#------------------------------------------------------------------------------ #$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/23/82/2238282.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_2238282 loop_ _publ_author_name 'Andrade, Marcelo B.' 'Doell, Donald' 'Downs, Robert T.' 'Yang, Hexiong' _publ_section_title ; Redetermination of katayamalite, KLi~3~Ca~7~Ti~2~(SiO~3~)~12~(OH)~2~ ; _journal_coeditor_code WM2749 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i41 _journal_paper_doi 10.1107/S1600536813016620 _journal_volume 69 _journal_year 2013 _chemical_formula_iupac 'K Li3 Ca7 Ti2 (Si O3)12 (O H)2' _chemical_formula_moiety '2(O18 Si6 Ti), 2(H O), 7(Ca), K, 3(Li)' _chemical_formula_structural 'K Li3 Ca7 Ti2 (Si O3)12 (O H)2' _chemical_formula_sum 'Ca7 H2 K Li3 O38 Si12 Ti2' _chemical_formula_weight 1383.38 _chemical_name_common ' katayamalite' _chemical_name_systematic ; Potassium trilithium heptacalcium dititanium dodecasilicate dihydroxide ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 112.396(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 16.9093(10) _cell_length_b 9.7287(5) _cell_length_c 20.9019(12) _cell_measurement_reflns_used 5222 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 32.180 _cell_measurement_theta_min 2.654 _cell_volume 3179.1(3) _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_molecular_graphics 'Xtal-Draw (Downs & Hall-Wallace, 2003)' _computing_publication_material 'publCIF (Westrip, 2010)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.961 _diffrn_measured_fraction_theta_max 0.853 _diffrn_measurement_device_type 'Bruker X8 APEXII CCD' _diffrn_measurement_method '\f and \w scan' _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 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0494 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 26611 _diffrn_reflns_theta_full 25.50 _diffrn_reflns_theta_max 32.40 _diffrn_reflns_theta_min 2.11 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.361 _exptl_absorpt_correction_T_max 0.8911 _exptl_absorpt_correction_T_min 0.8713 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2744 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.831 _refine_diff_density_min -0.561 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 290 _refine_ls_number_reflns 4873 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0348 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.7329P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.0825 _reflns_number_gt 3632 _reflns_number_total 4873 _reflns_threshold_expression I>2sigma(I) _iucr_refine_instructions_details ; TITL kata in C2/c CELL 0.71073 16.9093 9.7287 20.9019 90.000 112.396 90.000 ZERR 4.00 0.0010 0.0005 0.0012 0.000 0.003 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC LI H O SI K CA TI UNIT 12 8 152 48 4 28 8 rem shel 100 .66 L.S. 10 BOND FMAP 2 PLAN 20 OMIT -2 0 2 OMIT -2 4 4 OMIT 2 4 2 OMIT -7 1 2 OMIT 5 3 0 SIZE 0.06 0.05 0.05 ACTA 51 BOND $H CONF HTAB DFIX -0.72 O19 H1 WGHT 0.040800 1.374600 FVAR 0.04392 K 5 0.000000 0.071196 0.250000 10.50000 0.03523 0.03422 = 0.04102 0.00000 0.01702 0.00000 LI1 1 0.500000 0.083500 0.250000 10.50000 0.00618 0.02741 = 0.01647 0.00000 0.00418 0.00000 LI2 1 0.245800 0.317975 0.248619 11.00000 0.01589 0.01449 = 0.02394 -0.00154 0.00621 0.00258 CA1 6 0.220094 -0.072600 0.513111 11.00000 0.00838 0.01008 = 0.01555 -0.00022 0.00567 -0.00001 CA2 6 0.145296 0.283466 0.507103 11.00000 0.00809 0.01040 = 0.01549 0.00022 0.00533 0.00036 CA3 6 0.072475 0.638591 0.500047 11.00000 0.00792 0.01067 = 0.01431 0.00019 0.00541 -0.00007 CA4 6 0.000000 0.000000 0.500000 10.50000 0.00714 0.01009 = 0.01435 -0.00079 0.00420 0.00003 TI 7 0.334498 0.070409 0.251642 11.00000 0.00371 0.00631 = 0.00807 0.00031 0.00264 0.00022 SI1 4 0.614186 0.265048 0.360444 11.00000 0.00583 0.00923 = 0.01107 -0.00087 0.00405 -0.00051 SI2 4 0.430819 0.323460 0.359740 11.00000 0.00557 0.00910 = 0.01082 -0.00079 0.00293 0.00008 SI3 4 0.368717 0.635009 0.359265 11.00000 0.00520 0.00862 = 0.01089 0.00005 0.00260 -0.00020 SI4 4 0.491090 0.880118 0.360465 11.00000 0.00487 0.00962 = 0.01018 0.00091 0.00269 -0.00012 SI5 4 0.673946 0.815565 0.359093 11.00000 0.00644 0.00851 = 0.01129 0.00061 0.00464 0.00054 SI6 4 0.738644 0.507905 0.362076 11.00000 0.00680 0.00842 = 0.01114 -0.00015 0.00477 -0.00028 O1 3 0.658540 0.402718 0.345112 11.00000 0.01237 0.01298 = 0.02021 0.00075 0.00758 -0.00467 O2 3 0.659314 0.223138 0.440962 11.00000 0.01075 0.01431 = 0.01246 -0.00060 0.00528 0.00031 O3 3 0.613026 0.144153 0.308068 11.00000 0.00957 0.01297 = 0.01547 -0.00364 0.00644 -0.00037 O4 3 0.514861 0.310070 0.340259 11.00000 0.00690 0.01856 = 0.01765 0.00042 0.00612 0.00241 O5 3 0.352759 0.238856 0.305234 11.00000 0.00753 0.01301 = 0.01318 -0.00185 0.00221 -0.00053 O6 3 0.452623 0.283030 0.439175 11.00000 0.01240 0.01625 = 0.01444 -0.00028 0.00520 -0.00096 O7 3 0.409849 0.488209 0.350899 11.00000 0.01340 0.00877 = 0.02717 -0.00074 0.00836 0.00246 O8 3 0.273419 0.652928 0.304109 11.00000 0.00632 0.01389 = 0.01748 0.00113 0.00211 -0.00132 O9 3 0.378539 0.650304 0.438478 11.00000 0.01192 0.01614 = 0.01337 0.00000 0.00461 -0.00134 O10 3 0.427035 0.748367 0.340654 11.00000 0.00997 0.01542 = 0.01770 0.00172 0.00668 -0.00369 O11 3 0.520723 0.920802 0.440865 11.00000 0.01128 0.01340 = 0.01302 -0.00082 0.00503 -0.00055 O12 3 0.448279 0.004517 0.308239 11.00000 0.00680 0.01326 = 0.01502 0.00228 0.00421 0.00055 O13 3 0.572621 0.820689 0.345348 11.00000 0.00679 0.01719 = 0.02334 0.00031 0.00808 0.00184 O14 3 0.728712 0.853922 0.438470 11.00000 0.01273 0.01432 = 0.01337 -0.00050 0.00443 -0.00002 O15 3 0.694977 0.907010 0.303954 11.00000 0.01278 0.01088 = 0.01445 0.00305 0.00740 0.00193 O16 3 0.692324 0.656964 0.344646 11.00000 0.01830 0.01041 = 0.02039 0.00056 0.01085 0.00376 O17 3 0.785715 0.476595 0.309943 11.00000 0.01239 0.01210 = 0.01438 -0.00008 0.00922 0.00063 O18 3 0.801318 0.497998 0.442757 11.00000 0.01133 0.01544 = 0.01093 -0.00014 0.00372 0.00075 O19 3 0.101281 0.069215 0.457504 11.00000 0.01431 0.01558 = 0.00973 -0.00061 0.00469 0.00004 rem SADI 0.0 O19 H1 rem H1 2 0.101397 0.074226 0.434777 11.00000 10.04 rem H1 2 0.097083 0.074458 0.423046 11.00000 -1.20000 H1 2 0.096742 0.074340 0.423840 11.00000 -1.20000 HKLF 4 REM kata in C2/c REM R1 = 0.0348 for 3632 Fo > 4sig(Fo) and 0.0591 for all 4873 data REM 290 parameters refined using 1 restraints END WGHT 0.0407 1.3995 REM Highest difference peak 0.831, deepest hole -0.561, 1-sigma level 0.143 Q1 1 -0.0400 0.0737 0.1747 11.00000 0.05 0.83 Q2 1 0.0805 0.7243 0.5139 11.00000 0.05 0.70 Q3 1 0.0683 0.5606 0.4864 11.00000 0.05 0.69 Q4 1 0.3413 0.1549 0.2754 11.00000 0.05 0.68 Q5 1 -0.0256 -0.0013 0.4570 11.00000 0.05 0.65 Q6 1 0.7091 0.8074 0.4170 11.00000 0.05 0.65 Q7 1 0.2431 -0.0772 0.5580 11.00000 0.05 0.63 Q8 1 0.5036 0.8654 0.4158 11.00000 0.05 0.61 Q9 1 0.2784 0.7522 0.3075 11.00000 0.05 0.61 Q10 1 0.4629 -0.0958 0.3072 11.00000 0.05 0.60 Q11 1 0.3418 -0.0029 0.2635 11.00000 0.05 0.60 Q12 1 0.6494 0.3315 0.3446 11.00000 0.05 0.59 Q13 1 0.6626 0.7452 0.3271 11.00000 0.05 0.58 Q14 1 0.4445 0.3201 0.4080 11.00000 0.05 0.58 Q15 1 0.1036 0.6273 0.5475 11.00000 0.05 0.57 Q16 1 0.6848 0.9926 0.2979 11.00000 0.05 0.56 Q17 1 0.3908 0.6316 0.4078 11.00000 0.05 0.56 Q18 1 0.2272 -0.1429 0.5267 11.00000 0.05 0.56 Q19 1 0.6000 0.2258 0.3164 11.00000 0.05 0.55 Q20 1 0.3905 0.4178 0.3249 11.00000 0.05 0.55 ; _cod_data_source_file wm2749.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2238282 _cod_database_fobs_code 2238282 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity K K 0.0000 0.07120(12) 0.2500 0.0361(3) Uani d S 1 2 Li Li1 0.5000 0.0835(7) 0.2500 0.0167(15) Uani d S 1 2 Li Li2 0.2458(3) 0.3180(5) 0.2486(3) 0.0185(11) Uani d . 1 1 Ca Ca1 0.22009(3) -0.07260(5) 0.51311(3) 0.01101(12) Uani d . 1 1 Ca Ca2 0.14530(3) 0.28347(5) 0.50710(3) 0.01108(13) Uani d . 1 1 Ca Ca3 0.07248(3) 0.63859(5) 0.50005(3) 0.01062(12) Uani d . 1 1 Ca Ca4 0.0000 0.0000 0.5000 0.01050(17) Uani d S 1 2 Ti Ti 0.33450(3) 0.07041(4) 0.25164(3) 0.00591(11) Uani d . 1 1 Si Si1 0.61419(4) 0.26505(7) 0.36044(4) 0.00846(16) Uani d . 1 1 Si Si2 0.43082(4) 0.32346(7) 0.35974(4) 0.00856(16) Uani d . 1 1 Si Si3 0.36872(4) 0.63501(7) 0.35927(4) 0.00838(16) Uani d . 1 1 Si Si4 0.49109(4) 0.88012(7) 0.36047(4) 0.00828(16) Uani d . 1 1 Si Si5 0.67395(4) 0.81556(7) 0.35909(4) 0.00837(16) Uani d . 1 1 Si Si6 0.73864(4) 0.50791(7) 0.36208(4) 0.00839(16) Uani d . 1 1 O O1 0.65854(12) 0.40272(18) 0.34511(11) 0.0148(4) Uani d . 1 1 O O2 0.65931(12) 0.22314(18) 0.44096(11) 0.0123(4) Uani d . 1 1 O O3 0.61303(12) 0.14415(18) 0.30807(11) 0.0122(4) Uani d . 1 1 O O4 0.51486(12) 0.31007(19) 0.34026(11) 0.0139(4) Uani d . 1 1 O O5 0.35276(11) 0.23886(18) 0.30523(11) 0.0118(4) Uani d . 1 1 O O6 0.45262(12) 0.28303(19) 0.43917(11) 0.0143(4) Uani d . 1 1 O O7 0.40985(12) 0.48821(18) 0.35090(12) 0.0163(5) Uani d . 1 1 O O8 0.27342(12) 0.65293(18) 0.30411(11) 0.0133(4) Uani d . 1 1 O O9 0.37854(12) 0.65030(19) 0.43848(11) 0.0139(4) Uani d . 1 1 O O10 0.42704(12) 0.74837(18) 0.34065(11) 0.0139(4) Uani d . 1 1 O O11 0.52072(12) 0.92080(18) 0.44086(11) 0.0124(4) Uani d . 1 1 O O12 0.44828(11) 0.00452(18) 0.30824(11) 0.0117(4) Uani d . 1 1 O O13 0.57262(11) 0.82069(19) 0.34535(11) 0.0151(4) Uani d . 1 1 O O14 0.72871(12) 0.85392(18) 0.43847(11) 0.0136(4) Uani d . 1 1 O O15 0.69498(12) 0.90701(18) 0.30395(11) 0.0120(4) Uani d . 1 1 O O16 0.69232(13) 0.65696(18) 0.34465(11) 0.0153(4) Uani d . 1 1 O O17 0.78572(12) 0.47659(18) 0.30994(11) 0.0117(4) Uani d . 1 1 O O18 0.80132(12) 0.49800(19) 0.44276(11) 0.0127(4) Uani d . 1 1 O O19 0.10128(13) 0.0692(2) 0.45750(11) 0.0132(4) Uani d D 1 1 H H1 0.097(2) 0.074(4) 0.4238(11) 0.016 Uiso d D 1 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 K 0.0352(6) 0.0342(6) 0.0410(8) 0.000 0.0170(6) 0.000 Li1 0.006(3) 0.027(4) 0.016(4) 0.000 0.004(3) 0.000 Li2 0.016(2) 0.015(2) 0.023(3) 0.0026(18) 0.006(2) -0.002(2) Ca1 0.0084(2) 0.0101(2) 0.0156(4) 0.00000(18) 0.0057(2) -0.0002(2) Ca2 0.0081(2) 0.0104(2) 0.0155(4) 0.00035(17) 0.0053(2) 0.0002(2) Ca3 0.0079(2) 0.0107(2) 0.0142(4) -0.00007(17) 0.0054(2) 0.0002(2) Ca4 0.0072(3) 0.0101(3) 0.0142(5) 0.0000(2) 0.0042(3) -0.0008(3) Ti 0.00370(18) 0.00629(18) 0.0081(3) 0.00022(15) 0.00263(19) 0.00032(17) Si1 0.0058(3) 0.0092(3) 0.0110(5) -0.0005(2) 0.0040(3) -0.0009(3) Si2 0.0056(3) 0.0091(3) 0.0107(5) 0.0001(2) 0.0029(3) -0.0008(3) Si3 0.0052(3) 0.0086(3) 0.0108(5) -0.0002(2) 0.0026(3) 0.0000(3) Si4 0.0049(3) 0.0096(3) 0.0101(5) -0.0001(2) 0.0027(3) 0.0009(3) Si5 0.0065(3) 0.0085(3) 0.0112(5) 0.0005(2) 0.0046(3) 0.0006(3) Si6 0.0068(3) 0.0084(3) 0.0112(5) -0.0003(2) 0.0047(3) -0.0002(3) O1 0.0124(9) 0.0130(9) 0.0202(13) -0.0047(7) 0.0076(9) 0.0007(8) O2 0.0107(9) 0.0143(9) 0.0123(12) 0.0003(7) 0.0052(9) -0.0006(8) O3 0.0096(8) 0.0130(8) 0.0155(12) -0.0004(7) 0.0065(9) -0.0036(8) O4 0.0069(8) 0.0185(9) 0.0176(12) 0.0024(7) 0.0060(9) 0.0004(8) O5 0.0076(8) 0.0130(8) 0.0129(12) -0.0005(7) 0.0022(8) -0.0018(8) O6 0.0125(9) 0.0163(9) 0.0144(13) -0.0010(7) 0.0052(9) -0.0003(8) O7 0.0134(9) 0.0088(8) 0.0274(14) 0.0025(7) 0.0085(10) -0.0007(8) O8 0.0063(8) 0.0139(9) 0.0174(13) -0.0013(7) 0.0021(9) 0.0010(8) O9 0.0119(9) 0.0163(9) 0.0132(13) -0.0013(7) 0.0045(9) 0.0000(8) O10 0.0099(9) 0.0154(9) 0.0177(12) -0.0037(7) 0.0067(9) 0.0017(8) O11 0.0112(9) 0.0134(8) 0.0130(12) -0.0006(7) 0.0050(9) -0.0009(8) O12 0.0068(8) 0.0133(9) 0.0149(12) 0.0006(7) 0.0042(8) 0.0023(8) O13 0.0068(8) 0.0172(9) 0.0233(13) 0.0018(7) 0.0081(9) 0.0004(8) O14 0.0128(9) 0.0143(9) 0.0133(12) 0.0000(7) 0.0045(9) -0.0004(8) O15 0.0128(9) 0.0109(8) 0.0144(12) 0.0019(7) 0.0074(9) 0.0030(7) O16 0.0183(10) 0.0103(9) 0.0207(13) 0.0038(7) 0.0110(10) 0.0005(8) O17 0.0124(9) 0.0121(8) 0.0146(12) 0.0006(7) 0.0092(9) 0.0000(7) O18 0.0114(9) 0.0155(9) 0.0107(12) 0.0008(7) 0.0038(9) -0.0001(8) O19 0.0143(9) 0.0152(9) 0.0140(15) -0.0001(7) 0.0059(10) -0.0008(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Ca Ca 0.2262 0.3064 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O12 Li1 O12 2_655 . 132.6(4) O12 Li1 O3 2_655 . 86.53(8) O12 Li1 O3 . . 107.89(9) O12 Li1 O3 2_655 2_655 107.89(9) O12 Li1 O3 . 2_655 86.53(8) O3 Li1 O3 . 2_655 144.3(4) O15 Li2 O8 3_445 4_545 136.3(3) O15 Li2 O5 3_445 . 110.5(3) O8 Li2 O5 4_545 . 86.1(2) O15 Li2 O17 3_445 2_655 86.6(2) O8 Li2 O17 4_545 2_655 111.4(3) O5 Li2 O17 . 2_655 133.6(3) O15 Ti O3 2_645 2_655 89.64(8) O15 Ti O8 2_645 4_545 90.65(8) O3 Ti O8 2_655 4_545 90.97(8) O15 Ti O17 2_645 3_445 85.19(8) O3 Ti O17 2_655 3_445 173.77(8) O8 Ti O17 4_545 3_445 92.55(8) O15 Ti O5 2_645 . 174.56(8) O3 Ti O5 2_655 . 92.76(8) O8 Ti O5 4_545 . 84.44(8) O17 Ti O5 3_445 . 92.69(8) O15 Ti O12 2_645 . 93.66(8) O3 Ti O12 2_655 . 85.62(8) O8 Ti O12 4_545 . 174.48(8) O17 Ti O12 3_445 . 91.24(8) O5 Ti O12 . . 91.39(8) O3 Si1 O2 . . 113.90(11) O3 Si1 O1 . . 110.90(11) O2 Si1 O1 . . 110.09(11) O3 Si1 O4 . . 106.12(11) O2 Si1 O4 . . 111.69(11) O1 Si1 O4 . . 103.60(10) O5 Si2 O6 . . 114.28(11) O5 Si2 O4 . . 110.02(11) O6 Si2 O4 . . 111.16(11) O5 Si2 O7 . . 109.76(10) O6 Si2 O7 . . 108.12(11) O4 Si2 O7 . . 102.86(11) O8 Si3 O9 . . 114.47(11) O8 Si3 O10 . . 106.95(11) O9 Si3 O10 . . 110.52(11) O8 Si3 O7 . . 111.97(11) O9 Si3 O7 . . 108.15(11) O10 Si3 O7 . . 104.31(11) O12 Si4 O11 1_565 . 113.88(10) O12 Si4 O10 1_565 . 109.69(10) O11 Si4 O10 . . 111.83(11) O12 Si4 O13 1_565 . 109.30(11) O11 Si4 O13 . . 109.83(11) O10 Si4 O13 . . 101.60(10) O15 Si5 O14 . . 114.59(11) O15 Si5 O16 . . 106.47(11) O14 Si5 O16 . . 109.69(11) O15 Si5 O13 . . 111.35(11) O14 Si5 O13 . . 109.23(11) O16 Si5 O13 . . 105.04(11) O17 Si6 O18 . . 113.54(11) O17 Si6 O16 . . 109.83(11) O18 Si6 O16 . . 110.86(11) O17 Si6 O1 . . 108.67(11) O18 Si6 O1 . . 110.52(11) O16 Si6 O1 . . 102.88(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance K O13 3_445 3.083(2) K O13 4_545 3.083(2) K O4 4_545 3.117(2) K O4 3_445 3.117(2) K O1 4_545 3.125(2) K O1 3_445 3.125(2) K O10 4_545 3.141(2) K O10 3_445 3.141(2) K O7 4_545 3.142(2) K O7 3_445 3.142(2) K O16 3_445 3.207(2) K O16 4_545 3.207(2) Li1 O12 2_655 1.910(3) Li1 O12 . 1.910(3) Li1 O3 . 1.925(3) Li1 O3 2_655 1.925(3) Li2 O15 3_445 1.893(6) Li2 O8 4_545 1.904(5) Li2 O5 . 1.906(5) Li2 O17 2_655 1.915(5) Ca1 O19 . 2.348(2) Ca1 O14 5_666 2.3732(19) Ca1 O9 7_556 2.380(2) Ca1 O2 5_656 2.3943(19) Ca1 O18 3_445 2.462(2) Ca1 O2 3_445 2.469(2) Ca2 O19 . 2.321(2) Ca2 O18 5_666 2.3901(19) Ca2 O14 5_666 2.403(2) Ca2 O6 7_556 2.416(2) Ca2 O11 3_445 2.432(2) Ca2 O14 3_445 2.462(2) Ca3 O6 3_455 2.395(2) Ca3 O2 3_455 2.396(2) Ca3 O9 7_566 2.397(2) Ca3 O18 5_666 2.4094(19) Ca3 O11 7_566 2.414(2) Ca3 O11 3_445 2.4414(19) Ca4 O19 5_556 2.310(2) Ca4 O19 . 2.310(2) Ca4 O6 3_445 2.4367(19) Ca4 O6 7_556 2.4367(19) Ca4 O9 3_445 2.4490(19) Ca4 O9 7_556 2.4490(19) Ca4 O7 3_445 2.903(2) Ca4 O7 7_556 2.903(2) Ti O15 2_645 1.9195(19) Ti O3 2_655 1.924(2) Ti O8 4_545 1.9266(19) Ti O17 3_445 1.9402(19) Ti O5 . 1.9422(19) Ti O12 . 1.9436(18) Si1 O3 . 1.602(2) Si1 O2 . 1.613(2) Si1 O1 . 1.6255(19) Si1 O4 . 1.6281(19) Si2 O5 . 1.604(2) Si2 O6 . 1.607(2) Si2 O4 . 1.626(2) Si2 O7 . 1.6367(19) Si3 O8 . 1.594(2) Si3 O9 . 1.607(2) Si3 O10 . 1.622(2) Si3 O7 . 1.6269(19) Si4 O12 1_565 1.606(2) Si4 O11 . 1.609(2) Si4 O10 . 1.6266(19) Si4 O13 . 1.633(2) Si5 O15 . 1.600(2) Si5 O14 . 1.606(2) Si5 O16 . 1.6248(19) Si5 O13 . 1.6265(19) Si6 O17 . 1.605(2) Si6 O18 . 1.617(2) Si6 O16 . 1.6222(19) Si6 O1 . 1.6253(19) O1 K 3 3.125(2) O2 Ca1 5_656 2.3943(19) O2 Ca3 3_545 2.396(2) O2 Ca1 3 2.470(2) O3 Ti 2_655 1.924(2) O4 K 3 3.117(2) O6 Ca3 3_545 2.395(2) O6 Ca2 7_556 2.416(2) O6 Ca4 3 2.4367(19) O7 Ca4 3 2.903(2) O7 K 3 3.142(2) O8 Li2 4 1.904(5) O8 Ti 4 1.9266(19) O9 Ca1 7_556 2.380(2) O9 Ca3 7_566 2.397(2) O9 Ca4 3 2.4490(19) O10 K 3 3.141(2) O11 Ca3 7_566 2.414(2) O11 Ca2 3 2.432(2) O11 Ca3 3 2.4414(19) O12 Si4 1_545 1.606(2) O13 K 3 3.083(2) O14 Ca1 5_666 2.3732(19) O14 Ca2 5_666 2.403(2) O14 Ca2 3 2.462(2) O15 Li2 3 1.893(6) O15 Ti 2_665 1.9195(19) O16 K 3 3.207(2) O17 Li2 2_655 1.915(5) O17 Ti 3 1.9402(19) O18 Ca2 5_666 2.3901(19) O18 Ca3 5_666 2.4094(19) O18 Ca1 3 2.462(2) O19 H1 . 0.680(18)