data_CMN02 _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 'Ca0.03 H Mn1.98 Na O9 Si3' _chemical_formula_weight 361.78 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' 'H' 'H' 0.0000 0.0000 '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' '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' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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' _cell_length_a 7.6975(5) _cell_length_b 6.8875(5) _cell_length_c 6.7294(5) _cell_angle_alpha 90.296(3) _cell_angle_beta 93.990(3) _cell_angle_gamma 102.849(3) _cell_volume 346.91(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.463 _exptl_crystal_F_000 352 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 4.229 _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 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2277 _diffrn_reflns_av_unetI/netI 0.0122 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.721 _diffrn_reflns_theta_max 32.060 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.940 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.940 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.940 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 2277 _reflns_number_gt 2084 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _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 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^)+(0.0248P)^2^+0.1498P] 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 none _refine_ls_extinction_coef . _refine_ls_number_reflns 2277 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0208 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0485 _refine_ls_wR_factor_gt 0.0476 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _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 Na1 Na 0.55635(9) 0.25618(14) 0.35355(11) 0.01513(14) Uani 1 1 d . . . . . M1MN Mn 0.85291(3) 0.59425(7) 0.13463(4) 0.00884(7) Uani 0.975(6) 1 d . . P . . M1CA Ca 0.85291(3) 0.59425(7) 0.13463(4) 0.00884(7) Uani 0.025(6) 1 d . . P . . M2MN Mn 0.84885(3) 0.08382(7) 0.13275(3) 0.00816(7) Uani 1 1 d . . . . . Si1 Si 0.21473(6) 0.40125(8) 0.34258(7) 0.00698(11) Uani 1 1 d . . . . . Si2 Si 0.20587(6) 0.95078(9) 0.35060(7) 0.00651(11) Uani 1 1 d . . . . . Si3 Si 0.45412(5) 0.73724(8) 0.14342(6) 0.00655(8) Uani 1 1 d . . . . . O1 O 0.66421(15) 0.7939(3) 0.11413(17) 0.0101(2) Uani 1 1 d . . . . . O2 O 0.32246(15) 0.7063(3) 0.94386(16) 0.0099(2) Uani 1 1 d . . . . . O3 O 0.1780(2) 0.4913(2) 0.5555(2) 0.0101(3) Uani 1 1 d . . . . . O4 O 0.15983(19) 0.8446(2) 0.5571(2) 0.0106(2) Uani 1 1 d . . . . . O5 O 0.06129(15) 0.3917(4) 0.16758(16) 0.0099(2) Uani 1 1 d . . . . . O6 O 0.05190(15) 0.8912(4) 0.17231(17) 0.0094(2) Uani 1 1 d . . . . . O7 O 0.40701(18) 0.53418(19) 0.2776(2) 0.0104(3) Uani 1 1 d . . . . . O8 O 0.39717(18) 0.9061(2) 0.2869(2) 0.0106(2) Uani 1 1 d . . . . . O9 O 0.25903(15) 0.1886(2) 0.39305(17) 0.0100(2) Uani 1 1 d . . . . . H1 H 0.160(8) 0.565(9) 0.554(9) 0.015 Uiso 0.5 1 d . U P . . H2 H 0.143(7) 0.663(9) 0.564(7) 0.015 Uiso 0.5 1 d . U 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 Na1 0.0107(3) 0.0174(4) 0.0172(3) 0.0009(4) 0.0028(2) 0.0024(3) M1MN 0.00959(12) 0.00832(15) 0.00893(12) 0.0005(2) 0.00110(8) 0.0026(2) M1CA 0.00959(12) 0.00832(15) 0.00893(12) 0.0005(2) 0.00110(8) 0.0026(2) M2MN 0.00856(11) 0.00821(14) 0.00858(11) 0.0003(2) 0.00086(8) 0.0036(2) Si1 0.00732(19) 0.0061(3) 0.00779(19) 0.00044(16) 0.00008(15) 0.00215(17) Si2 0.00740(19) 0.0052(3) 0.00724(19) 0.00008(17) 0.00023(14) 0.00223(17) Si3 0.00619(17) 0.00663(19) 0.00715(17) 0.00012(19) 0.00042(13) 0.00212(19) O1 0.0075(5) 0.0096(5) 0.0133(5) 0.0005(7) 0.0018(4) 0.0019(6) O2 0.0102(5) 0.0110(5) 0.0086(5) -0.0004(7) -0.0004(4) 0.0031(6) O3 0.0131(6) 0.0096(6) 0.0088(6) -0.0009(5) 0.0008(5) 0.0049(5) O4 0.0148(6) 0.0077(5) 0.0094(6) 0.0015(4) 0.0022(5) 0.0026(5) O5 0.0092(5) 0.0113(6) 0.0086(5) 0.0001(9) -0.0008(4) 0.0015(8) O6 0.0086(5) 0.0102(6) 0.0095(5) -0.0018(9) -0.0008(4) 0.0026(8) O7 0.0087(6) 0.0084(5) 0.0137(6) 0.0040(4) 0.0011(5) 0.0011(4) O8 0.0086(6) 0.0114(5) 0.0124(6) -0.0035(5) 0.0001(5) 0.0038(5) O9 0.0110(5) 0.0061(5) 0.0132(5) 0.0004(5) 0.0000(4) 0.0029(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 Na1 O2 2.2585(13) 2_666 ? Na1 O9 2.2665(13) . ? Na1 O3 2.4112(17) 2_666 ? Na1 O4 2.4724(16) 2_666 ? Na1 O8 2.4725(16) 1_545 ? Na1 O7 2.4811(16) . ? Na1 O8 2.7050(16) 2_666 ? Na1 O7 2.8300(16) 2_666 ? Na1 Si1 3.0101(9) . ? Na1 Si2 3.0284(9) 1_545 ? Na1 Si2 3.1667(10) 2_666 ? Na1 M2MN 3.2129(8) . ? M1MN O5 2.1777(11) 2_665 ? M1MN O3 2.1840(15) 2_666 ? M1MN O1 2.2095(19) . ? M1MN O2 2.244(2) 2_666 ? M1MN O6 2.268(2) 1_655 ? M1MN O5 2.349(2) 1_655 ? M2MN O4 2.1512(14) 2_666 ? M2MN O1 2.176(2) 1_545 ? M2MN O2 2.203(2) 2_666 ? M2MN O6 2.2341(12) 2_665 ? M2MN O6 2.267(2) 1_645 ? M2MN O5 2.371(2) 1_655 ? Si1 O5 1.5991(12) . ? Si1 O9 1.6089(15) . ? Si1 O3 1.6261(15) . ? Si1 O7 1.6466(14) . ? Si2 O4 1.5983(14) . ? Si2 O6 1.6103(12) . ? Si2 O9 1.6163(16) 1_565 ? Si2 O8 1.6536(14) . ? Si3 O1 1.6034(12) . ? Si3 O2 1.6086(12) 1_554 ? Si3 O7 1.6541(14) . ? Si3 O8 1.6590(14) . ? 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 Na1 O9 124.51(5) 2_666 . ? O2 Na1 O3 80.31(6) 2_666 2_666 ? O9 Na1 O3 139.77(6) . 2_666 ? O2 Na1 O4 80.40(5) 2_666 2_666 ? O9 Na1 O4 144.93(6) . 2_666 ? O3 Na1 O4 60.70(4) 2_666 2_666 ? O2 Na1 O8 94.76(7) 2_666 1_545 ? O9 Na1 O8 64.56(5) . 1_545 ? O3 Na1 O8 152.22(6) 2_666 1_545 ? O4 Na1 O8 91.55(5) 2_666 1_545 ? O2 Na1 O7 89.93(7) 2_666 . ? O9 Na1 O7 64.79(5) . . ? O3 Na1 O7 86.55(5) 2_666 . ? O4 Na1 O7 146.88(6) 2_666 . ? O8 Na1 O7 120.95(5) 1_545 . ? O2 Na1 O8 140.41(6) 2_666 2_666 ? O9 Na1 O8 88.14(5) . 2_666 ? O3 Na1 O8 87.72(5) 2_666 2_666 ? O4 Na1 O8 61.01(5) 2_666 2_666 ? O8 Na1 O8 78.75(5) 1_545 2_666 ? O7 Na1 O8 127.09(5) . 2_666 ? O2 Na1 O7 138.11(7) 2_666 2_666 ? O9 Na1 O7 85.53(5) . 2_666 ? O3 Na1 O7 59.65(5) 2_666 2_666 ? O4 Na1 O7 89.47(5) 2_666 2_666 ? O8 Na1 O7 126.28(5) 1_545 2_666 ? O7 Na1 O7 76.75(5) . 2_666 ? O8 Na1 O7 55.52(4) 2_666 2_666 ? O2 Na1 Si1 111.17(5) 2_666 . ? O9 Na1 Si1 31.70(4) . . ? O3 Na1 Si1 114.44(5) 2_666 . ? O4 Na1 Si1 167.17(5) 2_666 . ? O8 Na1 Si1 92.91(4) 1_545 . ? O7 Na1 Si1 33.15(3) . . ? O8 Na1 Si1 108.16(4) 2_666 . ? O7 Na1 Si1 78.19(3) 2_666 . ? O2 Na1 Si2 114.39(5) 2_666 1_545 ? O9 Na1 Si2 31.57(4) . 1_545 ? O3 Na1 Si2 165.29(5) 2_666 1_545 ? O4 Na1 Si2 119.77(5) 2_666 1_545 ? O8 Na1 Si2 33.06(3) 1_545 1_545 ? O7 Na1 Si2 93.11(4) . 1_545 ? O8 Na1 Si2 80.76(4) 2_666 1_545 ? O7 Na1 Si2 105.95(4) 2_666 1_545 ? Si1 Na1 Si2 61.534(18) . 1_545 ? O2 Na1 Si2 109.15(5) 2_666 2_666 ? O9 Na1 Si2 116.85(4) . 2_666 ? O3 Na1 Si2 74.44(4) 2_666 2_666 ? O4 Na1 Si2 29.81(3) 2_666 2_666 ? O8 Na1 Si2 81.61(4) 1_545 2_666 ? O7 Na1 Si2 149.84(5) . 2_666 ? O8 Na1 Si2 31.48(3) 2_666 2_666 ? O7 Na1 Si2 73.47(3) 2_666 2_666 ? Si1 Na1 Si2 139.62(3) . 2_666 ? Si2 Na1 Si2 99.48(3) 1_545 2_666 ? O2 Na1 M2MN 43.26(5) 2_666 . ? O9 Na1 M2MN 140.84(5) . . ? O3 Na1 M2MN 79.34(4) 2_666 . ? O4 Na1 M2MN 41.99(3) 2_666 . ? O8 Na1 M2MN 78.56(4) 1_545 . ? O7 Na1 M2MN 132.56(4) . . ? O8 Na1 M2MN 97.56(4) 2_666 . ? O7 Na1 M2MN 129.22(4) 2_666 . ? Si1 Na1 M2MN 150.83(3) . . ? Si2 Na1 M2MN 111.07(3) 1_545 . ? Si2 Na1 M2MN 67.274(19) 2_666 . ? O5 M1MN O3 161.09(8) 2_665 2_666 ? O5 M1MN O1 100.79(7) 2_665 . ? O3 M1MN O1 98.07(5) 2_666 . ? O5 M1MN O2 88.52(7) 2_665 2_666 ? O3 M1MN O2 85.77(5) 2_666 2_666 ? O1 M1MN O2 103.21(5) . 2_666 ? O5 M1MN O6 83.16(7) 2_665 1_655 ? O3 M1MN O6 101.31(5) 2_666 1_655 ? O1 M1MN O6 80.98(6) . 1_655 ? O2 M1MN O6 171.29(4) 2_666 1_655 ? O5 M1MN O5 80.49(7) 2_665 1_655 ? O3 M1MN O5 80.73(5) 2_666 1_655 ? O1 M1MN O5 177.42(5) . 1_655 ? O2 M1MN O5 79.01(6) 2_666 1_655 ? O6 M1MN O5 96.99(4) 1_655 1_655 ? O5 M1MN Na1 131.30(6) 2_665 . ? O3 M1MN Na1 46.76(4) 2_666 . ? O1 M1MN Na1 90.22(5) . . ? O2 M1MN Na1 42.89(3) 2_666 . ? O6 M1MN Na1 145.53(3) 1_655 . ? O5 M1MN Na1 90.59(5) 1_655 . ? O4 M2MN O1 99.81(5) 2_666 1_545 ? O4 M2MN O2 89.21(5) 2_666 2_666 ? O1 M2MN O2 103.80(5) 1_545 2_666 ? O4 M2MN O6 157.80(7) 2_666 2_665 ? O1 M2MN O6 101.82(7) 1_545 2_665 ? O2 M2MN O6 90.48(7) 2_666 2_665 ? O4 M2MN O6 97.14(5) 2_666 1_645 ? O1 M2MN O6 81.71(6) 1_545 1_645 ? O2 M2MN O6 170.83(5) 2_666 1_645 ? O6 M2MN O6 81.14(7) 2_665 1_645 ? O4 M2MN O5 78.49(5) 2_666 1_655 ? O1 M2MN O5 176.48(5) 1_545 1_655 ? O2 M2MN O5 79.33(6) 2_666 1_655 ? O6 M2MN O5 79.64(7) 2_665 1_655 ? O6 M2MN O5 95.40(4) 1_645 1_655 ? O4 M2MN Na1 50.26(4) 2_666 . ? O1 M2MN Na1 88.67(4) 1_545 . ? O2 M2MN Na1 44.63(3) 2_666 . ? O6 M2MN Na1 134.96(6) 2_665 . ? O6 M2MN Na1 143.90(3) 1_645 . ? O5 M2MN Na1 92.53(5) 1_655 . ? O4 M2MN M1CA 103.20(4) 2_666 1_545 ? O1 M2MN M1CA 39.96(4) 1_545 1_545 ? O2 M2MN M1CA 142.76(5) 2_666 1_545 ? O6 M2MN M1CA 90.32(7) 2_665 1_545 ? O6 M2MN M1CA 41.83(6) 1_645 1_545 ? O5 M2MN M1CA 137.22(5) 1_655 1_545 ? Na1 M2MN M1CA 121.835(19) . 1_545 ? O5 Si1 O9 113.81(12) . . ? O5 Si1 O3 115.93(9) . . ? O9 Si1 O3 104.96(7) . . ? O5 Si1 O7 110.94(8) . . ? O9 Si1 O7 103.12(7) . . ? O3 Si1 O7 107.06(8) . . ? O5 Si1 Na1 130.64(8) . . ? O9 Si1 Na1 47.75(5) . . ? O3 Si1 Na1 113.31(6) . . ? O7 Si1 Na1 55.49(5) . . ? O5 Si1 Na1 135.26(11) . 2_666 ? O9 Si1 Na1 110.77(5) . 2_666 ? O3 Si1 Na1 46.16(6) . 2_666 ? O7 Si1 Na1 61.04(5) . 2_666 ? Na1 Si1 Na1 83.71(3) . 2_666 ? O4 Si2 O6 115.02(9) . . ? O4 Si2 O9 107.89(7) . 1_565 ? O6 Si2 O9 111.69(12) . 1_565 ? O4 Si2 O8 108.29(7) . . ? O6 Si2 O8 111.29(8) . . ? O9 Si2 O8 101.76(7) 1_565 . ? O4 Si2 Na1 116.21(6) . 1_565 ? O6 Si2 Na1 128.61(8) . 1_565 ? O9 Si2 Na1 47.24(5) 1_565 1_565 ? O8 Si2 Na1 54.67(5) . 1_565 ? O4 Si2 Na1 50.27(5) . 2_666 ? O6 Si2 Na1 139.36(11) . 2_666 ? O9 Si2 Na1 108.95(5) 1_565 2_666 ? O8 Si2 Na1 58.67(5) . 2_666 ? Na1 Si2 Na1 80.52(3) 1_565 2_666 ? O1 Si3 O2 116.56(6) . 1_554 ? O1 Si3 O7 109.50(9) . . ? O2 Si3 O7 108.83(9) 1_554 . ? O1 Si3 O8 110.72(9) . . ? O2 Si3 O8 107.95(9) 1_554 . ? O7 Si3 O8 102.31(6) . . ? O1 Si3 Na1 80.12(5) . 2_665 ? O2 Si3 Na1 36.44(4) 1_554 2_665 ? O7 Si3 Na1 125.13(6) . 2_665 ? O8 Si3 Na1 125.18(6) . 2_665 ? O1 Si3 Na1 102.51(5) . 2_666 ? O2 Si3 Na1 140.87(5) 1_554 2_666 ? O7 Si3 Na1 56.26(5) . 2_666 ? O8 Si3 Na1 51.92(5) . 2_666 ? Na1 Si3 Na1 176.57(3) 2_665 2_666 ? Si3 O1 M2MN 129.49(12) . 1_565 ? Si3 O1 M1MN 127.50(13) . . ? M2MN O1 M1MN 100.81(5) 1_565 . ? Si3 O2 M2MN 121.17(11) 1_556 2_666 ? Si3 O2 M1MN 120.09(11) 1_556 2_666 ? M2MN O2 M1MN 104.19(5) 2_666 2_666 ? Si3 O2 Na1 118.53(6) 1_556 2_666 ? M2MN O2 Na1 92.12(7) 2_666 2_666 ? M1MN O2 Na1 94.57(6) 2_666 2_666 ? Si1 O3 M1MN 140.69(8) . 2_666 ? Si1 O3 Na1 104.74(7) . 2_666 ? M1MN O3 Na1 91.95(6) 2_666 2_666 ? Si2 O4 M2MN 140.51(8) . 2_666 ? Si2 O4 Na1 99.92(7) . 2_666 ? M2MN O4 Na1 87.75(5) 2_666 2_666 ? Si1 O5 M1MN 116.07(7) . 2_665 ? Si1 O5 M1MN 127.08(13) . 1_455 ? M1MN O5 M1MN 99.51(7) 2_665 1_455 ? Si1 O5 M2MN 114.97(13) . 1_455 ? M1MN O5 M2MN 97.85(8) 2_665 1_455 ? M1MN O5 M2MN 96.02(4) 1_455 1_455 ? Si2 O6 M2MN 114.52(6) . 2_665 ? Si2 O6 M2MN 117.57(13) . 1_465 ? M2MN O6 M2MN 98.86(7) 2_665 1_465 ? Si2 O6 M1MN 125.45(13) . 1_455 ? M2MN O6 M1MN 99.34(7) 2_665 1_455 ? M2MN O6 M1MN 96.34(4) 1_465 1_455 ? Si1 O7 Si3 131.06(8) . . ? Si1 O7 Na1 91.36(6) . . ? Si3 O7 Na1 134.55(7) . . ? Si1 O7 Na1 88.35(6) . 2_666 ? Si3 O7 Na1 94.66(6) . 2_666 ? Na1 O7 Na1 103.25(5) . 2_666 ? Si2 O8 Si3 134.88(9) . . ? Si2 O8 Na1 92.27(6) . 1_565 ? Si3 O8 Na1 128.18(7) . 1_565 ? Si2 O8 Na1 89.85(6) . 2_666 ? Si3 O8 Na1 99.21(6) . 2_666 ? Na1 O8 Na1 101.25(5) 1_565 2_666 ? Si1 O9 Si2 146.59(8) . 1_545 ? Si1 O9 Na1 100.55(7) . . ? Si2 O9 Na1 101.19(7) 1_545 . ? _refine_diff_density_max 0.436 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.093 _shelx_res_file ; TITL al3_4i in P-1 CMN02.res created by SHELXL-2018/3 at 01:44:47 on 21-Aug-2020 CELL 0.71073 7.69750 6.88750 6.72940 90.2958 93.9903 102.8491 ZERR 2.00 0.00050 0.00050 0.00050 0.0030 0.0027 0.0028 LATT 1 SFAC O H NA SI MN CA UNIT 18 2 2 6 3.95 0.05 TEMP 25 ACTA L.S. 18 BOND FMAP 2 PLAN 20 EXYZ M1MN M1CA EADP M1MN M1CA WGHT 0.024800 0.149800 BASF 0.41922 FVAR 0.64717 0.97469 NA1 3 0.556346 0.256185 0.353549 11.00000 0.01072 0.01742 = 0.01717 0.00088 0.00279 0.00241 M1MN 5 0.852909 0.594246 0.134634 21.00000 0.00959 0.00832 = 0.00893 0.00049 0.00110 0.00256 M1CA 6 0.852909 0.594246 0.134634 -21.00000 0.00959 0.00832 = 0.00893 0.00049 0.00110 0.00256 M2MN 5 0.848846 0.083824 0.132753 11.00000 0.00856 0.00821 = 0.00858 0.00031 0.00086 0.00365 SI1 4 0.214728 0.401253 0.342579 11.00000 0.00732 0.00606 = 0.00779 0.00044 0.00008 0.00215 SI2 4 0.205869 0.950778 0.350599 11.00000 0.00740 0.00522 = 0.00724 0.00008 0.00023 0.00223 SI3 4 0.454118 0.737240 0.143421 11.00000 0.00619 0.00663 = 0.00715 0.00012 0.00042 0.00212 O1 1 0.664211 0.793888 0.114135 11.00000 0.00751 0.00958 = 0.01334 0.00050 0.00177 0.00193 O2 1 0.322457 0.706341 0.943860 11.00000 0.01016 0.01101 = 0.00858 -0.00040 -0.00043 0.00308 O3 1 0.177978 0.491327 0.555549 11.00000 0.01310 0.00958 = 0.00877 -0.00092 0.00084 0.00490 O4 1 0.159826 0.844599 0.557064 11.00000 0.01483 0.00773 = 0.00942 0.00154 0.00222 0.00262 O5 1 0.061290 0.391650 0.167585 11.00000 0.00920 0.01130 = 0.00860 0.00014 -0.00079 0.00148 O6 1 0.051900 0.891233 0.172310 11.00000 0.00859 0.01024 = 0.00946 -0.00182 -0.00079 0.00264 O7 1 0.407009 0.534176 0.277620 11.00000 0.00867 0.00845 = 0.01372 0.00401 0.00110 0.00111 O8 1 0.397170 0.906147 0.286923 11.00000 0.00865 0.01140 = 0.01238 -0.00347 0.00009 0.00377 O9 1 0.259032 0.188573 0.393046 11.00000 0.01105 0.00615 = 0.01316 0.00040 0.00005 0.00294 H1 2 0.159756 0.565123 0.554264 10.50000 10.01500 H2 2 0.143473 0.662770 0.563823 10.50000 10.01500 HKLF 5 REM al3_4i in P-1 REM wR2 = 0.048471, GooF = S = 1.10281, Restrained GooF = 1.10281 for all data REM R1 = 0.017965 for 2084 Fo > 4sig(Fo) and 0.020768 for all 2277 data REM 144 parameters refined using 0 restraints END WGHT 0.0248 0.1498 REM Highest difference peak 0.436, deepest hole -0.573, 1-sigma level 0.093 Q1 1 0.9126 0.1470 0.1458 11.00000 0.05 0.44 Q2 1 0.1723 0.8640 0.4422 11.00000 0.05 0.40 Q3 1 0.1649 0.4166 0.4721 11.00000 0.05 0.40 Q4 1 0.8259 0.0794 0.2264 11.00000 0.05 0.39 Q5 1 0.8840 0.6161 0.0366 11.00000 0.05 0.37 Q6 1 0.3190 0.9254 0.2897 11.00000 0.05 0.37 Q7 1 0.1432 0.9191 0.2242 11.00000 0.05 0.36 Q8 1 0.8430 0.0726 0.0398 11.00000 0.05 0.36 Q9 1 0.7960 0.5326 0.1332 11.00000 0.05 0.36 Q10 1 0.3519 0.7337 1.0417 11.00000 0.05 0.35 Q11 1 0.4333 0.7210 1.0038 11.00000 0.05 0.33 Q12 1 0.3368 0.4990 0.3157 11.00000 0.05 0.33 Q13 1 0.0981 0.4088 0.2778 11.00000 0.05 0.33 Q14 1 0.1147 0.3977 0.0973 11.00000 0.05 0.33 Q15 1 0.2091 0.9184 0.4890 11.00000 0.05 0.32 Q16 1 0.3707 0.7917 0.9127 11.00000 0.05 0.32 Q17 1 0.3172 0.4821 0.2558 11.00000 0.05 0.30 Q18 1 0.4361 0.6258 0.2536 11.00000 0.05 0.30 Q19 1 0.0950 0.9227 0.0888 11.00000 0.05 0.29 Q20 1 0.4403 0.9627 0.3005 11.00000 0.05 0.28 ; _shelx_res_checksum 40677 _shelx_hkl_file ; 1 0 0 378.105 2.09134 -2 1 0 0 378.105 2.09134 1 2 0 0 849.650 4.21646 -2 2 0 0 849.650 4.21646 1 3 0 0 3963.02 17.2288 -2 3 0 0 3963.02 17.2288 1 4 0 0 865.853 4.61603 -2 4 0 0 865.853 4.61603 1 5 0 0 511.201 3.22164 -2 5 0 0 511.201 3.22164 1 6 0 0 346.144 2.90245 -2 6 0 0 346.144 2.90245 1 7 0 0 295.702 2.70258 -2 7 0 0 295.702 2.70258 1 8 0 0 161.656 2.26770 -2 8 0 0 161.656 2.26770 1 9 0 0 1.18699 0.72897 -2 9 0 0 1.18699 0.72897 1 10 0 0 375.986 5.00091 -2 10 0 0 375.986 5.00091 1 11 0 0 114.162 8.16486 -2 11 0 0 114.162 8.16486 1 -11 1 0 3.62522 1.24185 1 -10 1 0 2.32123 0.88634 1 -9 1 0 6.32392 1.00320 1 -8 1 0 0.46622 0.66455 1 -7 1 0 140.267 2.58339 1 -6 1 0 195.406 2.55926 1 -5 1 0 37.0796 1.08242 1 -4 1 0 353.453 2.93301 1 -3 1 0 488.841 3.61861 1 -2 1 0 88.2775 0.95008 1 -1 1 0 12.4304 0.34269 1 0 1 0 1.17318 0.15498 1 1 1 0 40.9931 0.49435 1 2 1 0 224.552 1.65876 1 3 1 0 546.723 3.09899 1 4 1 0 248.478 2.07565 1 5 1 0 72.3013 1.13707 1 6 1 0 52.9160 0.99969 1 7 1 0 99.3659 1.42564 1 8 1 0 0.13942 0.43366 1 9 1 0 8.75930 1.03680 1 10 1 0 4.65651 1.19373 1 10 2 0 62.6286 4.18717 -2 -11 2 0 62.6286 4.18717 1 9 2 0 40.1166 1.84280 -2 -10 2 0 40.1166 1.84280 1 8 2 0 488.095 5.73943 -2 -9 2 0 488.095 5.73943 1 7 2 0 64.2770 2.05130 -2 -8 2 0 64.2770 2.05130 1 6 2 0 167.052 2.84838 -2 -7 2 0 167.052 2.84838 1 5 2 0 13.7630 1.04621 -2 -6 2 0 13.7630 1.04621 1 4 2 0 2285.33 13.3600 -2 -5 2 0 2285.33 13.3600 1 3 2 0 155.168 1.83393 -2 -4 2 0 155.168 1.83393 1 2 2 0 2371.71 10.1081 -2 -3 2 0 2371.71 10.1081 1 1 2 0 9999.99 39.6557 -2 -2 2 0 9999.99 39.6557 1 0 2 0 218.723 1.57748 -2 -1 2 0 218.723 1.57748 1 -1 2 0 205.846 1.39786 -2 0 2 0 205.846 1.39786 1 -2 2 0 9688.26 38.1979 -2 1 2 0 9688.26 38.1979 1 -3 2 0 2276.58 10.9344 -2 2 2 0 2276.58 10.9344 1 -4 2 0 139.900 1.55333 -2 3 2 0 139.900 1.55333 1 -5 2 0 2168.02 10.5476 -2 4 2 0 2168.02 10.5476 1 -6 2 0 14.1422 0.84772 -2 5 2 0 14.1422 0.84772 1 -7 2 0 162.773 2.14759 -2 6 2 0 162.773 2.14759 1 -8 2 0 50.8315 1.14217 -2 7 2 0 50.8315 1.14217 1 -9 2 0 446.799 3.55166 -2 8 2 0 446.799 3.55166 1 -10 2 0 34.0025 1.59127 -2 9 2 0 34.0025 1.59127 1 -11 2 0 67.7936 3.32625 -2 10 2 0 67.7936 3.32625 1 -11 3 0 3.59858 1.81005 1 -10 3 0 23.8720 2.04911 1 -9 3 0 106.963 3.22132 1 -8 3 0 186.265 3.31432 1 -7 3 0 7.46953 0.93267 1 -6 3 0 153.278 2.31707 1 -5 3 0 175.403 2.50794 1 -4 3 0 10.2147 0.61556 1 -3 3 0 5.16181 0.44803 1 -2 3 0 1.04406 0.34047 1 -1 3 0 0.55757 0.27082 1 0 3 0 35.2001 0.69779 1 1 3 0 4.64182 0.40581 1 2 3 0 11.0416 0.62475 1 3 3 0 85.3885 1.42683 1 4 3 0 117.015 1.81248 1 5 3 0 124.876 1.93683 1 6 3 0 115.992 1.94760 1 7 3 0 86.0128 1.95775 1 8 3 0 35.0445 1.53464 1 9 3 0 7.80669 1.23983 1 8 4 0 23.1520 2.26386 -2 -10 4 0 23.1520 2.26386 1 7 4 0 66.3258 2.76051 -2 -9 4 0 66.3258 2.76051 1 6 4 0 177.170 3.81264 -2 -8 4 0 177.170 3.81264 1 5 4 0 206.811 3.79393 -2 -7 4 0 206.811 3.79393 1 4 4 0 33.2147 1.30876 -2 -6 4 0 33.2147 1.30876 1 3 4 0 155.782 2.19633 -2 -5 4 0 155.782 2.19633 1 2 4 0 1546.31 7.62784 -2 -4 4 0 1546.31 7.62784 1 1 4 0 179.744 1.91468 -2 -3 4 0 179.744 1.91468 1 0 4 0 195.421 1.95241 -2 -2 4 0 195.421 1.95241 1 -1 4 0 9951.26 41.4503 -2 -1 4 0 9951.26 41.4503 1 -2 4 0 199.017 1.94125 -2 0 4 0 199.017 1.94125 1 -3 4 0 156.837 1.73500 -2 1 4 0 156.837 1.73500 1 -4 4 0 1491.19 7.64118 -2 2 4 0 1491.19 7.64118 1 -5 4 0 137.623 2.08505 -2 3 4 0 137.623 2.08505 1 -6 4 0 26.4575 1.24639 -2 4 4 0 26.4575 1.24639 1 -7 4 0 196.256 2.71357 -2 5 4 0 196.256 2.71357 1 -8 4 0 157.567 3.32780 -2 6 4 0 157.567 3.32780 1 -9 4 0 61.1197 2.46971 -2 7 4 0 61.1197 2.46971 1 -10 4 0 27.7674 2.09636 -2 8 4 0 27.7674 2.09636 1 -11 4 0 348.608 11.2315 -2 9 4 0 348.608 11.2315 1 -10 5 0 2.37322 1.25297 1 -9 5 0 41.2901 2.52656 1 -8 5 0 90.4922 2.94488 1 -7 5 0 157.075 2.72241 1 -6 5 0 1.94553 0.68453 1 -5 5 0 132.464 2.06795 1 -4 5 0 523.883 4.44296 1 -3 5 0 78.0828 1.60747 1 -2 5 0 40.4074 1.07977 1 -1 5 0 22.5861 0.76026 1 0 5 0 0.88741 0.42704 1 1 5 0 392.369 3.23462 1 2 5 0 210.484 2.34076 1 3 5 0 13.4666 1.05666 1 4 5 0 83.6575 2.13798 1 5 5 0 62.0685 2.34000 1 6 5 0 14.5550 1.55484 1 7 5 0 1.32208 1.18189 1 8 5 0 0.02153 1.34050 1 7 6 0 265.531 7.44513 -2 -10 6 0 265.531 7.44513 1 6 6 0 16.3565 2.16649 -2 -9 6 0 16.3565 2.16649 1 5 6 0 36.8572 1.86734 -2 -8 6 0 36.8572 1.86734 1 4 6 0 91.7801 2.28770 -2 -7 6 0 91.7801 2.28770 1 3 6 0 248.063 3.36429 -2 -6 6 0 248.063 3.36429 1 2 6 0 16.9925 1.23014 -2 -5 6 0 16.9925 1.23014 1 1 6 0 338.259 3.32710 -2 -4 6 0 338.259 3.32710 1 0 6 0 2105.51 11.0310 -2 -3 6 0 2105.51 11.0310 1 -1 6 0 55.0301 1.27051 -2 -2 6 0 55.0301 1.27051 1 -2 6 0 60.7869 1.36230 -2 -1 6 0 60.7869 1.36230 1 -3 6 0 2002.53 9.79355 -2 0 6 0 2002.53 9.79355 1 -4 6 0 332.584 3.26437 -2 1 6 0 332.584 3.26437 1 -5 6 0 14.6568 1.05082 -2 2 6 0 14.6568 1.05082 1 -6 6 0 234.909 3.90425 -2 3 6 0 234.909 3.90425 1 -7 6 0 80.8378 2.64321 -2 4 6 0 80.8378 2.64321 1 -8 6 0 35.8997 2.19549 -2 5 6 0 35.8997 2.19549 1 -9 6 0 7.76573 1.76477 -2 6 6 0 7.76573 1.76477 1 -10 6 0 219.415 6.97611 -2 7 6 0 219.415 6.97611 1 -9 7 0 102.753 4.42338 1 -8 7 0 0.65767 1.00766 1 -7 7 0 14.9474 1.51031 1 -6 7 0 198.062 3.03186 1 -5 7 0 13.2221 1.08290 1 -4 7 0 40.2643 1.45168 1 -3 7 0 108.689 2.08742 1 -2 7 0 40.5125 1.43266 1 -1 7 0 148.392 2.17108 1 0 7 0 6.02274 0.73455 1 1 7 0 13.7863 1.02253 1 2 7 0 249.477 3.87666 1 3 7 0 45.2739 2.65299 1 4 7 0 0.98165 1.23825 1 5 7 0 70.5103 3.43069 1 6 7 0 28.6366 4.03601 1 4 8 0 114.552 4.35556 -2 -8 8 0 114.552 4.35556 1 3 8 0 39.0033 2.36943 -2 -7 8 0 39.0033 2.36943 1 2 8 0 32.2953 1.79198 -2 -6 8 0 32.2953 1.79198 1 1 8 0 272.146 3.70329 -2 -5 8 0 272.146 3.70329 1 0 8 0 9.33127 1.39450 -2 -4 8 0 9.33127 1.39450 1 -1 8 0 49.0882 1.79790 -2 -3 8 0 49.0882 1.79790 1 -2 8 0 1207.86 8.06128 -2 -2 8 0 1207.86 8.06128 1 -3 8 0 55.2290 1.86028 -2 -1 8 0 55.2290 1.86028 1 -4 8 0 8.08483 1.42525 -2 0 8 0 8.08483 1.42525 1 -5 8 0 289.724 4.37523 -2 1 8 0 289.724 4.37523 1 -6 8 0 30.9630 2.01217 -2 2 8 0 30.9630 2.01217 1 -7 8 0 36.1761 2.83508 -2 3 8 0 36.1761 2.83508 1 -8 8 0 92.8484 4.67174 -2 4 8 0 92.8484 4.67174 1 -7 9 0 0.05531 1.91704 1 -6 9 0 8.62887 1.18009 1 -5 9 0 171.650 2.90703 1 -4 9 0 17.6736 1.34624 1 -3 9 0 167.289 2.98946 1 -2 9 0 75.8668 2.38436 1 -1 9 0 74.2848 2.60480 1 0 9 0 219.725 4.61967 1 1 9 0 6.81072 1.27255 1 2 9 0 16.4246 1.66963 1 -1 10 0 397.767 9.09477 -2 -4 10 0 397.767 9.09477 1 -2 10 0 19.8250 4.24440 -2 -3 10 0 19.8250 4.24440 1 -3 10 1 130.253 8.18233 -2 2 -10 1 130.253 8.18233 1 -2 -9 1 11.7241 1.69254 1 -1 -9 1 22.4592 1.80384 1 0 -9 1 13.4239 1.52988 1 1 -9 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6.01638 0.87805 1 1 -7 1 3.64995 0.71046 1 2 -7 1 38.7098 1.30471 1 3 -7 1 0.70951 0.60322 1 4 -7 1 17.4838 1.09361 1 5 -7 1 19.6927 1.23366 1 6 -7 1 57.0323 1.84320 1 7 -7 1 40.3714 1.93452 1 8 -7 1 9.39120 1.57644 1 9 -7 1 55.8317 3.50658 1 -10 6 1 363.226 8.46401 -2 -7 -6 1 363.226 8.46401 1 -9 6 1 854.234 9.11993 -2 -6 -6 1 854.234 9.11993 1 -8 6 1 116.737 3.23587 -2 -5 -6 1 116.737 3.23587 1 -7 6 1 116.543 3.03322 -2 -4 -6 1 116.543 3.03322 1 -6 6 1 469.049 4.91948 -2 -3 -6 1 469.049 4.91948 1 -5 6 1 474.932 4.50132 -2 -2 -6 1 474.932 4.50132 1 -4 6 1 190.037 3.04521 -2 -1 -6 1 190.037 3.04521 1 -3 6 1 470.930 4.31105 -2 0 -6 1 470.930 4.31105 1 -2 6 1 146.151 1.98281 -2 1 -6 1 146.151 1.98281 1 -1 6 1 12.3582 1.02463 -2 2 -6 1 12.3582 1.02463 1 0 6 1 517.010 4.18229 -2 3 -6 1 517.010 4.18229 1 1 6 1 540.598 4.37953 -2 4 -6 1 540.598 4.37953 1 2 6 1 484.148 3.98424 -2 5 -6 1 484.148 3.98424 1 3 6 1 51.8235 1.70230 -2 6 -6 1 51.8235 1.70230 1 4 6 1 93.3335 2.61121 -2 7 -6 1 93.3335 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