data_cb1b _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_mineral Fluor-tsilaisite _chemical_formula_sum 'H3.30 Al7.05 B3 Ca0.01 F0.35 Fe0.03 K0 Li0.31 Mn1.64 Na0.62 O30.65 Si5.94 Ti0.04' _chemical_formula_weight 1000.37 _chemical_compound_source 'San Piero in Campo, Elba, Italy' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 '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' 'Mn' 'Mn' 0.3368 0.7283 '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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Ca' 'Ca' 0.2262 0.3064 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system trigonal _space_group_IT_number 160 _space_group_name_H-M_alt 'R 3 m :H' _space_group_name_Hall 'R 3 -2"' _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' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 15.9619(4) _cell_length_b 15.9691(4) _cell_length_c 7.1426(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1576.71(9) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour green-yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.161 _exptl_crystal_F_000 1660 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.200 _exptl_absorpt_coefficient_mu 2.182 _shelx_estimated_absorpt_T_min 0.601 _shelx_estimated_absorpt_T_max 0.669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6630 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker KAPPA APEX-II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13288 _diffrn_reflns_av_unetI/netI 0.0176 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.551 _diffrn_reflns_theta_max 36.346 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 1746 _reflns_number_gt 1732 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.986 _reflns_Friedel_fraction_max 0.977 _reflns_Friedel_fraction_full 1.000 _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-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion twin. ; _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^)+(0.0169P)^2^+1.8832P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0057(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.02(3) _chemical_absolute_configuration ? _refine_ls_number_reflns 1746 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0166 _refine_ls_R_factor_gt 0.0164 _refine_ls_wR_factor_ref 0.0393 _refine_ls_wR_factor_gt 0.0392 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 Ca Ca 0.0000 0.0000 0.2257(5) 0.0269(11) Uani 0.0143 6 d S T P . . K K 0.0000 0.0000 0.2257(5) 0.0269(11) Uani 0.0046 6 d S T P . . Na Na 0.0000 0.0000 0.2257(5) 0.0269(11) Uani 0.614(11) 6 d S T P . . LiY Li 0.12432(4) 0.06216(2) 0.62286(10) 0.01170(15) Uani 0.1019 2 d S T P . . FeY Fe 0.12432(4) 0.06216(2) 0.62286(10) 0.01170(15) Uani 0.009 2 d S T P . . TiY Ti 0.12432(4) 0.06216(2) 0.62286(10) 0.01170(15) Uani 0.0137 2 d S T P . . AlY Al 0.12432(4) 0.06216(2) 0.62286(10) 0.01170(15) Uani 0.395(6) 2 d S T P . . MnY Mn 0.12432(4) 0.06216(2) 0.62286(10) 0.01170(15) Uani 0.481(6) 2 d S T P . . AlZ Al 0.29816(3) 0.26145(3) 0.61080(9) 0.00625(13) Uani 0.969(4) 1 d . . P . . MnZ Mn 0.29816(3) 0.26145(3) 0.61080(9) 0.00625(13) Uani 0.031(4) 1 d . . P . . B B 0.11012(8) 0.22025(16) 0.4541(3) 0.0068(3) Uani 1 2 d S T P . . Si Si 0.19185(3) 0.18988(3) 0.0000 0.00476(9) Uani 0.9895 1 d . . P . . AlT Al 0.19185(3) 0.18988(3) 0.0000 0.00476(9) Uani 0.0105 1 d . . P . . O1 O 0.0000 0.0000 0.7780(6) 0.0441(12) Uani 0.6537 6 d S T P . . F1 F 0.0000 0.0000 0.7780(6) 0.0441(12) Uani 0.3463 6 d S T P . . O2 O 0.06157(6) 0.12315(13) 0.4827(3) 0.0197(4) Uani 1 2 d S T P . . O3 O 0.26844(14) 0.13422(7) 0.5098(3) 0.0121(3) Uani 1 2 d S T P . . H3 H 0.260(3) 0.1301(14) 0.394(6) 0.018 Uiso 1 2 d S U P . . O4 O 0.09366(6) 0.18732(12) 0.0693(2) 0.0084(3) Uani 1 2 d S T P . . O5 O 0.18713(12) 0.09357(6) 0.0913(2) 0.0088(3) Uani 1 2 d S T P . . O6 O 0.19745(8) 0.18725(8) 0.77534(18) 0.00769(19) Uani 1 1 d . . . . . O7 O 0.28527(7) 0.28572(7) 0.07944(17) 0.00650(18) Uani 1 1 d . . . . . O8 O 0.20999(8) 0.27099(8) 0.44110(18) 0.00816(19) 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 Ca 0.0288(13) 0.0288(13) 0.0233(19) 0.000 0.000 0.0144(6) K 0.0288(13) 0.0288(13) 0.0233(19) 0.000 0.000 0.0144(6) Na 0.0288(13) 0.0288(13) 0.0233(19) 0.000 0.000 0.0144(6) LiY 0.0101(2) 0.00757(17) 0.0182(3) -0.00157(8) -0.00314(16) 0.00507(11) FeY 0.0101(2) 0.00757(17) 0.0182(3) -0.00157(8) -0.00314(16) 0.00507(11) TiY 0.0101(2) 0.00757(17) 0.0182(3) -0.00157(8) -0.00314(16) 0.00507(11) AlY 0.0101(2) 0.00757(17) 0.0182(3) -0.00157(8) -0.00314(16) 0.00507(11) MnY 0.0101(2) 0.00757(17) 0.0182(3) -0.00157(8) -0.00314(16) 0.00507(11) AlZ 0.00643(19) 0.00703(19) 0.0054(2) 0.00056(14) -0.00012(13) 0.00342(14) MnZ 0.00643(19) 0.00703(19) 0.0054(2) 0.00056(14) -0.00012(13) 0.00342(14) B 0.0074(6) 0.0057(8) 0.0067(9) 0.0000(6) 0.0000(3) 0.0029(4) Si 0.00481(16) 0.00467(15) 0.00484(18) -0.00042(12) -0.00017(12) 0.00239(11) AlT 0.00481(16) 0.00467(15) 0.00484(18) -0.00042(12) -0.00017(12) 0.00239(11) O1 0.062(2) 0.062(2) 0.0083(18) 0.000 0.000 0.0310(10) F1 0.062(2) 0.062(2) 0.0083(18) 0.000 0.000 0.0310(10) O2 0.0318(9) 0.0054(6) 0.0131(10) 0.0005(6) 0.0003(3) 0.0027(3) O3 0.0249(8) 0.0111(5) 0.0050(7) -0.0002(3) -0.0003(6) 0.0124(4) O4 0.0065(4) 0.0129(7) 0.0081(7) -0.0013(5) -0.0007(3) 0.0064(3) O5 0.0140(7) 0.0068(4) 0.0080(7) 0.0008(3) 0.0017(5) 0.0070(3) O6 0.0084(4) 0.0096(4) 0.0044(5) -0.0004(3) 0.0002(3) 0.0040(3) O7 0.0059(4) 0.0060(4) 0.0056(5) -0.0007(3) -0.0001(3) 0.0015(3) O8 0.0058(4) 0.0116(5) 0.0082(5) 0.0029(4) 0.0007(3) 0.0052(4) _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 Ca O2 2.503(3) 2 ? Ca O2 2.503(3) 3 ? Ca O2 2.504(3) . ? Ca O5 2.759(2) . ? Ca O5 2.760(2) 2 ? Ca O5 2.760(2) 3 ? Ca O4 2.820(2) 2 ? Ca O4 2.821(2) 3 ? Ca O4 2.821(2) . ? LiY O2 1.9823(13) . ? LiY O2 1.9826(13) 3 ? LiY O1 2.045(2) . ? LiY O6 2.0508(12) 6 ? LiY O6 2.0511(12) . ? LiY O3 2.150(2) . ? LiY MnY 2.9765(9) 2 ? LiY AlY 2.9765(9) 2 ? LiY TiY 2.9765(9) 2 ? LiY FeY 2.9765(9) 2 ? LiY LiY 2.9765(9) 2 ? AlZ O6 1.8613(12) . ? AlZ O7 1.8817(12) 8 ? AlZ O8 1.8837(12) 8 ? AlZ O8 1.9204(12) . ? AlZ O7 1.9588(11) 15 ? AlZ O3 1.9773(9) . ? AlZ MnZ 2.9382(5) 8 ? AlZ AlZ 2.9382(5) 8 ? AlZ MnZ 2.9383(5) 15_554 ? AlZ AlZ 2.9383(5) 15_554 ? B O2 1.358(3) . ? B O8 1.3836(16) . ? B O8 1.3840(16) 5 ? Si O6 1.6089(13) 1_554 ? Si O7 1.6142(11) . ? Si O4 1.6244(7) . ? Si O5 1.6373(8) . ? O1 MnY 2.045(2) 2 ? O1 AlY 2.045(2) 2 ? O1 LiY 2.045(2) 2 ? O1 TiY 2.045(2) 2 ? O1 FeY 2.045(2) 2 ? O1 MnY 2.045(2) 3 ? O1 FeY 2.045(2) 3 ? O2 MnY 1.9820(13) 2 ? O2 AlY 1.9820(13) 2 ? O2 TiY 1.9820(13) 2 ? O2 FeY 1.9820(13) 2 ? O2 LiY 1.9820(13) 2 ? O3 MnZ 1.9771(9) 6 ? O3 AlZ 1.9771(9) 6 ? O3 H3 0.83(4) . ? O4 AlT 1.6244(7) 5 ? O4 Si 1.6244(7) 5 ? O5 AlT 1.6373(8) 6 ? O5 Si 1.6373(8) 6 ? O6 AlT 1.6089(13) 1_556 ? O6 Si 1.6089(13) 1_556 ? O7 MnZ 1.8819(11) 15_554 ? O7 AlZ 1.8819(11) 15_554 ? O7 AlZ 1.9583(11) 8_554 ? O7 MnZ 1.9583(11) 8_554 ? O8 MnZ 1.8841(12) 15_554 ? O8 AlZ 1.8841(12) 15_554 ? 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 O2 Ca O2 72.16(12) 2 3 ? O2 Ca O2 72.17(12) 2 . ? O2 Ca O2 72.19(12) 3 . ? O2 Ca O5 153.22(15) 2 . ? O2 Ca O5 86.36(5) 3 . ? O2 Ca O5 86.35(5) . . ? O2 Ca O5 86.36(5) 2 2 ? O2 Ca O5 153.22(15) 3 2 ? O2 Ca O5 86.33(5) . 2 ? O5 Ca O5 108.54(8) . 2 ? O2 Ca O5 86.35(5) 2 3 ? O2 Ca O5 86.33(5) 3 3 ? O2 Ca O5 153.22(15) . 3 ? O5 Ca O5 108.56(8) . 3 ? O5 Ca O5 108.58(8) 2 3 ? O2 Ca O4 70.49(6) 2 2 ? O2 Ca O4 127.05(6) 3 2 ? O2 Ca O4 127.06(6) . 2 ? O5 Ca O4 136.29(15) . 2 ? O5 Ca O4 55.39(3) 2 2 ? O5 Ca O4 55.37(3) 3 2 ? O2 Ca O4 127.05(6) 2 3 ? O2 Ca O4 70.48(6) 3 3 ? O2 Ca O4 127.08(6) . 3 ? O5 Ca O4 55.39(3) . 3 ? O5 Ca O4 136.30(15) 2 3 ? O5 Ca O4 55.35(3) 3 3 ? O4 Ca O4 105.32(9) 2 3 ? O2 Ca O4 127.05(6) 2 . ? O2 Ca O4 127.07(6) 3 . ? O2 Ca O4 70.47(6) . . ? O5 Ca O4 55.37(3) . . ? O5 Ca O4 55.35(3) 2 . ? O5 Ca O4 136.31(15) 3 . ? O4 Ca O4 105.34(9) 2 . ? O4 Ca O4 105.36(9) 3 . ? O2 LiY O2 96.14(11) . 3 ? O2 LiY O1 84.61(8) . . ? O2 LiY O1 84.59(8) 3 . ? O2 LiY O6 175.30(6) . 6 ? O2 LiY O6 88.35(6) 3 6 ? O1 LiY O6 97.26(8) . 6 ? O2 LiY O6 88.34(6) . . ? O2 LiY O6 175.30(6) 3 . ? O1 LiY O6 97.28(8) . . ? O6 LiY O6 87.14(7) 6 . ? O2 LiY O3 102.45(6) . . ? O2 LiY O3 102.47(6) 3 . ? O1 LiY O3 169.26(11) . . ? O6 LiY O3 75.10(5) 6 . ? O6 LiY O3 75.08(5) . . ? O2 LiY MnY 41.33(5) . 2 ? O2 LiY MnY 89.60(5) 3 2 ? O1 LiY MnY 43.30(7) . 2 ? O6 LiY MnY 140.49(4) 6 2 ? O6 LiY MnY 94.71(3) . 2 ? O3 LiY MnY 143.37(3) . 2 ? O2 LiY AlY 41.33(5) . 2 ? O2 LiY AlY 89.60(5) 3 2 ? O1 LiY AlY 43.30(7) . 2 ? O6 LiY AlY 140.49(4) 6 2 ? O6 LiY AlY 94.71(3) . 2 ? O3 LiY AlY 143.37(3) . 2 ? MnY LiY AlY 0.00(3) 2 2 ? O2 LiY TiY 41.33(5) . 2 ? O2 LiY TiY 89.60(5) 3 2 ? O1 LiY TiY 43.30(7) . 2 ? O6 LiY TiY 140.49(4) 6 2 ? O6 LiY TiY 94.71(3) . 2 ? O3 LiY TiY 143.37(3) . 2 ? MnY LiY TiY 0.00(3) 2 2 ? AlY LiY TiY 0.00(3) 2 2 ? O2 LiY FeY 41.33(5) . 2 ? O2 LiY FeY 89.60(5) 3 2 ? O1 LiY FeY 43.30(7) . 2 ? O6 LiY FeY 140.49(4) 6 2 ? O6 LiY FeY 94.71(3) . 2 ? O3 LiY FeY 143.37(3) . 2 ? MnY LiY FeY 0.00(3) 2 2 ? AlY LiY FeY 0.00(3) 2 2 ? TiY LiY FeY 0.00(3) 2 2 ? O2 LiY LiY 41.33(5) . 2 ? O2 LiY LiY 89.60(5) 3 2 ? O1 LiY LiY 43.30(7) . 2 ? O6 LiY LiY 140.49(4) 6 2 ? O6 LiY LiY 94.71(3) . 2 ? O3 LiY LiY 143.37(3) . 2 ? MnY LiY LiY 0.00(3) 2 2 ? AlY LiY LiY 0.00(3) 2 2 ? TiY LiY LiY 0.00(3) 2 2 ? FeY LiY LiY 0.00(3) 2 2 ? O6 AlZ O7 169.03(6) . 8 ? O6 AlZ O8 94.46(6) . 8 ? O7 AlZ O8 96.50(5) 8 8 ? O6 AlZ O8 90.86(5) . . ? O7 AlZ O8 78.33(5) 8 . ? O8 AlZ O8 171.44(5) 8 . ? O6 AlZ O7 92.70(5) . 15 ? O7 AlZ O7 90.31(2) 8 15 ? O8 AlZ O7 77.36(5) 8 15 ? O8 AlZ O7 95.72(5) . 15 ? O6 AlZ O3 83.63(7) . . ? O7 AlZ O3 94.80(7) 8 . ? O8 AlZ O3 94.81(6) 8 . ? O8 AlZ O3 92.43(6) . . ? O7 AlZ O3 171.11(6) 15 . ? O6 AlZ MnZ 85.78(4) . 8 ? O7 AlZ MnZ 103.09(4) 8 8 ? O8 AlZ MnZ 39.90(4) 8 8 ? O8 AlZ MnZ 134.24(4) . 8 ? O7 AlZ MnZ 39.13(3) 15 8 ? O3 AlZ MnZ 132.23(5) . 8 ? O6 AlZ AlZ 85.78(4) . 8 ? O7 AlZ AlZ 103.09(4) 8 8 ? O8 AlZ AlZ 39.90(4) 8 8 ? O8 AlZ AlZ 134.24(4) . 8 ? O7 AlZ AlZ 39.13(3) 15 8 ? O3 AlZ AlZ 132.23(5) . 8 ? MnZ AlZ AlZ 0.000(15) 8 8 ? O6 AlZ MnZ 128.77(5) . 15_554 ? O7 AlZ MnZ 41.04(3) 8 15_554 ? O8 AlZ MnZ 134.11(4) 8 15_554 ? O8 AlZ MnZ 38.99(4) . 15_554 ? O7 AlZ MnZ 85.04(4) 15 15_554 ? O3 AlZ MnZ 103.57(5) . 15_554 ? MnZ AlZ MnZ 119.00(2) 8 15_554 ? AlZ AlZ MnZ 119.00(2) 8 15_554 ? O6 AlZ AlZ 128.77(5) . 15_554 ? O7 AlZ AlZ 41.04(3) 8 15_554 ? O8 AlZ AlZ 134.11(4) 8 15_554 ? O8 AlZ AlZ 38.99(4) . 15_554 ? O7 AlZ AlZ 85.04(4) 15 15_554 ? O3 AlZ AlZ 103.57(5) . 15_554 ? MnZ AlZ AlZ 119.00(2) 8 15_554 ? AlZ AlZ AlZ 119.00(2) 8 15_554 ? MnZ AlZ AlZ 0.00(2) 15_554 15_554 ? O2 B O8 120.75(9) . . ? O2 B O8 120.77(9) . 5 ? O8 B O8 118.46(18) . 5 ? O6 Si O7 109.77(6) 1_554 . ? O6 Si O4 111.64(7) 1_554 . ? O7 Si O4 109.82(7) . . ? O6 Si O5 110.46(7) 1_554 . ? O7 Si O5 109.72(8) . . ? O4 Si O5 105.33(8) . . ? O6 Si Ca 118.68(7) 1_554 . ? O7 Si Ca 131.51(7) . . ? O4 Si Ca 54.12(6) . . ? O5 Si Ca 51.98(6) . . ? LiY O1 MnY 93.40(14) . 2 ? LiY O1 AlY 93.40(14) . 2 ? MnY O1 AlY 0.00(4) 2 2 ? LiY O1 LiY 93.40(14) . 2 ? MnY O1 LiY 0.00(4) 2 2 ? AlY O1 LiY 0.00(4) 2 2 ? LiY O1 TiY 93.40(14) . 2 ? MnY O1 TiY 0.00(4) 2 2 ? AlY O1 TiY 0.00(4) 2 2 ? LiY O1 TiY 0.00(4) 2 2 ? LiY O1 FeY 93.40(14) . 2 ? MnY O1 FeY 0.00(4) 2 2 ? AlY O1 FeY 0.00(4) 2 2 ? LiY O1 FeY 0.00(4) 2 2 ? TiY O1 FeY 0.00(4) 2 2 ? LiY O1 MnY 93.42(14) . 3 ? MnY O1 MnY 93.44(14) 2 3 ? AlY O1 MnY 93.44(14) 2 3 ? LiY O1 MnY 93.44(14) 2 3 ? TiY O1 MnY 93.44(14) 2 3 ? FeY O1 MnY 93.44(14) 2 3 ? LiY O1 FeY 93.42(14) . 3 ? MnY O1 FeY 93.44(14) 2 3 ? AlY O1 FeY 93.44(14) 2 3 ? LiY O1 FeY 93.44(14) 2 3 ? TiY O1 FeY 93.44(14) 2 3 ? FeY O1 FeY 93.44(14) 2 3 ? MnY O1 FeY 0.00(4) 3 3 ? B O2 MnY 119.77(9) . 2 ? B O2 AlY 119.77(9) . 2 ? MnY O2 AlY 0.000(6) 2 2 ? B O2 TiY 119.77(9) . 2 ? MnY O2 TiY 0.000(6) 2 2 ? AlY O2 TiY 0.000(6) 2 2 ? B O2 FeY 119.77(9) . 2 ? MnY O2 FeY 0.000(6) 2 2 ? AlY O2 FeY 0.000(6) 2 2 ? TiY O2 FeY 0.000(6) 2 2 ? B O2 LiY 119.77(9) . 2 ? MnY O2 LiY 0.000(6) 2 2 ? AlY O2 LiY 0.000(6) 2 2 ? TiY O2 LiY 0.000(6) 2 2 ? FeY O2 LiY 0.000(6) 2 2 ? B O2 LiY 119.79(9) . . ? MnY O2 LiY 97.32(9) 2 . ? AlY O2 LiY 97.32(9) 2 . ? TiY O2 LiY 97.32(9) 2 . ? FeY O2 LiY 97.32(9) 2 . ? LiY O2 LiY 97.32(9) 2 . ? MnZ O3 AlZ 0.00(4) 6 6 ? MnZ O3 AlZ 130.34(10) 6 . ? AlZ O3 AlZ 130.34(10) 6 . ? MnZ O3 LiY 93.17(6) 6 . ? AlZ O3 LiY 93.17(6) 6 . ? AlZ O3 LiY 93.19(6) . . ? MnZ O3 H3 112.9(5) 6 . ? AlZ O3 H3 112.9(5) 6 . ? AlZ O3 H3 112.9(5) . . ? LiY O3 H3 104(3) . . ? AlT O4 Si 0.00(2) 5 5 ? AlT O4 Si 144.42(12) 5 . ? Si O4 Si 144.42(12) 5 . ? AlT O4 Ca 98.10(6) 5 . ? Si O4 Ca 98.10(6) 5 . ? Si O4 Ca 98.08(6) . . ? Si O5 AlT 132.82(11) . 6 ? Si O5 Si 132.82(11) . 6 ? AlT O5 Si 0.00(2) 6 6 ? Si O5 Ca 100.15(7) . . ? AlT O5 Ca 100.12(7) 6 . ? Si O5 Ca 100.12(7) 6 . ? AlT O6 Si 0.00(3) 1_556 1_556 ? AlT O6 AlZ 130.90(7) 1_556 . ? Si O6 AlZ 130.90(7) 1_556 . ? AlT O6 LiY 122.89(7) 1_556 . ? Si O6 LiY 122.89(7) 1_556 . ? AlZ O6 LiY 100.05(6) . . ? Si O7 MnZ 130.47(7) . 15_554 ? Si O7 AlZ 130.47(7) . 15_554 ? MnZ O7 AlZ 0.00(4) 15_554 15_554 ? Si O7 AlZ 126.91(7) . 8_554 ? MnZ O7 AlZ 99.80(5) 15_554 8_554 ? AlZ O7 AlZ 99.80(5) 15_554 8_554 ? Si O7 MnZ 126.91(7) . 8_554 ? MnZ O7 MnZ 99.80(5) 15_554 8_554 ? AlZ O7 MnZ 99.80(5) 15_554 8_554 ? AlZ O7 MnZ 0.00(5) 8_554 8_554 ? B O8 MnZ 132.86(12) . 15_554 ? B O8 AlZ 132.86(12) . 15_554 ? MnZ O8 AlZ 0.00(4) 15_554 15_554 ? B O8 AlZ 125.92(12) . . ? MnZ O8 AlZ 101.12(5) 15_554 . ? AlZ O8 AlZ 101.12(5) 15_554 . ? _refine_diff_density_max 1.069 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.064 _shelxl_version_number 2013-4 ########################################################### data_cb1b split-site SREF _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_mineral Fluor-tsilaisite _chemical_formula_sum 'H3.30 Al7.05 B3 Ca0.01 F0.35 Fe0.03 K0 Li0.31 Mn1.64 Na0.62 O30.65 Si5.94 Ti0.04' _chemical_formula_weight 1000.37 _chemical_compound_source 'San Piero in Campo, Elba, Italy' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 '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' 'Mn' 'Mn' 0.3368 0.7283 '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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Ca' 'Ca' 0.2262 0.3064 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system trigonal _space_group_IT_number 160 _space_group_name_H-M_alt 'R 3 m :H' _space_group_name_Hall 'R 3 -2"' _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' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 15.9619(4) _cell_length_b 15.9691(4) _cell_length_c 7.1426(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1576.71(9) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour green-yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.161 _exptl_crystal_F_000 1660 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.200 _exptl_absorpt_coefficient_mu 2.182 _shelx_estimated_absorpt_T_min 0.601 _shelx_estimated_absorpt_T_max 0.669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6630 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker KAPPA APEX-II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13288 _diffrn_reflns_av_unetI/netI 0.0176 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.551 _diffrn_reflns_theta_max 36.346 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 1746 _reflns_number_gt 1732 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.986 _reflns_Friedel_fraction_max 0.977 _reflns_Friedel_fraction_full 1.000 _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-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion twin. ; _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^)+(0.0171P)^2^+1.0631P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0056(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.03(2) _chemical_absolute_configuration ? _refine_ls_number_reflns 1746 _refine_ls_number_parameters 92 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0154 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0368 _refine_ls_wR_factor_gt 0.0368 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Ca Ca 0.0000 0.0000 0.2263(5) 0.0260(10) Uani 0.0143 6 d S T P . . K K 0.0000 0.0000 0.2263(5) 0.0260(10) Uani 0.0046 6 d S T P . . Na Na 0.0000 0.0000 0.2263(5) 0.0260(10) Uani 0.609(10) 6 d S T P . . LiY Li 0.12435(3) 0.06218(2) 0.62283(9) 0.01182(14) Uani 0.1019 2 d S T P . . FeY Fe 0.12435(3) 0.06218(2) 0.62283(9) 0.01182(14) Uani 0.009 2 d S T P . . TiY Ti 0.12435(3) 0.06218(2) 0.62283(9) 0.01182(14) Uani 0.0137 2 d S T P . . AlY Al 0.12435(3) 0.06218(2) 0.62283(9) 0.01182(14) Uani 0.387(5) 2 d S T P . . MnY Mn 0.12435(3) 0.06218(2) 0.62283(9) 0.01182(14) Uani 0.489(5) 2 d S T P . . AlZ Al 0.29815(3) 0.26144(3) 0.61085(8) 0.00620(12) Uani 0.969(3) 1 d . . P . . MnZ Mn 0.29815(3) 0.26144(3) 0.61085(8) 0.00620(12) Uani 0.031(3) 1 d . . P . . B B 0.11012(8) 0.22024(15) 0.4541(3) 0.0070(3) Uani 1 2 d S T P . . Si Si 0.19184(2) 0.18987(3) 0.0000 0.00467(8) Uani 0.9895 1 d . . P . . AlT Al 0.19184(2) 0.18987(3) 0.0000 0.00467(8) Uani 0.0105 1 d . . P . . O1 O 0.0199(3) 0.00995(13) 0.7783(5) 0.0121(10) Uiso 0.2179 2 d S . P . . F1 F 0.0199(3) 0.00995(13) 0.7783(5) 0.0121(10) Uiso 0.1154 2 d S . P . . O2 O 0.07173(15) 0.12324(12) 0.4828(3) 0.0086(4) Uiso 0.5 1 d . . P . . O3 O 0.26855(13) 0.13428(7) 0.5098(2) 0.0119(3) Uani 1 2 d S T P . . H3 H 0.259(3) 0.1295(13) 0.400(5) 0.018 Uiso 1 2 d S U P . . O4 O 0.09362(5) 0.18724(11) 0.0692(2) 0.0083(2) Uani 1 2 d S T P . . O5 O 0.18711(11) 0.09355(6) 0.0913(2) 0.0087(2) Uani 1 2 d S T P . . O6 O 0.19741(7) 0.18721(7) 0.77540(17) 0.00763(17) Uani 1 1 d . . . . . O7 O 0.28525(7) 0.28572(7) 0.07943(16) 0.00643(17) Uani 1 1 d . . . . . O8 O 0.20996(7) 0.27103(7) 0.44122(17) 0.00808(18) 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 Ca 0.0277(12) 0.0277(12) 0.0228(17) 0.000 0.000 0.0138(6) K 0.0277(12) 0.0277(12) 0.0228(17) 0.000 0.000 0.0138(6) Na 0.0277(12) 0.0277(12) 0.0228(17) 0.000 0.000 0.0138(6) LiY 0.0101(2) 0.00761(15) 0.0185(3) -0.00157(7) -0.00315(15) 0.00507(10) FeY 0.0101(2) 0.00761(15) 0.0185(3) -0.00157(7) -0.00315(15) 0.00507(10) TiY 0.0101(2) 0.00761(15) 0.0185(3) -0.00157(7) -0.00315(15) 0.00507(10) AlY 0.0101(2) 0.00761(15) 0.0185(3) -0.00157(7) -0.00315(15) 0.00507(10) MnY 0.0101(2) 0.00761(15) 0.0185(3) -0.00157(7) -0.00315(15) 0.00507(10) AlZ 0.00649(18) 0.00700(18) 0.0052(2) 0.00057(13) -0.00014(12) 0.00346(13) MnZ 0.00649(18) 0.00700(18) 0.0052(2) 0.00057(13) -0.00014(12) 0.00346(13) B 0.0077(5) 0.0066(7) 0.0063(9) 0.0000(6) 0.0000(3) 0.0033(4) Si 0.00463(14) 0.00463(14) 0.00482(16) -0.00042(11) -0.00012(11) 0.00236(10) AlT 0.00463(14) 0.00463(14) 0.00482(16) -0.00042(11) -0.00012(11) 0.00236(10) O3 0.0244(8) 0.0110(4) 0.0048(7) -0.0001(3) -0.0003(5) 0.0122(4) O4 0.0064(4) 0.0123(6) 0.0082(6) -0.0013(5) -0.0006(2) 0.0062(3) O5 0.0141(6) 0.0066(4) 0.0079(7) 0.0006(2) 0.0012(5) 0.0070(3) O6 0.0083(4) 0.0097(4) 0.0041(4) -0.0006(3) -0.0001(3) 0.0039(3) O7 0.0057(3) 0.0058(3) 0.0057(4) -0.0008(3) -0.0001(3) 0.0014(3) O8 0.0057(4) 0.0117(4) 0.0079(5) 0.0028(3) 0.0008(3) 0.0052(3) _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 Ca O2 2.507(3) 2 ? Ca O2 2.507(3) 4 ? Ca O2 2.507(3) 6 ? Ca O2 2.507(3) 3 ? Ca O2 2.507(3) . ? Ca O2 2.507(3) 5 ? Ca O5 2.7604(19) . ? Ca O5 2.7609(19) 2 ? Ca O5 2.7615(19) 3 ? Ca O4 2.821(2) 2 ? Ca O4 2.821(2) 3 ? Ca O4 2.822(2) . ? LiY O1 1.822(4) . ? LiY O2 1.865(2) . ? LiY O2 1.865(2) 6 ? LiY O6 2.0505(11) 6 ? LiY O6 2.0508(11) . ? LiY O2 2.107(2) 5 ? LiY O2 2.107(2) 3 ? LiY O3 2.1505(18) . ? LiY F1 2.177(3) 2 ? LiY O1 2.177(3) 2 ? LiY F1 2.177(3) 3 ? AlZ O6 1.8617(11) . ? AlZ O7 1.8820(11) 8 ? AlZ O8 1.8840(11) 8 ? AlZ O8 1.9206(11) . ? AlZ O7 1.9590(10) 15 ? AlZ O3 1.9769(8) . ? AlZ MnZ 2.9383(4) 8 ? AlZ AlZ 2.9383(4) 8 ? AlZ MnZ 2.9385(4) 15_554 ? AlZ AlZ 2.9385(4) 15_554 ? B O2 1.366(3) 5 ? B O2 1.367(3) . ? B O8 1.3832(15) . ? B O8 1.3835(15) 5 ? Si O6 1.6084(12) 1_554 ? Si O7 1.6141(10) . ? Si O4 1.6244(6) . ? Si O5 1.6371(7) . ? O1 F1 0.477(6) 2 ? O1 O1 0.477(6) 2 ? O1 F1 0.477(6) 3 ? O1 O1 0.477(6) 3 ? O1 LiY 2.177(3) 2 ? O1 FeY 2.177(3) 2 ? O1 TiY 2.177(3) 2 ? O2 O2 0.323(4) 5 ? O2 MnY 2.106(2) 2 ? O2 AlY 2.106(2) 2 ? O2 TiY 2.106(2) 2 ? O2 LiY 2.106(2) 2 ? O2 FeY 2.106(2) 2 ? O3 MnZ 1.9767(8) 6 ? O3 AlZ 1.9767(8) 6 ? O3 H3 0.80(4) . ? O4 AlT 1.6245(6) 5 ? O4 Si 1.6245(6) 5 ? O5 AlT 1.6370(7) 6 ? O5 Si 1.6370(7) 6 ? O6 AlT 1.6084(12) 1_556 ? O6 Si 1.6084(12) 1_556 ? O7 MnZ 1.8823(11) 15_554 ? O7 AlZ 1.8823(11) 15_554 ? O7 AlZ 1.9583(10) 8_554 ? O7 MnZ 1.9583(10) 8_554 ? O8 MnZ 1.8844(11) 15_554 ? O8 AlZ 1.8844(11) 15_554 ? 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 O2 Ca O2 7.38(10) 2 4 ? O2 Ca O2 76.74(13) 2 6 ? O2 Ca O2 72.48(11) 4 6 ? O2 Ca O2 72.48(11) 2 3 ? O2 Ca O2 67.61(12) 4 3 ? O2 Ca O2 7.38(10) 6 3 ? O2 Ca O2 72.49(11) 2 . ? O2 Ca O2 76.75(13) 4 . ? O2 Ca O2 67.63(12) 6 . ? O2 Ca O2 72.51(11) 3 . ? O2 Ca O2 67.62(12) 2 5 ? O2 Ca O2 72.50(11) 4 5 ? O2 Ca O2 72.51(11) 6 5 ? O2 Ca O2 76.77(13) 3 5 ? O2 Ca O2 7.38(10) . 5 ? O2 Ca O5 153.14(13) 2 . ? O2 Ca O5 153.14(13) 4 . ? O2 Ca O5 83.39(6) 6 . ? O2 Ca O5 89.39(6) 3 . ? O2 Ca O5 83.37(6) . . ? O2 Ca O5 89.37(6) 5 . ? O2 Ca O5 83.39(6) 2 2 ? O2 Ca O5 89.39(6) 4 2 ? O2 Ca O5 153.14(13) 6 2 ? O2 Ca O5 153.14(13) 3 2 ? O2 Ca O5 89.35(6) . 2 ? O2 Ca O5 83.36(6) 5 2 ? O5 Ca O5 108.46(8) . 2 ? O2 Ca O5 89.37(6) 2 3 ? O2 Ca O5 83.37(6) 4 3 ? O2 Ca O5 89.36(6) 6 3 ? O2 Ca O5 83.35(6) 3 3 ? O2 Ca O5 153.14(13) . 3 ? O2 Ca O5 153.14(13) 5 3 ? O5 Ca O5 108.48(8) . 3 ? O5 Ca O5 108.50(8) 2 3 ? O2 Ca O4 70.55(5) 2 2 ? O2 Ca O4 70.55(5) 4 2 ? O2 Ca O4 130.79(8) 6 2 ? O2 Ca O4 123.44(7) 3 2 ? O2 Ca O4 130.81(8) . 2 ? O2 Ca O4 123.45(7) 5 2 ? O5 Ca O4 136.12(14) . 2 ? O5 Ca O4 55.36(3) 2 2 ? O5 Ca O4 55.34(3) 3 2 ? O2 Ca O4 130.79(8) 2 3 ? O2 Ca O4 123.43(7) 4 3 ? O2 Ca O4 70.54(5) 6 3 ? O2 Ca O4 70.54(5) 3 3 ? O2 Ca O4 123.46(7) . 3 ? O2 Ca O4 130.82(8) 5 3 ? O5 Ca O4 55.36(3) . 3 ? O5 Ca O4 136.13(14) 2 3 ? O5 Ca O4 55.32(3) 3 3 ? O4 Ca O4 105.22(8) 2 3 ? O2 Ca O4 123.44(7) 2 . ? O2 Ca O4 130.80(8) 4 . ? O2 Ca O4 123.46(7) 6 . ? O2 Ca O4 130.82(8) 3 . ? O2 Ca O4 70.53(5) . . ? O2 Ca O4 70.53(5) 5 . ? O5 Ca O4 55.34(3) . . ? O5 Ca O4 55.32(3) 2 . ? O5 Ca O4 136.14(14) 3 . ? O4 Ca O4 105.24(8) 2 . ? O4 Ca O4 105.26(8) 3 . ? O1 LiY O2 91.04(10) . . ? O1 LiY O2 91.02(10) . 6 ? O2 LiY O2 96.89(11) . 6 ? O1 LiY O6 93.79(10) . 6 ? O2 LiY O6 173.22(7) . 6 ? O2 LiY O6 87.79(6) 6 6 ? O1 LiY O6 93.81(10) . . ? O2 LiY O6 87.79(6) . . ? O2 LiY O6 173.22(7) 6 . ? O6 LiY O6 87.14(6) 6 . ? O1 LiY O2 84.89(10) . 5 ? O2 LiY O2 6.18(9) . 5 ? O2 LiY O2 96.42(10) 6 5 ? O6 LiY O2 175.61(6) 6 5 ? O6 LiY O2 88.76(5) . 5 ? O1 LiY O2 84.87(10) . 3 ? O2 LiY O2 96.42(10) . 3 ? O2 LiY O2 6.17(9) 6 3 ? O6 LiY O2 88.76(5) 6 3 ? O6 LiY O2 175.61(6) . 3 ? O2 LiY O2 95.29(9) 5 3 ? O1 LiY O3 164.47(13) . . ? O2 LiY O3 99.21(7) . . ? O2 LiY O3 99.23(7) 6 . ? O6 LiY O3 75.11(5) 6 . ? O6 LiY O3 75.10(5) . . ? O2 LiY O3 105.34(6) 5 . ? O2 LiY O3 105.36(6) 3 . ? O1 LiY F1 9.17(12) . 2 ? O2 LiY F1 81.91(12) . 2 ? O2 LiY F1 91.31(9) 6 2 ? O6 LiY F1 102.96(11) 6 2 ? O6 LiY F1 94.22(8) . 2 ? O2 LiY F1 75.75(11) 5 2 ? O2 LiY F1 85.15(9) 3 2 ? O3 LiY F1 169.16(8) . 2 ? O1 LiY O1 9.17(12) . 2 ? O2 LiY O1 81.91(12) . 2 ? O2 LiY O1 91.31(9) 6 2 ? O6 LiY O1 102.96(11) 6 2 ? O6 LiY O1 94.22(8) . 2 ? O2 LiY O1 75.75(11) 5 2 ? O2 LiY O1 85.15(9) 3 2 ? O3 LiY O1 169.16(8) . 2 ? F1 LiY O1 0.00(19) 2 2 ? O1 LiY F1 9.17(12) . 3 ? O2 LiY F1 91.33(9) . 3 ? O2 LiY F1 81.89(12) 6 3 ? O6 LiY F1 94.20(8) 6 3 ? O6 LiY F1 102.97(11) . 3 ? O2 LiY F1 85.17(9) 5 3 ? O2 LiY F1 75.74(11) 3 3 ? O3 LiY F1 169.16(8) . 3 ? F1 LiY F1 12.58(16) 2 3 ? O1 LiY F1 12.58(16) 2 3 ? O6 AlZ O7 169.02(5) . 8 ? O6 AlZ O8 94.44(5) . 8 ? O7 AlZ O8 96.52(5) 8 8 ? O6 AlZ O8 90.85(5) . . ? O7 AlZ O8 78.35(4) 8 . ? O8 AlZ O8 171.45(4) 8 . ? O6 AlZ O7 92.72(5) . 15 ? O7 AlZ O7 90.31(2) 8 15 ? O8 AlZ O7 77.38(4) 8 15 ? O8 AlZ O7 95.69(4) . 15 ? O6 AlZ O3 83.67(6) . . ? O7 AlZ O3 94.76(6) 8 . ? O8 AlZ O3 94.76(6) 8 . ? O8 AlZ O3 92.49(6) . . ? O7 AlZ O3 171.11(6) 15 . ? O6 AlZ MnZ 85.79(4) . 8 ? O7 AlZ MnZ 103.09(4) 8 8 ? O8 AlZ MnZ 39.91(3) 8 8 ? O8 AlZ MnZ 134.21(4) . 8 ? O7 AlZ MnZ 39.14(3) 15 8 ? O3 AlZ MnZ 132.21(5) . 8 ? O6 AlZ AlZ 85.79(4) . 8 ? O7 AlZ AlZ 103.09(4) 8 8 ? O8 AlZ AlZ 39.91(3) 8 8 ? O8 AlZ AlZ 134.21(4) . 8 ? O7 AlZ AlZ 39.14(3) 15 8 ? O3 AlZ AlZ 132.21(5) . 8 ? MnZ AlZ AlZ 0.000(14) 8 8 ? O6 AlZ MnZ 128.77(4) . 15_554 ? O7 AlZ MnZ 41.05(3) 8 15_554 ? O8 AlZ MnZ 134.13(4) 8 15_554 ? O8 AlZ MnZ 39.00(3) . 15_554 ? O7 AlZ MnZ 85.02(3) 15 15_554 ? O3 AlZ MnZ 103.58(5) . 15_554 ? MnZ AlZ MnZ 118.991(18) 8 15_554 ? AlZ AlZ MnZ 118.991(18) 8 15_554 ? O6 AlZ AlZ 128.77(4) . 15_554 ? O7 AlZ AlZ 41.05(3) 8 15_554 ? O8 AlZ AlZ 134.13(4) 8 15_554 ? O8 AlZ AlZ 39.00(3) . 15_554 ? O7 AlZ AlZ 85.02(3) 15 15_554 ? O3 AlZ AlZ 103.58(5) . 15_554 ? MnZ AlZ AlZ 118.991(18) 8 15_554 ? AlZ AlZ AlZ 118.991(18) 8 15_554 ? MnZ AlZ AlZ 0.00(2) 15_554 15_554 ? O2 B O2 13.56(19) 5 . ? O2 B O8 127.56(14) 5 . ? O2 B O8 114.00(12) . . ? O2 B O8 114.02(12) 5 5 ? O2 B O8 127.58(14) . 5 ? O8 B O8 118.40(17) . 5 ? O6 Si O7 109.79(5) 1_554 . ? O6 Si O4 111.61(7) 1_554 . ? O7 Si O4 109.85(7) . . ? O6 Si O5 110.46(6) 1_554 . ? O7 Si O5 109.74(7) . . ? O4 Si O5 105.30(8) . . ? O6 Si Ca 118.73(6) 1_554 . ? O7 Si Ca 131.45(7) . . ? O4 Si Ca 54.09(5) . . ? O5 Si Ca 51.97(5) . . ? F1 O1 O1 0.0(10) 2 2 ? F1 O1 F1 60.019(6) 2 3 ? O1 O1 F1 60.019(6) 2 3 ? F1 O1 O1 60.019(6) 2 3 ? O1 O1 O1 60.019(6) 2 3 ? F1 O1 O1 0.0(16) 3 3 ? F1 O1 LiY 133.33(9) 2 . ? O1 O1 LiY 133.33(9) 2 . ? F1 O1 LiY 133.34(9) 3 . ? O1 O1 LiY 133.34(9) 3 . ? F1 O1 LiY 37.49(10) 2 2 ? O1 O1 LiY 37.49(10) 2 2 ? F1 O1 LiY 83.73(8) 3 2 ? O1 O1 LiY 83.73(8) 3 2 ? LiY O1 LiY 95.85(14) . 2 ? F1 O1 FeY 37.49(10) 2 2 ? O1 O1 FeY 37.49(10) 2 2 ? F1 O1 FeY 83.73(8) 3 2 ? O1 O1 FeY 83.73(8) 3 2 ? LiY O1 FeY 95.85(14) . 2 ? LiY O1 FeY 0.00(3) 2 2 ? F1 O1 TiY 37.49(10) 2 2 ? O1 O1 TiY 37.49(10) 2 2 ? F1 O1 TiY 83.73(8) 3 2 ? O1 O1 TiY 83.73(8) 3 2 ? LiY O1 TiY 95.85(14) . 2 ? LiY O1 TiY 0.00(3) 2 2 ? FeY O1 TiY 0.00(3) 2 2 ? O2 O2 B 83.20(9) 5 . ? O2 O2 LiY 135.40(7) 5 . ? B O2 LiY 127.53(14) . . ? O2 O2 MnY 38.44(5) 5 2 ? B O2 MnY 111.84(13) . 2 ? LiY O2 MnY 96.96(8) . 2 ? O2 O2 AlY 38.44(5) 5 2 ? B O2 AlY 111.84(13) . 2 ? LiY O2 AlY 96.96(8) . 2 ? MnY O2 AlY 0.00(3) 2 2 ? O2 O2 TiY 38.44(5) 5 2 ? B O2 TiY 111.84(13) . 2 ? LiY O2 TiY 96.96(8) . 2 ? MnY O2 TiY 0.00(3) 2 2 ? AlY O2 TiY 0.00(3) 2 2 ? O2 O2 LiY 38.44(5) 5 2 ? B O2 LiY 111.84(13) . 2 ? LiY O2 LiY 96.96(8) . 2 ? MnY O2 LiY 0.00(3) 2 2 ? AlY O2 LiY 0.00(3) 2 2 ? TiY O2 LiY 0.00(3) 2 2 ? O2 O2 FeY 38.44(5) 5 2 ? B O2 FeY 111.84(13) . 2 ? LiY O2 FeY 96.96(8) . 2 ? MnY O2 FeY 0.00(3) 2 2 ? AlY O2 FeY 0.00(3) 2 2 ? TiY O2 FeY 0.00(3) 2 2 ? LiY O2 FeY 0.00(3) 2 2 ? MnZ O3 AlZ 0.00(4) 6 6 ? MnZ O3 AlZ 130.38(9) 6 . ? AlZ O3 AlZ 130.38(9) 6 . ? MnZ O3 LiY 93.14(6) 6 . ? AlZ O3 LiY 93.14(6) 6 . ? AlZ O3 LiY 93.16(6) . . ? MnZ O3 H3 113.2(4) 6 . ? AlZ O3 H3 113.2(4) 6 . ? AlZ O3 H3 113.2(4) . . ? LiY O3 H3 102(3) . . ? Si O4 AlT 144.45(11) . 5 ? Si O4 Si 144.45(11) . 5 ? AlT O4 Si 0.00(2) 5 5 ? Si O4 Ca 98.13(6) . . ? AlT O4 Ca 98.15(6) 5 . ? Si O4 Ca 98.15(6) 5 . ? AlT O5 Si 0.00(2) 6 6 ? AlT O5 Si 132.82(10) 6 . ? Si O5 Si 132.82(10) 6 . ? AlT O5 Ca 100.16(6) 6 . ? Si O5 Ca 100.16(6) 6 . ? Si O5 Ca 100.18(6) . . ? AlT O6 Si 0.00(5) 1_556 1_556 ? AlT O6 AlZ 130.87(6) 1_556 . ? Si O6 AlZ 130.87(6) 1_556 . ? AlT O6 LiY 122.93(6) 1_556 . ? Si O6 LiY 122.93(6) 1_556 . ? AlZ O6 LiY 100.03(5) . . ? Si O7 MnZ 130.48(6) . 15_554 ? Si O7 AlZ 130.48(6) . 15_554 ? MnZ O7 AlZ 0.00(4) 15_554 15_554 ? Si O7 AlZ 126.92(6) . 8_554 ? MnZ O7 AlZ 99.79(4) 15_554 8_554 ? AlZ O7 AlZ 99.79(4) 15_554 8_554 ? Si O7 MnZ 126.92(6) . 8_554 ? MnZ O7 MnZ 99.79(4) 15_554 8_554 ? AlZ O7 MnZ 99.79(4) 15_554 8_554 ? AlZ O7 MnZ 0.00(5) 8_554 8_554 ? B O8 MnZ 132.88(11) . 15_554 ? B O8 AlZ 132.88(11) . 15_554 ? MnZ O8 AlZ 0.00(4) 15_554 15_554 ? B O8 AlZ 125.92(11) . . ? MnZ O8 AlZ 101.11(5) 15_554 . ? AlZ O8 AlZ 101.11(5) 15_554 . ? _refine_diff_density_max 0.423 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.059 _shelxl_version_number 2013-4