data_13279 _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 'Ca2 H36 O45 V10' _chemical_formula_weight 1345.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ca' 'Ca' 0.2262 0.3064 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 '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 8.779(2) _cell_length_b 10.311(2) _cell_length_c 12.060(2) _cell_angle_alpha 96.740(4) _cell_angle_beta 107.388(5) _cell_angle_gamma 114.439(6) _cell_volume 911.2(3) _cell_formula_units_Z 1 _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 2.453 _exptl_crystal_F_000 666 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 2.860 _shelx_estimated_absorpt_T_min 0.674 _shelx_estimated_absorpt_T_max 0.919 _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 0.71075 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11666 _diffrn_reflns_av_unetI/netI 0.0917 _diffrn_reflns_av_R_equivalents 0.1113 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.258 _diffrn_reflns_theta_max 25.051 _diffrn_reflns_theta_full 25.051 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 0.990 _reflns_number_total 3196 _reflns_number_gt 2711 _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^)+(0.1108P)^2^+1.8179P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3196 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1074 _refine_ls_R_factor_gt 0.0947 _refine_ls_wR_factor_ref 0.2742 _refine_ls_wR_factor_gt 0.2611 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.194 _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 V1 V 0.18925(19) 0.01871(18) -0.01147(14) 0.0566(5) Uani 1 1 d . . . . . V2 V 0.1531(2) 0.04788(19) 0.24205(14) 0.0599(5) Uani 1 1 d . . . . . V3 V 0.0610(2) 0.25860(19) -0.05625(15) 0.0595(5) Uani 1 1 d . . . . . V4 V 0.3879(2) 0.32622(19) 0.17727(15) 0.0621(5) Uani 1 1 d . . . . . V5 V 0.0295(2) 0.2883(2) 0.19460(15) 0.0632(5) Uani 1 1 d . . . . . Ca1 Ca 0.6060(2) -0.0998(2) 0.40626(18) 0.0629(6) Uani 1 1 d . . . . . O1 O 0.0892(7) 0.1318(7) 0.0793(5) 0.0570(16) Uani 1 1 d . . . . . O2 O 0.1022(7) 0.1021(7) -0.1364(6) 0.0578(15) Uani 1 1 d . . . . . O3 O 0.1831(8) -0.0739(7) 0.1179(6) 0.0578(15) Uani 1 1 d . . . . . O4 O 0.3973(8) 0.1664(8) 0.0650(6) 0.0618(16) Uani 1 1 d . . . . . O5 O 0.2134(8) -0.1056(8) -0.0998(6) 0.0602(16) Uani 1 1 d . . . . . O6 O 0.3787(7) 0.1988(7) 0.2768(6) 0.0599(16) Uani 1 1 d . . . . . O7 O 0.0690(8) 0.1681(8) 0.2935(6) 0.0648(17) Uani 1 1 d . . . . . O8 O 0.3026(8) 0.3725(8) 0.0323(6) 0.0631(16) Uani 1 1 d . . . . . O9 O 0.2787(8) 0.4074(7) 0.2451(6) 0.0630(16) Uani 1 1 d . . . . . O10 O -0.0094(8) 0.3397(7) 0.0496(6) 0.0648(17) Uani 1 1 d . . . . . O11 O 0.1946(8) -0.0226(8) 0.3544(6) 0.0611(16) Uani 1 1 d . . . . . O12 O 0.5966(8) 0.4494(8) 0.2328(6) 0.0703(18) Uani 1 1 d . . . . . O13 O 0.0267(9) 0.3355(8) -0.1656(6) 0.0688(18) Uani 1 1 d . . . . . O14 O -0.0356(9) 0.3806(8) 0.2664(6) 0.0742(19) Uani 1 1 d . . . . . OW1 O 0.5885(8) 0.1365(7) 0.4671(6) 0.0673(17) Uani 1 1 d . . . . . OW2 O 0.6985(9) -0.2289(8) 0.2727(7) 0.0754(19) Uani 1 1 d . . . . . OW3 O 0.5382(8) -0.0293(8) 0.2187(6) 0.0701(18) Uani 1 1 d . . . . . OW4 O 0.9107(8) 0.0811(9) 0.4488(6) 0.0745(19) Uani 1 1 d . . . . . OW5 O 0.3178(9) -0.3083(8) 0.2738(6) 0.0726(18) Uani 1 1 d . . . . . OW6 O 0.6084(10) -0.3133(8) 0.4764(6) 0.078(2) Uani 1 1 d . . . . . OW7 O 0.3443(10) -0.3429(10) 0.0246(8) 0.089(2) Uani 1 1 d . . . . . OW8 O 0.9705(13) 0.3506(12) 0.5740(10) 0.137(4) Uani 1 1 d . . . . . OW9 O 0.736(3) -0.527(2) 0.4850(18) 0.115(10) Uani 0.47(3) 1 d . . P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0535(9) 0.0680(11) 0.0620(10) 0.0236(8) 0.0282(7) 0.0352(8) V2 0.0590(9) 0.0706(11) 0.0598(10) 0.0224(8) 0.0251(7) 0.0366(8) V3 0.0573(9) 0.0651(11) 0.0658(10) 0.0228(8) 0.0269(8) 0.0343(8) V4 0.0571(9) 0.0669(11) 0.0681(11) 0.0207(8) 0.0254(8) 0.0332(8) V5 0.0633(10) 0.0703(12) 0.0689(11) 0.0211(9) 0.0310(8) 0.0388(9) Ca1 0.0610(11) 0.0728(13) 0.0708(12) 0.0250(10) 0.0323(9) 0.0395(10) O1 0.053(3) 0.066(4) 0.059(4) 0.019(3) 0.024(3) 0.034(3) O2 0.053(3) 0.067(4) 0.065(4) 0.023(3) 0.029(3) 0.034(3) O3 0.055(3) 0.069(4) 0.062(4) 0.027(3) 0.021(3) 0.039(3) O4 0.058(3) 0.078(4) 0.065(4) 0.028(3) 0.029(3) 0.040(3) O5 0.058(3) 0.077(4) 0.065(4) 0.024(3) 0.031(3) 0.042(3) O6 0.050(3) 0.066(4) 0.066(4) 0.018(3) 0.021(3) 0.030(3) O7 0.062(3) 0.075(5) 0.062(4) 0.015(3) 0.023(3) 0.038(3) O8 0.054(3) 0.076(4) 0.068(4) 0.027(3) 0.027(3) 0.034(3) O9 0.060(3) 0.055(4) 0.073(4) 0.011(3) 0.024(3) 0.028(3) O10 0.068(4) 0.067(4) 0.074(4) 0.026(3) 0.029(3) 0.042(3) O11 0.061(3) 0.069(4) 0.066(4) 0.025(3) 0.030(3) 0.037(3) O12 0.057(3) 0.068(4) 0.088(5) 0.035(4) 0.029(3) 0.028(3) O13 0.071(4) 0.078(5) 0.071(4) 0.030(4) 0.025(3) 0.047(4) O14 0.081(4) 0.080(5) 0.081(5) 0.018(4) 0.036(4) 0.054(4) OW1 0.064(4) 0.070(4) 0.078(4) 0.023(3) 0.030(3) 0.039(3) OW2 0.083(4) 0.079(5) 0.093(5) 0.030(4) 0.054(4) 0.048(4) OW3 0.064(4) 0.079(5) 0.074(4) 0.024(4) 0.026(3) 0.040(4) OW4 0.058(4) 0.099(5) 0.079(4) 0.033(4) 0.032(3) 0.042(4) OW5 0.065(4) 0.074(5) 0.081(5) 0.028(4) 0.030(3) 0.033(3) OW6 0.094(5) 0.077(5) 0.074(5) 0.031(4) 0.032(4) 0.049(4) OW7 0.080(5) 0.090(6) 0.109(6) 0.031(5) 0.045(4) 0.045(4) OW8 0.112(7) 0.124(9) 0.132(8) -0.022(7) 0.056(6) 0.025(6) OW9 0.122(17) 0.095(16) 0.111(17) 0.034(12) 0.040(12) 0.038(12) _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 V1 O5 1.692(6) . ? V1 O4 1.693(7) . ? V1 O3 1.925(6) . ? V1 O2 1.937(6) . ? V1 O1 2.103(6) 2 ? V1 O1 2.110(6) . ? V1 V5 3.063(2) 2 ? V1 V4 3.104(2) . ? V2 O11 1.629(6) . ? V2 O7 1.821(7) . ? V2 O6 1.822(6) . ? V2 O3 1.988(7) . ? V2 O2 2.001(6) 2 ? V2 O1 2.250(6) . ? V2 V3 3.073(2) 2 ? V2 V4 3.113(2) . ? V3 O13 1.632(7) . ? V3 O8 1.819(6) . ? V3 O10 1.833(7) . ? V3 O2 1.999(6) . ? V3 O3 2.027(6) 2 ? V3 O1 2.229(6) . ? V3 V2 3.073(2) 2 ? V3 V5 3.110(2) . ? V3 V4 3.115(2) . ? V4 O12 1.601(7) . ? V4 O9 1.806(6) . ? V4 O6 1.874(7) . ? V4 O8 1.885(6) . ? V4 O4 2.053(7) . ? V4 O1 2.352(6) . ? V4 V5 3.080(2) . ? V5 O14 1.592(7) . ? V5 O10 1.861(7) . ? V5 O9 1.862(6) . ? V5 O7 1.881(7) . ? V5 O5 2.029(7) 2 ? V5 O1 2.328(6) . ? V5 V1 3.063(2) 2 ? Ca1 OW4 2.393(7) . ? Ca1 OW5 2.419(7) . ? Ca1 OW3 2.437(7) . ? Ca1 OW6 2.456(7) . ? Ca1 OW2 2.490(7) . ? Ca1 OW1 2.541(7) . ? Ca1 OW1 2.559(7) 2_656 ? Ca1 O11 2.699(7) 2_656 ? Ca1 Ca1 4.171(4) 2_656 ? O1 V1 2.103(6) 2 ? O2 V2 2.001(6) 2 ? O3 V3 2.027(6) 2 ? O5 V5 2.029(7) 2 ? O11 Ca1 2.699(7) 2_656 ? OW1 Ca1 2.559(7) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 V1 O4 107.5(3) . . ? O5 V1 O3 97.0(3) . . ? O4 V1 O3 96.5(3) . . ? O5 V1 O2 97.1(3) . . ? O4 V1 O2 97.6(3) . . ? O3 V1 O2 156.0(3) . . ? O5 V1 O1 87.8(3) . 2 ? O4 V1 O1 164.8(3) . 2 ? O3 V1 O1 80.6(2) . 2 ? O2 V1 O1 80.6(2) . 2 ? O5 V1 O1 165.4(3) . . ? O4 V1 O1 87.2(3) . . ? O3 V1 O1 80.7(2) . . ? O2 V1 O1 80.7(2) . . ? O1 V1 O1 77.6(3) 2 . ? O5 V1 V5 38.4(2) . 2 ? O4 V1 V5 145.8(2) . 2 ? O3 V1 V5 89.6(2) . 2 ? O2 V1 V5 89.5(2) . 2 ? O1 V1 V5 49.40(17) 2 2 ? O1 V1 V5 126.99(17) . 2 ? O5 V1 V4 145.4(2) . . ? O4 V1 V4 38.0(2) . . ? O3 V1 V4 89.2(2) . . ? O2 V1 V4 90.2(2) . . ? O1 V1 V4 126.81(18) 2 . ? O1 V1 V4 49.23(17) . . ? V5 V1 V4 176.19(6) 2 . ? O11 V2 O7 102.7(3) . . ? O11 V2 O6 100.5(3) . . ? O7 V2 O6 94.5(3) . . ? O11 V2 O3 101.1(3) . . ? O7 V2 O3 154.5(3) . . ? O6 V2 O3 90.2(3) . . ? O11 V2 O2 102.0(3) . 2 ? O7 V2 O2 89.1(3) . 2 ? O6 V2 O2 155.8(3) . 2 ? O3 V2 O2 76.9(2) . 2 ? O11 V2 O1 176.6(3) . . ? O7 V2 O1 80.0(3) . . ? O6 V2 O1 81.4(2) . . ? O3 V2 O1 76.0(2) . . ? O2 V2 O1 75.7(2) 2 . ? O11 V2 V3 92.2(3) . 2 ? O7 V2 V3 128.8(2) . 2 ? O6 V2 V3 130.7(2) . 2 ? O3 V2 V3 40.52(18) . 2 ? O2 V2 V3 39.77(18) 2 2 ? O1 V2 V3 84.36(17) . 2 ? O11 V2 V4 133.4(2) . . ? O7 V2 V4 82.7(2) . . ? O6 V2 V4 33.16(19) . . ? O3 V2 V4 87.80(19) . . ? O2 V2 V4 124.56(19) 2 . ? O1 V2 V4 48.85(16) . . ? V3 V2 V4 120.54(7) 2 . ? O13 V3 O8 102.6(3) . . ? O13 V3 O10 102.5(3) . . ? O8 V3 O10 95.0(3) . . ? O13 V3 O2 99.5(3) . . ? O8 V3 O2 91.3(3) . . ? O10 V3 O2 155.1(3) . . ? O13 V3 O3 99.7(3) . 2 ? O8 V3 O3 155.9(3) . 2 ? O10 V3 O3 88.9(3) . 2 ? O2 V3 O3 76.1(3) . 2 ? O13 V3 O1 174.3(3) . . ? O8 V3 O1 81.7(3) . . ? O10 V3 O1 80.6(3) . . ? O2 V3 O1 76.5(2) . . ? O3 V3 O1 75.5(2) 2 . ? O13 V3 V2 89.8(3) . 2 ? O8 V3 V2 131.1(2) . 2 ? O10 V3 V2 128.4(2) . 2 ? O2 V3 V2 39.81(17) . 2 ? O3 V3 V2 39.59(18) 2 2 ? O1 V3 V2 84.50(17) . 2 ? O13 V3 V5 135.3(3) . . ? O8 V3 V5 84.1(2) . . ? O10 V3 V5 32.9(2) . . ? O2 V3 V5 124.79(19) . . ? O3 V3 V5 86.46(19) 2 . ? O1 V3 V5 48.32(16) . . ? V2 V3 V5 119.00(7) 2 . ? O13 V3 V4 135.9(3) . . ? O8 V3 V4 33.4(2) . . ? O10 V3 V4 83.6(2) . . ? O2 V3 V4 88.70(17) . . ? O3 V3 V4 124.31(18) 2 . ? O1 V3 V4 48.84(15) . . ? V2 V3 V4 120.66(6) 2 . ? V5 V3 V4 59.30(5) . . ? O12 V4 O9 104.4(3) . . ? O12 V4 O6 103.3(3) . . ? O9 V4 O6 92.8(3) . . ? O12 V4 O8 101.0(3) . . ? O9 V4 O8 91.0(3) . . ? O6 V4 O8 153.6(3) . . ? O12 V4 O4 100.3(3) . . ? O9 V4 O4 155.3(3) . . ? O6 V4 O4 82.8(3) . . ? O8 V4 O4 83.0(3) . . ? O12 V4 O1 173.4(3) . . ? O9 V4 O1 82.0(2) . . ? O6 V4 O1 77.6(2) . . ? O8 V4 O1 77.1(2) . . ? O4 V4 O1 73.3(2) . . ? O12 V4 V5 137.9(3) . . ? O9 V4 V5 33.5(2) . . ? O6 V4 V5 84.90(18) . . ? O8 V4 V5 83.93(18) . . ? O4 V4 V5 121.79(18) . . ? O1 V4 V5 48.51(15) . . ? O12 V4 V1 130.7(3) . . ? O9 V4 V1 124.8(2) . . ? O6 V4 V1 78.2(2) . . ? O8 V4 V1 78.2(2) . . ? O4 V4 V1 30.48(17) . . ? O1 V4 V1 42.79(15) . . ? V5 V4 V1 91.31(6) . . ? O12 V4 V2 135.4(2) . . ? O9 V4 V2 82.7(2) . . ? O6 V4 V2 32.13(17) . . ? O8 V4 V2 123.2(2) . . ? O4 V4 V2 80.67(19) . . ? O1 V4 V2 46.07(14) . . ? V5 V4 V2 60.87(5) . . ? V1 V4 V2 61.09(5) . . ? O12 V4 V3 133.0(3) . . ? O9 V4 V3 81.6(2) . . ? O6 V4 V3 123.12(19) . . ? O8 V4 V3 32.10(19) . . ? O4 V4 V3 80.58(17) . . ? O1 V4 V3 45.51(14) . . ? V5 V4 V3 60.26(5) . . ? V1 V4 V3 60.90(5) . . ? V2 V4 V3 91.40(6) . . ? O14 V5 O10 102.1(3) . . ? O14 V5 O9 105.2(3) . . ? O10 V5 O9 90.8(3) . . ? O14 V5 O7 102.9(3) . . ? O10 V5 O7 153.7(3) . . ? O9 V5 O7 90.3(3) . . ? O14 V5 O5 98.8(3) . 2 ? O10 V5 O5 84.2(3) . 2 ? O9 V5 O5 156.0(3) . 2 ? O7 V5 O5 84.2(3) . 2 ? O14 V5 O1 173.2(3) . . ? O10 V5 O1 77.4(2) . . ? O9 V5 O1 81.5(2) . . ? O7 V5 O1 76.7(2) . . ? O5 V5 O1 74.5(2) 2 . ? O14 V5 V1 130.0(3) . 2 ? O10 V5 V1 79.1(2) . 2 ? O9 V5 V1 124.8(2) . 2 ? O7 V5 V1 78.7(2) . 2 ? O5 V5 V1 31.18(16) 2 2 ? O1 V5 V1 43.29(15) . 2 ? O14 V5 V4 137.6(3) . . ? O10 V5 V4 84.21(19) . . ? O9 V5 V4 32.3(2) . . ? O7 V5 V4 82.77(19) . . ? O5 V5 V4 123.64(18) 2 . ? O1 V5 V4 49.18(15) . . ? V1 V5 V4 92.47(6) 2 . ? O14 V5 V3 134.5(3) . . ? O10 V5 V3 32.4(2) . . ? O9 V5 V3 81.0(2) . . ? O7 V5 V3 122.4(2) . . ? O5 V5 V3 82.29(18) 2 . ? O1 V5 V3 45.64(15) . . ? V1 V5 V3 61.94(5) 2 . ? V4 V5 V3 60.43(5) . . ? OW4 Ca1 OW5 152.2(3) . . ? OW4 Ca1 OW3 84.0(2) . . ? OW5 Ca1 OW3 76.7(2) . . ? OW4 Ca1 OW6 109.1(2) . . ? OW5 Ca1 OW6 75.4(2) . . ? OW3 Ca1 OW6 139.8(3) . . ? OW4 Ca1 OW2 77.3(2) . . ? OW5 Ca1 OW2 78.3(3) . . ? OW3 Ca1 OW2 74.1(2) . . ? OW6 Ca1 OW2 72.3(2) . . ? OW4 Ca1 OW1 80.0(2) . . ? OW5 Ca1 OW1 113.9(2) . . ? OW3 Ca1 OW1 76.4(2) . . ? OW6 Ca1 OW1 142.2(2) . . ? OW2 Ca1 OW1 144.2(2) . . ? OW4 Ca1 OW1 131.1(2) . 2_656 ? OW5 Ca1 OW1 76.6(2) . 2_656 ? OW3 Ca1 OW1 123.1(2) . 2_656 ? OW6 Ca1 OW1 77.2(2) . 2_656 ? OW2 Ca1 OW1 144.4(2) . 2_656 ? OW1 Ca1 OW1 70.3(2) . 2_656 ? OW4 Ca1 O11 67.4(2) . 2_656 ? OW5 Ca1 O11 138.5(2) . 2_656 ? OW3 Ca1 O11 140.6(2) . 2_656 ? OW6 Ca1 O11 77.4(2) . 2_656 ? OW2 Ca1 O11 121.7(2) . 2_656 ? OW1 Ca1 O11 72.6(2) . 2_656 ? OW1 Ca1 O11 67.1(2) 2_656 2_656 ? OW4 Ca1 Ca1 107.3(2) . 2_656 ? OW5 Ca1 Ca1 95.99(18) . 2_656 ? OW3 Ca1 Ca1 101.04(17) . 2_656 ? OW6 Ca1 Ca1 110.19(19) . 2_656 ? OW2 Ca1 Ca1 173.11(19) . 2_656 ? OW1 Ca1 Ca1 35.27(15) . 2_656 ? OW1 Ca1 Ca1 34.98(15) 2_656 2_656 ? O11 Ca1 Ca1 65.12(14) 2_656 2_656 ? V1 O1 V1 102.4(3) 2 . ? V1 O1 V3 94.3(2) 2 . ? V1 O1 V3 93.1(2) . . ? V1 O1 V2 93.7(2) 2 . ? V1 O1 V2 92.8(2) . . ? V3 O1 V2 168.8(3) . . ? V1 O1 V5 87.3(2) 2 . ? V1 O1 V5 170.3(3) . . ? V3 O1 V5 86.0(2) . . ? V2 O1 V5 86.5(2) . . ? V1 O1 V4 169.6(3) 2 . ? V1 O1 V4 88.0(2) . . ? V3 O1 V4 85.7(2) . . ? V2 O1 V4 85.09(19) . . ? V5 O1 V4 82.3(2) . . ? V1 O2 V3 106.4(3) . . ? V1 O2 V2 107.5(3) . 2 ? V3 O2 V2 100.4(2) . 2 ? V1 O3 V2 107.7(3) . . ? V1 O3 V3 107.0(3) . 2 ? V2 O3 V3 99.9(3) . 2 ? V1 O4 V4 111.6(3) . . ? V1 O5 V5 110.5(3) . 2 ? V2 O6 V4 114.7(3) . . ? V2 O7 V5 115.8(3) . . ? V3 O8 V4 114.5(4) . . ? V4 O9 V5 114.2(3) . . ? V3 O10 V5 114.7(3) . . ? V2 O11 Ca1 132.9(4) . 2_656 ? Ca1 OW1 Ca1 109.7(2) . 2_656 ? _refine_diff_density_max 0.679 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.146 _shelx_res_file ; 13279.res created by SHELXL-2014/7 TITL JM-13279 CELL 0.71075 8.77900 10.31110 12.06000 96.74010 107.38800 114.43900 ZERR 1 0.00200 0.00226 0.00237 0.00360 0.00510 0.00560 LATT 1 SFAC CA H O V UNIT 2 36 45 10 omit 0 0 1 L.S. 5 FMAP 2 PLAN 20 HTAB BOND $H ACTA SIZE 0.030 0.100 0.150 WGHT 0.110800 1.817900 FVAR 0.74009 0.46573 V1 4 0.189250 0.018715 -0.011471 11.00000 0.05350 0.06796 = 0.06201 0.02360 0.02825 0.03524 V2 4 0.153150 0.047885 0.242051 11.00000 0.05896 0.07061 = 0.05982 0.02239 0.02512 0.03660 V3 4 0.060957 0.258598 -0.056251 11.00000 0.05730 0.06514 = 0.06578 0.02278 0.02689 0.03430 V4 4 0.387851 0.326221 0.177271 11.00000 0.05713 0.06694 = 0.06814 0.02072 0.02540 0.03323 V5 4 0.029534 0.288338 0.194598 11.00000 0.06332 0.07027 = 0.06886 0.02105 0.03100 0.03882 CA1 1 0.605983 -0.099782 0.406259 11.00000 0.06101 0.07275 = 0.07079 0.02505 0.03234 0.03951 O1 3 0.089178 0.131828 0.079253 11.00000 0.05349 0.06585 = 0.05937 0.01861 0.02353 0.03361 O2 3 0.102212 0.102065 -0.136370 11.00000 0.05276 0.06729 = 0.06538 0.02252 0.02870 0.03398 O3 3 0.183056 -0.073878 0.117916 11.00000 0.05469 0.06854 = 0.06212 0.02675 0.02075 0.03871 O4 3 0.397258 0.166379 0.064950 11.00000 0.05752 0.07779 = 0.06521 0.02773 0.02877 0.03979 O5 3 0.213443 -0.105619 -0.099825 11.00000 0.05800 0.07664 = 0.06484 0.02424 0.03112 0.04238 O6 3 0.378724 0.198815 0.276777 11.00000 0.05011 0.06616 = 0.06586 0.01799 0.02138 0.03039 O7 3 0.069000 0.168070 0.293514 11.00000 0.06158 0.07540 = 0.06163 0.01469 0.02323 0.03771 O8 3 0.302577 0.372473 0.032261 11.00000 0.05353 0.07628 = 0.06774 0.02696 0.02675 0.03378 O9 3 0.278666 0.407446 0.245144 11.00000 0.06034 0.05453 = 0.07255 0.01130 0.02435 0.02828 O10 3 -0.009394 0.339666 0.049641 11.00000 0.06848 0.06678 = 0.07393 0.02590 0.02933 0.04220 O11 3 0.194581 -0.022619 0.354400 11.00000 0.06081 0.06948 = 0.06633 0.02524 0.02993 0.03720 O12 3 0.596622 0.449429 0.232771 11.00000 0.05747 0.06818 = 0.08755 0.03485 0.02862 0.02777 O13 3 0.026742 0.335451 -0.165643 11.00000 0.07116 0.07794 = 0.07112 0.03035 0.02475 0.04694 O14 3 -0.035569 0.380641 0.266352 11.00000 0.08081 0.08021 = 0.08112 0.01804 0.03560 0.05353 OW1 3 0.588479 0.136530 0.467105 11.00000 0.06415 0.06952 = 0.07839 0.02314 0.02951 0.03855 OW2 3 0.698534 -0.228861 0.272700 11.00000 0.08294 0.07871 = 0.09338 0.02973 0.05413 0.04833 OW3 3 0.538176 -0.029265 0.218662 11.00000 0.06423 0.07925 = 0.07413 0.02437 0.02647 0.03971 OW4 3 0.910740 0.081085 0.448755 11.00000 0.05836 0.09897 = 0.07873 0.03318 0.03242 0.04195 OW5 3 0.317831 -0.308317 0.273848 11.00000 0.06536 0.07424 = 0.08125 0.02761 0.02994 0.03289 OW6 3 0.608436 -0.313330 0.476437 11.00000 0.09419 0.07679 = 0.07442 0.03120 0.03182 0.04915 OW7 3 0.344262 -0.342878 0.024645 11.00000 0.07995 0.09026 = 0.10870 0.03142 0.04459 0.04529 OW8 3 0.970526 0.350559 0.574021 11.00000 0.11169 0.12365 = 0.13159 -0.02195 0.05600 0.02496 OW9 3 0.735635 -0.527488 0.484951 21.00000 0.12234 0.09456 = 0.11062 0.03370 0.04036 0.03769 HKLF 4 REM JM-13279 REM R1 = 0.0947 for 2711 Fo > 4sig(Fo) and 0.1074 for all 3196 data REM 263 parameters refined using 0 restraints END WGHT 0.1101 1.8171 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.679, deepest hole -0.568, 1-sigma level 0.146 Q1 1 0.6842 -0.2317 0.5124 11.00000 0.05 0.58 Q2 1 0.1732 0.0340 0.1134 11.00000 0.05 0.56 Q3 1 0.6463 -0.3249 0.5779 11.00000 0.05 0.51 Q4 1 0.0430 0.2803 0.0629 11.00000 0.05 0.48 Q5 1 0.0641 0.0063 0.1677 11.00000 0.05 0.46 Q6 1 0.1459 0.1877 0.1342 11.00000 0.05 0.45 Q7 1 0.2415 0.3962 0.0002 11.00000 0.05 0.45 Q8 1 0.6156 -0.3854 0.3647 11.00000 0.05 0.45 Q9 1 0.2041 -0.3750 0.2229 11.00000 0.05 0.45 Q10 1 0.0197 0.4004 0.0856 11.00000 0.05 0.45 Q11 1 0.2637 0.1397 0.2249 11.00000 0.05 0.45 Q12 1 0.4064 -0.1200 0.1756 11.00000 0.05 0.42 Q13 1 0.7692 -0.5525 0.6366 11.00000 0.05 0.42 Q14 1 0.6865 0.2009 0.5180 11.00000 0.05 0.41 Q15 1 0.4967 -0.5390 0.4212 11.00000 0.05 0.41 Q16 1 0.3955 -0.3204 0.1464 11.00000 0.05 0.40 Q17 1 0.5021 -0.3592 0.4833 11.00000 0.05 0.40 Q18 1 0.6650 -0.3670 0.4996 11.00000 0.05 0.38 Q19 1 -0.0196 0.1968 -0.0440 11.00000 0.05 0.38 Q20 1 0.4287 -0.3797 -0.0059 11.00000 0.05 0.38 ; _shelx_res_checksum 42664 _shelx_hkl_file ; 0 0 -1 1.91 2.13 0 0 1 -1.71 3.17 0 1 0 5597.52 119.23 -1 1 0 9190.59 208.63 1 -1 0 9344.95 206.97 1 -1 0 8930.27 203.54 -1 1 0 9450.53 209.03 1 -1 0 9060.23 198.71 -1 1 0 9253.81 202.67 -1 0 116113.93 347.56 -1 0 116048.92 344.76 1 0 -116014.71 343.88 1 0 -116734.54 128.85 1 0 0 3121.47 84.33 -1 0 0 3116.47 84.24 1 0 0 3154.09 84.38 -1 0 0 3147.74 84.25 -1 0 0 3244.71 86.71 1 0 0 3229.51 86.24 -1 1 1 1722.25 50.02 1 -1 -1 1776.83 51.75 1 -1 -1 1720.38 56.13 -1 1 1 1723.21 56.31 0 -1 -1 1603.86 51.46 0 1 1 1547.33 49.60 0 1 1 1430.54 37.03 -1 1 -1 3205.89 93.10 1 -1 1 2962.41 80.57 -1 1 -1 3060.95 96.80 1 -1 1 2998.45 84.34 1 -1 1 3215.70 93.08 -1 1 -1 2932.28 75.25 1 0 -2 1034.89 115.23 -1 0 2 818.10 34.88 1 0 -2 913.29 88.74 -1 0 2 778.25 65.79 0 0 2 144.64 20.42 0 0 -2 157.59 20.82 0 -1 2 3871.09 108.08 0 1 -2 3518.69 99.70 1 0 1 174.78 23.57 -1 0 -1 176.74 30.25 -1 0 -1 170.29 21.80 1 0 1 164.78 17.41 -1 0 -1 160.34 18.63 1 0 1 176.93 25.64 -1 -1 1 616.84 44.76 1 1 -1 568.63 86.94 -1 -1 1 587.69 31.15 1 1 -1 717.07 94.92 -1 -1 1 773.82 101.32 -1 2 0 15.06 4.18 -1 2 0 15.33 2.55 -1 1 2 7.76 4.43 -1 1 2 1.39 1.67 1 -1 -2 2.48 1.64 -1 1 2 3.35 7.18 1 1 0 1711.84 58.17 -1 -1 0 1952.08 182.19 1 1 0 1912.46 178.32 1 1 0 1740.58 60.28 -1 -1 0 1718.62 58.35 -1 -1 0 1679.65 67.73 1 -2 1 13.53 3.50 -1 2 -1 17.75 4.36 -1 2 -1 12.61 2.68 0 2 -1 2099.23 71.21 1 1 -2 486.35 88.46 -1 -1 2 545.49 88.04 1 1 -2 574.60 65.05 -1 2 1 2581.08 80.94 -1 2 1 2620.74 79.35 0 -2 0 382.99 17.68 0 2 0 481.15 57.94 0 2 0 431.66 46.78 2 -1 -1 556.82 65.76 -2 1 1 577.53 89.54 2 -1 -1 496.83 37.26 -2 1 1 586.53 66.54 -2 1 1 558.16 67.62 2 -1 -1 553.41 72.79 0 -1 -2 177.45 26.73 0 1 2 208.53 30.45 0 1 2 178.92 22.18 1 -1 2 2071.64 75.04 1 -1 2 2155.47 65.80 -1 1 -2 2219.04 105.87 -1 1 -2 2281.58 89.72 -1 1 -2 2344.89 102.50 1 -1 2 2328.34 81.00 -2 1 0 1759.80 187.78 -2 1 0 1494.82 63.54 -2 1 0 1886.25 197.73 2 -1 0 1844.81 212.32 2 -1 0 1627.19 180.25 2 -1 0 1681.89 184.31 0 -2 2 131.27 22.70 0 2 -2 145.48 27.15 0 2 -2 121.74 25.93 2 0 -1 67.28 10.87 2 0 -1 68.56 13.35 2 0 -1 80.13 12.70 -2 0 1 63.66 9.74 -2 0 1 61.08 12.90 -2 0 1 68.25 9.54 -2 1 2 16.21 3.51 -2 1 2 21.45 4.97 2 -1 -2 17.73 3.61 2 -1 -2 17.03 4.27 1 0 -3 1762.93 61.31 1 0 -3 1960.80 124.91 -1 0 3 1895.39 207.49 -1 0 3 2070.25 195.58 1 0 -3 1867.05 92.32 2 -2 0 4002.15 122.41 -2 2 0 3929.29 112.73 -2 2 0 3780.05 105.57 2 -2 0 3737.37 104.60 -2 2 0 3997.12 121.97 2 -2 0 3865.61 111.73 -2 2 1 880.42 43.49 -2 2 1 1248.89 137.02 2 -2 -1 1030.14 119.66 -2 2 1 1068.89 121.71 2 -2 -1 909.51 115.60 -1 -1 -1 33.44 8.14 1 1 1 47.91 9.27 1 1 1 35.99 6.93 1 1 1 34.09 8.06 -1 -1 -1 41.48 7.86 1 -2 2 162.58 22.94 -1 2 -2 131.17 15.76 1 -2 2 131.37 16.16 -1 2 -2 164.20 18.96 0 -2 -1 8.37 3.81 0 2 1 0.20 1.89 -2 0 2 5563.75 152.03 2 0 -2 5479.81 149.87 2 0 -2 5647.73 157.54 -2 0 2 5558.24 164.20 0 -1 3 614.55 66.22 0 1 -3 592.50 58.18 -1 0 -2 234.72 26.09 1 0 2 238.35 29.31 1 0 2 219.73 25.55 -1 0 -2 313.86 41.02 1 0 2 274.27 33.39 -1 0 -2 241.08 29.55 -2 0 0 1398.05 151.69 -2 0 0 1327.86 127.02 2 0 0 1336.65 168.33 -2 0 0 1300.79 171.58 2 0 0 1293.16 140.93 2 0 0 1415.56 124.18 1 1 -3 3254.92 89.45 -1 -1 3 3283.62 104.31 -1 -1 3 3298.39 90.69 0 0 -3 303.93 37.07 0 0 3 315.38 35.12 -1 2 2 0.40 2.94 -1 2 2 1.62 1.55 1 -2 -2 -0.12 4.08 1 -1 -3 3.16 3.17 -1 1 3 6.88 5.00 1 -1 -3 -0.91 1.18 -2 1 -1 345.55 31.57 2 -1 1 351.22 40.06 2 -1 1 349.68 33.64 2 -1 1 311.54 28.09 -2 1 -1 387.76 36.09 -2 1 -1 332.37 29.69 2 -2 1 8869.99 244.39 2 -2 1 8737.26 257.45 -2 2 -1 8727.71 232.85 2 -2 1 8461.89 210.26 -2 2 -1 8431.88 204.83 -2 2 -1 8886.70 236.43 2 -2 -2 74.59 12.61 2 -2 -2 81.54 14.55 -2 2 2 66.22 10.19 -2 2 2 80.10 11.36 1 2 -1 88.40 12.10 1 2 -1 77.18 15.84 -1 -2 1 76.36 10.23 -1 -2 1 96.81 13.51 1 -3 1 773.23 26.97 -1 3 -1 888.32 32.78 1 2 -2 30.20 10.39 -1 -2 2 49.47 8.59 1 2 -2 42.00 8.21 0 2 -3 928.43 25.23 0 -2 3 1387.16 163.28 0 2 -3 1262.59 110.02 2 0 -3 5882.94 159.88 -2 0 3 5863.96 160.37 -2 0 3 5959.91 177.62 2 0 -3 6080.44 170.03 2 -1 -3 1333.83 174.22 -2 1 3 1246.66 127.63 -2 1 3 1361.32 154.79 2 -1 -3 1214.00 123.91 -1 -2 0 567.61 78.48 1 2 0 481.18 51.29 1 2 0 530.97 58.65 -1 -2 0 447.03 44.87 -1 -2 0 504.38 64.97 1 2 0 489.33 52.74 2 1 -1 151.01 18.66 2 1 -1 122.52 22.67 2 1 -1 175.40 17.03 -2 -1 1 153.48 18.22 -2 -1 1 142.80 15.16 -2 -1 1 166.39 17.50 2 1 -2 253.40 26.36 2 1 -2 282.58 41.01 -2 -1 2 294.94 40.53 -2 -1 2 259.90 26.27 -2 -1 2 234.90 27.18 -2 3 0 90.42 12.33 2 -3 0 86.35 13.37 2 -3 0 91.97 16.39 2 -3 0 102.07 14.80 -2 3 0 82.10 14.83 -2 3 0 116.70 15.01 2 0 1 332.06 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196.44 6 -6 -3 1629.55 203.26 -6 6 3 1971.32 273.30 -6 6 3 2873.05 197.54 -6 6 3 1840.72 172.42 -5 -2 6 451.15 45.26 5 2 -6 286.62 55.02 -5 -2 6 243.45 44.59 5 2 -6 310.69 67.14 1 0 -9 21.37 10.21 -1 0 9 28.70 10.39 -1 0 9 22.56 8.80 1 6 1 824.69 104.84 2 5 -7 235.29 49.33 -2 -5 7 239.52 67.47 -2 -5 7 467.06 53.19 2 5 -7 318.56 48.65 -5 4 7 24.64 10.67 -5 4 7 16.71 5.91 5 -4 -7 14.67 5.67 -5 4 7 18.63 7.89 -5 1 -3 7.81 4.83 5 -1 3 14.07 6.56 5 -1 3 5.69 3.74 5 -1 3 19.66 9.86 -5 1 -3 1.02 6.94 -5 1 -3 8.06 6.01 1 3 -9 9.22 5.89 -1 -3 9 2.54 1.67 -1 -3 9 6.66 6.44 2 -1 -9 32.57 11.97 -2 1 9 15.31 8.56 -2 1 9 21.65 9.03 2 -1 -9 24.39 8.24 5 2 -1 209.81 34.85 -5 -2 1 70.87 17.40 5 2 -1 96.87 22.64 -5 -2 1 100.84 22.69 5 2 -1 46.96 18.51 -5 -2 1 204.59 36.31 5 -4 4 124.39 23.01 -5 4 -4 109.80 23.00 5 -4 4 108.59 18.69 5 -4 4 99.95 21.95 -5 4 -4 140.15 30.13 -5 4 -4 87.14 20.27 5 -2 -8 1511.03 219.75 5 -2 -8 2120.27 221.07 -5 2 8 1928.99 182.20 -5 2 8 1690.60 276.72 -5 2 8 1346.98 280.72 1 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20.06 10.15 -4 10 3 38.20 18.18 -4 10 3 62.60 19.25 -3 5 -10 157.91 36.69 -3 5 -10 150.74 41.70 3 -5 10 195.80 40.89 -6 8 7 4.41 2.93 -6 8 7 6.69 6.73 -6 8 7 8.37 6.25 -1 9 3 155.66 30.80 -1 9 3 299.87 81.26 -3 0 -9 28.28 11.00 -3 0 -9 82.33 18.69 3 0 9 108.06 30.31 3 0 9 45.18 11.89 -1 5 9 9.07 5.96 1 -5 -9 13.67 7.70 -1 5 9 5.69 6.47 -4 4 11 5.18 6.91 -4 4 11 18.89 9.86 -1 0 12 5.62 5.05 -1 0 12 3.01 4.22 -1 0 12 16.98 9.88 1 0 -12 7.30 6.55 1 0 -12 9.68 4.17 1 0 -12 5.10 2.75 9 -3 -3 5.28 6.01 9 -3 -3 4.53 9.79 -9 3 3 13.33 8.86 -9 3 3 9.70 8.28 1 -9 8 12.08 6.07 -4 3 -9 11.77 5.80 -4 3 -9 7.56 11.54 4 -3 9 7.45 6.08 4 -3 9 2.22 3.76 -8 7 -2 206.84 37.83 -8 7 -2 114.51 28.30 8 -7 2 142.05 32.52 8 -7 2 91.46 23.37 -8 7 -2 143.46 32.61 8 -7 2 129.55 34.78 2 -9 8 7.08 4.05 -9 6 4 9.24 5.75 9 -6 -4 12.74 7.58 -9 6 4 30.24 13.94 9 -6 -4 29.09 13.10 5 -4 -11 71.01 17.04 -2 -8 0 200.74 37.26 2 8 0 155.65 36.77 2 8 0 108.71 24.55 0 -3 12 4.02 2.10 0 3 -12 6.84 5.26 0 -3 12 1.47 2.06 0 3 -12 2.77 3.63 0 -3 12 22.89 11.10 -4 2 12 38.53 15.44 -4 2 12 19.73 11.51 4 -2 -12 5.02 3.59 5 -5 8 21.68 8.81 -5 5 -8 51.78 14.84 -5 5 -8 69.89 19.12 5 -5 8 37.82 16.84 -5 -1 12 467.78 88.11 5 1 -12 267.37 57.49 -4 -4 -4 26.30 14.13 4 4 4 28.22 12.86 4 4 4 10.86 4.61 -4 -4 -4 16.96 7.54 4 4 4 7.47 7.72 -3 9 5 5.85 2.71 8 -8 1 6.61 11.32 -8 8 -1 19.98 13.62 8 -8 1 2.08 4.19 -8 8 -1 -1.12 6.98 8 -8 1 5.07 3.84 -8 8 -1 17.54 7.59 -1 6 8 255.16 61.80 1 -6 -8 216.95 44.51 -1 -9 1 101.73 20.31 1 9 -1 80.16 19.55 1 9 -1 114.71 27.07 -5 9 -6 7.78 5.33 -5 9 -6 28.61 14.84 5 -9 6 4.16 2.74 -5 9 -6 2.49 1.45 -4 9 -7 3.07 3.89 4 -9 7 5.23 3.30 -4 9 -7 15.70 7.68 -9 4 6 16.55 11.22 -9 4 6 14.96 9.12 -9 4 6 19.42 11.21 9 -4 -6 17.44 10.62 9 -4 -6 34.32 15.46 7 1 1 191.42 38.82 -7 -1 -1 53.25 16.87 7 1 1 61.62 20.53 7 1 1 99.69 25.10 -7 -1 -1 182.68 38.65 -7 -1 -1 78.26 21.67 -9 6 2 8.04 8.96 -9 6 2 12.93 9.99 9 -6 -2 12.93 8.23 -9 6 2 13.09 9.64 9 -6 -2 -2.44 12.80 5 -1 7 2.80 4.63 -5 1 -7 11.41 7.91 5 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12.20 4.41 -3 9 -9 5.99 5.96 3 -9 9 7.59 5.68 2 9 -7 20.53 12.88 2 9 -7 21.89 6.44 -2 -9 7 16.09 5.08 -2 -9 7 35.59 11.05 -3 5 11 170.34 45.05 -3 5 11 180.56 54.12 -6 9 7 8.06 6.00 -6 9 7 8.20 5.11 -6 9 7 -3.03 11.24 6 5 -8 29.35 10.43 -6 -5 8 20.04 7.74 -6 -5 8 21.83 6.37 6 5 -8 17.07 7.49 -2 7 -11 33.39 14.07 2 -7 11 35.27 13.04 -2 7 -11 15.99 7.61 -6 10 -5 1.68 3.79 6 -10 5 3.77 3.87 -6 10 -5 9.39 8.08 -6 10 -5 9.12 7.93 -8 1 -2 115.20 34.40 -8 1 -2 17.54 6.87 8 -1 2 17.18 10.11 8 -1 2 28.36 13.09 -8 1 -2 14.15 8.96 -9 1 2 51.40 17.65 -9 1 2 44.40 21.19 9 -1 -2 18.53 10.02 -9 1 2 67.57 22.67 9 -1 -2 34.55 16.45 1 6 7 6.96 5.74 1 6 7 33.97 11.97 -1 -6 -7 14.18 6.65 -5 5 -9 46.36 16.01 5 -5 9 52.03 17.63 -5 5 -9 41.19 16.77 5 -5 9 9.87 5.91 3 -4 11 -1.09 8.67 -3 4 -11 21.65 8.77 -3 4 -11 7.78 6.61 6 2 -12 30.75 14.20 -6 -2 12 32.75 15.12 6 2 -12 36.61 15.57 -6 -2 12 54.91 18.04 2 8 2 7.79 5.74 -2 -8 -2 1.88 3.23 2 8 2 21.64 11.81 2 8 2 10.67 6.05 -9 7 -1 339.36 110.33 9 -7 1 448.82 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