data_shelx _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al1.50 H6.25 As0.75 O8' _chemical_formula_weight 230.96 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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.7730(16) _cell_length_b 26.991(5) _cell_length_c 15.867(3) _cell_angle_alpha 90 _cell_angle_beta 94.22(3) _cell_angle_gamma 90 _cell_volume 3319.9(12) _cell_formula_units_Z 16 _cell_measurement_temperature 293(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 1.848 _exptl_crystal_F_000 1832 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_absorpt_coefficient_mu 3.264 _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 293(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 22571 _diffrn_reflns_av_unetI/netI 0.0724 _diffrn_reflns_av_R_equivalents 0.1565 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.492 _diffrn_reflns_theta_max 19.979 _diffrn_reflns_theta_full 19.979 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measured_fraction_theta_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_point_group_measured_fraction_full 0.971 _reflns_number_total 3005 _reflns_number_gt 2164 _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-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+127.0000P] 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-2014/7 (Sheldrick 2014' _refine_ls_extinction_coef 0.0017(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3005 _refine_ls_number_parameters 414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2412 _refine_ls_wR_factor_gt 0.2124 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.336 _refine_ls_shift/su_mean 0.026 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 As01 As 1.0063(2) 0.60175(8) 0.55313(14) 0.0292(7) Uani 1 1 d . . . . . As02 As 0.5135(2) 0.68821(9) 0.52145(14) 0.0310(8) Uani 1 1 d . . . . . As03 As 0.2977(2) 0.72405(9) 0.25880(14) 0.0310(8) Uani 1 1 d . . . . . Al01 Al 0.6365(7) 0.5758(2) 0.4679(4) 0.0271(16) Uani 1 1 d . . . . . Al02 Al 0.3726(7) 0.6227(2) 0.3561(4) 0.0265(16) Uani 1 1 d . . . . . Al03 Al 0.1443(7) 0.7146(2) 0.6055(4) 0.0257(16) Uani 1 1 d . . . . . Al04 Al 0.1176(7) 0.6923(2) 0.4238(4) 0.0277(16) Uani 1 1 d . . . . . Al05 Al 0.6653(7) 0.6005(3) 0.6518(4) 0.0299(17) Uani 1 1 d . . . . . Al06 Al 0.4244(7) 0.6684(3) 0.7198(4) 0.0314(17) Uani 1 1 d . . . . . O01 O 0.9055(14) 0.6051(5) 0.6406(8) 0.024(3) Uani 1 1 d . . . . . O02 O 1.1817(15) 0.5672(6) 0.5674(10) 0.040(4) Uani 1 1 d . . . . . O03 O 0.8786(15) 0.5797(5) 0.4730(8) 0.028(3) Uani 1 1 d . . . . . O04 O 0.0678(15) 0.6597(5) 0.5292(8) 0.026(3) Uani 1 1 d . . . . . O05 O 0.652(2) 0.7300(9) 0.5011(14) 0.087(7) Uani 1 1 d . . . . . O06 O 0.3909(15) 0.6981(5) 0.6023(9) 0.032(4) Uani 1 1 d . . . . . O07 O 0.3662(15) 0.6771(5) 0.4386(8) 0.026(3) Uani 1 1 d . . . . . O08 O 0.6192(18) 0.6338(5) 0.5427(8) 0.035(4) Uani 1 1 d . . . . . O09 O 0.1576(15) 0.7335(5) 0.3309(8) 0.032(4) Uani 1 1 d . . . . . O10 O 0.1956(16) 0.7256(5) 0.1626(9) 0.033(4) Uani 1 1 d . . . . . O11 O 0.3880(18) 0.6681(5) 0.2681(8) 0.032(4) Uani 1 1 d . . . . . O12 O 0.4545(15) 0.7670(6) 0.2666(9) 0.037(4) Uani 1 1 d . . . . . OH1 O 0.3986(15) 0.5745(5) 0.4434(8) 0.024(3) Uani 1 1 d . . . . . OH2 O 0.6111(16) 0.6146(5) 0.3691(9) 0.034(4) Uani 1 1 d . . . . . OH3 O 0.6362(15) 0.5456(5) 0.5765(8) 0.026(3) Uani 1 1 d . . . . . OH4 O 0.1334(15) 0.6327(5) 0.3647(8) 0.029(3) Uani 1 1 d . . . . . OH5 O 0.1836(15) 0.6758(5) 0.7019(8) 0.030(4) Uani 1 1 d . . . . . OH6 O 0.1403(15) 0.7448(5) 0.4995(8) 0.031(4) Uani 1 1 d . . . . . OH7 O 0.4343(15) 0.6036(5) 0.6769(8) 0.028(3) Uani 1 1 d . . . . . OH8 O 0.6617(15) 0.6597(5) 0.7118(8) 0.034(4) Uani 1 1 d . . . . . OW1 O 0.6490(16) 0.5141(5) 0.4108(9) 0.033(4) Uani 1 1 d . . . . . OW2 O 0.3222(16) 0.5696(6) 0.2749(9) 0.038(4) Uani 1 1 d . . . . . OW3 O 0.9066(15) 0.7252(5) 0.6224(8) 0.030(3) Uani 1 1 d . . . . . OW4 O 0.8752(16) 0.6993(5) 0.3948(8) 0.035(4) Uani 1 1 d . . . . . OW5 O 0.7190(17) 0.5586(6) 0.7479(8) 0.037(4) Uani 1 1 d . . . . . OW6 O 0.4118(17) 0.6424(6) 0.8303(9) 0.040(4) Uani 1 1 d . . . . . W1 O 0.0792(17) 0.5180(5) 0.3643(9) 0.033(3) Uiso 1 1 d . . . . . W2 O 0.7545(17) 0.7811(5) 0.7365(9) 0.038(4) Uiso 1 1 d . . . . . W3 O 0.943(2) 0.8176(7) 0.3332(11) 0.060(5) Uiso 1 1 d . . . . . W4 O 0.418(3) 0.6888(8) 0.9772(13) 0.079(6) Uiso 1 1 d . . . . . W5 O 0.546(5) 0.6438(13) 1.123(2) 0.081(6) Uiso 0.62(4) 1 d . U . . . W6 O 0.859(6) 0.619(4) 0.228(4) 0.081(6) Uiso 0.47(12) 1 d . U . . . W7 O 0.482(5) 0.5447(15) 0.863(2) 0.081(6) Uiso 0.54(4) 1 d . U . . . W8 O 0.840(7) 0.467(2) 0.259(3) 0.081(6) Uiso 0.44(5) 1 d . U . . . W9 O 0.011(5) 0.6466(15) 0.103(2) 0.081(6) Uiso 0.54(4) 1 d . U . . . W10 O 1.006(5) 0.5828(15) 0.854(3) 0.081(6) Uiso 0.50(4) 1 d . U . . . W11 O 0.659(11) 0.505(3) 0.171(6) 0.081(6) Uiso 0.27(4) 1 d . U . . . W12 O 0.472(12) 0.494(3) 0.791(6) 0.081(6) Uiso 0.23(4) 1 d . U . . . W13 O 0.432(9) 0.626(2) 0.101(4) 0.081(6) Uiso 0.34(4) 1 d . U . . . W14 O 0.782(8) 0.799(3) 0.485(4) 0.081(6) Uiso 0.33(4) 1 d . U . . . W15 O 0.836(11) 0.836(4) 0.495(5) 0.081(6) Uiso 0.25(4) 1 d . U . . . W16 O 0.188(11) 0.565(3) 0.113(6) 0.081(6) Uiso 0.22(4) 1 d . U . . . W17 O 0.120(7) 0.625(2) 0.121(3) 0.081(6) Uiso 0.40(4) 1 d . U . . . W18 O 0.929(12) 0.452(3) 0.230(5) 0.081(6) Uiso 0.26(4) 1 d . U . . . W19 O 0.577(12) 0.503(4) 0.116(7) 0.081(6) Uiso 0.22(4) 1 d . U . . . W20 O 0.781(14) 0.504(4) 0.239(6) 0.081(6) Uiso 0.22(4) 1 d . U . . . W21 O 0.685(12) 0.533(4) 0.240(5) 0.081(6) Uiso 0.24(4) 1 d . U . . . W22 O 0.867(7) 0.598(4) 0.247(4) 0.081(6) Uiso 0.45(12) 1 d . U . . . W23 O 0.555(15) 0.531(4) 0.955(7) 0.081(6) Uiso 0.17(4) 1 d . U . . . W24 O 0.659(15) 0.550(5) 0.093(7) 0.081(6) Uiso 0.17(4) 1 d . U . . . 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 As01 0.0162(12) 0.0374(15) 0.0340(15) -0.0004(11) 0.0027(9) -0.0029(10) As02 0.0130(12) 0.0483(17) 0.0318(15) -0.0020(11) 0.0019(9) 0.0022(10) As03 0.0174(12) 0.0422(16) 0.0339(15) 0.0031(11) 0.0042(9) 0.0018(10) Al01 0.009(3) 0.035(4) 0.038(4) 0.000(3) 0.001(3) 0.004(3) Al02 0.011(3) 0.036(4) 0.032(4) -0.001(3) 0.002(3) 0.002(3) Al03 0.014(3) 0.034(4) 0.029(4) 0.000(3) 0.002(3) -0.002(3) Al04 0.015(3) 0.036(4) 0.031(4) 0.001(3) 0.001(3) 0.000(3) Al05 0.015(3) 0.039(4) 0.036(4) 0.000(3) 0.006(3) 0.000(3) Al06 0.010(3) 0.044(4) 0.040(4) -0.004(3) 0.002(3) -0.002(3) O01 0.014(7) 0.034(9) 0.025(8) -0.008(6) 0.000(5) -0.002(6) O02 0.010(7) 0.045(10) 0.066(11) 0.010(8) 0.005(7) -0.010(7) O03 0.019(7) 0.026(8) 0.040(9) 0.000(7) 0.000(6) 0.002(6) O04 0.021(7) 0.035(9) 0.021(8) -0.010(6) -0.015(6) 0.002(6) O05 0.044(11) 0.118(19) 0.096(16) 0.006(13) -0.009(10) 0.006(11) O06 0.015(7) 0.028(9) 0.052(10) 0.004(7) 0.008(6) -0.001(6) O07 0.016(7) 0.029(9) 0.035(9) 0.000(7) 0.005(6) 0.007(6) O08 0.050(9) 0.031(9) 0.022(8) 0.008(7) 0.003(6) 0.005(7) O09 0.014(7) 0.050(10) 0.031(9) -0.003(7) -0.005(6) -0.001(6) O10 0.021(7) 0.038(10) 0.042(9) -0.002(7) 0.009(6) 0.004(6) O11 0.050(9) 0.027(9) 0.020(8) 0.002(6) 0.013(7) -0.006(7) O12 0.002(7) 0.058(11) 0.052(10) 0.005(8) 0.001(6) 0.001(6) OH1 0.022(7) 0.021(8) 0.027(8) -0.002(6) -0.008(6) -0.001(6) OH2 0.021(8) 0.039(10) 0.043(9) 0.003(7) 0.007(6) 0.009(6) OH3 0.021(7) 0.026(9) 0.031(8) 0.000(6) 0.004(6) -0.002(6) OH4 0.016(7) 0.035(9) 0.036(9) 0.004(7) 0.005(6) -0.001(6) OH5 0.020(8) 0.045(10) 0.025(8) -0.006(7) -0.003(6) 0.002(6) OH6 0.012(7) 0.042(10) 0.039(9) -0.004(7) -0.005(6) 0.005(6) OH7 0.013(7) 0.044(9) 0.025(8) 0.010(7) 0.001(6) -0.001(6) OH8 0.018(8) 0.052(10) 0.031(9) -0.002(7) 0.004(6) 0.003(7) OW1 0.027(8) 0.039(9) 0.034(9) 0.004(7) 0.008(6) 0.001(7) OW2 0.022(8) 0.052(11) 0.039(9) -0.017(8) 0.003(6) 0.001(7) OW3 0.010(7) 0.047(10) 0.034(9) 0.005(7) 0.007(6) 0.000(6) OW4 0.020(8) 0.055(11) 0.030(9) 0.003(7) 0.002(6) 0.004(7) OW5 0.033(8) 0.051(10) 0.028(9) 0.004(7) 0.007(6) 0.000(7) OW6 0.031(8) 0.052(11) 0.036(9) 0.002(8) -0.002(7) 0.009(7) _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 As01 O01 1.645(12) . ? As01 O02 1.654(14) . ? As01 O03 1.663(13) . ? As01 O04 1.686(14) 1_655 ? As02 O05 1.61(2) . ? As02 O06 1.675(13) . ? As02 O07 1.705(13) . ? As02 O08 1.704(14) . ? As03 O09 1.656(13) . ? As03 O10 1.669(14) . ? As03 O11 1.668(14) . ? As03 O12 1.680(14) . ? Al01 OH1 1.862(13) . ? Al01 O03 1.880(13) . ? Al01 OH2 1.882(15) . ? Al01 OH3 1.908(14) . ? Al01 OW1 1.903(15) . ? Al01 O08 1.975(15) . ? Al01 Al02 2.901(8) . ? Al01 Al05 2.986(9) . ? Al02 OH2 1.863(13) . ? Al02 O11 1.868(14) . ? Al02 OH1 1.899(14) . ? Al02 OH4 1.894(13) . ? Al02 OW2 1.947(15) . ? Al02 O07 1.970(14) . ? Al02 Al04 2.988(8) . ? Al03 OH5 1.859(15) . ? Al03 OH6 1.868(15) . ? Al03 O10 1.879(15) 4_576 ? Al03 OW3 1.907(13) 1_455 ? Al03 O04 1.978(13) . ? Al03 O06 1.973(13) . ? Al03 Al04 2.938(9) . ? Al04 OH6 1.858(15) . ? Al04 OH4 1.872(15) . ? Al04 O09 1.891(15) . ? Al04 OW4 1.916(13) 1_455 ? Al04 O04 1.954(15) . ? Al04 O07 1.972(13) . ? Al05 OH7 1.870(13) . ? Al05 OH8 1.860(16) . ? Al05 O01 1.892(12) . ? Al05 OH3 1.908(14) . ? Al05 OW5 1.920(15) . ? Al05 O08 1.961(14) . ? Al05 Al06 2.886(9) . ? Al06 OH8 1.872(13) . ? Al06 OH7 1.882(16) . ? Al06 O12 1.902(16) 4_576 ? Al06 OH5 1.884(13) . ? Al06 OW6 1.898(15) . ? Al06 O06 2.028(15) . ? O04 As01 1.686(14) 1_455 ? O10 Al03 1.879(15) 4_575 ? O12 Al06 1.902(16) 4_575 ? OW3 Al03 1.907(12) 1_655 ? OW4 Al04 1.916(13) 1_655 ? W5 W13 1.05(6) 1_556 ? W6 W22 0.64(7) . ? W7 W19 1.42(10) 3_666 ? W7 W23 1.57(12) . ? W7 W12 1.77(10) . ? W8 W18 0.94(8) . ? W8 W20 1.14(11) . ? W9 W17 1.04(5) . ? W10 W18 1.74(11) 3_766 ? W11 W19 1.04(10) . ? W11 W12 1.22(10) 3_666 ? W11 W21 1.34(11) . ? W11 W20 1.38(13) . ? W11 W24 1.72(15) . ? W12 W11 1.22(10) 3_666 ? W12 W21 1.48(12) 3_666 ? W12 W19 1.54(13) 3_666 ? W13 W5 1.05(6) 1_554 ? W14 W15 1.08(9) . ? W16 W17 1.71(11) . ? W18 W10 1.74(11) 3_766 ? W19 W7 1.42(10) 3_666 ? W19 W24 1.47(15) . ? W19 W12 1.54(13) 3_666 ? W20 W21 1.09(12) . ? W21 W12 1.48(12) 3_666 ? 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 O01 As01 O02 110.7(7) . . ? O01 As01 O03 111.7(6) . . ? O02 As01 O03 110.1(7) . . ? O01 As01 O04 107.5(6) . 1_655 ? O02 As01 O04 108.0(6) . 1_655 ? O03 As01 O04 108.8(6) . 1_655 ? O05 As02 O06 118.0(9) . . ? O05 As02 O07 113.0(8) . . ? O06 As02 O07 103.4(6) . . ? O05 As02 O08 108.9(9) . . ? O06 As02 O08 106.2(6) . . ? O07 As02 O08 106.7(7) . . ? O09 As03 O10 109.6(6) . . ? O09 As03 O11 111.9(7) . . ? O10 As03 O11 105.8(7) . . ? O09 As03 O12 110.7(7) . . ? O10 As03 O12 110.1(7) . . ? O11 As03 O12 108.7(7) . . ? OH1 Al01 O03 170.3(7) . . ? OH1 Al01 OH2 78.2(6) . . ? O03 Al01 OH2 92.8(6) . . ? OH1 Al01 OH3 96.5(6) . . ? O03 Al01 OH3 93.0(6) . . ? OH2 Al01 OH3 169.5(7) . . ? OH1 Al01 OW1 88.2(6) . . ? O03 Al01 OW1 89.1(6) . . ? OH2 Al01 OW1 95.5(7) . . ? OH3 Al01 OW1 93.3(6) . . ? OH1 Al01 O08 91.7(6) . . ? O03 Al01 O08 92.4(6) . . ? OH2 Al01 O08 93.0(6) . . ? OH3 Al01 O08 78.0(6) . . ? OW1 Al01 O08 171.2(7) . . ? OH1 Al01 Al02 40.0(4) . . ? O03 Al01 Al02 131.5(5) . . ? OH2 Al01 Al02 39.0(4) . . ? OH3 Al01 Al02 133.7(4) . . ? OW1 Al01 Al02 98.6(5) . . ? O08 Al01 Al02 86.9(5) . . ? OH1 Al01 Al05 102.1(5) . . ? O03 Al01 Al05 86.7(5) . . ? OH2 Al01 Al05 133.3(5) . . ? OH3 Al01 Al05 38.5(4) . . ? OW1 Al01 Al05 131.1(5) . . ? O08 Al01 Al05 40.5(4) . . ? Al02 Al01 Al05 119.9(3) . . ? OH2 Al02 O11 92.4(7) . . ? OH2 Al02 OH1 77.7(6) . . ? O11 Al02 OH1 170.0(6) . . ? OH2 Al02 OH4 169.5(7) . . ? O11 Al02 OH4 94.4(6) . . ? OH1 Al02 OH4 95.6(6) . . ? OH2 Al02 OW2 97.9(6) . . ? O11 Al02 OW2 90.5(7) . . ? OH1 Al02 OW2 89.2(6) . . ? OH4 Al02 OW2 90.1(6) . . ? OH2 Al02 O07 95.1(6) . . ? O11 Al02 O07 90.8(6) . . ? OH1 Al02 O07 91.8(6) . . ? OH4 Al02 O07 76.9(6) . . ? OW2 Al02 O07 166.9(6) . . ? OH2 Al02 Al01 39.5(5) . . ? O11 Al02 Al01 131.4(5) . . ? OH1 Al02 Al01 39.1(4) . . ? OH4 Al02 Al01 132.2(5) . . ? OW2 Al02 Al01 100.6(5) . . ? O07 Al02 Al01 88.3(4) . . ? OH2 Al02 Al04 135.7(5) . . ? O11 Al02 Al04 86.4(5) . . ? OH1 Al02 Al04 101.9(5) . . ? OH4 Al02 Al04 37.2(4) . . ? OW2 Al02 Al04 126.4(5) . . ? O07 Al02 Al04 40.8(4) . . ? Al01 Al02 Al04 120.8(3) . . ? OH5 Al03 OH6 167.7(7) . . ? OH5 Al03 O10 94.1(7) . 4_576 ? OH6 Al03 O10 92.7(7) . 4_576 ? OH5 Al03 OW3 94.1(6) . 1_455 ? OH6 Al03 OW3 96.3(6) . 1_455 ? O10 Al03 OW3 88.7(6) 4_576 1_455 ? OH5 Al03 O04 96.0(6) . . ? OH6 Al03 O04 78.0(6) . . ? O10 Al03 O04 169.3(7) 4_576 . ? OW3 Al03 O04 87.0(6) 1_455 . ? OH5 Al03 O06 78.0(6) . . ? OH6 Al03 O06 91.6(6) . . ? O10 Al03 O06 92.0(6) 4_576 . ? OW3 Al03 O06 172.1(7) 1_455 . ? O04 Al03 O06 93.6(6) . . ? OH5 Al03 Al04 133.4(5) . . ? OH6 Al03 Al04 37.8(5) . . ? O10 Al03 Al04 130.2(5) 4_576 . ? OW3 Al03 Al04 99.7(5) 1_455 . ? O04 Al03 Al04 41.3(4) . . ? O06 Al03 Al04 85.8(5) . . ? OH6 Al04 OH4 166.8(7) . . ? OH6 Al04 O09 92.4(7) . . ? OH4 Al04 O09 95.4(6) . . ? OH6 Al04 OW4 97.2(6) . 1_455 ? OH4 Al04 OW4 93.7(6) . 1_455 ? O09 Al04 OW4 88.3(6) . 1_455 ? OH6 Al04 O04 78.8(6) . . ? OH4 Al04 O04 93.8(6) . . ? O09 Al04 O04 170.7(7) . . ? OW4 Al04 O04 89.8(6) 1_455 . ? OH6 Al04 O07 92.1(6) . . ? OH4 Al04 O07 77.3(6) . . ? O09 Al04 O07 90.0(6) . . ? OW4 Al04 O07 170.6(7) 1_455 . ? O04 Al04 O07 93.3(6) . . ? OH6 Al04 Al03 38.1(5) . . ? OH4 Al04 Al03 131.7(5) . . ? O09 Al04 Al03 129.9(5) . . ? OW4 Al04 Al03 102.3(5) 1_455 . ? O04 Al04 Al03 42.0(4) . . ? O07 Al04 Al03 85.9(4) . . ? OH6 Al04 Al02 132.7(5) . . ? OH4 Al04 Al02 37.7(4) . . ? O09 Al04 Al02 86.5(5) . . ? OW4 Al04 Al02 130.0(5) 1_455 . ? O04 Al04 Al02 101.7(5) . . ? O07 Al04 Al02 40.7(4) . . ? Al03 Al04 Al02 118.7(3) . . ? OH7 Al05 OH8 78.6(6) . . ? OH7 Al05 O01 170.8(7) . . ? OH8 Al05 O01 92.6(6) . . ? OH7 Al05 OH3 95.5(6) . . ? OH8 Al05 OH3 169.2(7) . . ? O01 Al05 OH3 93.7(6) . . ? OH7 Al05 OW5 90.8(6) . . ? OH8 Al05 OW5 96.4(7) . . ? O01 Al05 OW5 87.4(6) . . ? OH3 Al05 OW5 92.7(6) . . ? OH7 Al05 O08 93.0(6) . . ? OH8 Al05 O08 92.8(7) . . ? O01 Al05 O08 90.2(6) . . ? OH3 Al05 O08 78.3(6) . . ? OW5 Al05 O08 170.6(7) . . ? OH7 Al05 Al06 39.9(5) . . ? OH8 Al05 Al06 39.5(4) . . ? O01 Al05 Al06 131.8(5) . . ? OH3 Al05 Al06 132.7(5) . . ? OW5 Al05 Al06 100.8(5) . . ? O08 Al05 Al06 87.6(5) . . ? OH7 Al05 Al01 102.3(5) . . ? OH8 Al05 Al01 133.5(5) . . ? O01 Al05 Al01 85.7(4) . . ? OH3 Al05 Al01 38.5(4) . . ? OW5 Al05 Al01 129.9(5) . . ? O08 Al05 Al01 40.8(4) . . ? Al06 Al05 Al01 120.2(3) . . ? OH8 Al06 OH7 78.0(6) . . ? OH8 Al06 O12 92.8(6) . 4_576 ? OH7 Al06 O12 170.6(6) . 4_576 ? OH8 Al06 OH5 167.4(7) . . ? OH7 Al06 OH5 96.4(6) . . ? O12 Al06 OH5 93.1(6) 4_576 . ? OH8 Al06 OW6 97.7(6) . . ? OH7 Al06 OW6 89.8(7) . . ? O12 Al06 OW6 89.6(7) 4_576 . ? OH5 Al06 OW6 93.5(6) . . ? OH8 Al06 O06 92.7(6) . . ? OH7 Al06 O06 92.3(6) . . ? O12 Al06 O06 90.1(7) 4_576 . ? OH5 Al06 O06 76.1(6) . . ? OW6 Al06 O06 169.5(6) . . ? OH8 Al06 Al05 39.2(5) . . ? OH7 Al06 Al05 39.6(4) . . ? O12 Al06 Al05 131.6(4) 4_576 . ? OH5 Al06 Al05 132.5(5) . . ? OW6 Al06 Al05 100.9(5) . . ? O06 Al06 Al05 87.1(4) . . ? As01 O01 Al05 127.6(7) . . ? As01 O03 Al01 126.3(8) . . ? As01 O04 Al04 133.4(7) 1_455 . ? As01 O04 Al03 129.4(7) 1_455 . ? Al04 O04 Al03 96.7(6) . . ? As02 O06 Al03 131.6(8) . . ? As02 O06 Al06 126.9(7) . . ? Al03 O06 Al06 97.2(6) . . ? As02 O07 Al02 126.5(7) . . ? As02 O07 Al04 130.7(7) . . ? Al02 O07 Al04 98.5(6) . . ? As02 O08 Al05 128.6(8) . . ? As02 O08 Al01 128.1(8) . . ? Al05 O08 Al01 98.7(7) . . ? As03 O09 Al04 127.0(8) . . ? As03 O10 Al03 122.1(8) . 4_575 ? As03 O11 Al02 127.6(8) . . ? As03 O12 Al06 122.4(7) . 4_575 ? Al01 OH1 Al02 100.9(6) . . ? Al02 OH2 Al01 101.5(7) . . ? Al01 OH3 Al05 103.0(7) . . ? Al04 OH4 Al02 105.0(7) . . ? Al03 OH5 Al06 106.6(7) . . ? Al04 OH6 Al03 104.1(7) . . ? Al05 OH7 Al06 100.5(6) . . ? Al06 OH8 Al05 101.2(7) . . ? W19 W7 W23 71(7) 3_666 . ? W19 W7 W12 57(5) 3_666 . ? W23 W7 W12 115(6) . . ? W18 W8 W20 122(10) . . ? W19 W11 W12 86(9) . 3_666 ? W19 W11 W21 139(10) . . ? W12 W11 W21 70(7) 3_666 . ? W19 W11 W20 174(10) . . ? W12 W11 W20 99(9) 3_666 . ? W21 W11 W20 47(6) . . ? W19 W11 W24 58(8) . . ? W12 W11 W24 112(8) 3_666 . ? W21 W11 W24 100(7) . . ? W20 W11 W24 122(8) . . ? W11 W12 W21 59(6) 3_666 3_666 ? W11 W12 W19 42(5) 3_666 3_666 ? W21 W12 W19 95(7) 3_666 3_666 ? W11 W12 W7 71(6) 3_666 . ? W21 W12 W7 127(7) 3_666 . ? W19 W12 W7 50(5) 3_666 . ? W9 W17 W16 138(6) . . ? W8 W18 W10 150(9) . 3_766 ? W11 W19 W7 92(9) . 3_666 ? W11 W19 W24 85(10) . . ? W7 W19 W24 173(9) 3_666 . ? W11 W19 W12 52(7) . 3_666 ? W7 W19 W12 73(6) 3_666 3_666 ? W24 W19 W12 110(9) . 3_666 ? W21 W20 W8 154(10) . . ? W21 W20 W11 65(8) . . ? W8 W20 W11 119(9) . . ? W20 W21 W11 68(8) . . ? W20 W21 W12 100(10) . 3_666 ? W11 W21 W12 51(5) . 3_666 ? W19 W24 W11 37(5) . . ? _refine_diff_density_max 1.164 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.183 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL p21onc_a.res in P2(1)/c REM Old TITL p21onc in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.204, Rweak 0.027, Alpha 0.069, Orientation as input REM Formula found by SHELXT: O32 Al6 As3 CELL 0.71073 7.7730 26.9910 15.8670 90.000 94.221 90.000 ZERR 16.000 0.0016 0.0054 0.0032 0.000 0.030 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC O H AL AS UNIT 128 100 24 12 SHEL 20 1.04 L.S. 4 ACTA BOND $H LIST 4 FMAP 2 PLAN 20 WGHT 0.140000 127.000000 EXTI 0.001693 FVAR 0.25085 0.08070 AS01 4 1.006259 0.601750 0.553130 11.00000 0.01619 0.03736 = 0.03403 -0.00038 0.00272 -0.00287 AS02 4 0.513492 0.688210 0.521448 11.00000 0.01302 0.04826 = 0.03183 -0.00202 0.00194 0.00217 AS03 4 0.297741 0.724052 0.258799 11.00000 0.01735 0.04220 = 0.03388 0.00305 0.00419 0.00175 AL01 3 0.636536 0.575849 0.467881 11.00000 0.00863 0.03474 = 0.03789 -0.00017 0.00099 0.00390 AL02 3 0.372625 0.622679 0.356117 11.00000 0.01058 0.03645 = 0.03247 -0.00114 0.00157 0.00207 AL03 3 0.144271 0.714612 0.605530 11.00000 0.01384 0.03448 = 0.02877 0.00046 0.00170 -0.00245 AL04 3 0.117590 0.692292 0.423800 11.00000 0.01507 0.03644 = 0.03148 0.00062 0.00106 0.00027 AL05 3 0.665336 0.600521 0.651846 11.00000 0.01513 0.03888 = 0.03636 0.00020 0.00640 -0.00013 AL06 3 0.424446 0.668423 0.719839 11.00000 0.01020 0.04436 = 0.03983 -0.00360 0.00239 -0.00213 O01 1 0.905499 0.605068 0.640589 11.00000 0.01399 0.03361 = 0.02520 -0.00820 0.00016 -0.00231 O02 1 1.181654 0.567190 0.567448 11.00000 0.00979 0.04488 = 0.06642 0.01025 0.00471 -0.00955 O03 1 0.878614 0.579743 0.473049 11.00000 0.01914 0.02556 = 0.03962 -0.00009 0.00023 0.00225 O04 1 0.067849 0.659676 0.529222 11.00000 0.02094 0.03451 = 0.02075 -0.00990 -0.01513 0.00233 O05 1 0.652179 0.730018 0.501141 11.00000 0.04371 0.11846 = 0.09611 0.00638 -0.00939 0.00596 O06 1 0.390927 0.698058 0.602348 11.00000 0.01548 0.02767 = 0.05231 0.00445 0.00799 -0.00065 O07 1 0.366164 0.677088 0.438615 11.00000 0.01563 0.02857 = 0.03510 0.00002 0.00520 0.00709 O08 1 0.619243 0.633829 0.542692 11.00000 0.05029 0.03133 = 0.02242 0.00820 0.00263 0.00512 O09 1 0.157571 0.733508 0.330867 11.00000 0.01431 0.04990 = 0.03053 -0.00272 -0.00484 -0.00117 O10 1 0.195594 0.725574 0.162575 11.00000 0.02104 0.03789 = 0.04181 -0.00165 0.00851 0.00380 O11 1 0.388005 0.668055 0.268105 11.00000 0.05023 0.02731 = 0.01983 0.00247 0.01321 -0.00558 O12 1 0.454542 0.767012 0.266586 11.00000 0.00200 0.05792 = 0.05240 0.00482 0.00117 0.00075 OH1 1 0.398568 0.574546 0.443404 11.00000 0.02246 0.02142 = 0.02655 -0.00150 -0.00841 -0.00056 OH2 1 0.611144 0.614551 0.369088 11.00000 0.02096 0.03914 = 0.04341 0.00271 0.00656 0.00854 OH3 1 0.636194 0.545554 0.576548 11.00000 0.02079 0.02597 = 0.03132 0.00034 0.00406 -0.00177 OH4 1 0.133385 0.632659 0.364668 11.00000 0.01565 0.03528 = 0.03581 0.00357 0.00497 -0.00136 OH5 1 0.183571 0.675846 0.701904 11.00000 0.02028 0.04487 = 0.02470 -0.00631 -0.00265 0.00212 OH6 1 0.140346 0.744830 0.499477 11.00000 0.01166 0.04221 = 0.03930 -0.00433 -0.00461 0.00481 OH7 1 0.434275 0.603560 0.676881 11.00000 0.01342 0.04429 = 0.02526 0.00997 0.00084 -0.00145 OH8 1 0.661661 0.659693 0.711825 11.00000 0.01774 0.05194 = 0.03128 -0.00214 0.00358 0.00304 OW1 1 0.648951 0.514084 0.410837 11.00000 0.02748 0.03854 = 0.03443 0.00450 0.00838 0.00056 OW2 1 0.322158 0.569647 0.274876 11.00000 0.02221 0.05212 = 0.03938 -0.01683 0.00253 0.00057 OW3 1 0.906609 0.725195 0.622380 11.00000 0.00992 0.04728 = 0.03390 0.00484 0.00736 0.00010 OW4 1 0.875192 0.699278 0.394810 11.00000 0.02017 0.05458 = 0.02965 0.00279 0.00153 0.00396 OW5 1 0.719049 0.558563 0.747935 11.00000 0.03332 0.05101 = 0.02787 0.00440 0.00700 -0.00039 OW6 1 0.411759 0.642377 0.830318 11.00000 0.03140 0.05236 = 0.03595 0.00183 -0.00159 0.00870 W1 1 0.079183 0.518018 0.364281 11.00000 0.03330 W2 1 0.754542 0.781124 0.736473 11.00000 0.03805 W3 1 0.943328 0.817567 0.333175 11.00000 0.05995 W4 1 0.417504 0.688815 0.977244 11.00000 0.07936 W5 1 0.546050 0.643841 1.123126 0.61530 21.00000 W6 1 0.859028 0.618941 0.228042 0.47227 21.00000 W7 1 0.482499 0.544670 0.862983 0.54160 21.00000 W8 1 0.840487 0.466778 0.259294 0.44164 21.00000 W9 1 0.011224 0.646617 0.102534 0.54445 21.00000 W10 1 1.005892 0.582846 0.853912 0.50413 21.00000 W11 1 0.659456 0.504961 0.170743 0.27105 21.00000 W12 1 0.471520 0.494184 0.791318 0.23027 21.00000 W13 1 0.432322 0.625680 0.100613 0.34171 21.00000 W14 1 0.782311 0.799168 0.484911 0.32611 21.00000 W15 1 0.836244 0.835892 0.494850 0.24550 21.00000 W16 1 0.188336 0.565474 0.113316 0.22478 21.00000 W17 1 0.119860 0.625459 0.121008 0.39973 21.00000 W18 1 0.928780 0.451936 0.230129 0.26104 21.00000 W19 1 0.576870 0.503267 0.116150 0.22075 21.00000 W20 1 0.780784 0.503936 0.238519 0.21946 21.00000 W21 1 0.685108 0.533163 0.240039 0.23686 21.00000 W22 1 0.867419 0.598079 0.247241 0.45197 21.00000 W23 1 0.555092 0.531262 0.955366 0.17461 21.00000 W24 1 0.658840 0.549794 0.093255 0.16922 21.00000 HKLF 4 REM p21onc_a.res in P2(1)/c REM R1 = 0.0829 for 2164 Fo > 4sig(Fo) and 0.1182 for all 3005 data REM 414 parameters refined using 0 restraints END WGHT 0.0861 93.0595 REM Highest difference peak 1.164, deepest hole -0.677, 1-sigma level 0.183 Q1 1 0.3080 0.7717 0.2609 11.00000 0.05 1.16 Q2 1 1.0091 0.5568 0.5533 11.00000 0.05 1.12 Q3 1 0.5076 0.7338 0.5275 11.00000 0.05 1.07 Q4 1 0.1593 0.6924 0.2158 11.00000 0.05 0.73 Q5 1 0.1488 0.6659 0.6046 11.00000 0.05 0.72 Q6 1 0.5861 0.5661 0.9006 11.00000 0.05 0.71 Q7 1 0.5890 0.5431 0.1847 11.00000 0.05 0.71 Q8 1 0.0018 0.6488 0.5597 11.00000 0.05 0.70 Q9 1 0.2779 0.6604 0.9905 11.00000 0.05 0.70 Q10 1 0.7311 0.5876 0.9339 11.00000 0.05 0.69 Q11 1 0.1279 0.5638 0.0271 11.00000 0.05 0.67 Q12 1 -0.0759 0.6551 0.1183 11.00000 0.05 0.67 Q13 1 0.3353 0.5465 0.8622 11.00000 0.05 0.66 Q14 1 0.5654 0.4891 0.9983 11.00000 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54.49 8 12 -5 12.10 36.50 -7 -12 5 248.48 59.59 -7 -12 5 195.68 65.69 7 12 -5 185.08 38.00 7 12 -5 166.98 61.69 -6 -12 5 31.30 56.79 -6 -12 5 -67.09 57.39 6 12 -5 -18.20 34.50 6 12 -5 -0.80 54.49 -5 -12 5 6.80 57.09 -5 -12 5 -22.50 61.29 5 12 -5 33.50 53.99 5 12 -5 64.59 32.00 -4 -12 5 1465.05 97.39 -4 -12 5 1482.35 90.49 4 12 -5 1510.15 81.69 4 12 -5 1540.55 91.29 -3 -12 5 539.55 49.30 -3 -12 5 465.15 68.89 3 12 -5 432.06 59.39 3 12 -5 561.64 43.00 -2 -12 5 543.95 74.59 -2 -12 5 489.65 45.70 2 12 -5 498.25 64.29 2 12 -5 476.25 37.50 -1 -12 5 70.19 94.39 -1 -12 5 111.49 33.50 1 12 -5 50.39 61.49 1 12 -5 106.09 45.20 0 -12 5 470.75 123.39 0 -12 5 593.84 40.20 0 12 -5 533.65 52.89 0 12 -5 460.05 73.09 1 -12 5 -34.30 103.39 1 -12 5 -78.39 45.30 -1 12 -5 -6.50 42.90 -1 12 -5 -169.28 94.49 2 -12 5 308.47 85.19 2 -12 5 274.27 44.60 -2 12 -5 -56.19 118.89 -2 12 -5 260.87 44.80 3 -12 5 612.14 53.79 3 -12 5 536.95 90.39 -3 12 -5 388.26 99.39 -3 12 -5 602.24 52.69 4 -12 5 571.14 51.29 4 -12 5 338.37 77.29 -4 12 -5 625.34 92.59 -4 12 -5 506.15 51.59 5 -12 5 197.98 65.69 5 -12 5 74.79 37.40 -5 12 -5 -14.00 81.49 -5 12 -5 58.49 43.80 6 -12 5 431.36 48.30 6 -12 5 424.16 70.89 -6 12 -5 445.66 81.79 -6 12 -5 468.05 51.29 7 -12 5 94.79 38.20 7 -12 5 55.49 62.09 -7 12 -5 12.80 43.80 -7 12 -5 203.28 82.09 8 -12 5 66.59 40.30 8 -12 5 242.88 60.89 -8 12 -5 158.88 76.49 -8 12 -5 179.08 48.10 -9 -12 4 52.89 54.69 -9 -12 4 -22.00 50.79 9 12 -4 17.20 37.60 9 12 -4 -15.50 45.70 -8 -12 4 32.40 66.09 -8 -12 4 -73.49 61.39 8 12 -4 66.29 35.80 8 12 -4 47.80 55.39 -7 -12 4 33.70 67.89 -7 -12 4 36.70 64.29 7 12 -4 11.30 39.60 7 12 -4 17.40 61.49 -6 -12 4 45.40 65.49 -6 -12 4 10.60 56.89 6 12 -4 10.90 36.20 6 12 -4 90.49 56.09 -5 -12 4 47.30 57.09 -5 -12 4 11.40 56.19 5 12 -4 88.09 55.89 5 12 -4 1.30 33.40 -4 -12 4 1960.70 105.19 4 12 -4 1413.16 84.69 -3 -12 4 24.00 63.99 -3 -12 4 105.49 41.10 3 12 -4 -11.00 56.39 3 12 -4 88.59 30.90 -2 -12 4 57.99 71.19 -2 -12 4 65.29 38.60 2 12 -4 59.99 32.80 2 12 -4 59.69 59.29 -1 -12 4 -74.49 96.29 -1 -12 4 12.10 32.00 1 12 -4 -50.29 63.09 1 12 -4 36.80 47.20 0 -12 4 1311.17 79.39 0 -12 4 1530.65 138.69 0 12 -4 1782.42 90.89 0 12 -4 1561.54 113.59 1 -12 4 138.19 44.70 1 -12 4 -68.99 102.29 -1 12 -4 80.99 45.40 -1 12 -4 -85.79 107.79 2 -12 4 147.89 44.00 2 -12 4 80.99 91.99 -2 12 -4 -64.49 129.59 -2 12 -4 135.49 44.10 3 -12 4 73.29 85.89 3 -12 4 41.00 40.30 -3 12 -4 76.39 43.60 -3 12 -4 -65.79 97.29 4 -12 4 1369.56 82.59 4 -12 4 1284.37 105.49 -4 12 -4 1406.16 119.79 -4 12 -4 1410.46 81.29 5 -12 4 210.58 39.10 5 -12 4 357.56 70.29 -5 12 -4 140.09 43.10 -5 12 -4 202.58 78.09 6 -12 4 98.89 67.29 6 -12 4 20.50 39.90 -6 12 -4 35.40 80.69 -6 12 -4 -3.50 48.40 7 -12 4 71.49 61.89 7 -12 4 -15.50 40.40 -7 12 -4 24.20 49.50 -7 12 -4 -72.59 84.89 8 -12 4 324.97 63.79 8 -12 4 182.08 41.90 -8 12 -4 289.47 82.19 -8 12 -4 259.87 49.70 9 -12 4 8.90 53.19 9 -12 4 2.30 39.40 -9 12 -4 -98.69 77.09 -9 12 -4 -71.49 44.80 -9 -12 3 31.20 60.99 -9 -12 3 -43.70 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83.19 51.29 -4 -12 2 -35.60 58.69 -4 -12 2 -30.10 46.80 4 12 -2 63.39 53.49 4 12 -2 19.10 32.80 -3 -12 2 266.67 63.19 -3 -12 2 170.28 43.50 3 12 -2 166.78 32.50 3 12 -2 221.38 57.39 -2 -12 2 178.88 44.70 -2 -12 2 243.48 75.19 2 12 -2 226.78 33.40 2 12 -2 249.08 65.69 -1 -12 2 494.35 101.59 -1 -12 2 362.06 40.10 1 12 -2 366.26 55.49 1 12 -2 346.57 74.39 0 -12 2 -73.49 122.19 0 12 -2 162.68 46.80 0 12 -2 -72.19 94.79 1 -12 2 135.99 110.19 1 -12 2 68.89 47.80 -1 12 -2 196.68 49.60 -1 12 -2 425.86 120.79 2 -12 2 43.80 94.09 2 -12 2 56.09 48.90 -2 12 -2 242.58 112.29 -2 12 -2 42.10 42.40 3 -12 2 -64.19 83.49 3 -12 2 -69.29 43.40 -3 12 -2 -6.70 43.10 -3 12 -2 97.79 94.79 4 -12 2 -69.09 74.79 4 -12 2 31.80 45.90 -4 12 -2 -51.79 97.69 -4 12 -2 -30.60 43.60 5 -12 2 -42.90 71.59 5 -12 2 55.89 38.20 -5 12 -2 69.59 42.30 -5 12 -2 77.99 81.89 6 -12 2 -33.00 40.00 6 -12 2 -62.59 71.89 -6 12 -2 -45.10 49.70 -6 12 -2 -44.30 85.59 7 -12 2 -99.69 46.40 7 -12 2 32.80 58.39 -7 12 -2 -89.69 82.29 -7 12 -2 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