data_shelx _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al8 H16.50 Cs3.70 Na3.60 O39.90 Si8' _chemical_formula_weight 1670.12 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' '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' 'Cs' 'Cs' -0.3680 2.1192 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _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+1/2, -z' _cell_length_a 10.0349(3) _cell_length_b 10.0534(4) _cell_length_c 10.0586(4) _cell_angle_alpha 90 _cell_angle_beta 90.474(3) _cell_angle_gamma 90 _cell_volume 1014.73(6) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5667 _cell_measurement_theta_min 2.8497 _cell_measurement_theta_max 35.8055 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.733 _exptl_crystal_F_000 795 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_absorpt_coefficient_mu 3.869 _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_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14299 _diffrn_reflns_av_unetI/netI 0.0476 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.855 _diffrn_reflns_theta_max 34.069 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 0.726 _diffrn_reflns_point_group_measured_fraction_full 0.796 _reflns_number_total 6067 _reflns_number_gt 5639 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.397 _reflns_Friedel_fraction_max 0.433 _reflns_Friedel_fraction_full 0.586 _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. Completness statistics refer to single and composite reflections containing twin component 1 only. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _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^)+(0.0728P)^2^+6.6645P] 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 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_extinction_coef 0.0123(14) _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 0.48(3) _chemical_absolute_configuration ? _refine_ls_number_reflns 6067 _refine_ls_number_parameters 297 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _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 Cs1 Cs -0.09539(7) 0.12630(8) 0.26480(7) 0.0218(2) Uani 0.915(7) 1 d . . P . . O17 O -0.09539(7) 0.12630(8) 0.26480(7) 0.0218(2) Uani 0.085(7) 1 d . . P . . Cs2 Cs 0.23769(6) 0.37014(7) 0.41789(7) 0.0189(2) Uani 0.923(7) 1 d . . P . . O18 O 0.23769(6) 0.37014(7) 0.41789(7) 0.0189(2) Uani 0.077(7) 1 d . . P . . Na1 Na -0.4596(5) 0.9264(5) 0.1856(5) 0.0215(15) Uani 0.90(6) 1 d . . P . . O19 O -0.4596(5) 0.9264(5) 0.1856(5) 0.0215(15) Uani 0.10(6) 1 d . . P . . Na2 Na 0.3311(6) 0.1780(7) 0.0585(6) 0.033(2) Uani 0.88(7) 1 d . . P . . O20 O 0.3311(6) 0.1780(7) 0.0585(6) 0.033(2) Uani 0.12(7) 1 d . . P . . Si1 Si 0.3864(2) -0.2695(3) 0.3910(3) 0.0118(5) Uani 1 1 d . . . . . Si2 Si 0.1117(2) 0.0325(3) 0.5728(3) 0.0116(5) Uani 1 1 d . . . . . Si3 Si 0.0688(2) -0.2607(3) 0.0739(3) 0.0130(5) Uani 1 1 d . . . . . Si4 Si 0.5689(2) -0.5674(3) 0.1096(3) 0.0115(5) Uani 1 1 d . . . . . Al1 Al 0.4229(3) -0.0216(3) 0.5769(3) 0.0112(5) Uani 1 1 d . . . . . Al2 Al 0.0783(3) -0.2158(3) 0.3833(3) 0.0114(5) Uani 1 1 d . . . . . Al3 Al 0.3770(3) -0.3182(3) 0.0751(3) 0.0114(5) Uani 1 1 d . . . . . Al4 Al 0.8826(3) -0.5122(3) 0.1177(3) 0.0129(5) Uani 1 1 d . . . . . O1 O 0.4583(7) -0.4020(7) 0.4511(8) 0.0166(13) Uani 1 1 d . . . . . O2 O 0.2321(7) -0.2816(9) 0.4286(8) 0.0211(15) Uani 1 1 d . . . . . O3 O 0.4557(6) -0.1400(8) 0.4557(7) 0.0168(12) Uani 1 1 d . . . . . O4 O 0.2698(7) 0.0593(8) 0.5518(9) 0.0198(15) Uani 1 1 d . . . . . O5 O 0.0498(7) -0.0629(8) 0.4598(7) 0.0174(13) Uani 1 1 d . . . . . O6 O -0.0420(6) -0.3231(8) 0.4392(8) 0.0180(13) Uani 1 1 d . . . . . O7 O 0.0697(9) -0.1811(9) 0.2138(8) 0.0233(15) Uani 1 1 d . . . . . O8 O -0.0540(7) -0.3636(9) 0.0581(9) 0.0249(17) Uani 1 1 d . . . . . O9 O 0.0445(9) -0.1496(8) -0.0424(8) 0.0225(16) Uani 1 1 d . . . . . O10 O 0.2074(7) -0.3401(8) 0.0474(8) 0.0188(14) Uani 1 1 d . . . . . O11 O 0.4121(7) -0.2602(8) 0.2312(7) 0.0173(13) Uani 1 1 d . . . . . O12 O 0.4543(6) -0.2062(7) -0.0332(7) 0.0141(12) Uani 1 1 d . . . . . O13 O 0.4581(8) -0.4682(8) 0.0461(8) 0.0199(14) Uani 1 1 d . . . . . O14 O 0.5524(7) -0.5923(7) 0.2662(7) 0.0139(12) Uani 1 1 d . . . . . O15 O 0.7126(7) -0.5050(9) 0.0789(8) 0.0197(14) Uani 1 1 d . . . . . O16 O -0.0833(7) 0.4644(9) 0.2858(8) 0.0205(14) Uani 1 1 d . . . . . OW1 O -0.4101(8) 0.1178(9) 0.2787(8) 0.0241(15) Uani 1 1 d . . . . . OW2 O 0.2178(9) 0.3639(11) 0.1092(10) 0.034(2) Uani 1 1 d . . . . . OW3 O 0.2622(13) 0.0458(13) 0.2385(11) 0.027(3) Uani 0.75(4) 1 d . . P . . OW4 O -0.2615(9) -0.1987(13) 0.2298(12) 0.030(3) Uani 0.83(4) 1 d . . P . . 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 Cs1 0.0237(3) 0.0239(4) 0.0177(3) 0.0075(3) -0.0061(2) -0.0042(3) O17 0.0237(3) 0.0239(4) 0.0177(3) 0.0075(3) -0.0061(2) -0.0042(3) Cs2 0.0144(3) 0.0222(3) 0.0201(3) -0.0011(3) 0.00364(19) -0.0047(2) O18 0.0144(3) 0.0222(3) 0.0201(3) -0.0011(3) 0.00364(19) -0.0047(2) Na1 0.024(2) 0.021(2) 0.019(2) 0.0031(18) -0.0048(16) -0.0048(17) O19 0.024(2) 0.021(2) 0.019(2) 0.0031(18) -0.0048(16) -0.0048(17) Na2 0.029(3) 0.036(3) 0.034(3) -0.015(3) 0.014(2) -0.014(2) O20 0.029(3) 0.036(3) 0.034(3) -0.015(3) 0.014(2) -0.014(2) Si1 0.0110(9) 0.0140(11) 0.0104(11) -0.0012(9) -0.0004(7) 0.0012(8) Si2 0.0117(10) 0.0124(11) 0.0109(11) 0.0010(9) 0.0009(7) -0.0001(8) Si3 0.0118(10) 0.0165(12) 0.0108(11) 0.0014(9) 0.0008(8) -0.0023(8) Si4 0.0122(9) 0.0111(11) 0.0114(11) -0.0002(9) -0.0002(7) 0.0007(8) Al1 0.0089(10) 0.0139(12) 0.0107(12) 0.0004(10) -0.0006(8) -0.0017(8) Al2 0.0099(10) 0.0137(12) 0.0107(12) -0.0004(10) 0.0006(8) -0.0006(8) Al3 0.0110(10) 0.0129(12) 0.0102(12) 0.0022(10) 0.0032(8) 0.0016(9) Al4 0.0127(11) 0.0143(13) 0.0119(12) -0.0010(10) 0.0016(9) -0.0027(9) O1 0.019(3) 0.014(3) 0.017(3) 0.000(2) -0.002(2) 0.000(2) O2 0.014(3) 0.030(4) 0.019(3) 0.009(3) 0.003(2) 0.004(3) O3 0.019(3) 0.015(3) 0.016(3) -0.002(3) 0.001(2) -0.001(2) O4 0.011(3) 0.016(3) 0.032(4) 0.007(3) 0.001(3) -0.002(2) O5 0.022(3) 0.015(3) 0.015(3) 0.000(3) -0.005(2) 0.001(2) O6 0.011(3) 0.015(3) 0.028(4) -0.004(3) 0.002(2) -0.001(2) O7 0.042(4) 0.017(3) 0.011(3) 0.002(3) 0.003(3) 0.005(3) O8 0.011(3) 0.027(4) 0.036(4) 0.014(4) -0.005(3) 0.000(3) O9 0.037(4) 0.012(4) 0.019(4) 0.004(3) -0.008(3) -0.007(3) O10 0.013(3) 0.025(4) 0.018(3) -0.011(3) 0.002(2) 0.000(2) O11 0.019(3) 0.017(3) 0.015(3) 0.001(3) 0.003(2) 0.002(2) O12 0.012(3) 0.018(3) 0.012(3) -0.004(2) 0.001(2) -0.002(2) O13 0.030(4) 0.013(3) 0.017(3) 0.001(3) -0.006(3) 0.002(3) O14 0.016(3) 0.019(3) 0.007(3) 0.000(2) 0.002(2) 0.000(2) O15 0.014(3) 0.026(4) 0.019(3) 0.002(3) 0.003(2) -0.003(3) O16 0.020(3) 0.026(4) 0.015(3) -0.005(3) 0.003(2) 0.000(3) OW1 0.036(4) 0.015(3) 0.021(3) 0.003(3) -0.004(3) -0.002(3) OW2 0.029(4) 0.027(4) 0.044(5) 0.000(5) -0.016(4) -0.014(4) OW3 0.043(7) 0.027(6) 0.011(5) 0.004(4) 0.002(4) -0.012(5) OW4 0.014(4) 0.035(6) 0.041(7) 0.002(5) 0.004(4) 0.011(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 Cs1 O5 3.089(7) . ? Cs1 OW1 3.164(8) . ? Cs1 O9 3.219(8) 2 ? Cs1 O6 3.311(8) 2_556 ? Cs1 O10 3.344(7) 2 ? Cs1 O16 3.408(9) . ? Cs1 O2 3.510(8) 2_556 ? Cs1 O7 3.546(8) . ? Cs1 O8 3.590(9) 2 ? Cs1 Si3 3.603(3) 2 ? Cs1 OW4 3.684(13) . ? Cs1 OW3 3.690(13) . ? Cs2 OW2 3.110(10) . ? Cs2 O6 3.121(7) 2_556 ? Cs2 O1 3.201(7) 1_565 ? Cs2 O5 3.217(7) 2_556 ? Cs2 O3 3.321(7) 2_656 ? Cs2 O4 3.418(8) . ? Cs2 O2 3.504(9) 1_565 ? Cs2 O14 3.539(7) 1_565 ? Cs2 Al1 3.576(3) 2_656 ? Cs2 O16 3.601(8) . ? Cs2 OW4 3.617(13) 2_556 ? Cs2 OW3 3.736(13) . ? Na1 OW1 2.196(11) 1_565 ? Na1 O11 2.323(9) 1_465 ? Na1 OW4 2.391(11) 1_565 ? Na1 O13 2.560(9) 2_565 ? Na1 O12 2.708(9) 1_465 ? Na1 O3 2.931(9) 1_465 ? Na1 Al3 3.152(6) 1_465 ? Na1 Si4 3.157(5) 2_565 ? Na1 Si1 3.254(6) 1_465 ? Na1 Na2 3.521(9) 1_465 ? Na1 Na2 3.739(8) 2 ? Na2 OW2 2.249(13) . ? Na2 O15 2.340(10) 2_655 ? Na2 OW3 2.354(13) . ? Na2 O12 2.463(8) 2_655 ? Na2 O13 2.790(10) 2_655 ? Na2 Si4 3.159(7) 2_655 ? Na2 Al3 3.233(6) 2_655 ? Na2 Al4 3.366(6) 2_655 ? Si1 O2 1.601(7) . ? Si1 O3 1.611(8) . ? Si1 O1 1.629(8) . ? Si1 O11 1.632(8) . ? Si2 O16 1.606(8) 2_546 ? Si2 O5 1.608(8) . ? Si2 O6 1.616(8) 2_556 ? Si2 O4 1.625(7) . ? Si3 O8 1.615(8) . ? Si3 O7 1.618(9) . ? Si3 O10 1.628(7) . ? Si3 O9 1.633(8) . ? Si4 O14 1.605(7) . ? Si4 O15 1.605(8) . ? Si4 O12 1.610(8) 2_645 ? Si4 O13 1.621(8) . ? Al1 O1 1.718(8) 2_656 ? Al1 O3 1.737(8) . ? Al1 O14 1.747(7) 2_656 ? Al1 O4 1.754(8) . ? Al2 O6 1.717(8) . ? Al2 O2 1.736(7) . ? Al2 O7 1.742(8) . ? Al2 O5 1.744(8) . ? Al3 O11 1.709(8) . ? Al3 O10 1.736(7) . ? Al3 O13 1.739(8) . ? Al3 O12 1.752(8) . ? Al4 O8 1.733(9) 1_655 ? Al4 O16 1.738(9) 1_645 ? Al4 O9 1.740(8) 2_645 ? Al4 O15 1.748(8) . ? 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 O5 Cs1 OW1 114.9(2) . . ? O5 Cs1 O9 142.7(2) . 2 ? OW1 Cs1 O9 102.3(2) . 2 ? O5 Cs1 O6 48.15(19) . 2_556 ? OW1 Cs1 O6 111.89(19) . 2_556 ? O9 Cs1 O6 116.76(19) 2 2_556 ? O5 Cs1 O10 144.3(2) . 2 ? OW1 Cs1 O10 73.53(19) . 2 ? O9 Cs1 O10 47.97(19) 2 2 ? O6 Cs1 O10 164.47(19) 2_556 2 ? O5 Cs1 O16 123.96(19) . . ? OW1 Cs1 O16 93.4(2) . . ? O9 Cs1 O16 48.64(19) 2 . ? O6 Cs1 O16 77.09(19) 2_556 . ? O10 Cs1 O16 88.2(2) 2 . ? O5 Cs1 O2 77.9(2) . 2_556 ? OW1 Cs1 O2 64.57(19) . 2_556 ? O9 Cs1 O2 119.4(2) 2 2_556 ? O6 Cs1 O2 48.09(17) 2_556 2_556 ? O10 Cs1 O2 131.89(18) 2 2_556 ? O16 Cs1 O2 72.3(2) . 2_556 ? O5 Cs1 O7 48.45(19) . . ? OW1 Cs1 O7 116.8(2) . . ? O9 Cs1 O7 115.6(2) 2 . ? O6 Cs1 O7 94.16(19) 2_556 . ? O10 Cs1 O7 96.07(19) 2 . ? O16 Cs1 O7 149.52(19) . . ? O2 Cs1 O7 122.9(2) 2_556 . ? O5 Cs1 O8 113.18(19) . 2 ? OW1 Cs1 O8 117.73(18) . 2 ? O9 Cs1 O8 44.1(2) 2 2 ? O6 Cs1 O8 129.45(16) 2_556 2 ? O10 Cs1 O8 44.52(16) 2 2 ? O16 Cs1 O8 90.7(2) . 2 ? O2 Cs1 O8 163.1(2) 2_556 2 ? O7 Cs1 O8 72.2(2) . 2 ? O5 Cs1 Si3 139.14(15) . 2 ? OW1 Cs1 Si3 97.60(15) . 2 ? O9 Cs1 Si3 26.96(15) 2 2 ? O6 Cs1 Si3 140.20(13) 2_556 2 ? O10 Cs1 Si3 26.77(12) 2 2 ? O16 Cs1 Si3 74.99(14) . 2 ? O2 Cs1 Si3 141.26(16) 2_556 2 ? O7 Cs1 Si3 95.71(14) . 2 ? O8 Cs1 Si3 25.95(14) 2 2 ? O5 Cs1 OW4 74.0(2) . . ? OW1 Cs1 OW4 61.9(2) . . ? O9 Cs1 OW4 128.9(2) 2 . ? O6 Cs1 OW4 114.0(2) 2_556 . ? O10 Cs1 OW4 81.5(2) 2 . ? O16 Cs1 OW4 155.03(19) . . ? O2 Cs1 OW4 97.9(2) 2_556 . ? O7 Cs1 OW4 54.9(2) . . ? O8 Cs1 OW4 97.5(2) 2 . ? Si3 Cs1 OW4 103.1(2) 2 . ? O5 Cs1 OW3 57.1(2) . . ? OW1 Cs1 OW3 165.7(3) . . ? O9 Cs1 OW3 86.8(2) 2 . ? O6 Cs1 OW3 72.6(2) 2_556 . ? O10 Cs1 OW3 105.9(2) 2 . ? O16 Cs1 OW3 100.9(2) . . ? O2 Cs1 OW3 120.6(2) 2_556 . ? O7 Cs1 OW3 48.9(3) . . ? O8 Cs1 OW3 61.8(2) 2 . ? Si3 Cs1 OW3 85.50(18) 2 . ? OW4 Cs1 OW3 103.8(2) . . ? OW2 Cs2 O6 114.3(2) . 2_556 ? OW2 Cs2 O1 99.1(2) . 1_565 ? O6 Cs2 O1 146.5(2) 2_556 1_565 ? OW2 Cs2 O5 109.6(2) . 2_556 ? O6 Cs2 O5 52.01(19) 2_556 2_556 ? O1 Cs2 O5 115.60(19) 1_565 2_556 ? OW2 Cs2 O3 115.7(2) . 2_656 ? O6 Cs2 O3 112.88(19) 2_556 2_656 ? O1 Cs2 O3 49.03(18) 1_565 2_656 ? O5 Cs2 O3 133.71(18) 2_556 2_656 ? OW2 Cs2 O4 112.3(3) . . ? O6 Cs2 O4 46.13(17) 2_556 . ? O1 Cs2 O4 123.39(18) 1_565 . ? O5 Cs2 O4 97.04(18) 2_556 . ? O3 Cs2 O4 74.75(18) 2_656 . ? OW2 Cs2 O2 92.9(2) . 1_565 ? O6 Cs2 O2 126.68(18) 2_556 1_565 ? O1 Cs2 O2 45.00(17) 1_565 1_565 ? O5 Cs2 O2 76.38(18) 2_556 1_565 ? O3 Cs2 O2 91.94(18) 2_656 1_565 ? O4 Cs2 O2 154.6(2) . 1_565 ? OW2 Cs2 O14 67.80(19) . 1_565 ? O6 Cs2 O14 146.31(18) 2_556 1_565 ? O1 Cs2 O14 49.44(18) 1_565 1_565 ? O5 Cs2 O14 161.60(19) 2_556 1_565 ? O3 Cs2 O14 48.78(16) 2_656 1_565 ? O4 Cs2 O14 100.72(17) . 1_565 ? O2 Cs2 O14 85.48(16) 1_565 1_565 ? OW2 Cs2 Al1 94.26(16) . 2_656 ? O6 Cs2 Al1 141.76(14) 2_556 2_656 ? O1 Cs2 Al1 28.69(14) 1_565 2_656 ? O5 Cs2 Al1 141.98(14) 2_556 2_656 ? O3 Cs2 Al1 28.88(14) 2_656 2_656 ? O4 Cs2 Al1 100.71(12) . 2_656 ? O2 Cs2 Al1 73.19(12) 1_565 2_656 ? O14 Cs2 Al1 28.42(12) 1_565 2_656 ? OW2 Cs2 O16 65.6(2) . . ? O6 Cs2 O16 76.69(19) 2_556 . ? O1 Cs2 O16 117.76(19) 1_565 . ? O5 Cs2 O16 44.26(18) 2_556 . ? O3 Cs2 O16 166.5(2) 2_656 . ? O4 Cs2 O16 117.86(18) . . ? O2 Cs2 O16 74.56(18) 1_565 . ? O14 Cs2 O16 127.70(17) 1_565 . ? Al1 Cs2 O16 140.73(15) 2_656 . ? OW2 Cs2 OW4 167.8(3) . 2_556 ? O6 Cs2 OW4 57.7(2) 2_556 2_556 ? O1 Cs2 OW4 89.7(2) 1_565 2_556 ? O5 Cs2 OW4 73.6(2) 2_556 2_556 ? O3 Cs2 OW4 64.24(18) 2_656 2_556 ? O4 Cs2 OW4 55.5(2) . 2_556 ? O2 Cs2 OW4 99.3(2) 1_565 2_556 ? O14 Cs2 OW4 113.00(18) 1_565 2_556 ? Al1 Cs2 OW4 89.35(15) 2_656 2_556 ? O16 Cs2 OW4 117.6(2) . 2_556 ? OW2 Cs2 OW3 60.3(3) . . ? O6 Cs2 OW3 74.0(2) 2_556 . ? O1 Cs2 OW3 128.8(2) 1_565 . ? O5 Cs2 OW3 115.5(2) 2_556 . ? O3 Cs2 OW3 95.4(2) 2_656 . ? O4 Cs2 OW3 52.1(2) . . ? O2 Cs2 OW3 152.7(2) 1_565 . ? O14 Cs2 OW3 79.8(2) 1_565 . ? Al1 Cs2 OW3 101.9(2) 2_656 . ? O16 Cs2 OW3 96.5(2) . . ? OW4 Cs2 OW3 107.6(3) 2_556 . ? OW1 Na1 O11 138.3(4) 1_565 1_465 ? OW1 Na1 OW4 101.4(4) 1_565 1_565 ? O11 Na1 OW4 90.0(4) 1_465 1_565 ? OW1 Na1 O13 91.3(3) 1_565 2_565 ? O11 Na1 O13 121.4(3) 1_465 2_565 ? OW4 Na1 O13 112.1(4) 1_565 2_565 ? OW1 Na1 O12 148.0(4) 1_565 1_465 ? O11 Na1 O12 65.8(3) 1_465 1_465 ? OW4 Na1 O12 98.7(4) 1_565 1_465 ? O13 Na1 O12 57.9(3) 2_565 1_465 ? OW1 Na1 O3 82.5(3) 1_565 1_465 ? O11 Na1 O3 57.8(3) 1_465 1_465 ? OW4 Na1 O3 87.4(3) 1_565 1_465 ? O13 Na1 O3 160.4(3) 2_565 1_465 ? O12 Na1 O3 123.2(3) 1_465 1_465 ? OW1 Na1 Al3 161.6(3) 1_565 1_465 ? O11 Na1 Al3 32.1(2) 1_465 1_465 ? OW4 Na1 Al3 94.9(4) 1_565 1_465 ? O13 Na1 Al3 90.5(2) 2_565 1_465 ? O12 Na1 Al3 33.71(17) 1_465 1_465 ? O3 Na1 Al3 89.7(2) 1_465 1_465 ? OW1 Na1 Si4 117.3(3) 1_565 2_565 ? O11 Na1 Si4 90.8(2) 1_465 2_565 ? OW4 Na1 Si4 117.9(4) 1_565 2_565 ? O13 Na1 Si4 30.73(19) 2_565 2_565 ? O12 Na1 Si4 30.65(18) 1_465 2_565 ? O3 Na1 Si4 140.8(2) 1_465 2_565 ? Al3 Na1 Si4 60.55(11) 1_465 2_565 ? OW1 Na1 Si1 111.5(3) 1_565 1_465 ? O11 Na1 Si1 28.2(2) 1_465 1_465 ? OW4 Na1 Si1 87.8(3) 1_565 1_465 ? O13 Na1 Si1 146.6(3) 2_565 1_465 ? O12 Na1 Si1 93.9(2) 1_465 1_465 ? O3 Na1 Si1 29.61(16) 1_465 1_465 ? Al3 Na1 Si1 60.23(11) 1_465 1_465 ? Si4 Na1 Si1 116.49(16) 2_565 1_465 ? OW1 Na1 Na2 70.0(3) 1_565 1_465 ? O11 Na1 Na2 108.8(3) 1_465 1_465 ? OW4 Na1 Na2 159.7(4) 1_565 1_465 ? O13 Na1 Na2 51.7(2) 2_565 1_465 ? O12 Na1 Na2 82.7(2) 1_465 1_465 ? O3 Na1 Na2 108.9(2) 1_465 1_465 ? Al3 Na1 Na2 97.20(16) 1_465 1_465 ? Si4 Na1 Na2 56.14(13) 2_565 1_465 ? Si1 Na1 Na2 112.34(17) 1_465 1_465 ? OW1 Na1 Na2 142.0(3) 1_565 2 ? O11 Na1 Na2 77.6(2) 1_465 2 ? OW4 Na1 Na2 58.7(3) 1_565 2 ? O13 Na1 Na2 71.0(2) 2_565 2 ? O12 Na1 Na2 41.16(19) 1_465 2 ? O3 Na1 Na2 124.1(2) 1_465 2 ? Al3 Na1 Na2 55.17(14) 1_465 2 ? Si4 Na1 Na2 60.97(14) 2_565 2 ? Si1 Na1 Na2 100.43(17) 1_465 2 ? Na2 Na1 Na2 116.71(14) 1_465 2 ? OW1 Na1 Cs1 46.6(2) 1_565 1_565 ? O11 Na1 Cs1 145.5(3) 1_465 1_565 ? OW4 Na1 Cs1 60.0(3) 1_565 1_565 ? O13 Na1 Cs1 87.9(2) 2_565 1_565 ? O12 Na1 Cs1 130.9(2) 1_465 1_565 ? O3 Na1 Cs1 100.94(18) 1_465 1_565 ? Al3 Na1 Cs1 151.74(17) 1_465 1_565 ? Si4 Na1 Cs1 117.35(14) 2_565 1_565 ? Si1 Na1 Cs1 125.50(14) 1_465 1_565 ? Na2 Na1 Cs1 103.79(15) 1_465 1_565 ? Na2 Na1 Cs1 97.97(15) 2 1_565 ? OW2 Na2 O15 134.0(4) . 2_655 ? OW2 Na2 OW3 98.2(5) . . ? O15 Na2 OW3 87.5(4) 2_655 . ? OW2 Na2 O12 94.3(3) . 2_655 ? O15 Na2 O12 118.0(3) 2_655 2_655 ? OW3 Na2 O12 127.5(4) . 2_655 ? OW2 Na2 O13 155.5(4) . 2_655 ? O15 Na2 O13 60.1(3) 2_655 2_655 ? OW3 Na2 O13 102.8(5) . 2_655 ? O12 Na2 O13 62.8(3) 2_655 2_655 ? OW2 Na2 Si4 159.0(4) . 2_655 ? O15 Na2 Si4 29.41(19) 2_655 2_655 ? OW3 Na2 Si4 93.9(4) . 2_655 ? O12 Na2 Si4 91.8(2) 2_655 2_655 ? O13 Na2 Si4 30.83(17) 2_655 2_655 ? OW2 Na2 Al3 123.1(3) . 2_655 ? O15 Na2 Al3 86.0(2) 2_655 2_655 ? OW3 Na2 Al3 126.8(4) . 2_655 ? O12 Na2 Al3 32.37(19) 2_655 2_655 ? O13 Na2 Al3 32.52(18) 2_655 2_655 ? Si4 Na2 Al3 59.59(12) 2_655 2_655 ? OW2 Na2 Al4 105.7(3) . 2_655 ? O15 Na2 Al4 29.21(19) 2_655 2_655 ? OW3 Na2 Al4 83.9(3) . 2_655 ? O12 Na2 Al4 140.1(3) 2_655 2_655 ? O13 Na2 Al4 89.1(2) 2_655 2_655 ? Si4 Na2 Al4 58.57(12) 2_655 2_655 ? Al3 Na2 Al4 111.30(18) 2_655 2_655 ? OW2 Na2 Na1 144.7(4) . 1_645 ? O15 Na2 Na1 76.0(3) 2_655 1_645 ? OW3 Na2 Na1 59.6(4) . 1_645 ? O12 Na2 Na1 81.8(2) 2_655 1_645 ? O13 Na2 Na1 46.1(2) 2_655 1_645 ? Si4 Na2 Na1 56.10(15) 2_655 1_645 ? Al3 Na2 Na1 67.65(16) 2_655 1_645 ? Al4 Na2 Na1 99.13(19) 2_655 1_645 ? OW2 Na2 Na1 76.8(3) . 2_545 ? O15 Na2 Na1 101.6(3) 2_655 2_545 ? OW3 Na2 Na1 170.8(4) . 2_545 ? O12 Na2 Na1 46.3(2) 2_655 2_545 ? O13 Na2 Na1 80.6(2) 2_655 2_545 ? Si4 Na2 Na1 93.27(16) 2_655 2_545 ? Al3 Na2 Na1 53.16(12) 2_655 2_545 ? Al4 Na2 Na1 104.78(19) 2_655 2_545 ? Na1 Na2 Na1 120.67(15) 1_645 2_545 ? OW2 Na2 Cs2 46.2(3) . . ? O15 Na2 Cs2 145.7(3) 2_655 . ? OW3 Na2 Cs2 62.0(3) . . ? O12 Na2 Cs2 94.2(2) 2_655 . ? O13 Na2 Cs2 137.8(3) 2_655 . ? Si4 Na2 Cs2 153.1(2) 2_655 . ? Al3 Na2 Cs2 124.07(16) 2_655 . ? Al4 Na2 Cs2 124.56(15) 2_655 . ? Na1 Na2 Cs2 98.89(17) 1_645 . ? Na1 Na2 Cs2 109.73(17) 2_545 . ? OW2 Na2 Cs1 62.5(3) . . ? O15 Na2 Cs1 90.4(2) 2_655 . ? OW3 Na2 Cs1 48.5(3) . . ? O12 Na2 Cs1 151.6(3) 2_655 . ? O13 Na2 Cs1 142.0(3) 2_655 . ? Si4 Na2 Cs1 115.81(15) 2_655 . ? Al3 Na2 Cs1 174.3(2) 2_655 . ? Al4 Na2 Cs1 66.41(10) 2_655 . ? Na1 Na2 Cs1 107.26(17) 1_645 . ? Na1 Na2 Cs1 132.04(19) 2_545 . ? Cs2 Na2 Cs1 58.20(7) . . ? O2 Si1 O3 112.4(4) . . ? O2 Si1 O1 106.0(4) . . ? O3 Si1 O1 108.8(4) . . ? O2 Si1 O11 113.5(4) . . ? O3 Si1 O11 106.3(4) . . ? O1 Si1 O11 109.8(4) . . ? O2 Si1 Na1 131.4(3) . 1_645 ? O3 Si1 Na1 64.0(3) . 1_645 ? O1 Si1 Na1 121.3(3) . 1_645 ? O11 Si1 Na1 42.3(3) . 1_645 ? O2 Si1 Cs2 63.0(3) . 1_545 ? O3 Si1 Cs2 151.7(3) . 1_545 ? O1 Si1 Cs2 52.2(3) . 1_545 ? O11 Si1 Cs2 100.6(3) . 1_545 ? Na1 Si1 Cs2 141.68(12) 1_645 1_545 ? O16 Si2 O5 107.6(4) 2_546 . ? O16 Si2 O6 111.7(4) 2_546 2_556 ? O5 Si2 O6 108.6(4) . 2_556 ? O16 Si2 O4 111.5(4) 2_546 . ? O5 Si2 O4 112.2(4) . . ? O6 Si2 O4 105.3(4) 2_556 . ? O16 Si2 Cs1 136.2(3) 2_546 . ? O5 Si2 Cs1 51.1(3) . . ? O6 Si2 Cs1 59.2(3) 2_556 . ? O4 Si2 Cs1 112.2(3) . . ? O16 Si2 Cs2 68.4(3) 2_546 2_546 ? O5 Si2 Cs2 54.6(3) . 2_546 ? O6 Si2 Cs2 89.4(3) 2_556 2_546 ? O4 Si2 Cs2 163.5(3) . 2_546 ? Cs1 Si2 Cs2 68.79(4) . 2_546 ? O16 Si2 Cs2 140.9(3) 2_546 . ? O5 Si2 Cs2 110.9(3) . . ? O6 Si2 Cs2 48.5(3) 2_556 . ? O4 Si2 Cs2 59.3(3) . . ? Cs1 Si2 Cs2 69.06(5) . . ? Cs2 Si2 Cs2 131.73(7) 2_546 . ? O8 Si3 O7 113.6(5) . . ? O8 Si3 O10 108.8(4) . . ? O7 Si3 O10 112.7(4) . . ? O8 Si3 O9 105.0(4) . . ? O7 Si3 O9 106.5(4) . . ? O10 Si3 O9 109.9(5) . . ? O8 Si3 Cs1 76.6(3) . 2_545 ? O7 Si3 Cs1 167.9(3) . 2_545 ? O10 Si3 Cs1 67.7(3) . 2_545 ? O9 Si3 Cs1 63.3(3) . 2_545 ? O14 Si4 O15 110.5(4) . . ? O14 Si4 O12 108.5(4) . 2_645 ? O15 Si4 O12 111.9(4) . 2_645 ? O14 Si4 O13 114.0(4) . . ? O15 Si4 O13 107.4(4) . . ? O12 Si4 O13 104.4(4) 2_645 . ? O14 Si4 Na1 151.9(3) . 2_535 ? O15 Si4 Na1 97.6(3) . 2_535 ? O12 Si4 Na1 59.1(3) 2_645 2_535 ? O13 Si4 Na1 53.8(3) . 2_535 ? O14 Si4 Na2 133.1(3) . 2_645 ? O15 Si4 Na2 45.7(3) . 2_645 ? O12 Si4 Na2 117.8(3) 2_645 2_645 ? O13 Si4 Na2 61.9(3) . 2_645 ? Na1 Si4 Na2 67.76(17) 2_535 2_645 ? O1 Al1 O3 103.2(4) 2_656 . ? O1 Al1 O14 109.8(4) 2_656 2_656 ? O3 Al1 O14 109.2(4) . 2_656 ? O1 Al1 O4 105.1(4) 2_656 . ? O3 Al1 O4 112.8(4) . . ? O14 Al1 O4 115.9(4) 2_656 . ? O1 Al1 Cs2 63.4(3) 2_656 2_646 ? O3 Al1 Cs2 67.4(2) . 2_646 ? O14 Al1 Cs2 74.6(2) 2_656 2_646 ? O4 Al1 Cs2 167.4(3) . 2_646 ? O6 Al2 O2 107.5(4) . . ? O6 Al2 O7 114.6(4) . . ? O2 Al2 O7 111.7(4) . . ? O6 Al2 O5 106.9(4) . . ? O2 Al2 O5 111.6(4) . . ? O7 Al2 O5 104.4(4) . . ? O6 Al2 Cs2 52.3(3) . 2_546 ? O2 Al2 Cs2 132.9(3) . 2_546 ? O7 Al2 Cs2 115.4(3) . 2_546 ? O5 Al2 Cs2 55.6(3) . 2_546 ? O6 Al2 Cs1 58.0(3) . 2_546 ? O2 Al2 Cs1 64.7(3) . 2_546 ? O7 Al2 Cs1 167.4(3) . 2_546 ? O5 Al2 Cs1 87.9(3) . 2_546 ? Cs2 Al2 Cs1 69.48(5) 2_546 2_546 ? O6 Al2 Cs1 109.2(3) . . ? O2 Al2 Cs1 141.6(3) . . ? O7 Al2 Cs1 61.5(3) . . ? O5 Al2 Cs1 46.1(2) . . ? Cs2 Al2 Cs1 66.87(5) 2_546 . ? Cs1 Al2 Cs1 129.35(8) 2_546 . ? O11 Al3 O10 112.6(4) . . ? O11 Al3 O13 110.9(4) . . ? O10 Al3 O13 108.8(4) . . ? O11 Al3 O12 105.3(4) . . ? O10 Al3 O12 114.9(4) . . ? O13 Al3 O12 104.1(4) . . ? O11 Al3 Na1 46.2(3) . 1_645 ? O10 Al3 Na1 131.4(3) . 1_645 ? O13 Al3 Na1 119.5(3) . 1_645 ? O12 Al3 Na1 59.1(3) . 1_645 ? O11 Al3 Na2 101.9(3) . 2_645 ? O10 Al3 Na2 145.3(3) . 2_645 ? O13 Al3 Na2 59.6(3) . 2_645 ? O12 Al3 Na2 48.8(3) . 2_645 ? Na1 Al3 Na2 71.67(17) 1_645 2_645 ? O8 Al4 O16 112.5(4) 1_655 1_645 ? O8 Al4 O9 112.2(4) 1_655 2_645 ? O16 Al4 O9 103.7(4) 1_645 2_645 ? O8 Al4 O15 104.3(4) 1_655 . ? O16 Al4 O15 114.0(4) 1_645 . ? O9 Al4 O15 110.4(4) 2_645 . ? O8 Al4 Na2 64.0(3) 1_655 2_645 ? O16 Al4 Na2 135.1(3) 1_645 2_645 ? O9 Al4 Na2 119.3(3) 2_645 2_645 ? O15 Al4 Na2 40.8(3) . 2_645 ? O8 Al4 Cs1 155.3(3) 1_655 1_645 ? O16 Al4 Cs1 59.9(3) 1_645 1_645 ? O9 Al4 Cs1 53.6(3) 2_645 1_645 ? O15 Al4 Cs1 100.0(3) . 1_645 ? Na2 Al4 Cs1 139.21(14) 2_645 1_645 ? Si1 O1 Al1 144.8(5) . 2_646 ? Si1 O1 Cs2 104.0(3) . 1_545 ? Al1 O1 Cs2 87.9(3) 2_646 1_545 ? Si1 O2 Al2 140.2(5) . . ? Si1 O2 Cs2 93.0(4) . 1_545 ? Al2 O2 Cs2 112.8(4) . 1_545 ? Si1 O2 Cs1 127.8(4) . 2_546 ? Al2 O2 Cs1 88.8(3) . 2_546 ? Cs2 O2 Cs1 76.69(17) 1_545 2_546 ? Si1 O3 Al1 138.9(4) . . ? Si1 O3 Na1 86.4(3) . 1_645 ? Al1 O3 Na1 123.5(4) . 1_645 ? Si1 O3 Cs2 125.1(4) . 2_646 ? Al1 O3 Cs2 83.7(3) . 2_646 ? Na1 O3 Cs2 94.2(2) 1_645 2_646 ? Si2 O4 Al1 139.4(5) . . ? Si2 O4 Cs2 96.5(3) . . ? Al1 O4 Cs2 124.1(3) . . ? Si2 O5 Al2 140.7(5) . . ? Si2 O5 Cs1 105.0(4) . . ? Al2 O5 Cs1 109.9(3) . . ? Si2 O5 Cs2 101.3(3) . 2_546 ? Al2 O5 Cs2 97.8(3) . 2_546 ? Cs1 O5 Cs2 87.24(18) . 2_546 ? Si2 O6 Al2 147.7(5) 2_546 . ? Si2 O6 Cs2 108.7(3) 2_546 2_546 ? Al2 O6 Cs2 101.9(3) . 2_546 ? Si2 O6 Cs1 96.1(4) 2_546 2_546 ? Al2 O6 Cs1 95.9(3) . 2_546 ? Cs2 O6 Cs1 86.6(2) 2_546 2_546 ? Si3 O7 Al2 138.8(6) . . ? Si3 O7 Cs1 123.9(4) . . ? Al2 O7 Cs1 93.0(3) . . ? Si3 O8 Al4 143.1(5) . 1_455 ? Si3 O8 Cs1 77.5(3) . 2_545 ? Al4 O8 Cs1 116.4(4) 1_455 2_545 ? Si3 O9 Al4 142.5(5) . 2_655 ? Si3 O9 Cs1 89.8(3) . 2_545 ? Al4 O9 Cs1 100.6(4) 2_655 2_545 ? Si3 O10 Al3 138.5(5) . . ? Si3 O10 Cs1 85.5(3) . 2_545 ? Al3 O10 Cs1 119.0(3) . 2_545 ? Si1 O11 Al3 148.4(5) . . ? Si1 O11 Na1 109.5(4) . 1_645 ? Al3 O11 Na1 101.8(4) . 1_645 ? Si4 O12 Al3 142.3(4) 2_655 . ? Si4 O12 Na2 118.9(4) 2_655 2_645 ? Al3 O12 Na2 98.8(4) . 2_645 ? Si4 O12 Na1 90.3(3) 2_655 1_645 ? Al3 O12 Na1 87.2(3) . 1_645 ? Na2 O12 Na1 92.5(3) 2_645 1_645 ? Si4 O13 Al3 142.0(5) . . ? Si4 O13 Na1 95.4(4) . 2_535 ? Al3 O13 Na1 121.2(4) . 2_535 ? Si4 O13 Na2 87.3(4) . 2_645 ? Al3 O13 Na2 87.9(3) . 2_645 ? Na1 O13 Na2 82.2(3) 2_535 2_645 ? Si4 O14 Al1 143.9(5) . 2_646 ? Si4 O14 Cs2 122.6(3) . 1_545 ? Al1 O14 Cs2 77.0(2) 2_646 1_545 ? Si4 O15 Al4 144.8(6) . . ? Si4 O15 Na2 104.9(4) . 2_645 ? Al4 O15 Na2 110.0(4) . 2_645 ? Si2 O16 Al4 140.3(6) 2_556 1_465 ? Si2 O16 Cs1 118.2(4) 2_556 . ? Al4 O16 Cs1 93.9(3) 1_465 . ? Si2 O16 Cs2 87.1(3) 2_556 . ? Al4 O16 Cs2 124.3(3) 1_465 . ? Cs1 O16 Cs2 77.97(18) . . ? Na1 OW1 Cs1 103.1(3) 1_545 . ? Na2 OW2 Cs2 102.4(4) . . ? Na2 OW3 Cs1 102.9(4) . . ? Na2 OW3 Cs2 84.2(4) . . ? Cs1 OW3 Cs2 72.9(3) . . ? Na1 OW4 Cs2 97.5(4) 1_545 2_546 ? Na1 OW4 Cs1 85.8(4) 1_545 . ? Cs2 OW4 Cs1 73.2(2) 2_546 . ? _refine_diff_density_max 2.100 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.338 _shelx_res_file ; TITL a in P2(1) shelx.res created by SHELXL-2018/3 at 11:51:35 on 08-Oct-2019 CELL 0.71073 10.0349 10.0534 10.0586 90.000 90.474 90.000 ZERR 1.00 0.0003 0.0004 0.0004 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC O AL SI CS NA H UNIT 39.9 8 8 3.7 3.6 16.5 MERG 2 temp -173 OMIT -2 0 1 OMIT -4 0 4 OMIT -5 0 2 OMIT -2 0 4 OMIT -6 -1 1 OMIT -5 -2 1 OMIT -2 -2 2 OMIT 2 -4 5 OMIT 1 0 2 OMIT 0 0 4 OMIT 5 0 4 OMIT 2 -2 2 OMIT 4 -7 1 OMIT -2 -3 5 OMIT 5 -3 2 OMIT -2 2 2 OMIT 5 3 2 OMIT -1 0 6 OMIT 4 0 0 OMIT -4 0 5 OMIT 5 1 0 OMIT 2 0 5 OMIT -8 0 4 OMIT 5 -1 0 OMIT -5 2 1 OMIT -3 -2 5 OMIT -2 3 5 OMIT -6 1 1 OMIT 1 2 7 OMIT 2 2 2 OMIT 4 7 1 OMIT -3 0 7 OMIT 5 0 1 OMIT 1 2 5 OMIT 1 -2 7 OMIT 1 7 2 OMIT -5 -1 2 OMIT -4 0 10 OMIT 0 1 3 OMIT -2 1 7 OMIT 5 -3 7 OMIT -4 1 7 OMIT 1 -2 5 OMIT 1 -7 2 OMIT 6 0 7 OMIT -7 2 9 OMIT -3 2 5 OMIT 7 0 9 OMIT 2 0 6 OMIT 3 1 0 TWIN eadp cs1 o17 exyz cs1 o17 eadp cs2 o18 exyz cs2 o18 exyz na1 o19 eadp na1 o19 exyz na2 o20 eadp na2 o20 FMAP 2 omit -2 68.14 ACTA BOND L.S. 8 WGHT 0.072800 6.664500 EXTI 0.012315 BASF 0.48089 FVAR 3.63183 0.91519 0.92342 0.89751 0.88096 0.74522 0.82932 MOLE 1 CS1 4 -0.095385 0.126295 0.264805 21.00000 0.02368 0.02393 = 0.01773 0.00750 -0.00607 -0.00416 O17 1 -0.095385 0.126295 0.264805 -21.00000 0.02368 0.02393 = 0.01773 0.00750 -0.00607 -0.00416 CS2 4 0.237694 0.370142 0.417888 31.00000 0.01435 0.02224 = 0.02007 -0.00109 0.00364 -0.00470 O18 1 0.237694 0.370142 0.417888 -31.00000 0.01435 0.02224 = 0.02007 -0.00109 0.00364 -0.00470 NA1 5 -0.459598 0.926364 0.185574 41.00000 0.02431 0.02116 = 0.01894 0.00314 -0.00484 -0.00475 O19 1 -0.459598 0.926364 0.185574 -41.00000 0.02431 0.02116 = 0.01894 0.00314 -0.00484 -0.00475 NA2 5 0.331093 0.177954 0.058549 51.00000 0.02900 0.03615 = 0.03419 -0.01517 0.01439 -0.01423 O20 1 0.331093 0.177954 0.058549 -51.00000 0.02900 0.03615 = 0.03419 -0.01517 0.01439 -0.01423 SI1 3 0.386368 -0.269494 0.390968 11.00000 0.01102 0.01401 = 0.01040 -0.00117 -0.00036 0.00120 SI2 3 0.111651 0.032472 0.572833 11.00000 0.01165 0.01235 = 0.01090 0.00102 0.00085 -0.00010 SI3 3 0.068769 -0.260688 0.073886 11.00000 0.01181 0.01651 = 0.01083 0.00135 0.00079 -0.00226 SI4 3 0.568885 -0.567370 0.109618 11.00000 0.01220 0.01107 = 0.01136 -0.00025 -0.00024 0.00074 AL1 2 0.422882 -0.021557 0.576874 11.00000 0.00889 0.01390 = 0.01073 0.00037 -0.00062 -0.00174 AL2 2 0.078302 -0.215813 0.383267 11.00000 0.00991 0.01365 = 0.01067 -0.00039 0.00065 -0.00056 AL3 2 0.376995 -0.318180 0.075066 11.00000 0.01101 0.01286 = 0.01024 0.00217 0.00316 0.00160 AL4 2 0.882609 -0.512212 0.117681 11.00000 0.01266 0.01435 = 0.01185 -0.00101 0.00165 -0.00266 O1 1 0.458286 -0.402025 0.451109 11.00000 0.01880 0.01434 = 0.01678 0.00008 -0.00211 0.00033 O2 1 0.232089 -0.281576 0.428628 11.00000 0.01423 0.02968 = 0.01947 0.00911 0.00281 0.00444 O3 1 0.455709 -0.139999 0.455700 11.00000 0.01946 0.01470 = 0.01619 -0.00191 0.00130 -0.00125 O4 1 0.269819 0.059265 0.551812 11.00000 0.01113 0.01582 = 0.03239 0.00686 0.00131 -0.00177 O5 1 0.049800 -0.062929 0.459800 11.00000 0.02170 0.01547 = 0.01483 -0.00049 -0.00456 0.00080 O6 1 -0.042045 -0.323059 0.439154 11.00000 0.01113 0.01487 = 0.02798 -0.00429 0.00170 -0.00051 O7 1 0.069738 -0.181145 0.213753 11.00000 0.04161 0.01699 = 0.01142 0.00200 0.00289 0.00548 O8 1 -0.054023 -0.363556 0.058132 11.00000 0.01135 0.02700 = 0.03612 0.01405 -0.00548 -0.00032 O9 1 0.044485 -0.149645 -0.042351 11.00000 0.03664 0.01195 = 0.01889 0.00392 -0.00827 -0.00694 O10 1 0.207380 -0.340119 0.047413 11.00000 0.01349 0.02492 = 0.01789 -0.01063 0.00193 0.00042 O11 1 0.412087 -0.260187 0.231220 11.00000 0.01947 0.01745 = 0.01491 0.00091 0.00332 0.00152 O12 1 0.454312 -0.206227 -0.033181 11.00000 0.01241 0.01811 = 0.01179 -0.00423 0.00081 -0.00154 O13 1 0.458057 -0.468222 0.046128 11.00000 0.03011 0.01263 = 0.01672 0.00061 -0.00629 0.00185 O14 1 0.552400 -0.592265 0.266243 11.00000 0.01641 0.01852 = 0.00683 -0.00013 0.00245 -0.00004 O15 1 0.712604 -0.504965 0.078852 11.00000 0.01394 0.02576 = 0.01942 0.00187 0.00271 -0.00349 O16 1 -0.083253 0.464426 0.285770 11.00000 0.01996 0.02640 = 0.01522 -0.00497 0.00312 -0.00028 OW1 1 -0.410133 0.117830 0.278748 11.00000 0.03642 0.01542 = 0.02051 0.00319 -0.00374 -0.00201 OW2 1 0.217769 0.363918 0.109219 11.00000 0.02898 0.02743 = 0.04444 -0.00019 -0.01621 -0.01389 OW3 1 0.262213 0.045761 0.238464 61.00000 0.04295 0.02668 = 0.01087 0.00412 0.00207 -0.01236 OW4 1 -0.261528 -0.198704 0.229792 71.00000 0.01350 0.03513 = 0.04094 0.00218 0.00436 0.01136 HKLF 4 REM a in P2(1) REM wR2 = 0.1484, GooF = S = 1.134, Restrained GooF = 1.134 for all data REM R1 = 0.0531 for 5639 Fo > 4sig(Fo) and 0.0578 for all 6067 data REM 297 parameters refined using 1 restraints END WGHT 0.0716 8.6634 REM Highest difference peak 2.100, deepest hole -1.221, 1-sigma level 0.338 Q1 1 -0.2671 -0.1642 0.0970 11.00000 0.05 2.10 Q2 1 0.4168 0.0907 0.2450 11.00000 0.05 1.95 Q3 1 0.2709 0.3701 0.0759 11.00000 0.05 1.87 Q4 1 0.3021 0.3651 0.4270 11.00000 0.05 1.74 Q5 1 -0.3995 0.1624 0.2374 11.00000 0.05 1.74 Q6 1 0.0747 -0.1174 -0.1089 11.00000 0.05 1.70 Q7 1 0.2527 0.1150 0.2592 11.00000 0.05 1.63 Q8 1 0.4219 -0.2100 0.4222 11.00000 0.05 1.58 Q9 1 -0.1603 0.1496 0.2578 11.00000 0.05 1.56 Q10 1 0.0721 -0.3832 0.4270 11.00000 0.05 1.51 Q11 1 0.2115 0.2996 0.3960 11.00000 0.05 1.50 Q12 1 0.4027 -0.2481 0.1069 11.00000 0.05 1.50 Q13 1 0.4246 -0.3861 0.0763 11.00000 0.05 1.49 Q14 1 -0.3988 0.0832 0.2368 11.00000 0.05 1.47 Q15 1 0.4198 -0.1006 0.5831 11.00000 0.05 1.47 Q16 1 -0.1176 0.2180 0.2769 11.00000 0.05 1.46 Q17 1 -0.4251 0.1250 0.2263 11.00000 0.05 1.45 Q18 1 0.2660 0.4428 0.4307 11.00000 0.05 1.44 Q19 1 -0.0796 0.1201 0.1963 11.00000 0.05 1.42 Q20 1 0.0745 -0.1368 0.3764 11.00000 0.05 1.42 ; _shelx_res_checksum 37998 _shelx_hkl_file ; 0 -16 0 25767.6 2271.16 7 0 -16 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3724.64 953.141 4 -14 6 2 18669.9 2002.15 6 -14 6 2 19692.4 1888.68 4 -14 6 1 21279.1 2193.40 6 -14 6 1 20396.3 1914.41 4 -14 6 0 4441.51 1229.83 6 -14 7 3 3389.38 983.330 6 -14 7 3 2857.37 872.653 4 -14 7 2 2109.04 700.158 4 -14 7 2 57.4791 729.996 6 -14 7 1 1439.91 655.079 4 -15 -6 1 6072.59 1258.16 6 -15 -6 0 1820.80 887.012 6 -15 -6 -1 3356.15 1028.32 6 -15 -6 -2 5580.46 1229.20 6 -15 -6 -3 3023.96 857.458 6 -15 -5 2 6281.51 1250.57 6 -15 -5 1 4118.17 1086.30 6 -15 -5 0 2111.44 919.660 6 15 -5 1-844.190 1036.39 5 -15 -5 -1 69.9485 575.623 6 15 -5 2 4762.61 1383.17 5 -15 -5 -2 4949.08 1190.18 6 -15 -5 -3-510.348 781.965 6 -15 -5 -4 1804.54 717.585 6 -15 -4 3 418.559 591.235 6 -15 -4 2 635.694 695.489 6 -15 -4 1 472.184 630.870 6 -15 -4 0 18004.7 2041.78 6 -15 -4 -1 6483.00 1295.71 6 15 -4 2-1304.01 1179.89 5 -15 -4 -2-210.391 877.703 6 15 -4 3 447.785 926.389 5 -15 -4 -3 161.102 700.528 6 15 -4 4 4049.04 1331.38 5 -15 -4 -4 11.9502 798.381 6 -15 -4 -5-901.642 792.389 6 -15 -3 4 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5 4190.91 1003.67 6 -15 2 4 14069.0 1813.88 6 -15 2 4 14952.9 1616.99 4 -15 2 3 1935.24 755.033 4 -15 2 3 2115.58 900.502 6 -15 2 2 2440.71 856.590 6 -15 2 1 4828.58 1162.54 6 -15 2 0 3567.55 1039.86 6 -15 2 -1 1912.20 854.933 6 -15 2 -2 15487.5 2019.24 6 -15 2 -3 5693.99 1315.15 6 -15 2 -4 4074.79 1327.28 6 -15 3 5 2290.19 845.355 6 -15 3 5 911.835 558.030 4 -15 3 4 1403.07 597.125 4 -15 3 4 1291.42 790.266 6 -15 3 3 7711.61 1240.17 4 -15 3 3 6520.01 1389.19 6 -15 3 2 3322.73 911.062 6 -15 3 1 3824.28 1025.89 6 -15 3 0 741.845 648.613 6 -15 3 -1 5202.35 1345.42 6 -15 3 -2 2612.28 1070.41 6 -15 3 -3 4296.87 1428.81 6 -15 4 5 1835.04 617.330 6 -15 4 4 1435.39 752.470 6 -15 4 3 449.607 573.636 4 -15 4 3-257.296 729.780 6 -15 4 2 447.199 519.728 4 -15 4 2 1150.20 725.660 6 -15 4 1 219.791 754.148 6 -15 4 0 16272.2 2032.47 6 -15 4 -1 6777.33 1439.65 6 -15 4 -2 1035.27 947.173 6 -15 5 4 1436.58 694.266 6 -15 5 3 4652.37 1118.46 6 -15 5 2 6133.84 1128.55 4 -15 5 2 6602.75 1362.69 6 -15 5 1 2122.48 1028.46 6 -15 5 0 2450.05 996.711 6 -15 5 -1-371.768 787.032 6 -15 6 3 2148.50 871.611 6 -15 6 2 2565.28 999.825 6 -15 6 1 4597.48 1255.68 6 -15 6 0 2758.32 1099.16 6 0 0 0 0.00 0.00 0 TITL CHYKO1_100 in P2(1) REM P2(1) (#4 in standard setting) CELL 0.71073 10.034868 10.053412 10.058580 90.0000 90.4741 90.0000 ZERR 3.00 0.000340 0.000379 0.000383 0.0000 0.0031 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H O Cs UNIT 30.00 12.00 36.00 3.00 TREF HKLF 4 END ; _shelx_hkl_checksum 37651