data_KNR96 _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 'Ca0.90 H Mn1.11 Na O9 Si3' _chemical_formula_weight 348.85 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 7.83826(6) _cell_length_b 6.96973(6) _cell_length_c 6.90376(7) _cell_angle_alpha 90.7516(8) _cell_angle_beta 94.4374(7) _cell_angle_gamma 102.8940(7) _cell_volume 366.365(6) _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 3.162 _exptl_crystal_F_000 343 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 3.183 _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 31974 _diffrn_reflns_av_unetI/netI 0.0134 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.675 _diffrn_reflns_theta_max 35.313 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.928 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.928 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.928 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 3067 _reflns_number_gt 2965 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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-2018/3 (Sheldrick, 2018)' _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^)+(0.0310P)^2^+0.0999P] 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 3067 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0178 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0522 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.002 _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(5) 0.24471(7) 0.34917(7) 0.01720(9) Uani 1 1 d . . . . . M1MN Mn 0.84873(2) 0.59374(2) 0.14584(3) 0.00856(5) Uani 0.179(4) 1 d . . P . . M1CA Ca 0.84873(2) 0.59374(2) 0.14584(3) 0.00856(5) Uani 0.821(4) 1 d . . P . . M2MN Mn 0.85197(2) 0.08496(2) 0.13457(2) 0.00914(5) Uani 0.871(4) 1 d . . P . . M2CA Ca 0.85197(2) 0.08496(2) 0.13457(2) 0.00914(5) Uani 0.129(4) 1 d . . P . . Si1 Si 0.21972(3) 0.40701(3) 0.33581(4) 0.00685(6) Uani 1 1 d . . . . . Si2 Si 0.20655(3) 0.96037(3) 0.34968(4) 0.00696(6) Uani 1 1 d . . . . . Si3 Si 0.45078(3) 0.74673(3) 0.14285(4) 0.00688(6) Uani 1 1 d . . . . . O1 O 0.65738(9) 0.80722(10) 0.12181(11) 0.01115(12) Uani 1 1 d . . . . . O2 O 0.32548(9) 0.72413(10) -0.05598(10) 0.01097(12) Uani 1 1 d . . . . . O3 O 0.19130(9) 0.50997(10) 0.53876(10) 0.01079(12) Uani 1 1 d . . . . . O4 O 0.15523(9) 0.85318(10) 0.54988(10) 0.01165(12) Uani 1 1 d . . . . . O5 O 0.06036(9) 0.38494(10) 0.17148(10) 0.00992(12) Uani 1 1 d . . . . . O6 O 0.05638(9) 0.90403(10) 0.17316(11) 0.01070(12) Uani 1 1 d . . . . . O7 O 0.40393(9) 0.53320(10) 0.25603(11) 0.01180(12) Uani 1 1 d . . . . . O8 O 0.39130(9) 0.90464(10) 0.29325(11) 0.01075(12) Uani 1 1 d . . . . . O9 O 0.26545(9) 0.19703(9) 0.39263(10) 0.00955(12) Uani 1 1 d . . . . . H1 H 0.168(2) 0.649(2) 0.534(2) 0.015 Uiso 1 1 d . U . . . H2 H 0.201(4) 0.652(5) 0.012(5) 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 0.01053(17) 0.0193(2) 0.0205(2) -0.00052(17) 0.00337(15) -0.00005(15) M1MN 0.00948(8) 0.00651(7) 0.00985(9) 0.00063(5) 0.00119(6) 0.00197(5) M1CA 0.00948(8) 0.00651(7) 0.00985(9) 0.00063(5) 0.00119(6) 0.00197(5) M2MN 0.00889(7) 0.00767(7) 0.01126(8) 0.00058(5) 0.00076(5) 0.00269(5) M2CA 0.00889(7) 0.00767(7) 0.01126(8) 0.00058(5) 0.00076(5) 0.00269(5) Si1 0.00794(10) 0.00498(10) 0.00783(11) 0.00032(7) -0.00008(8) 0.00208(7) Si2 0.00760(10) 0.00468(10) 0.00861(11) -0.00010(7) 0.00000(8) 0.00164(7) Si3 0.00645(10) 0.00597(10) 0.00827(12) -0.00001(8) 0.00054(8) 0.00153(7) O1 0.0075(3) 0.0106(3) 0.0154(3) 0.0006(2) 0.0022(2) 0.0018(2) O2 0.0112(3) 0.0114(3) 0.0097(3) -0.0006(2) -0.0018(2) 0.0021(2) O3 0.0150(3) 0.0091(3) 0.0093(3) -0.0011(2) 0.0009(2) 0.0051(2) O4 0.0171(3) 0.0076(3) 0.0109(3) 0.0022(2) 0.0040(2) 0.0031(2) O5 0.0093(3) 0.0118(3) 0.0088(3) 0.0008(2) -0.0007(2) 0.0031(2) O6 0.0098(3) 0.0099(3) 0.0117(3) -0.0010(2) -0.0020(2) 0.0016(2) O7 0.0107(3) 0.0079(3) 0.0170(3) 0.0040(2) 0.0027(2) 0.0021(2) O8 0.0096(3) 0.0098(3) 0.0136(3) -0.0033(2) 0.0009(2) 0.0041(2) O9 0.0111(3) 0.0045(2) 0.0132(3) 0.0004(2) -0.0003(2) 0.00256(19) _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 O9 2.2738(8) . ? Na1 O2 2.2834(9) 2_665 ? Na1 O3 2.3777(8) 2_666 ? Na1 O8 2.4435(8) 1_545 ? Na1 O4 2.5532(9) 2_666 ? Na1 O7 2.6212(8) . ? Na1 O8 2.7290(9) 2_666 ? Na1 Si2 3.0037(5) 1_545 ? Na1 Si1 3.0899(5) . ? Na1 M2MN 3.2316(5) . ? Na1 Si2 3.2380(5) 2_666 ? M1CA O3 2.3255(7) 2_666 ? M1CA O1 2.3356(7) . ? M1CA O5 2.3520(7) 2_665 ? M1CA O2 2.3750(7) 2_665 ? M1CA O6 2.3943(7) 1_655 ? M1CA O5 2.4371(7) 1_655 ? M1CA Si1 3.3268(3) 2_665 ? M1CA M2MN 3.4200(2) 1_565 ? M1CA Si3 3.4323(3) 2_665 ? M1CA Si3 3.5132(3) . ? M1CA Si2 3.5316(3) 1_655 ? M2MN O2 2.1743(7) 2_665 ? M2MN O1 2.1768(7) 1_545 ? M2MN O4 2.2227(7) 2_666 ? M2MN O6 2.2522(7) 1_645 ? M2MN O6 2.2916(8) 2_665 ? M2MN O5 2.3456(7) 1_655 ? Si1 O5 1.6004(7) . ? Si1 O3 1.6190(7) . ? Si1 O9 1.6284(7) . ? Si1 O7 1.6525(7) . ? Si2 O6 1.6075(7) . ? Si2 O4 1.6153(7) . ? Si2 O9 1.6272(7) 1_565 ? Si2 O8 1.6535(7) . ? Si3 O1 1.5983(7) . ? Si3 O2 1.6094(7) . ? Si3 O8 1.6676(7) . ? Si3 O7 1.6707(7) . ? 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 O9 Na1 O2 125.30(3) . 2_665 ? O9 Na1 O3 133.81(3) . 2_666 ? O2 Na1 O3 84.87(3) 2_665 2_666 ? O9 Na1 O8 65.67(2) . 1_545 ? O2 Na1 O8 96.33(3) 2_665 1_545 ? O3 Na1 O8 153.54(3) 2_666 1_545 ? O9 Na1 O4 146.16(3) . 2_666 ? O2 Na1 O4 81.61(3) 2_665 2_666 ? O3 Na1 O4 60.04(2) 2_666 2_666 ? O8 Na1 O4 93.88(3) 1_545 2_666 ? O9 Na1 O7 63.05(2) . . ? O2 Na1 O7 88.20(3) 2_665 . ? O3 Na1 O7 87.15(3) 2_666 . ? O8 Na1 O7 119.29(3) 1_545 . ? O4 Na1 O7 146.25(3) 2_666 . ? O9 Na1 O8 89.14(3) . 2_666 ? O2 Na1 O8 140.31(3) 2_665 2_666 ? O3 Na1 O8 82.94(3) 2_666 2_666 ? O8 Na1 O8 79.36(3) 1_545 2_666 ? O4 Na1 O8 59.62(2) 2_666 2_666 ? O7 Na1 O8 128.55(3) . 2_666 ? O9 Na1 Si2 32.313(17) . 1_545 ? O2 Na1 Si2 115.17(3) 2_665 1_545 ? O3 Na1 Si2 159.85(3) 2_666 1_545 ? O8 Na1 Si2 33.372(17) 1_545 1_545 ? O4 Na1 Si2 122.28(2) 2_666 1_545 ? O7 Na1 Si2 91.18(2) . 1_545 ? O8 Na1 Si2 82.435(19) 2_666 1_545 ? O9 Na1 Si1 30.830(18) . . ? O2 Na1 Si1 110.70(3) 2_665 . ? O3 Na1 Si1 111.45(2) 2_666 . ? O8 Na1 Si1 92.93(2) 1_545 . ? O4 Na1 Si1 165.16(3) 2_666 . ? O7 Na1 Si1 32.330(16) . . ? O8 Na1 Si1 108.93(2) 2_666 . ? Si2 Na1 Si1 61.022(10) 1_545 . ? O9 Na1 M2MN 145.70(3) . . ? O2 Na1 M2MN 42.22(2) 2_665 . ? O3 Na1 M2MN 80.46(2) 2_666 . ? O8 Na1 M2MN 82.82(2) 1_545 . ? O4 Na1 M2MN 43.239(18) 2_666 . ? O7 Na1 M2MN 129.46(2) . . ? O8 Na1 M2MN 98.39(2) 2_666 . ? Si2 Na1 M2MN 115.387(16) 1_545 . ? Si1 Na1 M2MN 151.110(18) . . ? O9 Na1 Si2 117.41(2) . 2_666 ? O2 Na1 Si2 109.71(2) 2_665 2_666 ? O3 Na1 Si2 72.61(2) 2_666 2_666 ? O8 Na1 Si2 82.21(2) 1_545 2_666 ? O4 Na1 Si2 29.475(17) 2_666 2_666 ? O7 Na1 Si2 151.07(2) . 2_666 ? O8 Na1 Si2 30.688(16) 2_666 2_666 ? Si2 Na1 Si2 100.746(15) 1_545 2_666 ? Si1 Na1 Si2 139.586(18) . 2_666 ? M2MN Na1 Si2 68.347(11) . 2_666 ? O3 M1CA O1 99.53(3) 2_666 . ? O3 M1CA O5 161.08(3) 2_666 2_665 ? O1 M1CA O5 99.14(3) . 2_665 ? O3 M1CA O2 84.01(2) 2_666 2_665 ? O1 M1CA O2 105.86(3) . 2_665 ? O5 M1CA O2 88.00(2) 2_665 2_665 ? O3 M1CA O6 106.47(3) 2_666 1_655 ? O1 M1CA O6 79.98(2) . 1_655 ? O5 M1CA O6 79.80(3) 2_665 1_655 ? O2 M1CA O6 167.25(3) 2_665 1_655 ? O3 M1CA O5 81.37(2) 2_666 1_655 ? O1 M1CA O5 177.20(2) . 1_655 ? O5 M1CA O5 80.12(3) 2_665 1_655 ? O2 M1CA O5 76.84(2) 2_665 1_655 ? O6 M1CA O5 97.23(2) 1_655 1_655 ? O3 M1CA Si1 158.077(19) 2_666 2_665 ? O1 M1CA Si1 81.14(2) . 2_665 ? O5 M1CA Si1 26.228(17) 2_665 2_665 ? O2 M1CA Si1 74.838(18) 2_665 2_665 ? O6 M1CA Si1 95.259(19) 1_655 2_665 ? O5 M1CA Si1 99.030(18) 1_655 2_665 ? O3 M1CA Na1 45.164(19) 2_666 . ? O1 M1CA Na1 92.691(19) . . ? O5 M1CA Na1 130.73(2) 2_665 . ? O2 M1CA Na1 42.90(2) 2_665 . ? O6 M1CA Na1 149.47(2) 1_655 . ? O5 M1CA Na1 89.812(19) 1_655 . ? Si1 M1CA Na1 112.993(10) 2_665 . ? O3 M1CA M2MN 108.420(18) 2_666 1_565 ? O1 M1CA M2MN 39.012(17) . 1_565 ? O5 M1CA M2MN 88.152(18) 2_665 1_565 ? O2 M1CA M2MN 143.118(18) 2_665 1_565 ? O6 M1CA M2MN 41.016(17) 1_655 1_565 ? O5 M1CA M2MN 138.193(17) 1_655 1_565 ? Si1 M1CA M2MN 86.019(6) 2_665 1_565 ? Na1 M1CA M2MN 126.458(10) . 1_565 ? O3 M1CA Si3 104.783(18) 2_666 2_665 ? O1 M1CA Si3 89.438(18) . 2_665 ? O5 M1CA Si3 72.381(18) 2_665 2_665 ? O2 M1CA Si3 24.538(18) 2_665 2_665 ? O6 M1CA Si3 148.23(2) 1_655 2_665 ? O5 M1CA Si3 92.894(17) 1_655 2_665 ? Si1 M1CA Si3 53.311(6) 2_665 2_665 ? Na1 M1CA Si3 60.026(9) . 2_665 ? M2MN M1CA Si3 121.566(7) 1_565 2_665 ? O3 M1CA Si3 88.395(18) 2_666 . ? O1 M1CA Si3 21.746(17) . . ? O5 M1CA Si3 108.207(18) 2_665 . ? O2 M1CA Si3 86.228(18) 2_665 . ? O6 M1CA Si3 101.037(18) 1_655 . ? O5 M1CA Si3 160.988(18) 1_655 . ? Si1 M1CA Si3 84.580(7) 2_665 . ? Na1 M1CA Si3 71.730(10) . . ? M2MN M1CA Si3 60.407(5) 1_565 . ? Si3 M1CA Si3 74.200(7) 2_665 . ? O3 M1CA Si2 86.717(18) 2_666 1_655 ? O1 M1CA Si2 93.730(18) . 1_655 ? O5 M1CA Si2 95.080(18) 2_665 1_655 ? O2 M1CA Si2 159.451(18) 2_665 1_655 ? O6 M1CA Si2 22.527(18) 1_655 1_655 ? O5 M1CA Si2 83.665(17) 1_655 1_655 ? Si1 M1CA Si2 115.170(8) 2_665 1_655 ? Na1 M1CA Si2 131.830(11) . 1_655 ? M2MN M1CA Si2 57.405(5) 1_565 1_655 ? Si3 M1CA Si2 167.416(8) 2_665 1_655 ? Si3 M1CA Si2 111.843(7) . 1_655 ? O2 M2MN O1 97.77(3) 2_665 1_545 ? O2 M2MN O4 92.16(3) 2_665 2_666 ? O1 M2MN O4 96.00(3) 1_545 2_666 ? O2 M2MN O6 170.93(3) 2_665 1_645 ? O1 M2MN O6 86.67(3) 1_545 1_645 ? O4 M2MN O6 95.25(3) 2_666 1_645 ? O2 M2MN O6 91.09(3) 2_665 2_665 ? O1 M2MN O6 101.80(3) 1_545 2_665 ? O4 M2MN O6 161.30(3) 2_666 2_665 ? O6 M2MN O6 80.23(3) 1_645 2_665 ? O2 M2MN O5 82.77(2) 2_665 1_655 ? O1 M2MN O5 176.06(3) 1_545 1_655 ? O4 M2MN O5 80.08(3) 2_666 1_655 ? O6 M2MN O5 93.34(3) 1_645 1_655 ? O6 M2MN O5 82.07(2) 2_665 1_655 ? O2 M2MN Na1 44.88(2) 2_665 . ? O1 M2MN Na1 83.27(2) 1_545 . ? O4 M2MN Na1 51.90(2) 2_666 . ? O6 M2MN Na1 143.98(2) 1_645 . ? O6 M2MN Na1 135.69(2) 2_665 . ? O5 M2MN Na1 94.46(2) 1_655 . ? O2 M2MN M1CA 40.745(18) 2_665 . ? O1 M2MN M1CA 136.643(19) 1_545 . ? O4 M2MN M1CA 77.936(18) 2_666 . ? O6 M2MN M1CA 136.337(18) 1_645 . ? O6 M2MN M1CA 92.741(18) 2_665 . ? O5 M2MN M1CA 43.043(17) 1_655 . ? Na1 M2MN M1CA 59.013(9) . . ? O5 Si1 O3 115.12(4) . . ? O5 Si1 O9 112.92(4) . . ? O3 Si1 O9 105.84(4) . . ? O5 Si1 O7 110.67(4) . . ? O3 Si1 O7 108.00(4) . . ? O9 Si1 O7 103.50(4) . . ? O5 Si1 Na1 130.74(3) . . ? O3 Si1 Na1 113.74(3) . . ? O9 Si1 Na1 45.69(3) . . ? O7 Si1 Na1 58.03(3) . . ? O5 Si1 Na1 136.95(3) . 2_666 ? O3 Si1 Na1 41.74(3) . 2_666 ? O9 Si1 Na1 109.13(3) . 2_666 ? O7 Si1 Na1 66.77(3) . 2_666 ? Na1 Si1 Na1 86.249(14) . 2_666 ? O6 Si2 O4 114.23(4) . . ? O6 Si2 O9 112.01(4) . 1_565 ? O4 Si2 O9 108.87(4) . 1_565 ? O6 Si2 O8 111.17(4) . . ? O4 Si2 O8 107.16(4) . . ? O9 Si2 O8 102.67(4) 1_565 . ? O6 Si2 Na1 127.67(3) . 1_565 ? O4 Si2 Na1 118.06(3) . 1_565 ? O9 Si2 Na1 48.32(3) 1_565 1_565 ? O8 Si2 Na1 54.38(3) . 1_565 ? O6 Si2 Na1 140.56(3) . 2_666 ? O4 Si2 Na1 51.06(3) . 2_666 ? O9 Si2 Na1 107.41(3) 1_565 2_666 ? O8 Si2 Na1 57.38(3) . 2_666 ? Na1 Si2 Na1 79.253(15) 1_565 2_666 ? O1 Si3 O2 116.30(4) . . ? O1 Si3 O8 110.53(4) . . ? O2 Si3 O8 108.79(4) . . ? O1 Si3 O7 109.07(4) . . ? O2 Si3 O7 107.79(4) . . ? O8 Si3 O7 103.56(4) . . ? O1 Si3 Na1 80.93(3) . 2_665 ? O2 Si3 Na1 35.47(3) . 2_665 ? O8 Si3 Na1 128.00(3) . 2_665 ? O7 Si3 Na1 120.71(3) . 2_665 ? O1 Si3 Na1 100.79(3) . 2_666 ? O2 Si3 Na1 142.58(3) . 2_666 ? O8 Si3 Na1 49.12(3) . 2_666 ? O7 Si3 Na1 61.17(3) . 2_666 ? Na1 Si3 Na1 177.002(18) 2_665 2_666 ? O1 Si3 M1CA 32.78(3) . . ? O2 Si3 M1CA 118.92(3) . . ? O8 Si3 M1CA 129.41(3) . . ? O7 Si3 M1CA 77.91(3) . . ? Na1 Si3 M1CA 88.033(10) 2_665 . ? Na1 Si3 M1CA 94.731(10) 2_666 . ? Si3 O1 M2MN 134.52(4) . 1_565 ? Si3 O1 M1CA 125.47(4) . . ? M2MN O1 M1CA 98.50(3) 1_565 . ? Si3 O2 M2MN 124.42(4) . 2_665 ? Si3 O2 Na1 120.39(4) . 2_665 ? M2MN O2 Na1 92.90(3) 2_665 2_665 ? Si3 O2 M1MN 117.67(4) . 2_665 ? M2MN O2 M1MN 102.56(3) 2_665 2_665 ? Na1 O2 M1MN 92.03(3) 2_665 2_665 ? Si1 O3 M1MN 135.40(4) . 2_666 ? Si1 O3 Na1 111.31(4) . 2_666 ? M1MN O3 Na1 90.92(3) 2_666 2_666 ? Si2 O4 M2MN 141.98(4) . 2_666 ? Si2 O4 Na1 99.47(3) . 2_666 ? M2MN O4 Na1 84.87(3) 2_666 2_666 ? Si1 O5 M2MN 118.87(4) . 1_455 ? Si1 O5 M1MN 113.27(4) . 2_665 ? M2MN O5 M1MN 98.89(3) 1_455 2_665 ? Si1 O5 M1MN 125.34(4) . 1_455 ? M2MN O5 M1MN 95.89(2) 1_455 1_455 ? M1MN O5 M1MN 99.88(3) 2_665 1_455 ? Si2 O6 M2MN 118.90(4) . 1_465 ? Si2 O6 M2MN 116.80(4) . 2_665 ? M2MN O6 M2MN 99.77(3) 1_465 2_665 ? Si2 O6 M1MN 122.68(4) . 1_455 ? M2MN O6 M1MN 94.74(3) 1_465 1_455 ? M2MN O6 M1MN 99.20(3) 2_665 1_455 ? Si1 O7 Si3 131.82(4) . . ? Si1 O7 Na1 89.64(3) . . ? Si3 O7 Na1 138.25(4) . . ? Si2 O8 Si3 137.18(4) . . ? Si2 O8 Na1 92.25(3) . 1_565 ? Si3 O8 Na1 122.80(4) . 1_565 ? Si2 O8 Na1 91.93(3) . 2_666 ? Si3 O8 Na1 103.36(3) . 2_666 ? Na1 O8 Na1 100.64(3) 1_565 2_666 ? Si2 O9 Si1 143.81(5) 1_545 . ? Si2 O9 Na1 99.36(3) 1_545 . ? Si1 O9 Na1 103.48(3) . . ? _refine_diff_density_max 0.543 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.106 _shelx_res_file ; TITL Henrik Tutop pectolite exp_95_Mo in P-1 KNR96.res created by SHELXL-2018/3 at 01:47:19 on 21-Aug-2020 CELL 0.71073 7.838260 6.96973 6.903762 90.7516 94.4374 102.8940 ZERR 2.00 0.000064 0.000061 0.000071 0.0008 0.0007 0.0007 LATT 1 SFAC O H NA SI MN CA UNIT 18 2 2 6 2.21 1.79 TEMP 25 MERG 2 BOND HTAB LIST 6 FMAP 2 PLAN 10 ACTA L.S. 18 EXYZ M1CA M1MN EADP M1CA M1MN EXYZ M2MN M2CA EADP M2MN M2CA WGHT 0.031000 0.099900 FVAR 1.80619 0.17913 0.87066 NA1 3 0.556354 0.244715 0.349171 11.00000 0.01053 0.01932 = 0.02045 -0.00052 0.00337 -0.00005 M1MN 5 0.848733 0.593737 0.145844 21.00000 0.00948 0.00651 = 0.00985 0.00063 0.00119 0.00197 M1CA 6 0.848733 0.593737 0.145844 -21.00000 0.00948 0.00651 = 0.00985 0.00063 0.00119 0.00197 M2MN 5 0.851973 0.084956 0.134567 31.00000 0.00889 0.00767 = 0.01126 0.00058 0.00076 0.00269 M2CA 6 0.851973 0.084956 0.134567 -31.00000 0.00889 0.00767 = 0.01126 0.00058 0.00076 0.00269 SI1 4 0.219722 0.407010 0.335815 11.00000 0.00794 0.00498 = 0.00783 0.00032 -0.00008 0.00208 SI2 4 0.206550 0.960368 0.349676 11.00000 0.00760 0.00468 = 0.00861 -0.00010 0.00000 0.00164 SI3 4 0.450783 0.746734 0.142848 11.00000 0.00645 0.00597 = 0.00827 -0.00001 0.00054 0.00153 O1 1 0.657382 0.807219 0.121810 11.00000 0.00748 0.01064 = 0.01541 0.00063 0.00221 0.00179 O2 1 0.325485 0.724135 -0.055981 11.00000 0.01117 0.01142 = 0.00966 -0.00057 -0.00179 0.00207 O3 1 0.191296 0.509971 0.538765 11.00000 0.01503 0.00913 = 0.00927 -0.00110 0.00093 0.00508 O4 1 0.155234 0.853181 0.549876 11.00000 0.01710 0.00761 = 0.01089 0.00220 0.00398 0.00307 O5 1 0.060365 0.384938 0.171480 11.00000 0.00928 0.01184 = 0.00876 0.00085 -0.00069 0.00311 O6 1 0.056377 0.904028 0.173165 11.00000 0.00975 0.00993 = 0.01166 -0.00097 -0.00204 0.00165 O7 1 0.403928 0.533202 0.256027 11.00000 0.01075 0.00795 = 0.01704 0.00396 0.00274 0.00206 O8 1 0.391304 0.904644 0.293251 11.00000 0.00962 0.00981 = 0.01362 -0.00325 0.00090 0.00414 O9 1 0.265447 0.197029 0.392633 11.00000 0.01115 0.00447 = 0.01321 0.00036 -0.00032 0.00256 H1 2 0.168208 0.649168 0.533877 11.00000 10.01500 H2 2 0.200900 0.652480 0.011591 10.50000 10.01500 HKLF 4 1 0 0 1 0 1 0 1 0 0 REM Henrik Tutop pectolite exp_95_Mo in P-1 REM wR2 = 0.052549, GooF = S = 1.12987, Restrained GooF = 1.12987 for all data REM R1 = 0.017786 for 2965 Fo > 4sig(Fo) and 0.018429 for all 3067 data REM 144 parameters refined using 0 restraints END WGHT 0.0310 0.1000 REM Instructions for potential hydrogen bonds HTAB O3 O4 HTAB O4 O3 HTAB O2 O5 EQIV $12 -x, -y+1, -z HTAB O2 O5_$12 HTAB O2 O6 REM Highest difference peak 0.543, deepest hole -0.651, 1-sigma level 0.106 Q1 1 0.5576 0.8022 0.1411 11.00000 0.05 0.54 Q2 1 0.1359 0.3906 0.2410 11.00000 0.05 0.51 Q3 1 0.1255 0.9357 0.2599 11.00000 0.05 0.48 Q4 1 0.3271 0.4875 0.3112 11.00000 0.05 0.47 Q5 1 0.2004 0.9142 0.4731 11.00000 0.05 0.46 Q6 1 0.3686 0.7228 0.0509 11.00000 0.05 0.43 Q7 1 0.1994 0.1506 0.3639 11.00000 0.05 0.42 Q8 1 0.9397 0.1168 0.1527 11.00000 0.05 0.38 Q9 1 0.2151 0.2532 0.3547 11.00000 0.05 0.37 Q10 1 0.1579 0.7465 0.5475 11.00000 0.05 0.35 ; _shelx_res_checksum 50489 _shelx_hkl_file ; -3 -3 -3 6.30554 3.24853 0 -1 -5 -8 46.6040 10.0441 0 0 -2 -7 61.3850 9.69776 0 -2 -4 -6 14.7888 5.69855 0 2 -1 5 2.97148 2.56963 0 -3 -4 -4 41.6065 7.42308 0 5 1 1 2.21816 1.87981 0 -2 -3 -5 1.08690 3.43538 0 -4 -7 -3 13.8050 5.38470 0 3 -1 -8 37.3624 7.70931 0 -3 -6 -5 44.6115 8.69160 0 7 1 0 99.2747 6.21285 0 6 0 -7 35.2947 6.30558 0 4 -1 -8 7.00452 4.51566 0 2 -1 -7 39.1927 7.13468 0 -1 -5 -7-1.59061 3.55133 0 3 -3 -9-1.57947 4.72944 0 1 -1 -6 41.5378 7.03022 0 4 -3 -9 23.3187 7.43922 0 7 1 1 29.4809 4.64731 0 5 -3 -9 61.1324 11.2011 0 3 -1 -7 49.5875 8.02913 0 -4 -7 5 4.10915 1.77097 0 -3 -3 0 19.8579 2.87065 0 1 -5 -8 5.15257 5.42097 0 -2 -5 -5 41.3120 8.35832 0 4 0 -6 13.8038 4.19741 0 -2 -8 -5 48.0309 10.2224 0 -4 -7 -1 17.2110 5.15441 0 6 1 -4 18.7637 2.69069 0 2 -2 -7 68.8656 9.78417 0 5 -2 -8 85.2145 11.2132 0 3 1 2 3.32512 2.06882 0 6 0 -6 46.8970 6.49730 0 3 -3 -8-1.44393 4.55984 0 6 -2 -8 37.2006 8.20688 0 7 1 2 9.89238 3.32012 0 7 -1 -7 4.59002 3.03771 0 5 1 3-0.68153 2.04074 0 5 -1 -7 19.9997 5.37841 0 4 -3 -8 30.0826 8.21584 0 -1 -4 -5 5.78522 3.65675 0 2 1 0 10944.3 38.7764 0 5 -3 -8 25.5116 7.48489 0 3 -5 -8 84.0229 13.1430 0 7 1 3 5.80209 3.23249 0 4 -4 -8 39.3787 9.16673 0 -1 -5 -5 16.5605 6.10414 0 4 -2 -7 10.3262 4.28858 0 0 -6 -6 26.4399 7.76503 0 4 -5 -8 13.6795 7.03301 0 3 -3 -7 5.16318 4.07780 0 2 -5 -7 72.4027 11.9695 0 -2 -4 8 7.76102 3.37248 0 -2 -9 -3 35.7904 9.14003 0 -4 -8 1 12.2177 3.70924 0 7 -1 -6 46.7032 6.84233 0 -2 -10 -2 43.0140 9.06382 0 4 -3 -7 8.98938 5.13063 0 -3 -5 -1 2.69861 2.69684 0 1 -5 -6 60.7752 10.2789 0 5 -3 -7 2.56860 4.44225 0 4 -4 -7 11.4695 5.90263 0 -1 -5 -4 63.4901 8.97441 0 5 1 -3 5.80875 1.56507 0 0 -6 -5 9.82726 5.24696 0 -3 -5 8 38.3453 5.64592 0 -3 -3 3 4.03367 0.95467 0 7 -4 -7 17.2860 6.42287 0 2 -5 -6 44.0910 8.64208 0 2 -6 -6 1.57272 3.84662 0 7 -2 -6 52.1533 8.25457 0 -1 -10 -2 102.705 13.1603 0 1 1 3 28.1873 4.19179 0 1 1 2 8.69357 2.23501 0 4 -3 -6 47.0508 8.18804 0 -2 -7 -2 8.70300 4.34634 0 8 -3 -6 5.85199 4.36648 0 3 -5 -6 38.9268 8.14582 0 7 -1 -5 50.5513 6.66399 0 0 -7 -4 44.9265 9.08675 0 5 -3 -6 2.32321 3.06975 0 7 -3 -6 59.2066 9.22900 0 2 -8 -5 34.4706 8.76770 0 6 -3 -6 35.3277 7.34270 0 -1 -6 -3 28.7385 6.24778 0 4 -6 -6 14.5999 6.05843 0 0 -9 -3 93.9788 13.0415 0 1 -3 -4-0.84098 2.05952 0 7 -5 -6 44.4466 9.42078 0 3 -1 -4 13.2306 3.40112 0 6 -5 -6 4.55753 5.02751 0 5 2 0 18.5671 2.53692 0 1 -7 -4 15.7955 6.41363 0 5 -2 -5 7.11690 3.87462 0 6 -2 -5 39.1089 6.73746 0 -1 -4 -2 9.77385 3.19849 0 2 -8 -4 14.5950 6.47426 0 4 -7 -5 13.3603 6.23612 0 -2 -9 0 53.1169 8.76449 0 2 -3 -4 0.85152 2.69203 0 -3 -7 1 6.16805 3.13668 0 7 -3 -5 41.0545 7.67412 0 2 -1 -3 11.7925 2.90749 0 8 -4 -5 6.54621 5.22270 0 -3 -9 2 20.3520 4.80405 0 6 -3 -5 51.1853 8.21190 0 8 -5 -5 26.7160 8.10338 0 4 1 -2 147.557 4.45863 0 -1 -11 1 34.9759 7.95294 0 8 0 -3 6.01691 2.43517 0 7 -6 -5 13.0544 6.90289 0 5 -5 -5 96.5361 12.4965 0 7 -5 -5 4.41724 4.87199 0 6 -4 -5 1.26660 3.34624 0 2 -9 -3 13.2486 6.39887 0 2 -5 -4 55.7420 8.68505 0 0 -10 -1 81.9598 12.2110 0 0 -8 -2 63.1619 9.92089 0 -4 -7 4 5.38076 1.97296 0 8 -2 -4 21.0572 5.18039 0 3 -5 -4 4.83898 3.82287 0 5 -7 -4 50.9451 9.84094 0 7 1 -2 60.7771 3.32684 0 -3 -9 3 26.0723 5.40904 0 6 -7 -4 5.07176 5.59329 0 0 -6 -2 14.3097 5.00448 0 -1 1 6 27.7629 5.34445 0 8 -5 -4-1.45285 4.58183 0 5 -6 -4 5.95033 4.92655 0 6 -6 -4 75.5765 11.8252 0 3 3 3 8.09068 2.85584 0 4 3 2 20.3080 3.91359 0 5 1 -2 71.2928 3.38106 0 7 -5 -4 89.6189 12.6984 0 4 -8 -3 90.9331 13.2009 0 2 -3 -3 14.8723 4.07226 0 -4 -7 5 4.10915 1.77097 0 6 1 -2 1307.11 15.1839 0 -4 -3 7 7.95081 2.52781 0 -2 -1 2 376.214 6.66910 0 -4 -3 8 12.8512 3.55699 0 2 -8 -2 21.6886 6.92482 0 1 -10 0 1.48995 3.93227 0 9 -3 -3 18.1792 5.64330 0 9 -5 -3 79.0423 11.8107 0 7 -7 -3 85.8816 13.3295 0 5 -7 -3 4.72662 4.71875 0 9 -4 -3 16.4204 5.63213 0 -3 -9 4 7.56077 3.14113 0 3 -3 -3 18.8857 4.51928 0 1 3 5-0.89642 2.52987 0 3 0 -2 4978.89 34.8867 0 4 -8 -2 9.54612 5.94299 0 0 -8 0 56.4801 8.84370 0 8 0 -2 2936.35 34.4945 0 5 -8 -2 44.8906 10.0929 0 5 -5 -3 1.25148 3.53647 0 3 -7 -2 20.5270 6.55634 0 7 -3 -3 3.07362 3.96300 0 5 -4 -3 67.9401 9.20741 0 6 -4 -3 4.58321 4.28288 0 6 -3 -3 3.87283 3.35106 0 4 -7 -2 17.2927 5.93464 0 6 0 3 1633.90 35.4735 0 -2 -5 -7 470.185 28.7726 0 3 -1 5 340.391 17.3391 0 0 -2 5 14109.4 95.4826 0 -2 -2 -4 2122.56 43.1595 0 0 -1 -6 838.527 29.9773 0 -2 -6 -7 292.885 23.3908 0 0 -3 -8 509.652 28.6954 0 3 0 -7 6877.29 83.1108 0 1 -1 -7 110.605 11.7227 0 -1 -2 4 2044.52 30.4382 0 -3 -5 -5 179.038 16.2880 0 1 -2 -8 3555.42 71.5094 0 1 0 2 16820.6 76.8514 0 -4 -6 -3 3821.69 65.2167 0 -4 -5 -2 148.238 11.5017 0 4 1 -5 128.217 8.53522 0 2 0 3 5436.20 55.0071 0 3 -2 -9 1378.57 46.1233 0 1 0 -5 5789.54 67.4777 0 1 -4 -9 1363.00 50.4795 0 -3 -6 6 546.677 17.0283 0 1 -2 6 742.375 25.1297 0 -4 -8 -3 718.228 30.9495 0 2 0 -6 155.841 12.1221 0 4 1 1 2168.14 30.1779 0 2 -3 -9 804.041 37.3275 0 -3 -8 -5 342.472 24.2124 0 4 0 -7 2400.11 47.9651 0 3 1 -4 424.338 13.6031 0 0 -4 -8 642.665 33.3959 0 -1 -4 -7 2130.68 57.8561 0 -3 -7 -5 584.888 30.6686 0 5 1 -5 449.752 14.7543 0 4 0 4 6052.38 69.1745 0 5 0 4 1049.37 29.6193 0 4 -2 -9 138.329 14.9285 0 -1 -4 7 6719.46 73.6568 0 -2 -5 -6 133.109 14.8769 0 6 1 1 102.963 7.49117 0 -4 -5 -1 597.326 20.4250 0 5 0 -7 584.879 23.3586 0 -3 -4 4 243.790 8.38757 0 5 -2 -9 2229.73 57.4893 0 2 -2 -8 438.082 25.2223 0 -4 -6 -2 352.117 18.5328 0 6 -2 -9 272.244 20.2235 0 1 -3 -8 327.344 22.8724 0 -1 -3 6 164.331 10.8632 0 0 -1 -5 85.3628 9.02249 0 2 -4 -9 259.493 22.0279 0 3 0 4 4204.56 55.5974 0 -2 -5 7 517.576 19.4099 0 -2 -4 6 6266.40 61.7833 0 0 -3 7 163.475 12.2587 0 -2 -6 -6 113.319 14.2018 0 -3 -5 -4 1681.38 44.7927 0 -2 -7 -6 184.139 18.5545 0 -1 -1 2 2762.60 23.8514 0 0 -3 -7 1944.82 52.3179 0 5 -1 -8 1633.73 44.3932 0 6 -1 -8 593.924 26.2814 0 -3 -3 -1 416.842 14.2946 0 -3 -4 -3 5447.04 71.0611 0 -1 -6 -7 2186.11 62.9246 0 3 1 1 484.384 13.3662 0 -4 -7 -2 3167.86 57.9812 0 -4 -8 -2 606.664 26.9956 0 -2 -4 -5 138.255 13.4118 0 3 0 -6 3319.55 52.9408 0 1 -2 -7 12134.6 124.617 0 0 -2 -6 727.065 29.0893 0 1 0 -4 4374.56 51.4289 0 -2 -3 -4 2932.02 53.4794 0 -3 -6 -4 3306.50 66.0860 0 1 -4 -8 3255.19 74.3651 0 -3 -8 -4 991.114 39.0497 0 0 -2 6 189.036 12.3064 0 5 1 2 172.468 10.4225 0 3 -4 -9 1611.78 53.8616 0 3 -2 -8 6127.10 92.6326 0 -3 -7 -4 196.365 17.2429 0 -2 -2 -2 10432.9 75.4135 0 4 1 -4 1616.39 24.7953 0 2 0 -5 9158.72 81.7315 0 4 1 2 558.174 17.6473 0 2 -1 6 100.749 9.83639 0 2 0 4 925.202 25.3039 0 -2 -3 5 234.319 10.8803 0 2 -3 -8 141.599 15.2220 0 -1 -4 -6 1865.84 51.4109 0 6 -3 -9 810.216 36.4520 0 -4 -6 -1 1183.77 30.8445 0 1 0 3 1075.80 23.1475 0 6 1 2 1320.45 28.9407 0 -1 -2 5 2957.37 41.5932 0 -4 -5 1 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2 8 3434.89 65.8661 3 4 3 7 642.036 25.7991 3 -3 3 -5 1658.19 36.6841 3 3 1 3 412.172 13.0156 3 1 0 8 3313.30 67.8495 3 -2 -1 9 1081.03 43.1858 3 -7 3 -4 379.046 16.9025 3 3 3 9 387.969 23.9728 3 -6 -1 9 181.278 18.4610 3 -7 -1 8 1255.75 43.9583 3 0 -1 6 3934.88 65.3285 3 3 1 5 317.242 15.6199 3 -4 2 -4 668.778 20.8308 3 -4 3 -5 6648.05 74.9120 3 -2 3 -5 1004.26 28.6859 3 2 4 -4 6740.92 70.4036 3 -1 0 10 2264.33 64.5798 3 -2 2 -4 20537.9 113.119 3 2 3 -3 10013.3 74.3057 3 2 1 8 102.566 12.5479 3 3 1 4 1231.87 26.8555 3 0 -1 5 704.826 25.2195 3 -7 2 -3 288.487 12.7288 3 3 4 -3 3248.67 44.5851 3 -5 -1 9 284.661 23.0585 3 5 4 2 21.2289 1.77716 3 5 4 4 4574.13 45.0788 3 -4 -1 9 810.890 38.0973 3 2 3 10 618.617 32.9674 3 -7 -1 7 821.566 33.8583 3 3 5 -4 2437.49 44.6581 3 -6 -1 2 1231.43 20.8698 3 0 1 -2 1297.28 20.1807 3 2 5 -5 881.329 29.0759 3 -4 -1 1 31.0246 2.61284 3 1 3 -4 1174.52 28.2331 3 2 2 9 228.540 19.0665 3 1 0 7 4824.25 76.6983 3 -5 2 -4 637.316 20.5683 3 -6 -1 8 119.296 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3 -4 4685.00 57.3950 3 -3 2 -5 764.748 24.6455 3 -2 -1 3 129.635 9.04316 3 -7 1 9 238.640 21.9844 3 1 1 7 125.630 13.2142 3 -7 0 7 3862.80 76.9461 3 0 0 6 1139.32 36.4726 3 1 4 -6 5142.61 73.1686 3 2 1 5 1090.40 30.8822 3 -3 -1 5 4022.08 65.1921 3 -8 0 5 1655.63 42.9709 3 -4 2 -5 6086.34 69.3120 3 -2 2 -5 3699.22 54.1203 3 -8 1 8 136.005 16.3345 3 3 2 5 5940.26 70.9540 3 -3 -1 2 1367.63 24.5828 3 -5 -1 4 1466.68 35.8676 3 -4 -1 5 114.616 11.5280 3 -1 0 7 376.055 23.2791 3 -4 -1 2 137.716 8.13642 3 1 3 -5 281.027 15.5652 3 -5 0 8 4463.81 87.7938 3 4 3 4 1210.15 27.4857 3 -4 0 8 500.165 29.6491 3 1 3 9 345.353 24.9871 3 4 5 -4 2959.72 49.2331 3 -2 2 10 955.607 44.7254 3 -2 1 9 369.364 26.4108 3 1 2 8 4064.12 79.0491 3 -6 1 9 534.743 33.3207 3 -9 1 6 139.436 14.4613 3 -3 -1 3 1838.72 34.8236 3 -5 2 -5 618.492 22.3638 3 -7 0 6 3284.37 67.3408 3 -3 2 10 525.134 33.7771 3 -7 2 -4 1017.97 25.5955 3 -5 1 9 240.912 22.3707 3 -6 1 -3 41.5898 4.77690 3 -2 0 7 447.250 25.9423 3 0 0 5 4264.48 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1598.05 49.4465 9 -4 6 3 3615.54 72.1677 9 -4 5 4 190.684 16.8557 9 -2 1 9 358.771 20.4954 9 -4 7 3 2337.83 60.6233 9 -1 -1 6 1602.21 27.9713 9 -3 5 0 1193.47 31.5633 9 4 1 -4 1569.35 31.2017 9 -2 1 2 348.616 12.6941 9 -2 9 -2 3119.65 55.2838 9 -3 10 1 683.690 33.0938 9 -4 8 4 523.919 31.3480 9 -4 7 6 324.665 25.3398 9 -1 -1 5 163.567 8.26232 9 -4 5 3 836.940 32.9680 9 -1 -1 7 72.0861 6.82420 9 -4 8 3 119.571 14.6066 9 -2 0 6 147.781 10.4802 9 5 2 -5 5970.57 66.8570 9 -3 2 3 11959.1 97.9933 9 2 1 -3 144.654 7.13856 9 3 -3 3 4306.95 40.8988 9 -3 2 8 6580.25 91.6248 9 -1 0 10 2247.84 46.2468 9 -2 0 5 9086.04 74.7170 9 -4 5 7 128.539 15.4360 9 0 -1 10 67.5964 7.22454 9 -4 6 2 134.775 13.7588 9 4 4 -6 3531.51 45.3980 9 -4 4 4 1290.87 40.4920 9 -2 0 7 408.548 18.2916 9 5 -3 2 174.275 11.2353 9 -1 8 -4 485.704 15.4776 9 5 0 -3 7423.11 73.7781 9 -1 3 -2 4625.02 31.0780 9 5 1 -4 1410.23 32.4486 9 1 3 -4 1115.89 13.4593 9 -2 5 -2 509.978 16.1930 9 -4 5 2 2370.09 52.4593 9 -3 7 -1 434.202 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5099.12 79.3299 22 1 -6 2 81.4575 9.56065 22 2 -5 8 147.275 18.8336 22 3 -7 8 945.279 49.9558 22 1 -6 4 3726.70 73.2706 22 2 -7 6 618.155 36.1923 22 0 -3 1 206.270 10.0527 22 2 4 -3 14792.6 117.512 22 0 -2 4 1739.04 41.3797 22 2 -7 0 2678.39 42.4042 22 1 -3 7 155.332 17.0636 22 1 -2 7 17984.3 168.803 22 2 -4 -4 6935.57 51.8592 22 3 4 -5 4358.57 74.5892 22 3 0 9 3197.33 76.8288 22 1 3 -1 620.937 17.3259 22 0 0 3 22109.4 109.936 22 3 -8 7 1165.74 54.5687 22 0 -1 4 2197.72 43.4021 22 2 0 8 796.367 35.4869 22 2 3 -4 4584.90 67.9898 22 1 -6 5 3765.88 79.2414 22 1 -1 7 105.512 13.0176 22 3 -3 10 490.347 35.0652 22 2 1 -5 1950.01 44.0486 22 1 -6 1 1889.19 37.9868 22 3 -4 10 2359.27 77.7525 22 4 0 10 1818.45 60.7058 22 3 -9 4 632.450 34.6675 22 4 6 -3 2101.67 52.5875 22 3 -2 10 837.818 44.4160 22 2 -4 9 1185.74 52.5959 22 3 -9 3 854.132 37.1789 22 0 -4 3 1712.51 40.9177 22 2 -2 9 356.555 27.4980 22 2 -8 4 4286.83 85.5055 22 3 5 -3 1068.15 34.4587 22 2 -8 3 255.021 19.4903 22 3 -2 -6 3781.28 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6919.97 55.3652 22 2 -9 5 846.007 40.9398 22 0 -4 7 757.926 37.0487 22 0 -2 7 2120.25 58.0716 22 1 1 7 128.576 12.7729 22 2 -1 10 129.884 16.6230 22 2 -5 -3 741.095 11.2184 22 1 0 8 3288.19 70.4260 22 2 -9 4 631.659 32.7573 22 3 5 -1 1411.80 34.1475 22 2 -9 6 184.335 20.8436 22 4 6 1 1180.17 28.7262 22 3 -10 6 496.993 34.0664 22 3 -10 4 2171.15 62.1211 22 3 4 -3 3167.82 56.7418 22 0 -6 4 2527.21 58.7997 22 1 -7 8 417.200 32.2784 22 0 -6 5 505.670 28.7966 22 3 3 -4 285.756 17.8336 22 2 -9 7 2253.85 73.9493 22 2 -4 11 191.672 23.0345 22 1 -8 5 518.185 31.0745 22 2 -9 3 244.467 19.2011 22 2 -3 11 1123.63 53.3350 22 1 -8 4 524.558 28.8439 22 4 -5 -5 1482.50 32.6356 22 1 -8 6 3881.06 89.6319 22 0 -1 7 758.793 33.3549 22 0 0 6 1113.94 35.3083 22 3 1 -5 3953.09 65.0675 22 0 -6 6 728.173 36.3860 22 0 1 4 6908.07 65.5237 22 3 4 6 2445.33 35.9766 22 0 -6 3 11080.5 111.903 22 0 -3 8 2944.16 74.9074 22 1 3 1 1272.35 14.8064 22 1 -4 10 551.100 37.0573 22 0 -4 8 2571.17 71.7479 22 4 -2 -6 1914.44 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1508.71 46.2769 22 5 4 -2 899.990 32.7062 22 -2 -3 5 229.848 17.7072 22 -2 -5 6 5391.87 96.5462 22 1 2 0 775.212 14.1334 22 3 4 0 755.055 22.9557 22 4 -5 -4 186.250 12.0267 22 1 -3 -2 366.589 8.51684 22 0 -2 12 2376.83 73.9321 22 -1 -3 11 144.709 19.4151 22 5 3 -3 944.896 33.8307 22 -1 -8 5 2074.52 58.8937 22 -2 -3 8 1757.61 57.7823 22 -2 -5 5 793.646 34.8969 22 0 2 6 716.118 23.7135 22 -1 0 8 2549.74 60.9549 22 4 4 -1 14931.4 117.614 22 -2 -6 7 886.198 42.9060 22 -2 -2 5 3594.42 66.0522 22 1 3 6 129.040 8.93819 22 -2 -2 7 3409.89 74.4906 22 -2 -6 8 2680.62 77.5321 22 -2 -4 9 789.189 41.9030 22 1 2 9 2305.04 52.3016 22 -2 -4 4 6508.92 88.7704 22 -1 -3 1 642.844 18.0852 22 4 0 -4 3427.99 58.4216 22 2 -2 -3 32114.1 128.259 22 -1 -9 8 586.828 37.7200 22 0 -8 2 6449.37 75.6552 22 -1 -1 10 510.614 31.8543 22 -2 -2 8 877.096 39.6129 22 4 5 2 169.915 11.0559 22 -1 -9 7 394.592 29.3413 22 -1 -2 11 1288.23 54.2193 22 -1 -6 2 657.657 24.0444 22 -2 -6 5 9513.46 123.300 22 -2 -2 4 36492.4 194.709 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1479.88 36.9202 22 5 -5 -4 1033.07 31.2697 22 -2 -8 7 4854.13 101.778 22 -2 -1 4 582.545 23.3845 22 -2 -2 3 4407.95 61.8769 22 5 3 -2 1065.46 34.4704 22 -2 -3 11 925.360 47.7644 22 3 4 1 298.592 13.2528 22 -2 -5 3 7669.23 91.1496 22 4 4 0 1701.59 37.9473 22 0 2 8 2584.62 52.4174 22 -1 0 10 2107.44 60.5904 22 -1 -10 7 167.759 19.6741 22 0 -10 4 1473.64 44.0903 22 -2 -8 6 437.085 29.3484 22 4 1 -3 6282.13 76.4377 22 -2 -1 9 1010.71 42.8944 22 -3 -4 7 1465.64 53.4277 22 -3 -4 8 3272.22 82.9385 22 5 -1 -4 972.218 33.3096 22 2 4 3 1644.78 17.7700 22 -3 -5 9 1683.64 64.0542 22 -1 -7 2 379.481 18.6906 22 -3 -3 7 1416.59 50.6281 22 -3 -4 9 967.217 47.1377 22 -2 -7 4 2067.60 54.1462 22 -1 -10 6 2566.36 68.5065 22 5 -4 -4 7358.09 86.0211 22 -3 -6 8 629.144 37.8840 22 -1 -1 1 1479.02 22.1039 22 3 -5 -3 1200.62 24.7623 22 -2 -9 8 234.171 24.1381 22 -3 -3 8 691.128 37.0508 22 -2 0 6 126.279 12.4398 22 -3 -5 6 1167.14 45.8465 22 -2 -2 11 2265.48 71.3250 22 -3 -6 7 476.779 31.8390 22 -1 -9 4 438.701 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463.337 33.5648 22 -1 2 7 12357.6 108.131 22 -4 -6 9 889.852 47.5477 22 4 -5 -3 954.968 26.7099 22 -3 -1 5 3947.80 69.2921 22 -4 -6 8 1393.99 57.6292 22 -4 -5 10 1072.04 52.9082 22 -4 -4 7 326.628 25.7094 22 -2 -10 6 2506.62 67.1767 22 -1 -10 4 536.857 26.1902 22 -2 1 6 102.013 10.5231 22 2 -5 -2 1398.64 20.9355 22 0 3 5 2215.22 30.3644 22 -3 -9 7 1764.64 61.6578 22 -2 -6 2 5949.20 73.5271 22 -4 -6 7 2365.46 70.8101 22 -3 -1 10 159.573 18.8718 22 -1 2 5 2358.83 39.4974 22 -2 1 8 527.361 26.6921 22 5 -1 -3 215.452 15.3312 22 2 -1 -2 356.125 12.9021 22 -2 0 11 310.841 24.8984 22 -1 2 8 3798.30 64.2622 22 -2 0 3 8700.34 77.0105 22 4 -2 -3 4053.44 58.5501 22 -3 -4 3 3154.19 59.1616 22 -3 -8 5 1497.58 50.5970 22 -2 1 5 372.298 18.3545 22 4 -4 -3 95.8196 9.20078 22 -4 -3 6 385.096 26.1963 22 5 1 -2 72.8600 9.11439 22 -2 -9 4 1463.19 44.6151 22 -4 -6 6 873.827 41.0575 22 1 -8 0 364.374 8.70455 22 4 -3 -3 1713.69 37.7821 22 4 2 -1 2693.36 46.9393 22 -2 -8 3 3062.77 59.4003 22 -3 -5 3 996.605 34.2200 22 -2 1 9 385.576 24.1865 22 -3 0 7 6948.61 99.1429 22 -3 -9 6 628.607 34.9325 22 -4 -2 8 153.974 17.7572 22 4 4 2 12306.7 93.3397 22 -3 0 8 1419.48 47.6347 22 -3 -1 11 1087.95 48.4799 22 -3 -1 4 418.113 20.9797 22 -4 -2 7 3654.10 80.1404 22 -4 -8 8 402.153 31.3493 22 5 3 0 833.178 28.8496 22 -4 -2 9 1598.62 57.5709 22 5 -2 -3 10637.5 105.081 22 -4 -3 11 654.124 40.6965 22 -3 0 6 3333.09 65.0417 22 2 2 0 16431.9 81.9301 22 -2 -10 5 174.591 17.1790 22 3 -6 -2 4745.71 47.6544 22 -1 2 9 3456.47 63.6946 22 -4 -5 5 123.201 15.1110 22 -3 0 9 1225.91 46.3040 22 5 2 -1 1086.07 33.0073 22 -1 -7 1 607.613 19.1947 22 -4 -2 6 643.070 32.2878 22 -4 -7 6 2368.79 68.2939 22 -4 -2 10 138.568 18.3932 22 5 -3 -3 343.044 19.0220 22 -4 -8 7 1061.17 48.6149 22 2 4 4 10214.0 44.2797 22 -3 -10 7 501.667 32.9948 22 -3 -6 3 2398.25 54.0389 22 0 3 7 1954.80 36.1798 22 -4 -6 5 1044.10 42.3806 22 -2 1 10 949.869 38.6307 22 -1 -3 0 2806.73 28.7594 22 -2 -7 2 514.207 21.8831 22 -3 0 5 16306.5 134.235 22 -1 2 4 6029.57 55.0974 22 -3 0 10 4222.29 88.3029 22 3 4 3 5706.41 51.5891 22 -1 -4 0 1474.62 22.3975 22 -3 -9 5 806.727 36.5925 22 -5 -5 9 876.240 47.1973 22 -3 -8 4 703.185 31.8864 22 -2 -4 1 4938.91 55.6457 22 -4 -1 8 295.940 23.6207 22 -4 -2 5 131.689 14.0898 22 -5 -6 9 624.809 40.4178 22 -4 -1 7 236.339 20.0927 22 -1 1 2 2323.52 27.3009 22 -5 -4 9 1724.51 65.0063 22 2 -2 -2 9871.73 64.9344 22 -4 -1 9 719.987 37.6971 22 -4 -8 6 1720.81 58.2200 22 -5 -4 8 821.188 43.2822 22 -5 -4 10 655.634 41.3073 22 -5 -6 8 2030.19 69.5483 22 3 3 1 412.481 15.4390 22 0 3 8 553.940 20.7831 22 -4 -4 4 2523.53 59.5417 22 -4 -5 4 2887.77 65.0603 22 -5 -5 7 4506.18 98.3571 22 -4 -1 6 2012.89 54.6856 22 -3 0 11 497.053 31.4613 22 -5 -3 9 1370.68 56.3643 22 -3 -7 3 979.877 34.6384 22 -5 -3 8 1344.93 53.8110 22 0 3 4 2016.16 21.8318 22 -3 -1 3 2111.16 43.0618 22 -2 -5 1 7729.04 71.2055 22 6 3 1 229.671 16.4827 22 5 4 3 1278.39 33.4260 22 4 4 3 1281.17 29.4810 22 -5 -3 10 510.174 35.8301 22 0 -7 0 217.773 7.62594 22 -3 -4 2 4731.65 65.8013 22 -3 0 4 13839.9 114.541 22 -4 -6 4 461.372 26.7562 22 -2 -9 3 1065.25 33.7943 22 4 3 1 1947.30 38.2594 22 5 3 1 93.4179 9.76557 22 -3 -3 2 1631.24 37.8049 22 -5 -5 6 664.809 36.4915 22 -5 -7 7 1387.14 56.3275 22 3 2 0 4721.56 52.9754 22 -4 -1 5 135.732 13.7175 22 -1 -2 0 765.185 13.7085 22 2 -3 -2 3078.01 35.3571 22 -3 -5 2 575.248 23.6944 22 -4 -2 4 10076.9 112.474 22 -1 -5 0 39.2856 4.03961 22 6 2 0 5296.68 77.7697 22 -4 -8 5 463.450 28.9474 22 -2 2 7 87.0345 9.81816 22 -5 -6 6 485.689 31.4822 22 2 -4 -2 12965.5 69.5567 22 -5 -2 8 3690.41 87.3135 22 -5 -2 9 559.941 35.6910 22 -3 1 9 2278.57 59.5296 22 -5 -3 6 476.765 30.0906 22 -2 2 8 423.378 22.2251 22 -3 1 6 742.318 29.3397 22 -4 0 8 481.284 28.7965 22 -5 -2 10 1476.74 58.6335 22 -5 -2 7 2620.81 70.4606 22 -2 2 6 2457.00 46.8178 22 -4 0 7 2368.30 60.9535 22 4 2 0 5327.17 64.4056 22 -4 0 9 180.342 18.5517 22 1 2 1 92.1967 4.06123 22 -3 -10 5 1137.90 41.9730 22 -2 -8 2 662.801 24.1543 22 4 -6 -2 180.594 11.6436 22 5 -6 -2 6524.04 77.9599 22 -2 2 9 61.5411 9.59624 22 3 -2 -2 15116.6 97.0459 22 -3 1 10 250.684 21.0012 22 -2 1 3 8.45347 3.28570 22 -4 0 10 4371.85 92.2077 22 -3 1 5 257.116 16.3365 22 3 -5 -2 379.385 14.7142 22 -2 2 5 71.0690 7.67080 22 4 -5 -2 2309.40 42.3431 22 -1 2 3 3605.51 35.7159 22 -1 3 7 262.985 14.0154 22 -4 4 -10 31.4258 9.03780 23 -2 5 4 50.1194 6.91459 23 -6 4 -5 40.4767 7.32945 23 -1 1 -9 95.8001 13.5091 23 2 2 -12 1.92046 5.06841 23 -4 3 -9 3.41669 4.51352 23 -6 5 -8 44.4206 10.0179 23 -4 2 -7 8.24468 4.34212 23 -1 2 -11 15.7173 7.59647 23 0 1 -10 76.3534 13.0334 23 1 2 -12 95.6336 15.2679 23 3 2 3 44.6321 6.36327 23 3 1 2 3.91866 2.30564 23 2 -1 -4 36.1401 5.22731 23 2 1 -11 62.9939 12.3163 23 6 0 -7 30.8828 5.86973 23 -3 1 -7 20.8063 6.64879 23 3 -1 -4 13.3123 3.46271 23 4 1 -11 57.9561 11.0093 23 4 0 0 31441.6 93.0679 23 2 -1 -3 10.2859 2.89776 23 -6 4 -7 9.35922 4.81216 23 5 1 1 3.50772 2.54429 23 -4 2 -8 86.3224 12.4452 23 -5 3 -8 91.6578 13.0717 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