data_rakovanite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'rakovanite' _chemical_compound_source 'West Sunday mine, Colorado, USA' _chemical_formula_sum 'H36 N3 Na3 O40 V10' _chemical_formula_weight 1296.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' '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' 'N' 'N' 0.0061 0.0033 '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/n' _space_group_name_Hall '-P 2yn' _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+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0248(17) _cell_length_b 17.121(3) _cell_length_c 18.140(3) _cell_angle_alpha 90 _cell_angle_beta 106.242(8) _cell_angle_gamma 90 _cell_volume 3585.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8863 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 23.3 _exptl_crystal_description 'prism' _exptl_crystal_density_diffrn 2.402 _exptl_crystal_F_000 2560 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 2.647 _shelx_estimated_absorpt_T_min 0.778 _shelx_estimated_absorpt_T_max 0.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Higashi2001 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.821 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis RAPID II' _diffrn_reflns_number 42383 _diffrn_reflns_av_unetI/netI 0.0553 _diffrn_reflns_av_R_equivalents 0.1095 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.998 _diffrn_reflns_theta_max 23.256 _diffrn_reflns_theta_full 23.256 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 5138 _reflns_number_gt 2897 _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_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _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^)+(0.0379P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5138 _refine_ls_number_parameters 613 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.994 _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 0.06620(8) -0.12905(7) 0.10292(5) 0.0198(2) Uani 1 1 d . . . . . V2 V -0.01353(8) -0.12714(7) 0.24947(5) 0.0196(2) Uani 1 1 d . . . . . V3 V 0.13091(9) -0.21571(6) 0.39483(6) 0.0214(3) Uani 1 1 d . . . . . V4 V 0.12458(9) -0.03546(6) 0.39366(6) 0.0209(3) Uani 1 1 d . . . . . V5 V 0.28539(9) -0.03404(6) 0.10015(6) 0.0223(3) Uani 1 1 d . . . . . V6 V 0.29424(9) -0.21384(6) 0.10272(6) 0.0227(3) Uani 1 1 d . . . . . V7 V 0.43409(8) -0.12110(7) 0.24686(5) 0.0184(2) Uani 1 1 d . . . . . V8 V 0.35250(8) -0.12219(7) 0.39301(5) 0.0182(2) Uani 1 1 d . . . . . V9 V 0.21232(9) -0.22041(6) 0.24848(6) 0.0177(3) Uani 1 1 d . . . . . V10 V 0.20625(9) -0.02923(6) 0.24726(6) 0.0172(3) Uani 1 1 d . . . . . Na1 Na 0.2821(2) 0.12433(19) -0.06515(13) 0.0395(7) Uani 1 1 d . . . . . Na2 Na -0.1932(2) 0.13987(15) 0.16877(14) 0.0317(7) Uani 1 1 d . . . . . Na3 Na -0.3096(2) 0.10624(14) 0.32562(14) 0.0331(7) Uani 1 1 d . . . . . N1 N 0.1754(4) 0.1291(4) 0.5929(3) 0.0446(15) Uani 1 1 d D . . . . H1A H 0.214(4) 0.083(2) 0.597(3) 0.053 Uiso 1 1 d D U . . . H1B H 0.222(4) 0.167(2) 0.612(3) 0.053 Uiso 1 1 d D U . . . H1C H 0.146(4) 0.137(3) 0.5422(15) 0.053 Uiso 1 1 d D U . . . H1D H 0.117(3) 0.123(3) 0.613(3) 0.053 Uiso 1 1 d D U . . . N2 N 0.0922(4) 0.1547(3) 0.1097(3) 0.0214(13) Uani 1 1 d D . . . . H2A H 0.142(3) 0.118(2) 0.132(2) 0.026 Uiso 1 1 d D U . . . H2B H 0.096(4) 0.162(3) 0.0619(15) 0.026 Uiso 1 1 d D U . . . H2C H 0.021(2) 0.140(3) 0.107(2) 0.026 Uiso 1 1 d D U . . . H2D H 0.106(4) 0.1972(18) 0.136(2) 0.026 Uiso 1 1 d D U . . . N3 N 0.0948(4) -0.3993(3) 0.1081(3) 0.0288(14) Uani 1 1 d D . . . . H3A H 0.149(3) -0.366(2) 0.135(2) 0.035 Uiso 1 1 d D U . . . H3B H 0.057(4) -0.380(3) 0.0645(18) 0.035 Uiso 1 1 d D U . . . H3C H 0.134(4) -0.441(2) 0.100(3) 0.035 Uiso 1 1 d D U . . . H3D H 0.052(3) -0.417(3) 0.136(2) 0.035 Uiso 1 1 d D U . . . O1 O -0.0685(3) -0.1314(3) 0.0542(2) 0.0251(10) Uani 1 1 d . . . . . O2 O -0.1446(3) -0.1278(3) 0.1969(2) 0.0241(9) Uani 1 1 d . . . . . O3 O 0.1064(3) -0.2848(2) 0.4480(2) 0.0305(11) Uani 1 1 d . . . . . O4 O 0.0950(3) 0.0320(2) 0.4462(2) 0.0274(11) Uani 1 1 d . . . . . O5 O 0.3102(4) 0.0344(3) 0.0475(2) 0.0314(11) Uani 1 1 d . . . . . O6 O 0.3260(4) -0.2818(3) 0.0519(3) 0.0343(12) Uani 1 1 d . . . . . O7 O 0.5663(3) -0.1197(3) 0.2989(2) 0.0242(9) Uani 1 1 d . . . . . O8 O 0.4863(3) -0.1194(3) 0.4435(2) 0.0239(9) Uani 1 1 d . . . . . O9 O 0.2436(3) -0.1247(2) 0.18488(18) 0.0159(8) Uani 1 1 d . . . . . O10 O 0.1732(3) -0.1245(2) 0.31149(19) 0.0170(9) Uani 1 1 d . . . . . O11 O 0.0565(3) -0.1995(2) 0.1886(2) 0.0185(10) Uani 1 1 d . . . . . O12 O 0.0534(3) -0.0549(2) 0.1874(2) 0.0173(10) Uani 1 1 d . . . . . O13 O -0.0107(3) -0.2059(2) 0.3191(2) 0.0226(10) Uani 1 1 d . . . . . O14 O -0.0162(3) -0.0488(2) 0.3178(2) 0.0213(10) Uani 1 1 d . . . . . O15 O 0.1007(3) -0.1256(3) 0.44126(19) 0.0222(9) Uani 1 1 d . . . . . O16 O 0.2911(3) -0.2011(2) 0.4361(2) 0.0194(10) Uani 1 1 d . . . . . O17 O 0.1773(3) -0.2787(2) 0.3142(2) 0.0211(10) Uani 1 1 d . . . . . O18 O 0.2860(3) -0.0441(2) 0.4350(2) 0.0206(10) Uani 1 1 d . . . . . O19 O 0.1676(3) 0.0297(2) 0.3111(2) 0.0201(10) Uani 1 1 d . . . . . O20 O 0.3661(3) -0.1947(2) 0.3095(2) 0.0174(10) Uani 1 1 d . . . . . O21 O 0.3612(3) -0.0503(2) 0.3077(2) 0.0158(10) Uani 1 1 d . . . . . O22 O 0.4275(3) -0.0438(2) 0.1781(2) 0.0203(10) Uani 1 1 d . . . . . O23 O 0.4334(3) -0.2003(2) 0.1802(2) 0.0214(10) Uani 1 1 d . . . . . O24 O 0.3173(3) -0.1240(3) 0.0548(2) 0.0238(9) Uani 1 1 d . . . . . O25 O 0.2401(3) 0.0302(2) 0.1819(2) 0.0180(10) Uani 1 1 d . . . . . O26 O 0.1324(3) -0.2056(2) 0.0609(2) 0.0238(10) Uani 1 1 d . . . . . O27 O 0.1273(3) -0.0486(2) 0.0603(2) 0.0213(10) Uani 1 1 d . . . . . O28 O 0.2499(3) -0.2792(2) 0.1849(2) 0.0216(10) Uani 1 1 d . . . . . O29 O 0.3862(4) 0.0314(3) -0.1111(3) 0.0439(14) Uani 1 1 d D . . . . H29A H 0.393(5) -0.013(2) -0.096(4) 0.053 Uiso 1 1 d D U . . . H29B H 0.446(4) 0.042(3) -0.123(4) 0.053 Uiso 1 1 d D U . . . O30 O 0.3744(4) 0.2152(3) -0.1222(3) 0.0378(13) Uani 1 1 d D . . . . H30A H 0.425(4) 0.200(3) -0.141(4) 0.045 Uiso 1 1 d D U . . . H30B H 0.393(5) 0.2621(19) -0.114(4) 0.045 Uiso 1 1 d D U . . . O31 O -0.1391(4) 0.2459(3) 0.0976(3) 0.0399(13) Uani 1 1 d D . . . . H31A H -0.083(4) 0.269(4) 0.124(3) 0.048 Uiso 1 1 d D U . . . H31B H -0.130(5) 0.250(4) 0.0548(16) 0.048 Uiso 1 1 d D U . . . O32 O -0.1071(5) 0.0518(3) 0.1008(3) 0.0397(14) Uani 1 1 d D . . . . H32A H -0.113(6) 0.043(4) 0.0556(15) 0.048 Uiso 1 1 d D U . . . H32B H -0.071(6) 0.021(4) 0.125(3) 0.048 Uiso 1 1 d D U . . . O33 O -0.3838(4) 0.1283(4) 0.0764(3) 0.0434(13) Uani 1 1 d . . . . . H33A H -0.354(5) 0.145(4) 0.038(4) 0.052 Uiso 1 1 d D U . . . H33B H -0.424(6) 0.166(4) 0.076(4) 0.052 Uiso 1 1 d D U . . . O34 O -0.0070(4) 0.1487(3) 0.2554(3) 0.0497(15) Uani 1 1 d D . . . . H34A H 0.045(5) 0.117(3) 0.275(4) 0.060 Uiso 1 1 d D U . . . H34B H 0.021(5) 0.190(2) 0.270(4) 0.060 Uiso 1 1 d D U . . . O35 O -0.2763(4) 0.2186(3) 0.2426(3) 0.0430(15) Uani 1 1 d D . . . . H35A H -0.336(4) 0.243(4) 0.223(3) 0.052 Uiso 1 1 d D U . . . H35B H -0.244(5) 0.247(4) 0.279(3) 0.052 Uiso 1 1 d D U . . . O36 O -0.2302(4) 0.0292(3) 0.2482(3) 0.0390(14) Uani 1 1 d D . . . . H36A H -0.274(4) -0.001(3) 0.218(3) 0.047 Uiso 1 1 d D U . . . H36B H -0.170(3) 0.007(3) 0.266(3) 0.047 Uiso 1 1 d D U . . . O37 O -0.1204(4) 0.1232(4) 0.4046(2) 0.0390(12) Uani 1 1 d D . . . . H37A H -0.061(4) 0.103(4) 0.397(3) 0.047 Uiso 1 1 d D U . . . H37B H -0.105(5) 0.125(5) 0.4520(17) 0.047 Uiso 1 1 d D U . . . O38 O -0.5031(4) 0.1016(3) 0.2516(3) 0.0477(15) Uani 1 1 d D . . . . H38A H -0.513(6) 0.064(3) 0.226(4) 0.057 Uiso 1 1 d D U . . . H38B H -0.557(4) 0.131(3) 0.235(4) 0.057 Uiso 1 1 d D U . . . O39 O -0.3417(5) 0.0023(3) 0.4102(3) 0.0485(15) Uani 1 1 d D . . . . H39A H -0.388(5) -0.034(3) 0.401(4) 0.058 Uiso 1 1 d D U . . . H39B H -0.332(6) 0.014(4) 0.454(2) 0.058 Uiso 1 1 d D U . . . O40 O -0.3769(5) 0.1956(3) 0.4014(3) 0.0431(14) Uani 1 1 d D . . . . H40A H -0.373(6) 0.190(4) 0.4446(19) 0.052 Uiso 1 1 d D U . . . H40B H -0.417(5) 0.233(3) 0.383(3) 0.052 Uiso 1 1 d 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 V1 0.0198(5) 0.0256(6) 0.0123(5) 0.0001(6) 0.0016(4) -0.0011(5) V2 0.0166(5) 0.0238(6) 0.0177(5) 0.0003(6) 0.0035(4) -0.0012(5) V3 0.0251(6) 0.0206(7) 0.0190(7) 0.0031(5) 0.0067(5) -0.0025(5) V4 0.0239(6) 0.0216(7) 0.0176(7) -0.0009(5) 0.0065(5) 0.0011(5) V5 0.0261(7) 0.0236(7) 0.0173(7) 0.0046(5) 0.0064(5) -0.0003(5) V6 0.0282(7) 0.0219(7) 0.0187(7) -0.0031(5) 0.0077(5) 0.0010(5) V7 0.0188(5) 0.0207(6) 0.0155(5) 0.0002(6) 0.0045(4) 0.0005(5) V8 0.0192(5) 0.0201(6) 0.0144(5) 0.0006(5) 0.0030(4) -0.0003(5) V9 0.0206(6) 0.0155(6) 0.0156(6) -0.0009(5) 0.0029(4) 0.0001(5) V10 0.0198(6) 0.0135(6) 0.0178(6) -0.0001(5) 0.0045(4) 0.0004(5) Na1 0.0357(15) 0.0568(18) 0.0265(14) 0.0050(17) 0.0095(11) 0.0021(15) Na2 0.0322(14) 0.0290(17) 0.0350(15) -0.0019(13) 0.0112(12) 0.0057(12) Na3 0.0325(15) 0.0338(19) 0.0324(15) -0.0036(13) 0.0081(12) 0.0037(12) N1 0.039(4) 0.057(4) 0.044(4) -0.002(4) 0.021(3) -0.004(4) N2 0.025(3) 0.017(3) 0.021(3) 0.007(2) 0.006(2) 0.002(2) N3 0.034(3) 0.021(4) 0.027(3) 0.001(3) 0.000(3) 0.001(3) O1 0.019(2) 0.033(3) 0.019(2) -0.001(2) -0.0015(17) 0.000(2) O2 0.016(2) 0.029(2) 0.023(2) -0.001(2) -0.0009(17) 0.000(2) O3 0.035(3) 0.028(3) 0.028(3) 0.006(2) 0.008(2) -0.003(2) O4 0.029(3) 0.027(3) 0.029(3) -0.011(2) 0.011(2) 0.003(2) O5 0.037(3) 0.036(3) 0.023(3) 0.010(2) 0.011(2) -0.003(2) O6 0.043(3) 0.035(3) 0.028(3) -0.006(2) 0.014(2) 0.007(2) O7 0.015(2) 0.030(2) 0.025(2) 0.000(2) 0.0025(18) -0.001(2) O8 0.019(2) 0.031(2) 0.018(2) -0.003(2) -0.0008(17) -0.001(2) O9 0.020(2) 0.016(2) 0.0093(19) 0.003(2) 0.0012(16) 0.0024(19) O10 0.018(2) 0.017(2) 0.017(2) -0.001(2) 0.0052(16) 0.0026(19) O11 0.020(2) 0.018(2) 0.016(2) -0.0005(19) 0.0035(18) -0.0035(18) O12 0.015(2) 0.024(3) 0.011(2) 0.0036(19) 0.0010(18) -0.0007(18) O13 0.026(2) 0.024(3) 0.017(2) 0.000(2) 0.0039(19) 0.003(2) O14 0.018(2) 0.022(2) 0.024(3) -0.005(2) 0.0064(19) -0.0007(19) O15 0.024(2) 0.028(2) 0.016(2) -0.002(2) 0.0061(17) 0.000(2) O16 0.025(2) 0.018(2) 0.013(2) 0.0031(19) 0.0032(19) -0.0015(19) O17 0.020(2) 0.021(3) 0.021(3) 0.000(2) 0.0039(19) -0.0023(19) O18 0.019(2) 0.025(3) 0.018(3) 0.000(2) 0.0060(19) -0.0032(19) O19 0.022(2) 0.015(2) 0.023(3) -0.003(2) 0.0051(19) -0.0009(18) O20 0.021(2) 0.016(2) 0.013(2) -0.0045(19) 0.0019(18) 0.0007(18) O21 0.018(2) 0.015(2) 0.013(2) -0.0034(18) 0.0015(18) -0.0006(18) O22 0.018(2) 0.025(2) 0.018(3) 0.001(2) 0.0049(18) 0.0010(19) O23 0.023(2) 0.019(2) 0.022(3) 0.000(2) 0.0065(19) 0.0037(19) O24 0.027(2) 0.030(2) 0.016(2) -0.001(2) 0.0081(18) 0.001(2) O25 0.019(2) 0.017(2) 0.018(2) 0.0013(19) 0.0057(19) -0.0008(18) O26 0.027(3) 0.027(3) 0.015(2) -0.004(2) 0.0025(19) -0.003(2) O27 0.023(2) 0.025(3) 0.015(3) 0.002(2) 0.0043(19) -0.0024(19) O28 0.027(3) 0.018(3) 0.017(2) -0.0034(19) 0.002(2) 0.0000(18) O29 0.037(3) 0.044(3) 0.057(4) 0.011(3) 0.023(3) 0.003(3) O30 0.038(3) 0.041(3) 0.038(3) -0.006(3) 0.015(2) 0.004(2) O31 0.048(3) 0.038(3) 0.030(3) -0.005(3) 0.004(3) -0.013(2) O32 0.054(4) 0.039(4) 0.023(3) 0.004(3) 0.006(3) 0.023(3) O33 0.041(3) 0.060(4) 0.033(3) 0.001(4) 0.017(2) 0.008(3) O34 0.040(3) 0.030(3) 0.062(4) -0.009(3) -0.013(3) 0.002(2) O35 0.032(3) 0.049(4) 0.042(4) -0.016(3) -0.001(2) 0.015(3) O36 0.036(3) 0.043(4) 0.034(4) -0.006(2) 0.002(3) 0.008(3) O37 0.034(3) 0.055(3) 0.027(2) -0.004(3) 0.007(2) 0.012(3) O38 0.047(3) 0.031(4) 0.053(4) -0.008(3) -0.006(3) 0.011(2) O39 0.066(4) 0.045(4) 0.030(3) -0.004(3) 0.007(3) -0.023(3) O40 0.060(4) 0.044(4) 0.021(3) 0.001(3) 0.004(3) 0.027(3) _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 O1 1.614(3) . ? V1 O26 1.809(4) . ? V1 O27 1.831(4) . ? V1 O11 1.997(4) . ? V1 O12 2.029(4) . ? V1 O9 2.234(3) . ? V1 V2 3.0679(14) . ? V1 V6 3.1036(15) . ? V1 V5 3.1097(15) . ? V1 N2 3.818(5) 3 ? V1 N3 4.638(5) . ? V2 O2 1.598(3) . ? V2 O14 1.833(4) . ? V2 O13 1.842(4) . ? V2 O12 1.989(4) . ? V2 O11 1.995(4) . ? V2 O10 2.213(3) . ? V2 V4 3.1037(15) . ? V2 V3 3.1157(15) . ? V2 N1 3.883(5) 3_556 ? V3 O3 1.604(4) . ? V3 O15 1.842(4) . ? V3 O13 1.872(4) . ? V3 O16 1.878(4) . ? V3 O17 2.017(4) . ? V3 O10 2.327(4) . ? V3 V9 3.0767(17) . ? V3 V4 3.0869(14) . ? V3 V8 3.1168(14) . ? V3 N2 4.022(5) 2_545 ? V3 N1 4.034(6) 3_556 ? V4 O4 1.600(4) . ? V4 O15 1.829(4) . ? V4 O14 1.872(4) . ? V4 O18 1.881(4) . ? V4 O19 2.047(4) . ? V4 O10 2.318(4) . ? V4 V10 3.0802(17) . ? V4 N1 4.017(6) 3_556 ? V4 N3 4.109(5) 2 ? V4 N1 4.488(6) . ? V5 O5 1.592(4) . ? V5 O24 1.837(4) . ? V5 O27 1.852(4) . ? V5 O22 1.896(4) . ? V5 O25 2.039(4) . ? V5 O9 2.337(4) . ? V5 V10 3.0748(17) . ? V5 V6 3.0802(15) . ? V5 N2 4.011(5) . ? V6 O6 1.597(4) . ? V6 O24 1.826(4) . ? V6 O23 1.874(4) . ? V6 O26 1.886(4) . ? V6 O28 2.049(4) . ? V6 O9 2.330(4) . ? V6 V9 3.0710(17) . ? V6 V7 3.1185(15) . ? V6 N3 3.996(5) . ? V6 N1 4.547(6) 2_545 ? V7 O7 1.606(3) . ? V7 O22 1.806(4) . ? V7 O23 1.815(4) . ? V7 O21 1.999(4) . ? V7 O20 2.016(4) . ? V7 O9 2.253(3) . ? V7 V8 3.0735(14) . ? V7 N3 4.688(5) 2 ? V7 N2 4.698(5) 2_545 ? V7 N1 4.783(5) 3_656 ? V8 O8 1.614(4) . ? V8 O16 1.817(4) . ? V8 O18 1.830(4) . ? V8 O20 2.000(4) . ? V8 O21 2.003(4) . ? V8 O10 2.248(3) . ? V8 N3 3.870(5) 2 ? V8 N2 3.881(5) 2_545 ? V8 N3 4.182(5) 4_656 ? V9 O28 1.685(4) . ? V9 O17 1.696(4) . ? V9 O11 1.919(4) . ? V9 O20 1.922(4) . ? V9 O9 2.097(4) . ? V9 O10 2.127(4) . ? V9 N2 3.652(5) 2_545 ? V9 N3 3.981(5) . ? V10 O19 1.696(4) . ? V10 O25 1.696(4) . ? V10 O12 1.907(4) . ? V10 O21 1.914(4) . ? V10 O10 2.106(4) . ? V10 O9 2.107(4) . ? V10 N3 3.748(5) 2 ? V10 N2 4.014(5) . ? Na1 O30 2.317(6) . ? Na1 O29 2.319(6) . ? Na1 O2 2.497(4) 3 ? Na1 O5 2.504(5) . ? Na1 O1 2.633(4) 3 ? Na1 O3 2.673(5) 2 ? Na1 N2 4.426(6) . ? Na2 O35 2.314(5) . ? Na2 O34 2.354(5) . ? Na2 O32 2.363(5) . ? Na2 O31 2.420(6) . ? Na2 O33 2.439(5) . ? Na2 O36 2.495(6) . ? Na2 Na3 3.551(3) . ? Na2 N2 3.879(5) . ? Na2 N1 4.337(7) 4_565 ? Na3 O36 2.318(6) . ? Na3 O38 2.340(5) . ? Na3 O37 2.343(5) . ? Na3 O40 2.347(5) . ? Na3 O39 2.451(6) . ? Na3 O35 2.543(7) . ? Na3 N3 3.941(6) 2_455 ? Na3 N1 4.437(7) 3_556 ? N1 O39 3.021(9) 3_556 ? N1 O6 3.032(7) 2 ? N1 O4 3.056(7) . ? N1 O31 3.075(8) 4_666 ? N1 O14 3.149(7) 3_556 ? N1 O13 3.157(7) 3_556 ? N1 O7 3.180(6) 3_656 ? N1 O15 3.204(6) 3_556 ? N2 O25 2.849(6) . ? N2 O1 2.932(6) 3 ? N2 O20 2.940(6) 2 ? N2 O32 2.941(8) . ? N2 O17 2.959(6) 2 ? N2 O16 3.067(6) 2 ? N2 O31 3.143(7) . ? N2 O34 3.192(8) . ? N3 O28 2.862(6) . ? N3 O8 2.923(6) 4 ? N3 O21 2.975(6) 2_545 ? N3 O38 3.043(9) 2_445 ? N3 O40 3.046(8) 2_445 ? N3 O18 3.072(6) 2_545 ? N3 O19 3.073(6) 2_545 ? N3 O39 3.414(8) 2_445 ? 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 O1 V1 O26 104.1(2) . . ? O1 V1 O27 104.3(2) . . ? O26 V1 O27 95.23(16) . . ? O1 V1 O11 98.21(18) . . ? O26 V1 O11 91.12(18) . . ? O27 V1 O11 154.28(17) . . ? O1 V1 O12 98.79(18) . . ? O26 V1 O12 155.15(17) . . ? O27 V1 O12 88.38(17) . . ? O11 V1 O12 75.94(14) . . ? O1 V1 O9 172.00(16) . . ? O26 V1 O9 81.59(16) . . ? O27 V1 O9 80.50(16) . . ? O11 V1 O9 75.81(14) . . ? O12 V1 O9 74.76(14) . . ? O1 V1 V2 88.05(13) . . ? O26 V1 V2 130.87(14) . . ? O27 V1 V2 128.10(14) . . ? O11 V1 V2 39.76(11) . . ? O12 V1 V2 39.73(11) . . ? O9 V1 V2 83.95(9) . . ? O1 V1 V6 137.64(16) . . ? O26 V1 V6 33.65(12) . . ? O27 V1 V6 83.83(13) . . ? O11 V1 V6 87.86(11) . . ? O12 V1 V6 123.20(11) . . ? O9 V1 V6 48.46(10) . . ? V2 V1 V6 119.76(4) . . ? O1 V1 V5 136.85(16) . . ? O26 V1 V5 84.09(13) . . ? O27 V1 V5 32.61(12) . . ? O11 V1 V5 124.28(11) . . ? O12 V1 V5 85.90(11) . . ? O9 V1 V5 48.53(10) . . ? V2 V1 V5 118.69(4) . . ? V6 V1 V5 59.44(3) . . ? O1 V1 N2 45.84(15) . 3 ? O26 V1 N2 69.19(14) . 3 ? O27 V1 N2 78.80(14) . 3 ? O11 V1 N2 126.55(13) . 3 ? O12 V1 N2 135.44(13) . 3 ? O9 V1 N2 142.13(12) . 3 ? V2 V1 N2 133.46(8) . 3 ? V6 V1 N2 97.83(8) . 3 ? V5 V1 N2 103.25(8) . 3 ? O1 V1 N3 92.48(18) . . ? O26 V1 N3 41.17(15) . . ? O27 V1 N3 136.29(15) . . ? O11 V1 N3 53.27(13) . . ? O12 V1 N3 129.06(13) . . ? O9 V1 N3 88.15(13) . . ? V2 V1 N3 91.87(8) . . ? V6 V1 N3 58.19(7) . . ? V5 V1 N3 117.62(7) . . ? N2 V1 N3 85.36(10) 3 . ? O2 V2 O14 102.0(2) . . ? O2 V2 O13 103.3(2) . . ? O14 V2 O13 94.14(16) . . ? O2 V2 O12 98.86(18) . . ? O14 V2 O12 90.81(18) . . ? O13 V2 O12 155.71(17) . . ? O2 V2 O11 99.39(19) . . ? O14 V2 O11 156.69(16) . . ? O13 V2 O11 89.72(17) . . ? O12 V2 O11 76.88(14) . . ? O2 V2 O10 174.19(17) . . ? O14 V2 O10 81.27(15) . . ? O13 V2 O10 81.06(16) . . ? O12 V2 O10 76.21(14) . . ? O11 V2 O10 76.64(14) . . ? O2 V2 V1 88.71(14) . . ? O14 V2 V1 131.50(14) . . ? O13 V2 V1 129.52(14) . . ? O12 V2 V1 40.69(12) . . ? O11 V2 V1 39.80(11) . . ? O10 V2 V1 85.54(9) . . ? O2 V2 V4 135.48(16) . . ? O14 V2 V4 33.52(12) . . ? O13 V2 V4 83.63(13) . . ? O12 V2 V4 87.53(12) . . ? O11 V2 V4 124.83(11) . . ? O10 V2 V4 48.20(10) . . ? V1 V2 V4 120.82(4) . . ? O2 V2 V3 136.47(16) . . ? O14 V2 V3 83.96(13) . . ? O13 V2 V3 33.27(12) . . ? O12 V2 V3 124.35(11) . . ? O11 V2 V3 86.81(12) . . ? O10 V2 V3 48.20(10) . . ? V1 V2 V3 119.52(4) . . ? V4 V2 V3 59.51(3) . . ? O2 V2 N1 79.96(16) . 3_556 ? O14 V2 N1 53.23(16) . 3_556 ? O13 V2 N1 53.51(16) . 3_556 ? O12 V2 N1 142.02(16) . 3_556 ? O11 V2 N1 141.04(16) . 3_556 ? O10 V2 N1 105.80(12) . 3_556 ? V1 V2 N1 168.63(9) . 3_556 ? V4 V2 N1 69.16(9) . 3_556 ? V3 V2 N1 69.40(9) . 3_556 ? O3 V3 O15 104.5(2) . . ? O3 V3 O13 103.0(2) . . ? O15 V3 O13 90.29(17) . . ? O3 V3 O16 101.5(2) . . ? O15 V3 O16 91.01(17) . . ? O13 V3 O16 154.33(18) . . ? O3 V3 O17 100.1(2) . . ? O15 V3 O17 155.37(17) . . ? O13 V3 O17 83.99(16) . . ? O16 V3 O17 84.22(16) . . ? O3 V3 O10 174.6(2) . . ? O15 V3 O10 80.89(15) . . ? O13 V3 O10 77.43(15) . . ? O16 V3 O10 77.47(15) . . ? O17 V3 O10 74.49(15) . . ? O3 V3 V9 130.94(17) . . ? O15 V3 V9 124.56(13) . . ? O13 V3 V9 79.23(13) . . ? O16 V3 V9 78.97(13) . . ? O17 V3 V9 30.82(11) . . ? O10 V3 V9 43.68(9) . . ? O3 V3 V4 137.13(17) . . ? O15 V3 V4 32.65(12) . . ? O13 V3 V4 83.66(13) . . ? O16 V3 V4 83.69(13) . . ? O17 V3 V4 122.73(12) . . ? O10 V3 V4 48.24(10) . . ? V9 V3 V4 91.91(4) . . ? O3 V3 V2 135.63(16) . . ? O15 V3 V2 81.07(12) . . ? O13 V3 V2 32.67(13) . . ? O16 V3 V2 122.63(13) . . ? O17 V3 V2 81.27(11) . . ? O10 V3 V2 45.16(8) . . ? V9 V3 V2 61.25(3) . . ? V4 V3 V2 60.05(4) . . ? O3 V3 V8 133.34(16) . . ? O15 V3 V8 81.54(12) . . ? O13 V3 V8 123.43(13) . . ? O16 V3 V8 31.90(12) . . ? O17 V3 V8 81.74(11) . . ? O10 V3 V8 46.00(8) . . ? V9 V3 V8 61.64(3) . . ? V4 V3 V8 60.39(3) . . ? V2 V3 V8 90.96(4) . . ? O3 V3 N2 84.12(17) . 2_545 ? O15 V3 N2 137.88(13) . 2_545 ? O13 V3 N2 128.54(15) . 2_545 ? O16 V3 N2 47.05(14) . 2_545 ? O17 V3 N2 44.92(13) . 2_545 ? O10 V3 N2 91.40(11) . 2_545 ? V9 V3 N2 60.20(8) . 2_545 ? V4 V3 N2 124.79(8) . 2_545 ? V2 V3 N2 121.35(8) . 2_545 ? V8 V3 N2 64.41(7) . 2_545 ? O3 V3 N1 85.06(18) . 3_556 ? O15 V3 N1 50.75(14) . 3_556 ? O13 V3 N1 49.48(15) . 3_556 ? O16 V3 N1 141.25(16) . 3_556 ? O17 V3 N1 132.70(14) . 3_556 ? O10 V3 N1 99.10(13) . 3_556 ? V9 V3 N1 124.96(9) . 3_556 ? V4 V3 N1 67.17(11) . 3_556 ? V2 V3 N1 64.30(9) . 3_556 ? V8 V3 N1 127.47(11) . 3_556 ? N2 V3 N1 167.94(12) 2_545 3_556 ? O4 V4 O15 103.7(2) . . ? O4 V4 O14 102.69(19) . . ? O15 V4 O14 90.88(17) . . ? O4 V4 O18 101.3(2) . . ? O15 V4 O18 91.51(17) . . ? O14 V4 O18 154.60(18) . . ? O4 V4 O19 100.7(2) . . ? O15 V4 O19 155.53(17) . . ? O14 V4 O19 83.71(16) . . ? O18 V4 O19 83.69(16) . . ? O4 V4 O10 174.85(19) . . ? O15 V4 O10 81.37(15) . . ? O14 V4 O10 77.67(15) . . ? O18 V4 O10 77.70(15) . . ? O19 V4 O10 74.16(15) . . ? O4 V4 V10 131.79(17) . . ? O15 V4 V10 124.47(13) . . ? O14 V4 V10 79.14(13) . . ? O18 V4 V10 78.69(13) . . ? O19 V4 V10 31.06(11) . . ? O10 V4 V10 43.10(10) . . ? O4 V4 V3 136.63(17) . . ? O15 V4 V3 32.90(12) . . ? O14 V4 V3 84.20(13) . . ? O18 V4 V3 84.16(13) . . ? O19 V4 V3 122.63(12) . . ? O10 V4 V3 48.47(10) . . ? V10 V4 V3 91.57(4) . . ? O4 V4 V2 135.37(15) . . ? O15 V4 V2 81.59(12) . . ? O14 V4 V2 32.73(12) . . ? O18 V4 V2 123.06(13) . . ? O19 V4 V2 81.04(11) . . ? O10 V4 V2 45.37(8) . . ? V10 V4 V2 61.02(3) . . ? V3 V4 V2 60.44(4) . . ? O4 V4 N1 84.21(18) . 3_556 ? O15 V4 N1 51.15(15) . 3_556 ? O14 V4 N1 49.72(15) . 3_556 ? O18 V4 N1 142.07(16) . 3_556 ? O19 V4 N1 132.63(14) . 3_556 ? O10 V4 N1 99.72(13) . 3_556 ? V10 V4 N1 125.06(9) . 3_556 ? V3 V4 N1 67.75(11) . 3_556 ? V2 V4 N1 64.61(9) . 3_556 ? O4 V4 N3 85.10(17) . 2 ? O15 V4 N3 136.03(13) . 2 ? O14 V4 N3 129.70(15) . 2 ? O18 V4 N3 44.71(14) . 2 ? O19 V4 N3 46.26(13) . 2 ? O10 V4 N3 90.73(12) . 2 ? V10 V4 N3 60.86(8) . 2 ? V3 V4 N3 123.28(8) . 2 ? V2 V4 N3 121.83(8) . 2 ? N1 V4 N3 168.62(13) 3_556 2 ? O4 V4 N1 21.51(16) . . ? O15 V4 N1 98.83(15) . . ? O14 V4 N1 124.02(14) . . ? O18 V4 N1 80.52(15) . . ? O19 V4 N1 103.98(14) . . ? O10 V4 N1 158.21(11) . . ? V10 V4 N1 131.92(9) . . ? V3 V4 N1 128.65(9) . . ? V2 V4 N1 156.42(8) . . ? N1 V4 N1 97.14(12) 3_556 . ? N3 V4 N1 73.90(10) 2 . ? O5 V5 O24 104.5(2) . . ? O5 V5 O27 102.1(2) . . ? O24 V5 O27 91.88(17) . . ? O5 V5 O22 103.4(2) . . ? O24 V5 O22 90.16(17) . . ? O27 V5 O22 153.10(18) . . ? O5 V5 O25 99.9(2) . . ? O24 V5 O25 155.52(17) . . ? O27 V5 O25 84.40(16) . . ? O22 V5 O25 82.74(16) . . ? O5 V5 O9 174.2(2) . . ? O24 V5 O9 81.24(15) . . ? O27 V5 O9 77.33(15) . . ? O22 V5 O9 76.48(14) . . ? O25 V5 O9 74.33(15) . . ? O5 V5 V10 131.05(17) . . ? O24 V5 V10 124.43(13) . . ? O27 V5 V10 78.98(13) . . ? O22 V5 V10 77.79(12) . . ? O25 V5 V10 31.12(11) . . ? O9 V5 V10 43.21(10) . . ? O5 V5 V6 137.16(17) . . ? O24 V5 V6 32.65(12) . . ? O27 V5 V6 84.19(13) . . ? O22 V5 V6 83.16(13) . . ? O25 V5 V6 122.91(12) . . ? O9 V5 V6 48.59(10) . . ? V10 V5 V6 91.80(4) . . ? O5 V5 V1 134.16(16) . . ? O24 V5 V1 81.53(12) . . ? O27 V5 V1 32.18(12) . . ? O22 V5 V1 122.23(13) . . ? O25 V5 V1 82.56(11) . . ? O9 V5 V1 45.76(8) . . ? V10 V5 V1 62.00(3) . . ? V6 V5 V1 60.18(4) . . ? O5 V5 N2 68.97(18) . . ? O24 V5 N2 152.98(14) . . ? O27 V5 N2 65.25(15) . . ? O22 V5 N2 116.79(14) . . ? O25 V5 N2 42.13(13) . . ? O9 V5 N2 105.85(12) . . ? V10 V5 N2 67.51(8) . . ? V6 V5 N2 145.31(8) . . ? V1 V5 N2 85.23(8) . . ? O6 V6 O24 104.3(2) . . ? O6 V6 O23 102.5(2) . . ? O24 V6 O23 91.74(17) . . ? O6 V6 O26 102.0(2) . . ? O24 V6 O26 91.26(17) . . ? O23 V6 O26 153.73(18) . . ? O6 V6 O28 100.1(2) . . ? O24 V6 O28 155.64(18) . . ? O23 V6 O28 83.18(17) . . ? O26 V6 O28 83.38(17) . . ? O6 V6 O9 174.1(2) . . ? O24 V6 O9 81.65(15) . . ? O23 V6 O9 77.15(14) . . ? O26 V6 O9 77.48(15) . . ? O28 V6 O9 74.00(15) . . ? O6 V6 V9 131.06(17) . . ? O24 V6 V9 124.67(13) . . ? O23 V6 V9 78.05(13) . . ? O26 V6 V9 78.81(13) . . ? O28 V6 V9 30.97(11) . . ? O9 V6 V9 43.02(10) . . ? O6 V6 V5 137.13(18) . . ? O24 V6 V5 32.86(12) . . ? O23 V6 V5 84.70(13) . . ? O26 V6 V5 83.76(13) . . ? O28 V6 V5 122.78(12) . . ? O9 V6 V5 48.79(10) . . ? V9 V6 V5 91.81(4) . . ? O6 V6 V1 134.09(17) . . ? O24 V6 V1 81.86(12) . . ? O23 V6 V1 123.02(13) . . ? O26 V6 V1 32.09(12) . . ? O28 V6 V1 81.07(11) . . ? O9 V6 V1 45.87(8) . . ? V9 V6 V1 61.30(3) . . ? V5 V6 V1 60.38(4) . . ? O6 V6 V7 134.09(17) . . ? O24 V6 V7 81.50(12) . . ? O23 V6 V7 31.73(12) . . ? O26 V6 V7 123.57(13) . . ? O28 V6 V7 81.78(11) . . ? O9 V6 V7 46.09(8) . . ? V9 V6 V7 61.60(3) . . ? V5 V6 V7 60.80(4) . . ? V1 V6 V7 91.74(4) . . ? O6 V6 N3 71.14(18) . . ? O24 V6 N3 148.54(14) . . ? O23 V6 N3 119.72(15) . . ? O26 V6 N3 60.72(15) . . ? O28 V6 N3 43.02(13) . . ? O9 V6 N3 103.80(12) . . ? V9 V6 N3 67.09(8) . . ? V5 V6 N3 140.89(8) . . ? V1 V6 N3 80.51(8) . . ? V7 V6 N3 124.79(9) . . ? O6 V6 N1 14.91(18) . 2_545 ? O24 V6 N1 94.04(15) . 2_545 ? O23 V6 N1 114.12(14) . 2_545 ? O26 V6 N1 91.67(14) . 2_545 ? O28 V6 N1 109.81(14) . 2_545 ? O9 V6 N1 168.17(11) . 2_545 ? V9 V6 N1 139.93(9) . 2_545 ? V5 V6 N1 126.09(9) . 2_545 ? V1 V6 N1 122.76(8) . 2_545 ? V7 V6 N1 144.41(7) . 2_545 ? N3 V6 N1 74.27(11) . 2_545 ? O7 V7 O22 103.9(2) . . ? O7 V7 O23 102.87(19) . . ? O22 V7 O23 95.54(16) . . ? O7 V7 O21 100.40(18) . . ? O22 V7 O21 89.75(17) . . ? O23 V7 O21 154.10(16) . . ? O7 V7 O20 99.72(18) . . ? O22 V7 O20 154.31(16) . . ? O23 V7 O20 88.93(17) . . ? O21 V7 O20 76.01(14) . . ? O7 V7 O9 174.22(17) . . ? O22 V7 O9 80.43(15) . . ? O23 V7 O9 80.33(16) . . ? O21 V7 O9 75.57(14) . . ? O20 V7 O9 75.39(14) . . ? O7 V7 V8 89.71(14) . . ? O22 V7 V8 129.61(13) . . ? O23 V7 V8 128.81(14) . . ? O21 V7 V8 39.87(11) . . ? O20 V7 V8 39.88(11) . . ? O9 V7 V8 84.54(9) . . ? O7 V7 V6 135.54(15) . . ? O22 V7 V6 83.40(13) . . ? O23 V7 V6 32.88(12) . . ? O21 V7 V6 123.70(11) . . ? O20 V7 V6 86.89(11) . . ? O9 V7 V6 48.16(10) . . ? V8 V7 V6 119.52(4) . . ? O7 V7 N3 82.77(17) . 2 ? O22 V7 N3 78.34(14) . 2 ? O23 V7 N3 172.62(14) . 2 ? O21 V7 N3 23.96(12) . 2 ? O20 V7 N3 94.85(13) . 2 ? O9 V7 N3 94.46(12) . 2 ? V8 V7 N3 55.19(7) . 2 ? V6 V7 N3 140.87(7) . 2 ? O7 V7 N2 84.00(17) . 2_545 ? O22 V7 N2 170.14(14) . 2_545 ? O23 V7 N2 76.70(14) . 2_545 ? O21 V7 N2 94.70(13) . 2_545 ? O20 V7 N2 22.59(12) . 2_545 ? O9 V7 N2 92.14(12) . 2_545 ? V8 V7 N2 55.26(7) . 2_545 ? V6 V7 N2 86.81(7) . 2_545 ? N3 V7 N2 108.91(8) 2 2_545 ? O7 V7 N1 2.85(18) . 3_656 ? O22 V7 N1 106.65(14) . 3_656 ? O23 V7 N1 101.79(14) . 3_656 ? O21 V7 N1 100.91(13) . 3_656 ? O20 V7 N1 97.10(13) . 3_656 ? O9 V7 N1 172.23(12) . 3_656 ? V8 V7 N1 88.37(7) . 3_656 ? V6 V7 N1 134.61(8) . 3_656 ? N3 V7 N1 84.06(10) 2 3_656 ? N2 V7 N1 81.17(10) 2_545 3_656 ? O8 V8 O16 103.8(2) . . ? O8 V8 O18 102.95(19) . . ? O16 V8 O18 95.01(16) . . ? O8 V8 O20 99.71(18) . . ? O16 V8 O20 89.62(17) . . ? O18 V8 O20 155.02(17) . . ? O8 V8 O21 99.23(18) . . ? O16 V8 O21 154.73(17) . . ? O18 V8 O21 89.76(17) . . ? O20 V8 O21 76.29(14) . . ? O8 V8 O10 173.81(16) . . ? O16 V8 O10 80.77(15) . . ? O18 V8 O10 80.58(15) . . ? O20 V8 O10 75.95(14) . . ? O21 V8 O10 75.55(14) . . ? O8 V8 V7 88.92(14) . . ? O16 V8 V7 129.89(13) . . ? O18 V8 V7 129.53(14) . . ? O20 V8 V7 40.27(11) . . ? O21 V8 V7 39.77(11) . . ? O10 V8 V7 84.92(9) . . ? O8 V8 V3 136.79(16) . . ? O16 V8 V3 33.11(12) . . ? O18 V8 V3 84.08(12) . . ? O20 V8 V3 86.59(11) . . ? O21 V8 V3 123.62(11) . . ? O10 V8 V3 48.12(10) . . ? V7 V8 V3 119.50(4) . . ? O8 V8 N3 80.48(18) . 2 ? O16 V8 N3 145.30(15) . 2 ? O18 V8 N3 51.13(15) . 2 ? O20 V8 N3 124.05(14) . 2 ? O21 V8 N3 49.15(13) . 2 ? O10 V8 N3 98.17(13) . 2 ? V7 V8 N3 84.11(9) . 2 ? V3 V8 N3 130.42(9) . 2 ? O8 V8 N2 83.65(18) . 2_545 ? O16 V8 N2 50.59(15) . 2_545 ? O18 V8 N2 145.21(15) . 2_545 ? O20 V8 N2 47.86(13) . 2_545 ? O21 V8 N2 123.30(13) . 2_545 ? O10 V8 N2 96.36(13) . 2_545 ? V7 V8 N2 84.14(8) . 2_545 ? V3 V8 N2 69.17(8) . 2_545 ? N3 V8 N2 160.39(10) 2 2_545 ? O8 V8 N3 31.15(15) . 4_656 ? O16 V8 N3 85.70(14) . 4_656 ? O18 V8 N3 79.58(14) . 4_656 ? O20 V8 N3 125.31(13) . 4_656 ? O21 V8 N3 119.57(13) . 4_656 ? O10 V8 N3 154.83(12) . 4_656 ? V7 V8 N3 119.80(8) . 4_656 ? V3 V8 N3 114.20(8) . 4_656 ? N3 V8 N3 81.13(11) 2 4_656 ? N2 V8 N3 91.20(10) 2_545 4_656 ? O28 V9 O17 107.3(2) . . ? O28 V9 O11 97.50(18) . . ? O17 V9 O11 96.44(18) . . ? O28 V9 O20 97.58(18) . . ? O17 V9 O20 96.80(18) . . ? O11 V9 O20 155.97(18) . . ? O28 V9 O9 88.04(18) . . ? O17 V9 O9 164.67(18) . . ? O11 V9 O9 80.79(15) . . ? O20 V9 O9 81.15(15) . . ? O28 V9 O10 166.11(18) . . ? O17 V9 O10 86.61(17) . . ? O11 V9 O10 80.35(15) . . ? O20 V9 O10 80.52(14) . . ? O9 V9 O10 78.07(14) . . ? O28 V9 V6 38.76(14) . . ? O17 V9 V6 146.04(14) . . ? O11 V9 V6 90.22(12) . . ? O20 V9 V6 89.92(12) . . ? O9 V9 V6 49.28(10) . . ? O10 V9 V6 127.35(11) . . ? O28 V9 V3 144.84(15) . . ? O17 V9 V3 37.56(14) . . ? O11 V9 V3 89.27(12) . . ? O20 V9 V3 89.10(12) . . ? O9 V9 V3 127.12(11) . . ? O10 V9 V3 49.06(10) . . ? V6 V9 V3 176.40(5) . . ? O28 V9 N2 83.67(16) . 2_545 ? O17 V9 N2 52.96(15) . 2_545 ? O11 V9 N2 147.39(14) . 2_545 ? O20 V9 N2 53.31(14) . 2_545 ? O9 V9 N2 131.75(12) . 2_545 ? O10 V9 N2 105.61(12) . 2_545 ? V6 V9 N2 109.25(9) . 2_545 ? V3 V9 N2 72.84(8) . 2_545 ? O28 V9 N3 38.55(15) . . ? O17 V9 N3 83.31(15) . . ? O11 V9 N3 70.47(14) . . ? O20 V9 N3 131.06(14) . . ? O9 V9 N3 109.57(13) . . ? O10 V9 N3 147.71(12) . . ? V6 V9 N3 67.62(8) . . ? V3 V9 N3 115.50(9) . . ? N2 V9 N3 92.50(10) 2_545 . ? O19 V10 O25 106.59(19) . . ? O19 V10 O12 96.98(18) . . ? O25 V10 O12 96.97(17) . . ? O19 V10 O21 97.45(17) . . ? O25 V10 O21 97.35(18) . . ? O12 V10 O21 155.82(18) . . ? O19 V10 O10 87.30(17) . . ? O25 V10 O10 166.11(17) . . ? O12 V10 O10 80.56(15) . . ? O21 V10 O10 80.86(15) . . ? O19 V10 O9 165.60(18) . . ? O25 V10 O9 87.80(17) . . ? O12 V10 O9 80.30(15) . . ? O21 V10 O9 80.90(14) . . ? O10 V10 O9 78.32(14) . . ? O19 V10 V5 144.98(14) . . ? O25 V10 V5 38.41(13) . . ? O12 V10 V5 88.99(12) . . ? O21 V10 V5 90.23(12) . . ? O10 V10 V5 127.70(11) . . ? O9 V10 V5 49.39(10) . . ? O19 V10 V4 38.51(14) . . ? O25 V10 V4 145.10(14) . . ? O12 V10 V4 89.67(12) . . ? O21 V10 V4 89.64(12) . . ? O10 V10 V4 48.79(10) . . ? O9 V10 V4 127.10(11) . . ? V5 V10 V4 176.44(5) . . ? O19 V10 N3 53.96(15) . 2 ? O25 V10 N3 84.39(15) . 2 ? O12 V10 N3 149.37(15) . 2 ? O21 V10 N3 51.85(14) . 2 ? O10 V10 N3 104.76(13) . 2 ? O9 V10 N3 130.29(12) . 2 ? V5 V10 N3 109.37(9) . 2 ? V4 V10 N3 73.26(9) . 2 ? O19 V10 N2 81.18(15) . . ? O25 V10 N2 37.04(14) . . ? O12 V10 N2 73.67(14) . . ? O21 V10 N2 127.80(14) . . ? O10 V10 N2 150.12(12) . . ? O9 V10 N2 111.22(13) . . ? V5 V10 N2 67.43(8) . . ? V4 V10 N2 115.30(8) . . ? N3 V10 N2 90.56(10) 2 . ? O30 Na1 O29 85.74(18) . . ? O30 Na1 O2 80.11(18) . 3 ? O29 Na1 O2 87.27(19) . 3 ? O30 Na1 O5 143.60(19) . . ? O29 Na1 O5 84.71(19) . . ? O2 Na1 O5 134.23(19) 3 . ? O30 Na1 O1 127.02(19) . 3 ? O29 Na1 O1 134.0(2) . 3 ? O2 Na1 O1 70.90(12) 3 3 ? O5 Na1 O1 83.04(15) . 3 ? O30 Na1 O3 76.56(18) . 2 ? O29 Na1 O3 118.93(18) . 2 ? O2 Na1 O3 142.90(19) 3 2 ? O5 Na1 O3 77.64(14) . 2 ? O1 Na1 O3 101.30(15) 3 2 ? O30 Na1 N2 130.47(18) . . ? O29 Na1 N2 140.95(18) . . ? O2 Na1 N2 110.28(12) 3 . ? O5 Na1 N2 57.78(12) . . ? O1 Na1 N2 39.73(10) 3 . ? O3 Na1 N2 66.83(12) 2 . ? O35 Na2 O34 93.5(2) . . ? O35 Na2 O32 175.5(2) . . ? O34 Na2 O32 85.2(2) . . ? O35 Na2 O31 95.5(2) . . ? O34 Na2 O31 87.7(2) . . ? O32 Na2 O31 88.7(2) . . ? O35 Na2 O33 88.27(19) . . ? O34 Na2 O33 178.3(2) . . ? O32 Na2 O33 93.1(2) . . ? O31 Na2 O33 92.07(19) . . ? O35 Na2 O36 86.13(19) . . ? O34 Na2 O36 87.31(19) . . ? O32 Na2 O36 89.5(2) . . ? O31 Na2 O36 174.87(19) . . ? O33 Na2 O36 92.85(19) . . ? O35 Na2 Na3 45.60(16) . . ? O34 Na2 Na3 89.41(18) . . ? O32 Na2 Na3 130.04(17) . . ? O31 Na2 Na3 140.72(16) . . ? O33 Na2 Na3 91.83(13) . . ? O36 Na2 Na3 40.55(13) . . ? O35 Na2 N2 132.87(18) . . ? O34 Na2 N2 55.28(18) . . ? O32 Na2 N2 49.19(17) . . ? O31 Na2 N2 54.04(15) . . ? O33 Na2 N2 123.33(15) . . ? O36 Na2 N2 121.58(15) . . ? Na3 Na2 N2 144.02(10) . . ? O35 Na2 N1 58.31(17) . 4_565 ? O34 Na2 N1 110.33(16) . 4_565 ? O32 Na2 N1 126.16(17) . 4_565 ? O31 Na2 N1 43.54(15) . 4_565 ? O33 Na2 N1 70.58(18) . 4_565 ? O36 Na2 N1 140.16(15) . 4_565 ? Na3 Na2 N1 102.24(9) . 4_565 ? N2 Na2 N1 97.15(11) . 4_565 ? O36 Na3 O38 98.3(2) . . ? O36 Na3 O37 86.96(19) . . ? O38 Na3 O37 174.1(2) . . ? O36 Na3 O40 173.6(2) . . ? O38 Na3 O40 84.7(2) . . ? O37 Na3 O40 89.8(2) . . ? O36 Na3 O39 97.4(2) . . ? O38 Na3 O39 91.7(2) . . ? O37 Na3 O39 90.2(2) . . ? O40 Na3 O39 88.0(2) . . ? O36 Na3 O35 84.96(18) . . ? O38 Na3 O35 88.96(19) . . ? O37 Na3 O35 89.0(2) . . ? O40 Na3 O35 89.5(2) . . ? O39 Na3 O35 177.4(2) . . ? O36 Na3 Na2 44.43(16) . . ? O38 Na3 Na2 95.59(17) . . ? O37 Na3 Na2 86.38(13) . . ? O40 Na3 Na2 129.91(17) . . ? O39 Na3 Na2 141.82(17) . . ? O35 Na3 Na2 40.55(12) . . ? O36 Na3 N3 135.40(18) . 2_455 ? O38 Na3 N3 50.45(18) . 2_455 ? O37 Na3 N3 126.58(16) . 2_455 ? O40 Na3 N3 50.53(18) . 2_455 ? O39 Na3 N3 59.23(17) . 2_455 ? O35 Na3 N3 119.57(15) . 2_455 ? Na2 Na3 N3 145.08(11) . 2_455 ? O36 Na3 N1 60.78(16) . 3_556 ? O38 Na3 N1 111.76(16) . 3_556 ? O37 Na3 N1 73.05(19) . 3_556 ? O40 Na3 N1 123.34(17) . 3_556 ? O39 Na3 N1 40.36(17) . 3_556 ? O35 Na3 N1 141.39(14) . 3_556 ? Na2 Na3 N1 103.07(9) . 3_556 ? N3 Na3 N1 98.22(11) 2_455 3_556 ? O39 N1 O6 101.6(2) 3_556 2 ? O39 N1 O4 68.18(18) 3_556 . ? O6 N1 O4 66.15(16) 2 . ? O39 N1 O31 92.30(18) 3_556 4_666 ? O6 N1 O31 60.17(17) 2 4_666 ? O4 N1 O31 117.0(2) . 4_666 ? O39 N1 O14 100.7(2) 3_556 3_556 ? O6 N1 O14 143.9(2) 2 3_556 ? O4 N1 O14 96.9(2) . 3_556 ? O31 N1 O14 146.2(2) 4_666 3_556 ? O39 N1 O13 146.3(2) 3_556 3_556 ? O6 N1 O13 112.1(2) 2 3_556 ? O4 N1 O13 125.2(2) . 3_556 ? O31 N1 O13 104.4(2) 4_666 3_556 ? O14 N1 O13 50.52(12) 3_556 3_556 ? O39 N1 O7 55.70(16) 3_556 3_656 ? O6 N1 O7 109.1(2) 2 3_656 ? O4 N1 O7 121.7(2) . 3_656 ? O31 N1 O7 56.13(15) 4_666 3_656 ? O14 N1 O7 106.9(2) 3_556 3_656 ? O13 N1 O7 110.6(2) 3_556 3_656 ? O39 N1 O15 129.6(3) 3_556 3_556 ? O6 N1 O15 95.02(19) 2 3_556 ? O4 N1 O15 76.27(16) . 3_556 ? O31 N1 O15 136.3(3) 4_666 3_556 ? O14 N1 O15 49.05(12) 3_556 3_556 ? O13 N1 O15 48.90(12) 3_556 3_556 ? O7 N1 O15 154.0(2) 3_656 3_556 ? O25 N2 O1 103.64(19) . 3 ? O25 N2 O20 115.41(19) . 2 ? O1 N2 O20 125.4(2) 3 2 ? O25 N2 O32 88.39(17) . . ? O1 N2 O32 90.95(19) 3 . ? O20 N2 O32 125.1(2) 2 . ? O25 N2 O17 71.98(15) . 2 ? O1 N2 O17 109.76(19) 3 2 ? O20 N2 O17 54.67(13) 2 2 ? O32 N2 O17 154.0(2) . 2 ? O25 N2 O16 116.90(19) . 2 ? O1 N2 O16 75.94(16) 3 2 ? O20 N2 O16 53.23(13) 2 2 ? O32 N2 O16 153.4(2) . 2 ? O17 N2 O16 51.38(13) 2 2 ? O25 N2 O31 146.1(2) . . ? O1 N2 O31 99.43(18) 3 . ? O20 N2 O31 67.85(15) 2 . ? O32 N2 O31 66.58(16) . . ? O17 N2 O31 122.4(2) 2 . ? O16 N2 O31 92.52(17) 2 . ? O25 N2 O34 85.69(17) . . ? O1 N2 O34 152.0(2) 3 . ? O20 N2 O34 70.50(16) 2 . ? O32 N2 O34 62.56(16) . . ? O17 N2 O34 98.27(18) 2 . ? O16 N2 O34 123.72(19) 2 . ? O31 N2 O34 62.96(16) . . ? O28 N3 O8 117.6(2) . 4 ? O28 N3 O21 112.1(2) . 2_545 ? O8 N3 O21 125.7(2) 4 2_545 ? O28 N3 O38 85.92(19) . 2_445 ? O8 N3 O38 133.7(2) 4 2_445 ? O21 N3 O38 68.21(16) 2_545 2_445 ? O28 N3 O40 94.45(19) . 2_445 ? O8 N3 O40 75.69(16) 4 2_445 ? O21 N3 O40 121.3(2) 2_545 2_445 ? O38 N3 O40 62.44(16) 2_445 2_445 ? O28 N3 O18 114.6(2) . 2_545 ? O8 N3 O18 86.27(18) 4 2_545 ? O21 N3 O18 53.17(13) 2_545 2_545 ? O38 N3 O18 121.4(2) 2_445 2_545 ? O40 N3 O18 150.6(2) 2_445 2_545 ? O28 N3 O19 70.13(15) . 2_545 ? O8 N3 O19 128.3(2) 4 2_545 ? O21 N3 O19 53.35(13) 2_545 2_545 ? O38 N3 O19 96.27(19) 2_445 2_545 ? O40 N3 O19 155.2(2) 2_445 2_545 ? O18 N3 O19 50.54(13) 2_545 2_545 ? O28 N3 O39 147.6(2) . 2_445 ? O8 N3 O39 79.81(16) 4 2_445 ? O21 N3 O39 69.28(15) 2_545 2_445 ? O38 N3 O39 64.02(16) 2_445 2_445 ? O40 N3 O39 61.84(16) 2_445 2_445 ? O18 N3 O39 92.48(17) 2_545 2_445 ? O19 N3 O39 122.38(19) 2_545 2_445 ? V1 O1 Na1 143.9(2) . 3 ? V1 O1 N2 110.9(2) . 3 ? Na1 O1 N2 105.23(15) 3 3 ? V2 O2 Na1 148.2(2) . 3 ? V2 O2 N1 76.46(15) . 3_556 ? Na1 O2 N1 135.32(15) 3 3_556 ? V3 O3 Na1 140.5(2) . 2_545 ? V4 O4 N1 147.4(2) . . ? V5 O5 Na1 159.5(3) . . ? V5 O5 N2 87.67(18) . . ? Na1 O5 N2 87.79(15) . . ? V6 O6 N1 157.3(3) . 2_545 ? V6 O6 N3 85.39(19) . . ? N1 O6 N3 98.02(18) 2_545 . ? V7 O7 N1 175.7(3) . 3_656 ? V8 O8 N3 132.2(2) . 4_656 ? V8 O8 N3 75.68(17) . 2 ? N3 O8 N3 98.54(16) 4_656 2 ? V8 O8 N2 72.92(17) . 2_545 ? N3 O8 N2 110.88(17) 4_656 2_545 ? N3 O8 N2 146.59(13) 2 2_545 ? V9 O9 V10 102.29(14) . . ? V9 O9 V1 93.19(14) . . ? V10 O9 V1 94.35(14) . . ? V9 O9 V7 93.49(14) . . ? V10 O9 V7 92.87(14) . . ? V1 O9 V7 168.91(17) . . ? V9 O9 V6 87.69(16) . . ? V10 O9 V6 170.0(2) . . ? V1 O9 V6 85.67(12) . . ? V7 O9 V6 85.75(12) . . ? V9 O9 V5 170.3(2) . . ? V10 O9 V5 87.40(16) . . ? V1 O9 V5 85.71(12) . . ? V7 O9 V5 86.21(13) . . ? V6 O9 V5 82.62(11) . . ? V10 O10 V9 101.32(14) . . ? V10 O10 V2 93.22(14) . . ? V9 O10 V2 93.23(14) . . ? V10 O10 V8 93.19(14) . . ? V9 O10 V8 92.95(14) . . ? V2 O10 V8 170.05(17) . . ? V10 O10 V4 88.11(15) . . ? V9 O10 V4 170.56(19) . . ? V2 O10 V4 86.43(12) . . ? V8 O10 V4 86.19(12) . . ? V10 O10 V3 171.40(19) . . ? V9 O10 V3 87.27(15) . . ? V2 O10 V3 86.65(13) . . ? V8 O10 V3 85.88(12) . . ? V4 O10 V3 83.30(11) . . ? V9 O11 V2 107.41(18) . . ? V9 O11 V1 107.01(18) . . ? V2 O11 V1 100.43(18) . . ? V9 O11 N3 81.09(15) . . ? V2 O11 N3 152.56(18) . . ? V1 O11 N3 101.81(16) . . ? V10 O12 V2 107.38(18) . . ? V10 O12 V1 108.03(18) . . ? V2 O12 V1 99.58(18) . . ? V10 O12 N2 78.58(14) . . ? V2 O12 N2 151.48(18) . . ? V1 O12 N2 105.02(15) . . ? V2 O13 V3 114.1(2) . . ? V2 O13 N1 98.5(2) . 3_556 ? V3 O13 N1 103.73(19) . 3_556 ? V2 O14 V4 113.7(2) . . ? V2 O14 N1 99.0(2) . 3_556 ? V4 O14 N1 103.31(19) . 3_556 ? V4 O15 V3 114.44(18) . . ? V4 O15 N1 102.4(2) . 3_556 ? V3 O15 N1 102.81(19) . 3_556 ? V8 O16 V3 115.0(2) . . ? V8 O16 N2 102.16(18) . 2_545 ? V3 O16 N2 106.32(18) . 2_545 ? V9 O17 V3 111.6(2) . . ? V9 O17 N2 99.82(19) . 2_545 ? V3 O17 N2 106.30(18) . 2_545 ? V9 O17 N3 72.69(15) . . ? V3 O17 N3 151.18(17) . . ? N2 O17 N3 100.70(15) 2_545 . ? V8 O18 V4 114.4(2) . . ? V8 O18 N3 101.24(18) . 2 ? V4 O18 N3 109.77(19) . 2 ? V10 O19 V4 110.4(2) . . ? V10 O19 N3 99.54(18) . 2 ? V4 O19 N3 104.97(18) . 2 ? V10 O19 N2 74.76(15) . . ? V4 O19 N2 153.63(16) . . ? N3 O19 N2 99.36(16) 2 . ? V9 O20 V8 108.01(18) . . ? V9 O20 V7 107.18(18) . . ? V8 O20 V7 99.85(17) . . ? V9 O20 N2 95.09(17) . 2_545 ? V8 O20 N2 101.84(17) . 2_545 ? V7 O20 N2 142.14(19) . 2_545 ? V10 O21 V7 107.76(18) . . ? V10 O21 V8 107.78(18) . . ? V7 O21 V8 100.36(17) . . ? V10 O21 N3 97.75(17) . 2 ? V7 O21 N3 140.21(19) . 2 ? V8 O21 N3 100.23(18) . 2 ? V7 O22 V5 115.8(2) . . ? V7 O23 V6 115.4(2) . . ? V6 O24 V5 114.49(18) . . ? V10 O25 V5 110.5(2) . . ? V10 O25 N2 121.9(2) . . ? V5 O25 N2 109.18(18) . . ? V10 O25 N3 70.38(15) . 2 ? V5 O25 N3 134.44(16) . 2 ? N2 O25 N3 107.15(16) . 2 ? V1 O26 V6 114.3(2) . . ? V1 O26 N3 118.87(19) . . ? V6 O26 N3 91.12(17) . . ? V1 O26 N2 82.78(16) . 3 ? V6 O26 N2 143.7(2) . 3 ? N3 O26 N2 108.91(15) . 3 ? V1 O27 V5 115.2(2) . . ? V1 O27 N2 121.79(18) . . ? V5 O27 N2 87.28(16) . . ? V1 O27 N2 73.79(14) . 3 ? V5 O27 N2 139.86(19) . 3 ? N2 O27 N2 122.62(12) . 3 ? V9 O28 V6 110.3(2) . . ? V9 O28 N3 119.9(2) . . ? V6 O28 N3 107.74(19) . . ? V9 O28 N2 70.55(15) . 2_545 ? V6 O28 N2 134.94(17) . 2_545 ? N3 O28 N2 109.72(17) . 2_545 ? Na2 O31 N1 103.6(2) . 4_565 ? Na2 O31 N2 87.42(19) . . ? N1 O31 N2 165.6(2) 4_565 . ? Na2 O32 N2 93.4(2) . . ? Na2 O34 N2 87.4(2) . . ? Na2 O35 Na3 93.9(2) . . ? Na2 O35 N1 89.5(2) . 4_565 ? Na3 O35 N1 162.1(2) . 4_565 ? Na3 O36 Na2 95.0(2) . . ? Na3 O36 N1 87.76(19) . 3_556 ? Na2 O36 N1 160.0(2) . 3_556 ? Na3 O38 N3 93.2(2) . 2_455 ? Na3 O39 N1 107.9(2) . 3_556 ? Na3 O39 N3 82.7(2) . 2_455 ? N1 O39 N3 160.5(2) 3_556 2_455 ? Na3 O40 N3 93.0(2) . 2_455 ? _refine_diff_density_max 0.426 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.092 _shelx_res_file ; TITL JM-7955 7955.res created by SHELXL-2016/6 at 15:29:41 on 04-Jul-2020 CELL 0.71075 12.0248 17.1212 18.1397 90.0000 106.2421 90.0000 ZERR 4 0.0017 0.0026 0.0029 0.0000 0.0075 0.0000 LATT 1 SYMM .50-X, .50+Y, .50-Z SFAC H NA O V N UNIT 144 12 160 40 12 L.S. 30 OMIT 2 6 1 OMIT -5 1 5 CONN 8 3 N1 CONN 8 3 N2 CONN 8 3 N3 FMAP 2 DFIX 0.82 0.03 O29 H29A O29 H29B O30 H30A O30 H30B O31 H31A O31 H31B DFIX 0.82 0.03 O32 H32A O32 H32A O31 H31A O31 H31B O34 H34A O34 H34B DFIX 0.82 0.03 O35 H35A O35 H35B O36 H36A O36 H36B O37 H37A O37 H37B DFIX 0.82 0.03 O38 H38A O38 H38B O39 H39A O39 H39B O40 H40A O40 H40B DFIX 1.30 0.03 H29a H29b H30a H30b H31a H31b H32a H32b H33a H33b H34a H34b DFIX 1.30 0.03 H35a H35b H36a H36b H37a H37b H38a H38b H39a H39b H40a H40b DFIX 0.9 0.03 N1 H1a N1 H1b N1 H1c N1 H1d N2 H2a N2 H2b N2 H2c N2 H2d DFIX 0.9 0.03 N3 H3a N3 H3b N3 H3c N3 H3d DFIX 1.45 0.03 H1a H1b H1a H1c H1a H1d H1b H1c H1b H1d H1c H1d DFIX 1.45 0.03 H2a H2b H2a H2c H2a H2d H2b H2c H2b H2d H2c H2d DFIX 1.45 0.03 H3a H3b H3a H3c H3a H3d H3b H3c H3b H3d H3c H3d PLAN 40 HTAB ACTA SIZE 0.050 0.060 0.100 WGHT 0.037900 FVAR 0.25135 V1 4 0.066201 -0.129053 0.102924 11.00000 0.01980 0.02564 = 0.01231 0.00008 0.00161 -0.00112 V2 4 -0.013533 -0.127135 0.249466 11.00000 0.01663 0.02379 = 0.01772 0.00026 0.00353 -0.00123 V3 4 0.130907 -0.215706 0.394833 11.00000 0.02507 0.02056 = 0.01896 0.00306 0.00671 -0.00247 V4 4 0.124576 -0.035463 0.393656 11.00000 0.02386 0.02156 = 0.01760 -0.00091 0.00649 0.00105 V5 4 0.285393 -0.034035 0.100145 11.00000 0.02615 0.02365 = 0.01727 0.00457 0.00643 -0.00028 V6 4 0.294241 -0.213839 0.102722 11.00000 0.02817 0.02188 = 0.01870 -0.00305 0.00769 0.00097 V7 4 0.434085 -0.121102 0.246855 11.00000 0.01879 0.02073 = 0.01555 0.00016 0.00449 0.00048 V8 4 0.352499 -0.122188 0.393008 11.00000 0.01918 0.02012 = 0.01439 0.00060 0.00296 -0.00025 V9 4 0.212316 -0.220410 0.248482 11.00000 0.02058 0.01555 = 0.01556 -0.00090 0.00294 0.00009 V10 4 0.206253 -0.029231 0.247257 11.00000 0.01978 0.01349 = 0.01785 -0.00011 0.00454 0.00036 NA1 2 0.282055 0.124327 -0.065150 11.00000 0.03566 0.05682 = 0.02652 0.00501 0.00948 0.00211 NA2 2 -0.193219 0.139872 0.168773 11.00000 0.03224 0.02904 = 0.03504 -0.00188 0.01117 0.00569 NA3 2 -0.309554 0.106239 0.325619 11.00000 0.03248 0.03383 = 0.03239 -0.00365 0.00813 0.00369 N1 5 0.175448 0.129140 0.592919 11.00000 0.03855 0.05698 = 0.04400 -0.00224 0.02117 -0.00373 H1A 1 0.214482 0.083186 0.597301 11.00000 -1.20000 H1B 1 0.221978 0.167403 0.612081 11.00000 -1.20000 H1C 1 0.145554 0.136808 0.542225 11.00000 -1.20000 H1D 1 0.117075 0.122589 0.613143 11.00000 -1.20000 N2 5 0.092155 0.154662 0.109658 11.00000 0.02547 0.01737 = 0.02100 0.00718 0.00578 0.00237 H2A 1 0.141698 0.117559 0.131876 11.00000 -1.20000 H2B 1 0.095559 0.161513 0.061884 11.00000 -1.20000 H2C 1 0.020691 0.139958 0.106748 11.00000 -1.20000 H2D 1 0.106257 0.197223 0.136117 11.00000 -1.20000 N3 5 0.094833 -0.399268 0.108099 11.00000 0.03404 0.02077 = 0.02664 0.00130 0.00038 0.00150 H3A 1 0.148888 -0.365936 0.134736 11.00000 -1.20000 H3B 1 0.056980 -0.380035 0.064482 11.00000 -1.20000 H3C 1 0.134384 -0.441391 0.099542 11.00000 -1.20000 H3D 1 0.052135 -0.416730 0.136007 11.00000 -1.20000 O1 3 -0.068514 -0.131447 0.054172 11.00000 0.01899 0.03271 = 0.01932 -0.00107 -0.00152 -0.00022 O2 3 -0.144599 -0.127836 0.196861 11.00000 0.01611 0.02906 = 0.02336 -0.00069 -0.00089 0.00020 O3 3 0.106424 -0.284780 0.447965 11.00000 0.03486 0.02837 = 0.02776 0.00575 0.00810 -0.00294 O4 3 0.095003 0.032035 0.446228 11.00000 0.02856 0.02693 = 0.02870 -0.01109 0.01122 0.00290 O5 3 0.310193 0.034403 0.047461 11.00000 0.03746 0.03551 = 0.02296 0.00969 0.01119 -0.00313 O6 3 0.325965 -0.281847 0.051861 11.00000 0.04347 0.03457 = 0.02751 -0.00644 0.01421 0.00691 O7 3 0.566258 -0.119662 0.298920 11.00000 0.01541 0.03019 = 0.02522 -0.00027 0.00249 -0.00051 O8 3 0.486288 -0.119354 0.443483 11.00000 0.01946 0.03058 = 0.01800 -0.00336 -0.00079 -0.00135 O9 3 0.243570 -0.124749 0.184877 11.00000 0.02006 0.01637 = 0.00935 0.00343 0.00116 0.00245 O10 3 0.173209 -0.124495 0.311491 11.00000 0.01760 0.01659 = 0.01710 -0.00114 0.00517 0.00257 O11 3 0.056459 -0.199510 0.188629 11.00000 0.02036 0.01835 = 0.01592 -0.00046 0.00351 -0.00349 O12 3 0.053360 -0.054865 0.187352 11.00000 0.01506 0.02410 = 0.01107 0.00362 0.00098 -0.00071 O13 3 -0.010675 -0.205883 0.319140 11.00000 0.02600 0.02366 = 0.01694 0.00023 0.00389 0.00329 O14 3 -0.016178 -0.048760 0.317832 11.00000 0.01811 0.02202 = 0.02418 -0.00511 0.00644 -0.00070 O15 3 0.100730 -0.125578 0.441258 11.00000 0.02365 0.02774 = 0.01556 -0.00246 0.00606 -0.00042 O16 3 0.291131 -0.201090 0.436077 11.00000 0.02516 0.01838 = 0.01326 0.00307 0.00318 -0.00149 O17 3 0.177288 -0.278691 0.314195 11.00000 0.02034 0.02077 = 0.02091 -0.00047 0.00387 -0.00229 O18 3 0.286019 -0.044066 0.434979 11.00000 0.01898 0.02488 = 0.01835 -0.00034 0.00597 -0.00315 O19 3 0.167641 0.029693 0.311100 11.00000 0.02220 0.01494 = 0.02253 -0.00270 0.00511 -0.00094 O20 3 0.366082 -0.194677 0.309484 11.00000 0.02059 0.01642 = 0.01346 -0.00453 0.00185 0.00073 O21 3 0.361237 -0.050308 0.307698 11.00000 0.01828 0.01468 = 0.01276 -0.00341 0.00152 -0.00058 O22 3 0.427537 -0.043754 0.178083 11.00000 0.01751 0.02530 = 0.01809 0.00133 0.00488 0.00103 O23 3 0.433352 -0.200315 0.180195 11.00000 0.02292 0.01938 = 0.02216 -0.00007 0.00652 0.00372 O24 3 0.317303 -0.123995 0.054784 11.00000 0.02699 0.02971 = 0.01591 -0.00078 0.00814 0.00145 O25 3 0.240106 0.030222 0.181886 11.00000 0.01860 0.01729 = 0.01836 0.00132 0.00567 -0.00082 O26 3 0.132380 -0.205554 0.060860 11.00000 0.02706 0.02746 = 0.01492 -0.00378 0.00251 -0.00254 O27 3 0.127274 -0.048595 0.060332 11.00000 0.02347 0.02457 = 0.01523 0.00234 0.00430 -0.00242 O28 3 0.249907 -0.279153 0.184882 11.00000 0.02719 0.01836 = 0.01711 -0.00345 0.00244 -0.00004 O29 3 0.386231 0.031412 -0.111057 11.00000 0.03677 0.04394 = 0.05709 0.01123 0.02327 0.00271 H29A 1 0.392663 -0.012603 -0.095563 11.00000 -1.20000 H29B 1 0.445830 0.042436 -0.123458 11.00000 -1.20000 O30 3 0.374430 0.215201 -0.122191 11.00000 0.03754 0.04072 = 0.03785 -0.00563 0.01484 0.00363 H30A 1 0.424918 0.200090 -0.141322 11.00000 -1.20000 H30B 1 0.392535 0.262139 -0.113595 11.00000 -1.20000 O31 3 -0.139077 0.245895 0.097627 11.00000 0.04762 0.03803 = 0.02984 -0.00503 0.00393 -0.01340 H31A 1 -0.083071 0.268815 0.123766 11.00000 -1.20000 H31B 1 -0.130154 0.249974 0.054778 11.00000 -1.20000 O32 3 -0.107077 0.051813 0.100750 11.00000 0.05433 0.03880 = 0.02323 0.00384 0.00632 0.02287 H32A 1 -0.113239 0.043048 0.055620 11.00000 -1.20000 H32B 1 -0.071426 0.020643 0.124702 11.00000 -1.20000 O33 3 -0.383830 0.128290 0.076433 11.00000 0.04149 0.06001 = 0.03268 0.00061 0.01685 0.00778 H33A 1 -0.354313 0.145397 0.037647 11.00000 -1.20000 H33B 1 -0.424279 0.165793 0.076420 11.00000 -1.20000 O34 3 -0.006958 0.148675 0.255449 11.00000 0.04031 0.02980 = 0.06215 -0.00933 -0.01340 0.00217 H34A 1 0.045225 0.116734 0.275449 11.00000 -1.20000 H34B 1 0.021117 0.189881 0.270065 11.00000 -1.20000 O35 3 -0.276294 0.218573 0.242564 11.00000 0.03179 0.04883 = 0.04162 -0.01602 -0.00105 0.01485 H35A 1 -0.336177 0.242895 0.222581 11.00000 -1.20000 H35B 1 -0.243505 0.246596 0.278681 11.00000 -1.20000 O36 3 -0.230243 0.029165 0.248225 11.00000 0.03598 0.04256 = 0.03366 -0.00627 0.00173 0.00800 H36A 1 -0.273704 -0.000848 0.218372 11.00000 -1.20000 H36B 1 -0.170233 0.006606 0.265630 11.00000 -1.20000 O37 3 -0.120358 0.123176 0.404561 11.00000 0.03411 0.05498 = 0.02673 -0.00357 0.00664 0.01207 H37A 1 -0.061149 0.103484 0.397494 11.00000 -1.20000 H37B 1 -0.104776 0.125293 0.452019 11.00000 -1.20000 O38 3 -0.503056 0.101612 0.251648 11.00000 0.04668 0.03078 = 0.05343 -0.00809 -0.00632 0.01064 H38A 1 -0.512565 0.064192 0.225917 11.00000 -1.20000 H38B 1 -0.556697 0.131043 0.234838 11.00000 -1.20000 O39 3 -0.341665 0.002277 0.410245 11.00000 0.06564 0.04548 = 0.03043 -0.00402 0.00684 -0.02332 H39A 1 -0.387977 -0.033531 0.401010 11.00000 -1.20000 H39B 1 -0.332312 0.013775 0.454232 11.00000 -1.20000 O40 3 -0.376928 0.195557 0.401395 11.00000 0.05969 0.04415 = 0.02096 0.00054 0.00409 0.02716 H40A 1 -0.373274 0.190119 0.444614 11.00000 -1.20000 H40B 1 -0.416574 0.232541 0.383197 11.00000 -1.20000 HKLF 4 REM JM-7955 REM R1 = 0.0389 for 2897 Fo > 4sig(Fo) and 0.0889 for all 5138 data REM 613 parameters refined using 66 restraints END WGHT 0.0379 0.0000 REM Instructions for potential hydrogen bonds EQIV $2 -x, -y, -z+1 HTAB N1 O39_$2 EQIV $7 x+1/2, -y+1/2, z+1/2 HTAB N1 O31_$7 HTAB N1 O4 EQIV $3 -x+1/2, y+1/2, -z+1/2 HTAB N1 O6_$3 HTAB N1 O13_$2 HTAB N1 O14_$2 HTAB N1 O15_$2 HTAB N2 O25 EQIV $1 -x, -y, -z HTAB N2 O1_$1 HTAB N2 O31 HTAB N2 O32 HTAB N2 O17_$3 HTAB N2 O20_$3 HTAB N3 O28 EQIV $6 x-1/2, -y-1/2, z-1/2 HTAB N3 O8_$6 EQIV $4 -x+1/2, y-1/2, -z+1/2 HTAB N3 O18_$4 HTAB N3 O19_$4 HTAB N3 O21_$4 EQIV $8 -x-1/2, y-1/2, -z+1/2 HTAB N3 O38_$8 HTAB O29 O33_$1 EQIV $13 -x+1, -y, -z HTAB O29 O22_$13 HTAB O30 O23_$13 EQIV $14 x+1/2, -y+1/2, z-1/2 HTAB O30 O37_$14 HTAB O31 O7_$3 HTAB O31 O20_$3 HTAB O31 O6_$1 HTAB O31 O26_$1 HTAB O32 O27_$1 HTAB O32 O12 EQIV $11 -x-1/2, y+1/2, -z+1/2 HTAB O33 O3_$11 HTAB O34 O19 HTAB O34 O23_$3 HTAB O35 O13_$11 HTAB O35 O2_$11 EQIV $15 x-1/2, -y+1/2, z+1/2 HTAB O35 O30_$15 HTAB O36 O29_$1 HTAB O36 O14 HTAB O37 O4 HTAB O37 O15_$2 EQIV $16 x-1, y, z HTAB O38 O22_$16 HTAB O38 O17_$11 HTAB O39 O7_$16 HTAB O39 O8_$16 HTAB O39 O18_$2 HTAB O40 O16_$2 HTAB O40 O1_$11 HTAB O40 O11_$11 REM Highest difference peak 0.426, deepest hole -0.368, 1-sigma level 0.092 Q1 1 0.3365 -0.2992 0.0147 11.00000 0.05 0.43 Q2 1 0.3354 -0.1598 0.3392 11.00000 0.05 0.35 Q3 1 -0.1581 -0.0705 0.1514 11.00000 0.05 0.32 Q4 1 0.1564 -0.2666 0.2751 11.00000 0.05 0.31 Q5 1 0.0685 -0.2596 0.5026 11.00000 0.05 0.31 Q6 1 0.2971 0.1273 0.0998 11.00000 0.05 0.31 Q7 1 0.3578 -0.0628 0.3477 11.00000 0.05 0.30 Q8 1 0.2429 0.0219 0.2067 11.00000 0.05 0.30 Q9 1 0.0354 -0.1928 0.1533 11.00000 0.05 0.30 Q10 1 -0.3308 0.0780 0.3446 11.00000 0.05 0.30 Q11 1 -0.2152 0.0591 0.3758 11.00000 0.05 0.30 Q12 1 -0.4636 0.2187 0.1273 11.00000 0.05 0.30 Q13 1 -0.2808 0.2338 0.1805 11.00000 0.05 0.30 Q14 1 0.5330 -0.1132 0.4855 11.00000 0.05 0.29 Q15 1 0.1411 -0.0273 0.1815 11.00000 0.05 0.29 Q16 1 0.3748 -0.2627 0.0664 11.00000 0.05 0.29 Q17 1 0.4545 0.1401 -0.0431 11.00000 0.05 0.29 Q18 1 0.2810 0.0248 -0.0014 11.00000 0.05 0.29 Q19 1 -0.0637 0.0591 0.2929 11.00000 0.05 0.29 Q20 1 0.2392 -0.0223 0.1673 11.00000 0.05 0.29 Q21 1 -0.3345 0.1340 0.3233 11.00000 0.05 0.28 Q22 1 0.0337 0.0678 0.2123 11.00000 0.05 0.28 Q23 1 0.1224 -0.2404 0.1909 11.00000 0.05 0.28 Q24 1 0.1594 0.0980 0.3329 11.00000 0.05 0.28 Q25 1 -0.0967 -0.1201 0.1703 11.00000 0.05 0.28 Q26 1 0.0329 -0.0678 0.1530 11.00000 0.05 0.28 Q27 1 0.1126 -0.1659 0.1978 11.00000 0.05 0.28 Q28 1 0.0261 -0.0660 0.2186 11.00000 0.05 0.28 Q29 1 0.4325 0.2875 -0.1752 11.00000 0.05 0.28 Q30 1 0.1181 -0.2946 0.1426 11.00000 0.05 0.28 Q31 1 0.5816 -0.1202 0.4546 11.00000 0.05 0.28 Q32 1 0.2258 0.1753 0.1439 11.00000 0.05 0.28 Q33 1 0.2163 -0.1145 -0.0001 11.00000 0.05 0.28 Q34 1 0.1600 0.0196 0.4945 11.00000 0.05 0.27 Q35 1 0.2012 -0.1699 0.0662 11.00000 0.05 0.27 Q36 1 -0.1750 0.0013 0.0177 11.00000 0.05 0.27 Q37 1 -0.1568 -0.1721 0.1518 11.00000 0.05 0.27 Q38 1 0.2335 0.0390 0.3074 11.00000 0.05 0.27 Q39 1 0.5360 -0.0803 0.2769 11.00000 0.05 0.27 Q40 1 0.4389 0.1498 -0.1704 11.00000 0.05 0.27 ; _shelx_res_checksum 66664 _shelx_hkl_file ; -1 -2 1 -11.78 7.51 1 2 -1 1.03 10.83 1 2 -1 -10.80 10.18 1 2 -1 -10.72 11.98 1 -2 -1 6.91 12.87 1 -2 -1 -1.69 2.26 -1 -2 1 0.13 6.22 -1 -2 1 12.26 8.40 -1 2 1 -3.61 12.38 -1 2 1 1.41 2.65 1 0 2 4.18 9.02 1 0 2 -15.53 6.78 -1 0 -2 26.04 13.88 -1 0 -2 -6.64 7.10 0 2 -2 1.73 8.52 0 -2 2 -27.69 13.96 0 2 2 -4.01 9.28 0 -2 2 4.68 9.04 0 -2 -2 13.04 7.67 0 2 2 6.18 11.38 0 -2 2 3.64 13.11 0 2 -2 -11.60 13.83 0 2 -2 4.57 8.80 0 -2 -2 -2.29 9.81 -1 -2 -1 12.25 8.68 1 -2 1 -1.14 6.78 1 2 1 -13.59 9.20 1 -2 1 0.01 11.84 1 2 1 7.37 8.71 -1 2 -1 7.46 7.10 -1 -2 -1 11.22 7.75 1 2 1 4.22 5.20 -1 2 -1 -20.69 7.66 2 0 -1 3.99 6.28 2 0 -1 -6.71 6.44 -2 0 1 5.21 4.98 -2 0 1 1.97 6.59 2 0 -1 8.35 5.30 -1 -2 2 810.18 38.56 1 -2 -2 776.02 17.77 1 2 -2 841.82 28.31 1 2 -2 785.49 28.33 -1 2 2 799.38 18.09 1 -2 -2 778.89 28.97 -1 -2 2 880.75 37.44 -1 -2 2 866.47 30.00 1 2 -2 775.92 28.89 -1 2 2 792.13 38.54 -1 0 3 1349.52 37.67 -1 0 3 1370.54 48.24 -1 0 3 1319.99 41.82 1 0 -3 1364.06 35.83 1 0 -3 1361.16 53.46 1 0 -3 1448.94 49.16 1 -1 2 13.15 10.32 0 0 3 13.28 8.61 1 1 2 3.50 4.45 -1 1 -2 8.40 9.81 0 0 3 19.64 10.86 -1 -1 -2 10.42 14.34 1 -1 2 -1.34 9.02 1 1 2 7.08 9.28 0 0 -3 -10.57 8.52 -1 1 -2 -13.69 13.05 0 0 3 28.10 12.78 0 0 -3 21.29 10.43 0 0 -3 12.32 13.33 -2 0 0 3353.50 70.05 2 0 0 3280.25 89.39 -2 0 0 3295.80 91.38 0 -3 0 10.03 10.47 0 3 0 12.26 7.59 0 3 0 -22.70 15.05 0 -3 0 12.42 11.73 0 -3 0 -12.83 9.33 2 -1 -1 49.29 8.02 2 1 -1 28.04 9.32 2 1 -1 51.82 15.77 -2 1 1 43.73 12.32 2 -1 -1 15.73 12.23 -2 1 1 47.46 8.21 -2 -1 1 30.31 5.84 -2 -1 1 70.08 10.09 2 0 -2 2086.59 59.05 2 0 -2 1865.72 62.25 -2 0 2 2099.11 51.78 -2 0 2 1884.31 61.58 1 -1 -3 7.60 5.89 1 -1 -3 10.82 10.78 1 1 -3 31.84 15.33 1 -1 -3 -1.75 6.83 1 1 -3 45.82 15.04 -1 1 3 18.74 15.40 -1 -1 3 39.28 9.96 1 1 -3 17.03 10.07 -1 -1 3 14.05 10.04 -1 1 3 37.72 8.60 -1 -1 3 27.92 10.59 0 1 3 11.06 11.83 0 1 -3 -12.52 8.30 0 1 -3 0.99 9.05 0 -1 3 6.26 14.37 0 -1 3 7.52 14.89 0 -1 -3 3.56 8.00 0 -1 -3 -2.02 4.22 0 1 3 16.56 12.72 0 1 3 3.50 6.72 0 -1 3 27.68 14.30 0 -1 -3 5.60 12.82 0 1 -3 33.67 9.90 2 -1 0 168.08 10.34 2 -1 0 186.89 9.22 2 1 0 189.08 14.98 2 1 0 181.70 14.83 -2 -1 0 167.14 14.49 -2 -1 0 157.43 7.21 2 1 0 182.31 7.59 -2 1 0 169.87 13.19 -2 1 0 193.26 16.61 0 -3 -1 41.63 18.41 0 -3 1 58.77 11.01 0 3 1 62.48 11.66 0 3 1 35.34 13.25 0 3 -1 89.05 10.62 0 -3 1 35.45 11.02 0 3 -1 42.51 19.47 0 -3 1 52.87 12.91 0 -3 -1 68.72 5.81 0 -3 -1 83.32 13.79 -2 1 2 250.54 15.38 -2 -1 2 306.38 23.72 2 1 -2 270.97 13.63 -2 1 2 277.12 11.23 2 1 -2 289.60 22.10 -2 -1 2 266.64 13.59 2 -1 -2 256.77 11.06 1 3 0 69.30 20.27 -1 -3 0 40.51 12.42 -1 3 0 80.96 20.11 1 3 0 82.58 8.37 1 -3 0 60.19 7.56 -1 -3 0 71.18 12.90 -1 -3 0 71.87 10.42 -1 3 0 70.95 7.64 1 3 0 56.39 10.06 1 -3 0 55.26 13.19 -1 -3 1 202.77 21.80 1 -3 -1 156.76 16.48 -1 -3 1 189.85 16.31 1 3 -1 146.53 13.17 1 3 -1 165.67 16.51 1 3 -1 208.02 21.99 -1 3 1 143.50 24.40 1 -3 -1 166.29 7.15 -1 3 1 154.69 6.64 -1 -3 1 164.51 13.26 2 0 1 16.72 4.92 -2 0 -1 10.34 10.28 -2 0 -1 10.41 3.11 2 0 1 -5.67 15.85 1 2 2 196.44 15.61 -1 -2 -2 191.14 24.01 1 2 2 178.52 14.91 -1 2 -2 180.24 20.32 -1 2 -2 157.55 14.35 -1 -2 -2 137.66 14.49 1 -2 2 152.35 14.13 1 -2 2 191.88 21.00 -2 2 1 189.88 8.92 2 2 -1 184.99 25.36 2 -2 -1 142.10 7.52 2 -2 -1 219.69 21.25 -2 -2 1 186.89 16.15 -2 2 1 143.22 21.37 -2 -2 1 183.78 14.84 2 2 -1 183.68 15.54 -2 1 -1 318.73 15.89 2 -1 1 294.93 24.92 -2 -1 -1 354.60 30.73 2 1 1 383.79 20.16 2 -1 1 352.55 16.59 -2 1 -1 351.95 26.21 -1 -2 3 -0.21 11.13 -1 -2 3 11.76 11.96 1 -2 -3 14.18 7.73 1 2 -3 50.89 11.55 1 2 -3 -2.53 10.54 -1 -2 3 -4.89 11.40 -1 2 3 -2.21 17.28 1 2 -3 -1.14 11.38 -1 2 3 12.26 7.65 -2 0 3 -0.88 9.58 2 0 -3 12.27 15.04 -2 0 3 5.80 11.59 2 0 -3 1.22 7.16 0 -2 3 782.48 32.95 0 -2 3 756.76 42.13 0 -2 -3 777.48 35.17 0 2 3 776.30 34.47 0 2 3 783.42 26.74 0 2 -3 827.97 42.93 0 -2 3 756.69 30.34 0 2 -3 779.79 31.50 0 2 -3 775.65 43.40 0 -2 -3 782.05 13.64 2 -2 0 0.46 8.51 2 2 0 -0.81 17.19 -2 -2 0 -8.73 10.56 -2 -2 0 -0.60 4.24 2 -2 0 -11.60 12.61 2 2 0 17.22 6.62 -2 2 0 1.75 9.27 -2 2 0 -7.56 7.84 0 3 2 23.35 7.60 0 3 -2 16.17 18.77 0 3 2 18.66 10.43 0 -3 2 29.26 18.04 0 -3 2 58.92 17.65 0 3 -2 20.17 17.42 0 3 -2 10.04 11.38 0 -3 2 6.94 11.68 0 -3 -2 9.99 16.41 0 3 2 5.56 12.16 -1 -3 -1 65.14 9.90 1 -3 1 72.20 10.17 1 -3 1 71.99 19.63 -1 3 -1 57.89 15.93 1 3 1 107.49 14.62 -1 -3 -1 72.05 12.87 1 3 1 61.90 9.10 -1 -3 -1 47.87 6.23 -1 3 -1 86.70 20.54 1 3 1 102.39 20.01 -1 0 -3 1553.77 54.75 1 0 3 1631.45 41.24 1 0 3 1597.26 54.11 -1 0 -3 1509.54 40.11 -2 -2 2 0.80 8.37 2 2 -2 3.28 8.25 2 2 -2 -10.37 10.49 2 -2 -2 -1.36 0.98 -2 2 2 19.65 15.56 -2 -2 2 -26.03 10.72 2 -2 -2 3.96 9.99 2 -2 -2 2.74 1.96 2 2 -2 -3.33 17.09 1 -3 -2 131.96 16.21 -1 -3 2 105.32 14.56 -1 3 2 110.85 16.27 -1 3 2 122.06 8.96 -1 -3 2 138.76 15.68 1 3 -2 161.71 21.78 -1 -3 2 115.74 15.58 -1 3 2 131.18 9.30 1 3 -2 146.54 14.50 1 3 -2 134.38 16.20 -2 -1 3 308.19 27.45 -2 1 3 319.13 20.46 -2 -1 3 347.74 19.37 2 1 -3 375.39 18.83 -2 1 3 352.80 15.01 2 1 -3 376.09 28.28 2 1 -3 336.67 22.22 2 -1 -3 356.65 14.58 1 1 3 27.98 7.25 -1 1 -3 31.88 9.13 -1 -1 -3 14.78 12.15 -1 1 -3 28.37 17.60 1 -1 3 16.20 18.96 -1 -1 -3 25.52 7.37 1 1 3 -8.83 19.22 1 -1 3 34.98 14.15 -1 0 4 6.97 16.24 -1 0 4 -1.77 8.58 -1 0 4 19.25 14.12 1 0 -4 -16.31 8.35 1 0 -4 16.24 10.46 2 2 1 1419.86 34.32 -1 1 4 33.07 14.48 2 2 1 1399.26 49.19 -1 1 4 40.43 13.14 -1 -1 4 39.29 19.72 2 -2 1 1489.82 41.46 1 1 -4 54.79 18.95 -2 -2 -1 1339.77 66.16 -1 -1 4 30.27 19.02 -2 -2 -1 1396.14 33.91 1 -1 -4 42.01 13.88 -1 -1 4 47.58 19.86 2 -2 1 1292.19 39.31 1 -1 -4 61.18 14.41 -2 2 -1 1363.30 51.15 -2 2 -1 1389.28 40.49 1 1 -4 84.14 21.14 1 -1 -4 37.61 13.38 1 1 -4 59.16 18.89 0 0 4 3047.85 97.54 0 0 -4 2899.94 107.06 0 0 4 2923.22 90.30 0 0 4 2931.60 94.02 0 0 -4 2763.39 88.93 0 0 -4 3083.61 86.56 -2 0 -2 283.07 10.79 2 0 2 259.98 21.17 -2 0 -2 319.09 31.78 2 0 2 280.46 11.19 0 4 0 264.76 19.41 0 -4 0 264.14 20.82 0 -4 0 246.97 16.42 0 -4 0 294.01 14.61 0 4 0 226.76 24.86 0 -1 -4 5.45 15.00 0 -1 -4 -14.66 14.65 0 -1 -4 9.15 8.83 0 1 4 -15.48 8.74 0 -1 4 14.05 11.30 0 1 4 -18.14 13.86 0 -1 4 14.48 10.80 0 1 4 -9.39 9.23 0 -1 4 0.36 9.69 0 1 -4 1.31 15.47 0 1 -4 2.19 11.10 0 1 -4 -1.42 15.18 2 2 -3 1047.43 49.73 -2 -2 3 1025.18 41.63 -2 2 3 1007.81 20.29 -2 2 3 973.15 39.46 2 2 -3 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48.00 8 12 -1 83.41 49.50 3 16 1 1514.65 166.61 8 -12 -1 58.03 25.68 -8 -12 1 -1.62 38.74 -3 -16 -1 1399.40 116.98 6 -2 -17 28.65 45.84 4 -3 14 59.78 40.40 -4 12 12 1652.94 83.05 -4 12 12 2066.27 162.98 -4 12 12 1707.60 98.63 -3 16 -1 1352.71 123.75 -8 12 1 105.13 59.91 7 8 8 -12.35 44.64 7 8 8 -89.09 63.96 -6 2 17 -28.85 41.67 -4 -12 12 1939.06 225.36 -4 -3 -14 -90.45 40.70 8 12 -1 6.43 48.87 -4 3 -14 38.99 41.07 -4 -12 12 1830.24 164.66 3 16 1 1308.60 125.64 7 8 8 4.21 12.55 3 -16 1 1148.40 156.84 4 12 -12 2236.57 164.08 3 -16 1 1494.45 96.20 4 3 14 -9.42 39.42 4 -3 14 -16.68 33.12 4 -12 -12 1675.62 77.07 0 0 -17 -41.98 39.73 6 -2 -17 49.03 39.37 7 8 8 0.69 13.48 4 3 14 5.55 29.94 4 12 -12 2009.02 169.70 3 -16 1 1558.85 199.32 4 12 -12 2191.25 165.59 -8 12 1 37.05 29.44 0 0 -17 -18.86 37.77 7 -8 8 -22.99 33.89 0 0 17 -1.56 43.39 7 -8 8 -41.31 41.07 0 0 17 -15.43 59.52 -6 -2 17 -4.17 34.78 8 -12 -1 53.47 40.80 8 12 -1 32.98 74.81 4 7 -16 71.01 68.39 4 7 -16 31.40 68.00 -4 -7 16 26.72 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