data_Polylithionite _audit_creation_method SHELXL-2014 _chemical_name_systematic Potassium lithium aluminium silicate fluoride ; ? ; _chemical_name_common Mica _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al2 F4 K2 Li4 O20 Si8' _chemical_formula_weight 780.64 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' 'O' 'O' 0.0106 0.0060 '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' '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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_H-M_alt 'C 2' _space_group_name_Hall 'C 2y' _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' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 5.1973(4) _cell_length_b 8.9753(6) _cell_length_c 10.0556(7) _cell_angle_alpha 90 _cell_angle_beta 100.4538(9) _cell_angle_gamma 90 _cell_volume 461.28(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6003 _cell_measurement_theta_min 4 _cell_measurement_theta_max 60 _exptl_crystal_description Thin flake _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.810 _exptl_crystal_F_000 384 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 150 microns _exptl_crystal_size_mid 150 microns _exptl_crystal_size_min 5 microns _exptl_absorpt_coefficient_mu 1.280 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type SADABS _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 Rotaing-anode generato _diffrn_measurement_device_type Area detector _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2718 _diffrn_reflns_av_unetI/netI 0.0163 _diffrn_reflns_av_R_equivalents 0.0112 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.059 _diffrn_reflns_theta_max 30.065 _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 1370 _reflns_number_gt 1358 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.890 _reflns_Friedel_fraction_max 1.000 _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-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^)+(0.0309P)^2^] 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_abs_structure_details ; Flack x determined using 632 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.07(3) _chemical_absolute_configuration ? _refine_ls_number_reflns 1370 _refine_ls_number_parameters 97 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0200 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0579 _refine_ls_goodness_of_fit_ref 1.438 _refine_ls_restrained_S_all 1.438 _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 T(1) Si 0.07675(11) 0.16735(6) 0.23177(6) 0.00804(17) Uani 1 1 d . . . . . T(2) Si 0.58485(11) 0.33116(6) 0.23133(6) 0.00807(17) Uani 1 1 d . . . . . M(1) Li 0.0000 0.9926(9) 0.5000 0.0106(19) Uani 0.93(3) 2 d S T . . . M(2) Al 0.0000 0.32883(13) 0.5000 0.0111(3) Uani 1.122(7) 2 d S T . . . M(3) Li 0.5000 0.1558(8) 0.5000 0.009(2) Uani 1.02(4) 2 d S T . . . A K 0.0000 0.49958(13) 0.0000 0.0239(3) Uani 1.023(5) 2 d S T . . . O1 O 0.0506(3) -0.0004(2) 0.16906(15) 0.0128(3) Uani 1 1 d . . . . . O2 O 0.3135(4) 0.2452(2) 0.17008(17) 0.0127(4) Uani 1 1 d . . . . . O3 O 0.8090(4) 0.2530(2) 0.15973(18) 0.0117(3) Uani 1 1 d . . . . . O4 O 0.1166(3) 0.1721(2) 0.39177(17) 0.0101(3) Uani 1 1 d . . . . . O5 O 0.6557(3) 0.3263(2) 0.39131(16) 0.0100(3) Uani 1 1 d . . . . . F6 F 0.1112(3) 0.47344(17) 0.39556(16) 0.0152(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 T(1) 0.0070(3) 0.0071(3) 0.0103(3) 0.0001(3) 0.0023(2) 0.0003(2) T(2) 0.0070(3) 0.0070(3) 0.0103(3) 0.0000(3) 0.0017(2) 0.0002(2) M(1) 0.014(3) 0.006(3) 0.011(3) 0.000 0.002(2) 0.000 M(2) 0.0068(4) 0.0127(5) 0.0128(5) 0.000 -0.0004(3) 0.000 M(3) 0.007(3) 0.012(3) 0.008(3) 0.000 0.000(2) 0.000 A 0.0236(4) 0.0221(4) 0.0262(4) 0.000 0.0049(3) 0.000 O1 0.0176(7) 0.0076(6) 0.0127(7) -0.0006(7) 0.0017(5) 0.0007(8) O2 0.0104(8) 0.0159(9) 0.0123(9) -0.0007(6) 0.0030(6) -0.0035(7) O3 0.0111(8) 0.0132(9) 0.0110(8) 0.0005(6) 0.0022(6) 0.0045(7) O4 0.0092(7) 0.0100(8) 0.0111(7) 0.0006(7) 0.0018(6) 0.0020(7) O5 0.0097(7) 0.0100(7) 0.0106(7) 0.0009(7) 0.0023(5) 0.0008(7) F6 0.0144(7) 0.0133(9) 0.0183(7) 0.0021(5) 0.0037(5) -0.0001(5) _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 T(1) O4 1.5851(18) . ? T(1) O1 1.628(2) . ? T(1) O2 1.6323(19) . ? T(1) O3 1.6388(19) 1_455 ? T(1) M(3) 3.1578(7) . ? T(1) A 3.7610(10) . ? T(1) A 3.7615(8) 3_445 ? T(1) A 3.7944(7) 3_545 ? T(2) O5 1.5844(16) . ? T(2) O2 1.6272(19) . ? T(2) O1 1.634(2) 3 ? T(2) O3 1.6348(19) . ? T(2) M(1) 3.166(4) 3_545 ? T(2) A 3.7536(11) 3_545 ? T(2) A 3.7647(8) 1_655 ? T(2) A 3.7908(8) . ? M(1) O4 2.094(7) 2_566 ? M(1) O4 2.094(7) 1_565 ? M(1) O5 2.098(6) 3_455 ? M(1) O5 2.098(6) 4_556 ? M(1) F6 2.1085(17) 3_455 ? M(1) F6 2.1085(17) 4_556 ? M(1) M(3) 2.983(5) 1_565 ? M(1) M(3) 2.983(5) 1_465 ? M(1) M(2) 2.986(4) 3_455 ? M(1) M(2) 2.986(4) 3 ? M(1) M(2) 3.018(8) 1_565 ? M(1) M(3) 3.023(10) 3_455 ? M(2) F6 1.8281(19) . ? M(2) F6 1.8281(18) 2_556 ? M(2) O5 1.9202(16) 2_656 ? M(2) O5 1.9202(16) 1_455 ? M(2) O4 1.942(2) . ? M(2) O4 1.942(2) 2_556 ? M(2) M(3) 2.935(7) 3_455 ? M(2) M(1) 2.986(4) 3_545 ? M(2) M(1) 2.986(4) 3_445 ? M(2) M(1) 3.018(8) 1_545 ? M(2) M(3) 3.027(3) . ? M(2) M(3) 3.027(3) 1_455 ? M(3) F6 2.083(6) 3_545 ? M(3) F6 2.083(6) 4_546 ? M(3) O4 2.0949(18) . ? M(3) O4 2.0949(18) 2_656 ? M(3) O5 2.124(5) . ? M(3) O5 2.124(5) 2_656 ? M(3) M(2) 2.935(7) 3_545 ? M(3) M(1) 2.983(5) 1_545 ? M(3) M(1) 2.983(5) 1_645 ? M(3) M(1) 3.023(10) 3_545 ? M(3) M(2) 3.027(3) 1_655 ? A O3 3.007(2) 2_655 ? A O3 3.007(2) 1_455 ? A O1 3.0519(15) 4_455 ? A O1 3.0519(15) 3 ? A O2 3.054(2) 3_455 ? A O2 3.054(2) 4 ? A O3 3.065(2) 3_455 ? A O3 3.065(2) 4 ? A O2 3.128(2) 2 ? A O2 3.128(2) . ? A O1 3.1282(15) 4 ? A O1 3.1282(15) 3_455 ? O1 T(2) 1.634(2) 3_445 ? O1 A 3.0519(15) 3_445 ? O1 A 3.1282(15) 3_545 ? O2 A 3.054(2) 3_545 ? O3 T(1) 1.6388(19) 1_655 ? O3 A 3.007(2) 1_655 ? O3 A 3.065(2) 3_545 ? O4 M(1) 2.094(7) 1_545 ? O5 M(2) 1.9202(16) 1_655 ? O5 M(1) 2.097(6) 3_545 ? F6 M(3) 2.083(6) 3_455 ? F6 M(1) 2.1085(17) 3_545 ? 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 O4 T(1) O1 113.83(10) . . ? O4 T(1) O2 113.92(9) . . ? O1 T(1) O2 105.33(9) . . ? O4 T(1) O3 112.35(9) . 1_455 ? O1 T(1) O3 104.94(9) . 1_455 ? O2 T(1) O3 105.64(11) . 1_455 ? O4 T(1) M(3) 36.03(7) . . ? O1 T(1) M(3) 107.26(14) . . ? O2 T(1) M(3) 83.24(9) . . ? O3 T(1) M(3) 142.84(11) 1_455 . ? O4 T(1) A 125.98(8) . . ? O1 T(1) A 120.07(6) . . ? O2 T(1) A 55.08(7) . . ? O3 T(1) A 50.82(7) 1_455 . ? M(3) T(1) A 122.30(12) . . ? O4 T(1) A 125.62(7) . 3_445 ? O1 T(1) A 52.33(6) . 3_445 ? O2 T(1) A 120.46(7) . 3_445 ? O3 T(1) A 52.88(7) 1_455 3_445 ? M(3) T(1) A 150.39(11) . 3_445 ? A T(1) A 87.160(14) . 3_445 ? O4 T(1) A 130.57(7) . 3_545 ? O1 T(1) A 54.00(6) . 3_545 ? O2 T(1) A 51.35(7) . 3_545 ? O3 T(1) A 117.06(7) 1_455 3_545 ? M(3) T(1) A 96.89(5) . 3_545 ? A T(1) A 86.684(14) . 3_545 ? A T(1) A 86.918(18) 3_445 3_545 ? O5 T(2) O2 113.39(9) . . ? O5 T(2) O1 113.82(10) . 3 ? O2 T(2) O1 105.49(10) . 3 ? O5 T(2) O3 112.48(10) . . ? O2 T(2) O3 105.52(11) . . ? O1 T(2) O3 105.38(9) 3 . ? O5 T(2) M(1) 35.81(12) . 3_545 ? O2 T(2) M(1) 107.14(9) . 3_545 ? O1 T(2) M(1) 83.18(15) 3 3_545 ? O3 T(2) M(1) 142.46(8) . 3_545 ? O5 T(2) A 125.93(9) . 3_545 ? O2 T(2) A 52.64(7) . 3_545 ? O1 T(2) A 120.25(6) 3 3_545 ? O3 T(2) A 53.11(7) . 3_545 ? M(1) T(2) A 150.78(13) 3_545 3_545 ? O5 T(2) A 125.78(7) . 1_655 ? O2 T(2) A 120.73(6) . 1_655 ? O1 T(2) A 54.99(6) 3 1_655 ? O3 T(2) A 50.67(7) . 1_655 ? M(1) T(2) A 121.84(12) 3_545 1_655 ? A T(2) A 87.220(14) 3_545 1_655 ? O5 T(2) A 130.31(7) . . ? O2 T(2) A 54.09(7) . . ? O1 T(2) A 51.41(6) 3 . ? O3 T(2) A 117.20(7) . . ? M(1) T(2) A 96.94(7) 3_545 . ? A T(2) A 86.842(13) 3_545 . ? A T(2) A 86.925(19) 1_655 . ? O4 M(1) O4 79.5(3) 2_566 1_565 ? O4 M(1) O5 173.6(3) 2_566 3_455 ? O4 M(1) O5 95.81(6) 1_565 3_455 ? O4 M(1) O5 95.81(6) 2_566 4_556 ? O4 M(1) O5 173.6(3) 1_565 4_556 ? O5 M(1) O5 89.2(3) 3_455 4_556 ? O4 M(1) F6 88.85(17) 2_566 3_455 ? O4 M(1) F6 98.4(2) 1_565 3_455 ? O5 M(1) F6 96.2(2) 3_455 3_455 ? O5 M(1) F6 77.05(16) 4_556 3_455 ? O4 M(1) F6 98.4(2) 2_566 4_556 ? O4 M(1) F6 88.85(17) 1_565 4_556 ? O5 M(1) F6 77.05(16) 3_455 4_556 ? O5 M(1) F6 96.2(2) 4_556 4_556 ? F6 M(1) F6 170.6(5) 3_455 4_556 ? O4 M(1) M(3) 87.5(2) 2_566 1_565 ? O4 M(1) M(3) 44.60(11) 1_565 1_565 ? O5 M(1) M(3) 86.05(11) 3_455 1_565 ? O5 M(1) M(3) 140.18(12) 4_556 1_565 ? F6 M(1) M(3) 142.8(2) 3_455 1_565 ? F6 M(1) M(3) 44.27(14) 4_556 1_565 ? O4 M(1) M(3) 44.60(11) 2_566 1_465 ? O4 M(1) M(3) 87.5(2) 1_565 1_465 ? O5 M(1) M(3) 140.18(12) 3_455 1_465 ? O5 M(1) M(3) 86.05(11) 4_556 1_465 ? F6 M(1) M(3) 44.27(14) 3_455 1_465 ? F6 M(1) M(3) 142.8(2) 4_556 1_465 ? M(3) M(1) M(3) 121.2(3) 1_565 1_465 ? O4 M(1) M(2) 92.56(6) 2_566 3_455 ? O4 M(1) M(2) 135.46(12) 1_565 3_455 ? O5 M(1) M(2) 93.9(2) 3_455 3_455 ? O5 M(1) M(2) 39.77(8) 4_556 3_455 ? F6 M(1) M(2) 37.28(10) 3_455 3_455 ? F6 M(1) M(2) 135.7(3) 4_556 3_455 ? M(3) M(1) M(2) 179.9(3) 1_565 3_455 ? M(3) M(1) M(2) 58.91(11) 1_465 3_455 ? O4 M(1) M(2) 135.46(12) 2_566 3 ? O4 M(1) M(2) 92.56(6) 1_565 3 ? O5 M(1) M(2) 39.77(8) 3_455 3 ? O5 M(1) M(2) 93.9(2) 4_556 3 ? F6 M(1) M(2) 135.7(3) 3_455 3 ? F6 M(1) M(2) 37.28(10) 4_556 3 ? M(3) M(1) M(2) 58.91(11) 1_565 3 ? M(3) M(1) M(2) 179.9(3) 1_465 3 ? M(2) M(1) M(2) 121.0(3) 3_455 3 ? O4 M(1) M(2) 39.73(16) 2_566 1_565 ? O4 M(1) M(2) 39.73(16) 1_565 1_565 ? O5 M(1) M(2) 135.38(17) 3_455 1_565 ? O5 M(1) M(2) 135.38(17) 4_556 1_565 ? F6 M(1) M(2) 94.7(2) 3_455 1_565 ? F6 M(1) M(2) 94.7(2) 4_556 1_565 ? M(3) M(1) M(2) 60.59(16) 1_565 1_565 ? M(3) M(1) M(2) 60.59(16) 1_465 1_565 ? M(2) M(1) M(2) 119.50(14) 3_455 1_565 ? M(2) M(1) M(2) 119.50(14) 3 1_565 ? O4 M(1) M(3) 140.27(16) 2_566 3_455 ? O4 M(1) M(3) 140.27(16) 1_565 3_455 ? O5 M(1) M(3) 44.62(17) 3_455 3_455 ? O5 M(1) M(3) 44.62(17) 4_556 3_455 ? F6 M(1) M(3) 85.3(2) 3_455 3_455 ? F6 M(1) M(3) 85.3(2) 4_556 3_455 ? M(3) M(1) M(3) 119.41(16) 1_565 3_455 ? M(3) M(1) M(3) 119.41(16) 1_465 3_455 ? M(2) M(1) M(3) 60.50(14) 3_455 3_455 ? M(2) M(1) M(3) 60.50(14) 3 3_455 ? M(2) M(1) M(3) 180.0 1_565 3_455 ? F6 M(2) F6 89.53(11) . 2_556 ? F6 M(2) O5 88.65(8) . 2_656 ? F6 M(2) O5 92.32(9) 2_556 2_656 ? F6 M(2) O5 92.32(9) . 1_455 ? F6 M(2) O5 88.65(8) 2_556 1_455 ? O5 M(2) O5 178.64(16) 2_656 1_455 ? F6 M(2) O4 91.67(7) . . ? F6 M(2) O4 178.79(10) 2_556 . ? O5 M(2) O4 87.53(8) 2_656 . ? O5 M(2) O4 91.48(9) 1_455 . ? F6 M(2) O4 178.79(10) . 2_556 ? F6 M(2) O4 91.67(7) 2_556 2_556 ? O5 M(2) O4 91.48(9) 2_656 2_556 ? O5 M(2) O4 87.53(8) 1_455 2_556 ? O4 M(2) O4 87.14(13) . 2_556 ? F6 M(2) M(3) 44.76(5) . 3_455 ? F6 M(2) M(3) 44.76(5) 2_556 3_455 ? O5 M(2) M(3) 90.68(8) 2_656 3_455 ? O5 M(2) M(3) 90.68(8) 1_455 3_455 ? O4 M(2) M(3) 136.43(6) . 3_455 ? O4 M(2) M(3) 136.43(6) 2_556 3_455 ? F6 M(2) M(1) 44.32(10) . 3_545 ? F6 M(2) M(1) 90.93(12) 2_556 3_545 ? O5 M(2) M(1) 44.33(10) 2_656 3_545 ? O5 M(2) M(1) 136.64(10) 1_455 3_545 ? O4 M(2) M(1) 89.80(13) . 3_545 ? O4 M(2) M(1) 135.80(10) 2_556 3_545 ? M(3) M(2) M(1) 60.50(14) 3_455 3_545 ? F6 M(2) M(1) 90.93(12) . 3_445 ? F6 M(2) M(1) 44.32(10) 2_556 3_445 ? O5 M(2) M(1) 136.64(10) 2_656 3_445 ? O5 M(2) M(1) 44.33(10) 1_455 3_445 ? O4 M(2) M(1) 135.80(10) . 3_445 ? O4 M(2) M(1) 89.80(13) 2_556 3_445 ? M(3) M(2) M(1) 60.50(14) 3_455 3_445 ? M(1) M(2) M(1) 121.0(3) 3_545 3_445 ? F6 M(2) M(1) 135.24(5) . 1_545 ? F6 M(2) M(1) 135.24(5) 2_556 1_545 ? O5 M(2) M(1) 89.32(8) 2_656 1_545 ? O5 M(2) M(1) 89.32(8) 1_455 1_545 ? O4 M(2) M(1) 43.57(6) . 1_545 ? O4 M(2) M(1) 43.57(6) 2_556 1_545 ? M(3) M(2) M(1) 180.0 3_455 1_545 ? M(1) M(2) M(1) 119.50(14) 3_545 1_545 ? M(1) M(2) M(1) 119.50(14) 3_445 1_545 ? F6 M(2) M(3) 90.19(11) . . ? F6 M(2) M(3) 136.47(8) 2_556 . ? O5 M(2) M(3) 44.16(10) 2_656 . ? O5 M(2) M(3) 134.84(8) 1_455 . ? O4 M(2) M(3) 43.37(8) . . ? O4 M(2) M(3) 89.06(10) 2_556 . ? M(3) M(2) M(3) 120.86(11) 3_455 . ? M(1) M(2) M(3) 60.35(16) 3_545 . ? M(1) M(2) M(3) 178.64(19) 3_445 . ? M(1) M(2) M(3) 59.14(11) 1_545 . ? F6 M(2) M(3) 136.47(8) . 1_455 ? F6 M(2) M(3) 90.19(11) 2_556 1_455 ? O5 M(2) M(3) 134.84(8) 2_656 1_455 ? O5 M(2) M(3) 44.16(10) 1_455 1_455 ? O4 M(2) M(3) 89.06(10) . 1_455 ? O4 M(2) M(3) 43.37(8) 2_556 1_455 ? M(3) M(2) M(3) 120.86(11) 3_455 1_455 ? M(1) M(2) M(3) 178.64(19) 3_545 1_455 ? M(1) M(2) M(3) 60.35(16) 3_445 1_455 ? M(1) M(2) M(3) 59.14(11) 1_545 1_455 ? M(3) M(2) M(3) 118.3(2) . 1_455 ? F6 M(3) F6 76.4(3) 3_545 4_546 ? F6 M(3) O4 96.74(17) 3_545 . ? F6 M(3) O4 89.53(16) 4_546 . ? F6 M(3) O4 89.53(16) 3_545 2_656 ? F6 M(3) O4 96.74(17) 4_546 2_656 ? O4 M(3) O4 172.0(4) . 2_656 ? F6 M(3) O5 98.06(7) 3_545 . ? F6 M(3) O5 172.8(2) 4_546 . ? O4 M(3) O5 95.62(19) . . ? O4 M(3) O5 78.58(14) 2_656 . ? F6 M(3) O5 172.8(2) 3_545 2_656 ? F6 M(3) O5 98.06(7) 4_546 2_656 ? O4 M(3) O5 78.58(14) . 2_656 ? O4 M(3) O5 95.62(19) 2_656 2_656 ? O5 M(3) O5 87.8(3) . 2_656 ? F6 M(3) M(2) 38.18(13) 3_545 3_545 ? F6 M(3) M(2) 38.18(13) 4_546 3_545 ? O4 M(3) M(2) 94.0(2) . 3_545 ? O4 M(3) M(2) 94.0(2) 2_656 3_545 ? O5 M(3) M(2) 136.08(15) . 3_545 ? O5 M(3) M(2) 136.08(15) 2_656 3_545 ? F6 M(3) M(1) 86.3(2) 3_545 1_545 ? F6 M(3) M(1) 44.97(11) 4_546 1_545 ? O4 M(3) M(1) 44.58(14) . 1_545 ? O4 M(3) M(1) 141.3(2) 2_656 1_545 ? O5 M(3) M(1) 140.09(12) . 1_545 ? O5 M(3) M(1) 86.59(13) 2_656 1_545 ? M(2) M(3) M(1) 60.59(16) 3_545 1_545 ? F6 M(3) M(1) 44.97(11) 3_545 1_645 ? F6 M(3) M(1) 86.3(2) 4_546 1_645 ? O4 M(3) M(1) 141.3(2) . 1_645 ? O4 M(3) M(1) 44.58(14) 2_656 1_645 ? O5 M(3) M(1) 86.59(13) . 1_645 ? O5 M(3) M(1) 140.09(12) 2_656 1_645 ? M(2) M(3) M(1) 60.59(16) 3_545 1_645 ? M(1) M(3) M(1) 121.2(3) 1_545 1_645 ? F6 M(3) M(1) 141.82(13) 3_545 3_545 ? F6 M(3) M(1) 141.82(13) 4_546 3_545 ? O4 M(3) M(1) 86.0(2) . 3_545 ? O4 M(3) M(1) 86.0(2) 2_656 3_545 ? O5 M(3) M(1) 43.92(15) . 3_545 ? O5 M(3) M(1) 43.92(15) 2_656 3_545 ? M(2) M(3) M(1) 180.0 3_545 3_545 ? M(1) M(3) M(1) 119.41(16) 1_545 3_545 ? M(1) M(3) M(1) 119.41(16) 1_645 3_545 ? F6 M(3) M(2) 136.05(10) 3_545 . ? F6 M(3) M(2) 94.96(4) 4_546 . ? O4 M(3) M(2) 39.54(10) . . ? O4 M(3) M(2) 134.4(2) 2_656 . ? O5 M(3) M(2) 92.2(2) . . ? O5 M(3) M(2) 39.04(6) 2_656 . ? M(2) M(3) M(2) 120.86(11) 3_545 . ? M(1) M(3) M(2) 60.27(14) 1_545 . ? M(1) M(3) M(2) 178.6(2) 1_645 . ? M(1) M(3) M(2) 59.14(11) 3_545 . ? F6 M(3) M(2) 94.96(4) 3_545 1_655 ? F6 M(3) M(2) 136.05(10) 4_546 1_655 ? O4 M(3) M(2) 134.4(2) . 1_655 ? O4 M(3) M(2) 39.54(10) 2_656 1_655 ? O5 M(3) M(2) 39.04(6) . 1_655 ? O5 M(3) M(2) 92.2(2) 2_656 1_655 ? M(2) M(3) M(2) 120.86(11) 3_545 1_655 ? M(1) M(3) M(2) 178.6(2) 1_545 1_655 ? M(1) M(3) M(2) 60.27(14) 1_645 1_655 ? M(1) M(3) M(2) 59.14(11) 3_545 1_655 ? M(2) M(3) M(2) 118.3(2) . 1_655 ? O3 A O3 85.21(7) 2_655 1_455 ? O3 A O1 93.99(5) 2_655 4_455 ? O3 A O1 86.01(5) 1_455 4_455 ? O3 A O1 86.01(5) 2_655 3 ? O3 A O1 93.99(5) 1_455 3 ? O1 A O1 180.00(9) 4_455 3 ? O3 A O2 178.27(6) 2_655 3_455 ? O3 A O2 93.62(4) 1_455 3_455 ? O1 A O2 87.20(5) 4_455 3_455 ? O1 A O2 92.80(5) 3 3_455 ? O3 A O2 93.62(4) 2_655 4 ? O3 A O2 178.27(6) 1_455 4 ? O1 A O2 92.80(5) 4_455 4 ? O1 A O2 87.20(5) 3 4 ? O2 A O2 87.58(8) 3_455 4 ? O3 A O3 129.321(17) 2_655 3_455 ? O3 A O3 117.30(6) 1_455 3_455 ? O1 A O3 129.87(6) 4_455 3_455 ? O1 A O3 50.13(6) 3 3_455 ? O2 A O3 50.23(6) 3_455 3_455 ? O2 A O3 64.44(5) 4 3_455 ? O3 A O3 117.30(6) 2_655 4 ? O3 A O3 129.321(17) 1_455 4 ? O1 A O3 50.13(6) 4_455 4 ? O1 A O3 129.87(6) 3 4 ? O2 A O3 64.44(5) 3_455 4 ? O2 A O3 50.23(6) 4 4 ? O3 A O3 84.20(8) 3_455 4 ? O3 A O2 50.23(6) 2_655 2 ? O3 A O2 64.22(5) 1_455 2 ? O1 A O2 49.65(5) 4_455 2 ? O1 A O2 130.35(6) 3 2 ? O2 A O2 130.274(17) 3_455 2 ? O2 A O2 114.05(5) 4 2 ? O3 A O2 178.49(6) 3_455 2 ? O3 A O2 94.80(4) 4 2 ? O3 A O2 64.22(5) 2_655 . ? O3 A O2 50.23(6) 1_455 . ? O1 A O2 130.35(6) 4_455 . ? O1 A O2 49.65(5) 3 . ? O2 A O2 114.05(5) 3_455 . ? O2 A O2 130.274(17) 4 . ? O3 A O2 94.80(4) 3_455 . ? O3 A O2 178.49(6) 4 . ? O2 A O2 86.23(7) 2 . ? O3 A O1 50.09(5) 2_655 4 ? O3 A O1 129.91(6) 1_455 4 ? O1 A O1 114.48(5) 4_455 4 ? O1 A O1 65.52(5) 3 4 ? O2 A O1 130.43(6) 3_455 4 ? O2 A O1 49.57(5) 4 4 ? O3 A O1 85.00(5) 3_455 4 ? O3 A O1 95.00(5) 4 4 ? O2 A O1 93.96(5) 2 4 ? O2 A O1 86.04(5) . 4 ? O3 A O1 129.91(6) 2_655 3_455 ? O3 A O1 50.09(5) 1_455 3_455 ? O1 A O1 65.52(5) 4_455 3_455 ? O1 A O1 114.48(5) 3 3_455 ? O2 A O1 49.57(5) 3_455 3_455 ? O2 A O1 130.43(6) 4 3_455 ? O3 A O1 95.00(5) 3_455 3_455 ? O3 A O1 85.00(5) 4 3_455 ? O2 A O1 86.04(5) 2 3_455 ? O2 A O1 93.96(5) . 3_455 ? O1 A O1 180.00(9) 4 3_455 ? T(1) O1 T(2) 135.36(10) . 3_445 ? T(1) O1 A 102.69(8) . 3_445 ? T(2) O1 A 103.85(8) 3_445 3_445 ? T(1) O1 A 101.09(8) . 3_545 ? T(2) O1 A 99.68(8) 3_445 3_545 ? A O1 A 114.48(5) 3_445 3_545 ? T(2) O2 T(1) 136.09(11) . . ? T(2) O2 A 102.30(8) . 3_545 ? T(1) O2 A 103.98(9) . 3_545 ? T(2) O2 A 100.99(9) . . ? T(1) O2 A 99.58(8) . . ? A O2 A 114.05(5) 3_545 . ? T(2) O3 T(1) 128.49(12) . 1_655 ? T(2) O3 A 104.47(9) . 1_655 ? T(1) O3 A 104.19(9) 1_655 1_655 ? T(2) O3 A 101.64(9) . 3_545 ? T(1) O3 A 101.88(8) 1_655 3_545 ? A O3 A 117.30(6) 1_655 3_545 ? T(1) O4 M(2) 126.27(12) . . ? T(1) O4 M(1) 120.67(16) . 1_545 ? M(2) O4 M(1) 96.71(17) . 1_545 ? T(1) O4 M(3) 117.54(10) . . ? M(2) O4 M(3) 97.09(16) . . ? M(1) O4 M(3) 90.82(18) 1_545 . ? T(2) O5 M(2) 126.76(10) . 1_655 ? T(2) O5 M(1) 117.96(14) . 3_545 ? M(2) O5 M(1) 95.90(8) 1_655 3_545 ? T(2) O5 M(3) 120.15(13) . . ? M(2) O5 M(3) 96.80(9) 1_655 . ? M(1) O5 M(3) 91.5(2) 3_545 . ? M(2) F6 M(3) 97.06(13) . 3_455 ? M(2) F6 M(1) 98.40(18) . 3_545 ? M(3) F6 M(1) 90.8(2) 3_455 3_545 ? _refine_diff_density_max 0.761 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.080 _shelxl_version_number 2014-3 _shelx_res_file ; TITL c2 in C2 CELL 0.71073 5.1973 8.9753 10.0556 90.000 100.4538 90.000 ZERR 1.00 0.0004 0.0006 0.0007 0.000 0.0009 0.000 LATT -7 SYMM -X, Y, -Z SFAC LI O F AL SI K UNIT 4 20 4 2 8 2 L.S. 10 BOND FMAP 2 PLAN 20 ACTA WGHT 0.030900 FVAR 0.78126 T(1) 5 0.076752 0.167348 0.231765 11.00000 0.00696 0.00715 = 0.01028 0.00010 0.00230 0.00028 T(2) 5 0.584849 0.331160 0.231333 11.00000 0.00704 0.00696 = 0.01026 0.00000 0.00172 0.00018 M(1) 1 0.000000 0.992618 0.500000 0.46411 0.01445 0.00609 = 0.01111 0.00000 0.00211 0.00000 M(2) 4 0.000000 0.328826 0.500000 0.56076 0.00683 0.01272 = 0.01280 0.00000 -0.00040 0.00000 M(3) 1 0.500000 0.155842 0.500000 0.50924 0.00677 0.01240 = 0.00793 0.00000 0.00036 0.00000 A 6 0.000000 0.499584 0.000000 0.51126 0.02362 0.02214 = 0.02620 0.00000 0.00489 0.00000 O1 2 0.050614 -0.000408 0.169059 11.00000 0.01761 0.00760 = 0.01269 -0.00056 0.00171 0.00071 O2 2 0.313528 0.245201 0.170083 11.00000 0.01041 0.01586 = 0.01227 -0.00066 0.00301 -0.00347 O3 2 0.809007 0.252958 0.159731 11.00000 0.01113 0.01316 = 0.01099 0.00045 0.00221 0.00452 O4 2 0.116638 0.172061 0.391771 11.00000 0.00920 0.00995 = 0.01114 0.00062 0.00182 0.00196 O5 2 0.655713 0.326279 0.391307 11.00000 0.00971 0.01001 = 0.01057 0.00087 0.00234 0.00081 F6 3 0.111193 0.473442 0.395562 11.00000 0.01438 0.01331 = 0.01830 0.00206 0.00368 -0.00013 HKLF 4 1 1 0 0 0 -1 0 0 0 1 REM c2 in C2 REM R1 = 0.0199 for 1358 Fo > 4sig(Fo) and 0.0200 for all 1370 data REM 97 parameters refined using 1 restraints END WGHT 0.0420 0.1211 REM Highest difference peak 0.761, deepest hole -0.292, 1-sigma level 0.080 Q1 1 0.6154 0.3313 0.3160 11.00000 0.05 0.76 Q2 1 0.1036 0.1619 0.3153 11.00000 0.05 0.75 Q3 1 0.0256 0.3347 0.5763 11.00000 0.05 0.41 Q4 1 0.0247 0.5048 0.0895 11.00000 0.05 0.33 Q5 1 0.1033 0.4969 0.3049 11.00000 0.05 0.28 Q6 1 0.7867 0.2725 0.0953 11.00000 0.05 0.28 Q7 1 0.2611 0.2612 0.0962 11.00000 0.05 0.27 Q8 1 0.0489 -0.0039 0.0985 11.00000 0.05 0.24 Q9 1 0.0729 0.3795 0.4830 11.00000 0.05 0.23 Q10 1 0.4487 0.2773 0.1824 11.00000 0.05 0.23 Q11 1 0.9472 0.2233 0.1883 11.00000 0.05 0.23 Q12 1 0.0746 0.0013 0.2079 11.00000 0.05 0.22 Q13 1 0.7196 0.2683 0.2052 11.00000 0.05 0.21 Q14 1 -0.0737 -0.0023 0.0367 11.00000 0.05 0.21 Q15 1 0.6845 0.3188 0.4798 11.00000 0.05 0.21 Q16 1 0.8681 0.2766 0.2183 11.00000 0.05 0.20 Q17 1 0.5590 0.3405 0.1469 11.00000 0.05 0.20 Q18 1 0.0186 0.9847 0.5421 11.00000 0.05 0.19 Q19 1 0.0008 0.0809 0.1838 11.00000 0.05 0.18 Q20 1 0.0517 0.1644 0.1439 11.00000 0.05 0.18 ; _shelx_res_checksum 75236 _shelx_hkl_file ; -2 0 0 3804.13 55.97 2 0 0 3814.66 50.84 -4 0 0 186.90 4.04 4 0 0 194.78 4.83 -6 0 0 63.81 3.05 6 0 0 66.27 5.85 -1 -1 0 632.71 7.13 1 -1 0 614.23 6.27 -1 1 0 662.82 12.74 1 1 0 677.55 9.39 -3 -1 0 466.77 5.70 3 -1 0 468.37 7.17 -3 1 0 480.37 9.26 3 1 0 486.29 8.19 -5 -1 0 499.51 8.79 5 -1 0 512.93 11.38 -5 1 0 490.77 8.33 5 1 0 490.52 11.16 -7 -1 0 302.59 8.75 7 -1 0 300.83 12.46 -7 1 0 299.82 8.02 7 1 0 279.68 11.88 0 -2 0 2440.78 24.92 0 2 0 2541.36 33.58 -2 -2 0 1679.15 17.12 2 -2 0 1641.02 16.44 -2 2 0 1580.93 21.62 2 2 0 1636.53 19.53 -4 -2 0 280.86 5.43 4 -2 0 291.14 6.32 -4 2 0 272.19 6.69 4 2 0 279.19 6.92 -6 -2 0 104.16 3.70 6 -2 0 103.89 6.56 -6 2 0 87.58 6.19 6 2 0 99.80 6.18 -1 -3 0 5094.25 58.02 1 -3 0 5192.70 48.73 -1 3 0 5285.66 100.87 1 3 0 5372.15 80.86 -3 -3 0 801.75 9.19 3 -3 0 785.75 9.59 -3 3 0 755.30 11.42 3 3 0 796.21 11.68 -5 -3 0 1627.96 25.63 5 -3 0 1604.91 28.72 -5 3 0 1560.61 34.35 5 3 0 1545.30 27.44 -7 -3 0 226.26 7.87 7 -3 0 209.00 14.82 -7 3 0 224.81 14.10 7 3 0 206.51 14.80 0 -4 0 1562.97 17.97 0 4 0 1627.56 23.97 -2 -4 0 47.79 1.39 2 -4 0 48.03 1.40 -2 4 0 43.27 1.94 2 4 0 43.12 2.05 -4 -4 0 340.16 6.24 4 -4 0 339.18 8.37 -4 4 0 332.55 7.75 4 4 0 332.33 7.99 -6 -4 0 402.25 9.01 6 -4 0 382.25 13.87 -6 4 0 380.34 13.16 6 4 0 377.19 12.69 -1 -5 0 259.25 4.76 1 -5 0 271.81 3.65 -1 5 0 260.48 5.86 1 5 0 259.12 5.51 -3 -5 0 454.70 7.84 3 -5 0 451.98 7.09 -3 5 0 438.89 7.99 3 5 0 441.57 7.73 -5 -5 0 595.87 15.67 5 -5 0 579.33 10.27 -5 5 0 582.67 13.69 5 5 0 602.25 16.34 0 -6 0 8894.58 97.93 0 6 0 9172.96 136.54 -2 -6 0 4284.56 48.56 2 -6 0 4291.48 45.83 -2 6 0 4367.49 59.47 2 6 0 4403.44 83.66 -4 -6 0 86.24 3.36 4 -6 0 84.27 4.07 -4 6 0 77.79 4.12 4 6 0 83.38 5.21 -6 -6 0 262.67 14.70 6 -6 0 269.91 11.46 -6 6 0 262.35 8.99 6 6 0 259.93 10.63 -1 -7 0 354.63 5.72 1 -7 0 353.58 4.89 -1 7 0 395.70 7.40 1 7 0 399.16 10.95 -3 -7 0 166.89 3.89 3 -7 0 171.07 4.51 -3 7 0 174.97 4.21 3 7 0 178.93 5.55 -5 -7 0 255.13 9.46 5 -7 0 258.88 14.81 -5 7 0 245.11 8.14 5 7 0 260.20 10.08 0 -8 0 202.28 4.46 0 8 0 205.27 7.45 -2 -8 0 59.77 2.88 2 -8 0 64.81 2.86 -2 8 0 67.79 3.01 2 8 0 69.27 3.76 -4 -8 0 294.37 7.86 4 -8 0 281.82 10.05 -4 8 0 263.31 8.34 4 8 0 262.30 9.86 -1 -9 0 950.76 14.55 1 -9 0 955.46 17.38 -1 9 0 887.14 21.91 1 9 0 953.41 22.03 -3 -9 0 213.93 6.50 3 -9 0 202.64 6.39 -3 9 0 197.16 6.69 3 9 0 208.22 6.66 -5 -9 0 451.64 20.66 5 -9 0 452.13 21.86 -5 9 0 457.93 12.90 5 9 0 455.54 22.03 0 -10 0 149.58 4.07 0 10 0 142.74 6.84 -2 -10 0 70.90 3.56 2 -10 0 82.20 5.73 -2 10 0 76.83 5.87 2 10 0 68.14 4.47 -4 -10 0 135.05 5.73 4 -10 0 149.69 10.74 -4 10 0 124.36 7.20 4 10 0 130.07 7.47 -1 -11 0 243.97 5.95 1 -11 0 236.31 7.26 -1 11 0 211.87 9.10 1 11 0 230.51 7.49 -3 -11 0 212.87 7.69 3 -11 0 200.50 12.01 -3 11 0 191.56 7.07 3 11 0 195.19 7.18 0 -12 0 2571.42 42.81 0 12 0 2525.90 43.24 -2 -12 0 378.84 9.69 2 -12 0 395.97 13.04 -2 12 0 362.66 12.43 2 12 0 371.28 10.56 6 0 -1 118.14 5.24 -6 0 1 111.32 4.31 4 0 -1 5331.14 83.27 -4 0 1 5359.87 66.83 2 0 -1 5024.15 64.95 -2 0 1 5010.97 53.96 0 0 -1 120.09 3.68 0 0 1 132.79 4.05 -2 0 -1 5414.27 77.77 2 0 1 5299.62 75.81 -4 0 -1 1787.65 30.06 4 0 1 1830.43 26.47 -6 0 -1 7.65 1.45 6 0 1 4.84 2.40 7 -1 -1 47.69 5.68 7 1 -1 45.62 5.38 -7 -1 1 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