 A O3 85.09(9) 12_565 . ? O3 A O3 91.85(6) 3_565 . ? O3 A O3 175.64(9) 10_665 . ? O3 A O3 91.85(6) 2_665 . ? O3 A O3 91.36(9) 11 . ? O3 A T2 42.55(4) 12_565 . ? O3 A T2 92.18(4) 3_565 . ? O3 A T2 134.32(5) 10_665 . ? O3 A T2 134.32(5) 2_665 . ? O3 A T2 92.18(4) 11 . ? O3 A T2 42.55(4) . . ? O3 A T2 92.18(4) 12_565 3_565 ? O3 A T2 42.55(4) 3_565 3_565 ? O3 A T2 42.55(4) 10_665 3_565 ? O3 A T2 92.18(4) 2_665 3_565 ? O3 A T2 134.32(5) 11 3_565 ? O3 A T2 134.32(4) . 3_565 ? T2 A T2 120.0 . 3_565 ? O3 A T2 134.32(5) 12_565 2_665 ? O3 A T2 134.32(5) 3_565 2_665 ? O3 A T2 92.18(4) 10_665 2_665 ? O3 A T2 42.55(4) 2_665 2_665 ? O3 A T2 42.55(4) 11 2_665 ? O3 A T2 92.18(4) . 2_665 ? T2 A T2 120.0 . 2_665 ? T2 A T2 120.0 3_565 2_665 ? O2 C O2 162.30(6) 7 4 ? O2 C O2 49.48(2) 7 11 ? O2 C O2 147.70(6) 4 11 ? O2 C O2 147.70(6) 7 2 ? O2 C O2 49.48(2) 4 2 ? O2 C O2 101.07(6) 11 2 ? O2 C O2 49.48(2) 7 12 ? O2 C O2 114.01(6) 4 12 ? O2 C O2 92.91(4) 11 12 ? O2 C O2 162.30(6) 2 12 ? O2 C O2 114.01(6) 7 3 ? O2 C O2 49.48(2) 4 3 ? O2 C O2 162.30(6) 11 3 ? O2 C O2 92.91(4) 2 3 ? O2 C O2 75.74(6) 12 3 ? O2 C O2 113.65(7) 7 10 ? O2 C O2 69.28(6) 4 10 ? O2 C O2 92.91(5) 11 10 ? O2 C O2 75.74(6) 2 10 ? O2 C O2 92.91(5) 12 10 ? O2 C O2 101.07(6) 3 10 ? O2 C O2 92.91(5) 7 9 ? O2 C O2 101.07(6) 4 9 ? O2 C O2 49.48(2) 11 9 ? O2 C O2 69.28(6) 2 9 ? O2 C O2 113.65(7) 12 9 ? O2 C O2 147.70(6) 3 9 ? O2 C O2 49.48(2) 10 9 ? O2 C O2 92.91(5) 7 8 ? O2 C O2 75.74(6) 4 8 ? O2 C O2 113.65(7) 11 8 ? O2 C O2 114.01(6) 2 8 ? O2 C O2 49.48(2) 12 8 ? O2 C O2 69.28(6) 3 8 ? O2 C O2 49.48(2) 10 8 ? O2 C O2 92.91(5) 9 8 ? O2 C O2 101.07(6) 7 6 ? O2 C O2 92.91(5) 4 6 ? O2 C O2 69.28(6) 11 6 ? O2 C O2 49.48(2) 2 6 ? O2 C O2 147.70(6) 12 6 ? O2 C O2 113.65(7) 3 6 ? O2 C O2 114.01(6) 10 6 ? O2 C O2 75.74(6) 9 6 ? O2 C O2 162.30(6) 8 6 ? O2 C O2 75.74(6) 7 5 ? O2 C O2 92.91(5) 4 5 ? O2 C O2 114.01(6) 11 5 ? O2 C O2 113.65(7) 2 5 ? O2 C O2 69.28(6) 12 5 ? O2 C O2 49.48(2) 3 5 ? O2 C O2 147.70(6) 10 5 ? O2 C O2 162.30(6) 9 5 ? O2 C O2 101.07(6) 8 5 ? O2 C O2 92.91(5) 6 5 ? O2 C O2 69.28(6) 7 . ? O2 C O2 113.65(7) 4 . ? O2 C O2 75.74(6) 11 . ? O2 C O2 92.91(4) 2 . ? O2 C O2 101.07(6) 12 . ? O2 C O2 92.91(5) 3 . ? O2 C O2 162.30(6) 10 . ? O2 C O2 114.01(6) 9 . ? O2 C O2 147.70(6) 8 . ? O2 C O2 49.48(2) 6 . ? O2 C O2 49.48(2) 5 . ? O3 T1 O1 111.25(10) . . ? O3 T1 O2 111.84(8) . . ? O1 T1 O2 110.44(11) . . ? O3 T1 O2 108.61(8) . 6 ? O1 T1 O2 110.27(11) . 6 ? O2 T1 O2 104.18(12) . 6 ? O3 T1 T2 35.21(5) . . ? O1 T1 T2 121.39(9) . . ? O2 T1 T2 125.57(6) . . ? O2 T1 T2 73.63(6) 6 . ? O3 T1 C 111.67(7) . . ? O1 T1 C 137.06(8) . . ? O2 T1 C 53.14(6) . . ? O2 T1 C 53.17(6) 6 . ? T2 T1 C 93.67(3) . . ? O3 T2 O3 135.20(9) 12_565 4_565 ? O3 T2 O3 112.18(9) 12_565 9 ? O3 T2 O3 85.01(9) 4_565 9 ? O3 T2 O3 85.01(9) 12_565 . ? O3 T2 O3 112.18(9) 4_565 . ? O3 T2 O3 135.20(9) 9 . ? O3 T2 A 42.50(4) 12_565 . ? O3 T2 A 137.50(4) 4_565 . ? O3 T2 A 137.50(4) 9 . ? O3 T2 A 42.51(4) . . ? O3 T2 A 137.49(4) 12_565 4_565 ? O3 T2 A 42.50(4) 4_565 4_565 ? O3 T2 A 42.51(4) 9 4_565 ? O3 T2 A 137.49(4) . 4_565 ? A T2 A 180.0 . 4_565 ? O3 T2 T1 28.31(4) 12_565 12_565 ? O3 T2 T1 112.33(5) 4_565 12_565 ? O3 T2 T1 97.71(5) 9 12_565 ? O3 T2 T1 111.49(5) . 12_565 ? A T2 T1 69.598(13) . 12_565 ? A T2 T1 110.401(13) 4_565 12_565 ? O3 T2 T1 112.33(5) 12_565 4_565 ? O3 T2 T1 28.31(4) 4_565 4_565 ? O3 T2 T1 111.49(5) 9 4_565 ? O3 T2 T1 97.71(5) . 4_565 ? A T2 T1 110.402(13) . 4_565 ? A T2 T1 69.597(13) 4_565 4_565 ? T1 T2 T1 97.91(3) 12_565 4_565 ? O3 T2 T1 97.71(5) 12_565 9 ? O3 T2 T1 111.49(5) 4_565 9 ? O3 T2 T1 28.31(4) 9 9 ? O3 T2 T1 112.33(5) . 9 ? A T2 T1 110.402(13) . 9 ? A T2 T1 69.599(13) 4_565 9 ? T1 T2 T1 96.05(4) 12_565 9 ? T1 T2 T1 139.20(3) 4_565 9 ? O3 T2 T1 111.49(5) 12_565 . ? O3 T2 T1 97.71(5) 4_565 . ? O3 T2 T1 112.33(5) 9 . ? O3 T2 T1 28.31(4) . . ? A T2 T1 69.599(13) . . ? A T2 T1 110.402(13) 4_565 . ? T1 T2 T1 139.20(3) 12_565 . ? T1 T2 T1 96.05(4) 4_565 . ? T1 T2 T1 97.91(3) 9 . ? T1 O1 T1 151.03(16) . 16 ? T1 O2 T1 152.81(11) . 5 ? T1 O2 C 101.77(7) . . ? T1 O2 C 101.68(7) 5 . ? T1 O3 A 142.90(9) . . ? T1 O3 T2 116.48(8) . . ? A O3 T2 94.95(7) . . ? _refine_diff_density_max 0.404 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.077 _shelxl_version_number 2014-3 _shelx_res_file ; TITL p6mcc in P6/mcc CELL 0.71073 9.898 9.898 14.276 90.000 90.000 120.000 ZERR 2.00 0.004 0.004 0.006 0.000 0.000 0.000 LATT 1 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM -X, -Y, Z SYMM Y, -X+Y, Z SYMM X-Y, X, Z SYMM Y, X, 0.5-Z SYMM X-Y, -Y, 0.5-Z SYMM -X, -X+Y, 0.5-Z SYMM -Y, -X, 0.5-Z SYMM -X+Y, Y, 0.5-Z SYMM X, X-Y, 0.5-Z SFAC O2- 3.04484 7.98437 0.50181 3.73146 1.55609 0.32297 4.20924 = 23.9207 0.23641 0.0106 0.006 32.5 0.66 15.9994 SFAC LI SI K TI UNIT 6 60 24 2 4 L.S. 10 BOND ACTA WGHT 0.024900 2.278000 FVAR 0.35165 A 5 0.333333 0.666667 0.250000 0.16682 0.00381 0.00381 = 0.00553 0.00000 0.00000 0.00190 C 4 0.000000 0.000000 0.250000 0.08640 0.02178 0.02178 = 0.02259 0.00000 0.00000 0.01089 T1 3 0.122431 0.361488 0.108963 11.00000 0.00599 0.00646 = 0.00562 -0.00060 -0.00026 0.00317 T2 2 0.000000 0.500000 0.250000 0.24922 0.00786 0.01296 = 0.02007 0.00000 0.00000 0.00393 O1 1 0.137778 0.407528 0.000000 10.50000 0.02144 0.01617 = 0.00614 0.00000 0.00000 0.00841 O2 1 0.226661 0.281520 0.132826 11.00000 0.01110 0.01347 = 0.01617 -0.00130 -0.00253 0.00868 O3 1 0.166787 0.508723 0.174210 11.00000 0.00622 0.00744 = 0.00955 -0.00258 -0.00098 0.00263 HKLF 4 REM p6mcc in P6/mcc REM R1 = 0.0208 for 392 Fo > 4sig(Fo) and 0.0367 for all 497 data REM 44 parameters refined using 0 restraints END WGHT 0.0196 1.0817 REM Highest difference peak 0.404, deepest hole -0.308, 1-sigma level 0.077 Q1 1 0.3044 0.3943 0.0000 10.50000 0.05 0.40 Q2 1 0.0000 0.5000 0.0000 10.25000 0.05 0.38 Q3 1 0.0000 0.0000 0.0639 10.16667 0.05 0.29 Q4 1 0.0000 0.6259 0.2500 10.50000 0.05 0.28 Q5 1 0.2348 0.2226 0.0353 11.00000 0.05 0.27 Q6 1 0.2872 0.5522 0.0000 10.50000 0.05 0.26 Q7 1 0.0000 0.5000 0.1776 10.50000 0.05 0.26 Q8 1 0.3688 0.4948 0.0000 10.50000 0.05 0.25 Q9 1 -0.0466 0.4119 0.0335 11.00000 0.05 0.25 Q10 1 0.0870 0.2558 0.0000 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