# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name W.Bensch _publ_contact_author_email WBENSCH@AC.UNI-KIEL.DE loop_ _publ_author_name W.Bensch E.Antonova C.Nather P.Koegerler data_ea669r _database_code_depnum_ccdc_archive 'CCDC 866641' #TrackingRef '- compound1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; _publ_requested_journal 'Dalton Trans' ; _chemical_name_common "_publ_requested_journal 'Dalton Trans'" _chemical_melting_point ? _chemical_formula_moiety 'O42 Sb4 V16, 2(C12 H38 N8 Zn), 7(H2O)' _chemical_formula_sum 'C24 H90 N16 O49 Sb4 V16 Zn2' _chemical_formula_weight 2819.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.7070(19) _cell_length_b 13.9512(5) _cell_length_c 23.1435(14) _cell_angle_alpha 90.00 _cell_angle_beta 128.076(6) _cell_angle_gamma 90.00 _cell_volume 7804.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36771 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.03 _exptl_crystal_description ? _exptl_crystal_colour brown _exptl_crystal_size_max 0.1056 _exptl_crystal_size_mid 0.0910 _exptl_crystal_size_min 0.0801 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5480 _exptl_absorpt_coefficient_mu 3.877 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5302 _exptl_absorpt_correction_T_max 0.5729 _exptl_absorpt_process_details 'X-Shape (STOE & CIE, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Imaging Plate Diffraction System' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 36771 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 28.03 _reflns_number_total 9130 _reflns_number_gt 6726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE-IPDS Program Package' _computing_cell_refinement 'STOE-IPDS Program Package' _computing_data_reduction 'STOE-IPDS Program Package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+75.5622P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9130 _refine_ls_number_parameters 501 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.200965(14) 0.31376(3) 0.39016(2) 0.01782(8) Uani 1 1 d . . . Sb2 Sb 0.161855(15) 0.07893(3) 0.40199(2) 0.01903(9) Uani 1 1 d . . . Zn1 Zn -0.12832(3) 0.80579(5) 0.33000(4) 0.02114(14) Uani 1 1 d . . . V1 V 0.01485(4) 0.35809(6) 0.41211(5) 0.01401(17) Uani 1 1 d . . . V2 V 0.11004(4) 0.47243(6) 0.38309(5) 0.01440(18) Uani 1 1 d . . . V3 V 0.05073(4) 0.10892(6) 0.40316(5) 0.01541(18) Uani 1 1 d . . . V4 V -0.03914(4) 0.02117(6) 0.26047(5) 0.01690(19) Uani 1 1 d . . . V5 V -0.09702(4) 0.17984(6) 0.28489(5) 0.01518(18) Uani 1 1 d . . . V6 V 0.12233(4) 0.28506(6) 0.45912(5) 0.01498(18) Uani 1 1 d . . . V7 V -0.09938(4) 0.39989(6) 0.28215(5) 0.01558(18) Uani 1 1 d . . . V8 V 0.03700(4) 0.54721(6) 0.22915(5) 0.01451(18) Uani 1 1 d . . . O1 O 0.04104(16) 0.0330(3) 0.3238(2) 0.0192(8) Uani 1 1 d . . . O2 O 0.04125(16) 0.5419(3) 0.3163(2) 0.0192(8) Uani 1 1 d . . . O3 O -0.02791(15) 0.4603(3) 0.3419(2) 0.0181(8) Uani 1 1 d . . . O4 O 0.11988(16) 0.1572(3) 0.4219(2) 0.0210(9) Uani 1 1 d . . . O5 O 0.11144(16) 0.0936(3) 0.2955(2) 0.0212(8) Uani 1 1 d . . . O6 O -0.02903(16) 0.1071(3) 0.3330(2) 0.0205(8) Uani 1 1 d . . . O7 O 0.17003(18) 0.2851(3) 0.5479(2) 0.0282(9) Uani 1 1 d . . . O8 O 0.10687(16) 0.4736(3) 0.2958(2) 0.0186(8) Uani 1 1 d . . . O9 O 0.06861(19) 0.0409(3) 0.4707(2) 0.0269(10) Uani 1 1 d . . . O10 O 0.21352(16) 0.1809(3) 0.4246(2) 0.0246(9) Uani 1 1 d . . . O11 O -0.05634(16) 0.2930(3) 0.3448(2) 0.0199(8) Uani 1 1 d . . . O12 O 0.08128(16) 0.4048(3) 0.4259(2) 0.0180(8) Uani 1 1 d . . . O13 O 0.15585(17) 0.5506(3) 0.4409(2) 0.0248(9) Uani 1 1 d . . . O14 O 0.02584(17) 0.3837(3) 0.4892(2) 0.0224(9) Uani 1 1 d . . . O15 O 0.04833(18) 0.6589(3) 0.2188(3) 0.0262(9) Uani 1 1 d . . . O17 O 0.05280(16) 0.2387(3) 0.4310(2) 0.0204(8) Uani 1 1 d . . . O16 O -0.13790(17) 0.4488(3) 0.3011(3) 0.0279(10) Uani 1 1 d . . . O18 O 0.15095(16) 0.3475(3) 0.4123(2) 0.0187(8) Uani 1 1 d . . . O19 O 0.14052(16) 0.2879(3) 0.2860(2) 0.0201(8) Uani 1 1 d . . . O20 O -0.13229(18) 0.1364(3) 0.3087(3) 0.0275(9) Uani 1 1 d . . . O21 O -0.05011(18) -0.0916(3) 0.2670(3) 0.0281(10) Uani 1 1 d . . . O22 O 0.0000 0.2887(13) 0.2500 0.148(7) Uani 1 2 d S . . N6 N 0.07841(19) 0.7658(3) 0.4763(3) 0.0204(10) Uani 1 1 d . . . N4 N -0.2203(2) 0.8385(4) 0.2542(3) 0.0245(11) Uani 1 1 d . . . N8 N 0.1089(2) 0.5209(4) 0.5588(3) 0.0285(12) Uani 1 1 d . . . H8A H 0.0869 0.4707 0.5462 0.043 Uiso 1 1 calc R . . H8B H 0.1220 0.5409 0.6033 0.043 Uiso 1 1 calc R . . H8C H 0.1370 0.5041 0.5589 0.043 Uiso 1 1 calc R . . N3 N -0.1419(2) 0.8019(4) 0.2308(3) 0.0291(12) Uani 1 1 d . . . H3A H -0.1126 0.8268 0.2361 0.035 Uiso 1 1 calc R . . H3B H -0.1463 0.7409 0.2155 0.035 Uiso 1 1 calc R . . N2 N -0.1276(2) 0.9387(4) 0.3724(3) 0.0274(11) Uani 1 1 d . . . H2A H -0.1019 0.9386 0.4215 0.033 Uiso 1 1 calc R . . H2B H -0.1189 0.9851 0.3541 0.033 Uiso 1 1 calc R . . N5 N -0.0441(2) 0.7719(4) 0.4060(3) 0.0254(11) Uani 1 1 d . . . H5A H -0.0401 0.7307 0.4388 0.030 Uiso 1 1 calc R . . H5B H -0.0341 0.7406 0.3818 0.030 Uiso 1 1 calc R . . N1 N -0.1591(3) 0.6769(4) 0.3393(3) 0.0331(13) Uani 1 1 d . . . H1C H -0.1433 0.6273 0.3336 0.040 Uiso 1 1 calc R . . H1D H -0.1495 0.6731 0.3847 0.040 Uiso 1 1 calc R . . C10 C 0.1072(3) 0.8306(4) 0.4600(4) 0.0278(13) Uani 1 1 d . . . H10A H 0.1440 0.8438 0.5049 0.033 Uiso 1 1 calc R . . H10B H 0.0873 0.8908 0.4415 0.033 Uiso 1 1 calc R . . N7 N 0.0549(3) 0.7680(4) 0.3345(3) 0.0356(13) Uani 1 1 d . . . H7C H 0.0575 0.7428 0.3014 0.053 Uiso 1 1 calc R . . H7D H 0.0359 0.8226 0.3172 0.053 Uiso 1 1 calc R . . H7E H 0.0376 0.7271 0.3436 0.053 Uiso 1 1 calc R . . C12 C 0.0772(3) 0.5994(4) 0.5051(3) 0.0238(12) Uani 1 1 d . . . H12A H 0.0462 0.6170 0.5043 0.029 Uiso 1 1 calc R . . H12B H 0.0624 0.5773 0.4564 0.029 Uiso 1 1 calc R . . C8 C 0.0543(2) 0.8182(4) 0.5060(3) 0.0249(12) Uani 1 1 d . . . H8D H 0.0771 0.8736 0.5332 0.030 Uiso 1 1 calc R . . H8E H 0.0547 0.7769 0.5401 0.030 Uiso 1 1 calc R . . C11 C 0.1138(2) 0.6873(4) 0.5250(3) 0.0236(12) Uani 1 1 d . . . H11A H 0.1324 0.7051 0.5758 0.028 Uiso 1 1 calc R . . H11B H 0.1417 0.6731 0.5188 0.028 Uiso 1 1 calc R . . C9 C 0.1118(3) 0.7876(5) 0.4040(4) 0.0306(14) Uani 1 1 d . . . H9A H 0.1310 0.8317 0.3943 0.037 Uiso 1 1 calc R . . H9B H 0.1328 0.7284 0.4229 0.037 Uiso 1 1 calc R . . C7 C -0.0044(2) 0.8514(4) 0.4473(3) 0.0254(12) Uani 1 1 d . . . H7A H -0.0166 0.8895 0.4700 0.030 Uiso 1 1 calc R . . H7B H -0.0049 0.8924 0.4130 0.030 Uiso 1 1 calc R . . C5 C -0.1832(3) 0.9579(5) 0.3523(4) 0.0354(16) Uani 1 1 d . . . H5C H -0.1856 1.0242 0.3626 0.042 Uiso 1 1 calc R . . H5D H -0.1892 0.9171 0.3807 0.042 Uiso 1 1 calc R . . C6 C -0.2387(3) 0.8283(5) 0.1783(4) 0.0297(14) Uani 1 1 d . . . H6A H -0.2709 0.8682 0.1452 0.036 Uiso 1 1 calc R . . H6B H -0.2489 0.7622 0.1625 0.036 Uiso 1 1 calc R . . C2 C -0.2461(3) 0.7679(6) 0.2720(4) 0.0362(16) Uani 1 1 d . . . H2C H -0.2855 0.7642 0.2320 0.043 Uiso 1 1 calc R . . H2D H -0.2413 0.7879 0.3158 0.043 Uiso 1 1 calc R . . C4 C -0.2268(3) 0.9372(5) 0.2704(4) 0.0356(16) Uani 1 1 d . . . H4A H -0.2635 0.9453 0.2566 0.043 Uiso 1 1 calc R . . H4B H -0.2226 0.9820 0.2420 0.043 Uiso 1 1 calc R . . C3 C -0.1921(3) 0.8582(6) 0.1762(4) 0.0334(15) Uani 1 1 d . . . H3C H -0.2030 0.8471 0.1275 0.040 Uiso 1 1 calc R . . H3D H -0.1846 0.9260 0.1871 0.040 Uiso 1 1 calc R . . C1 C -0.2196(3) 0.6692(5) 0.2847(4) 0.0399(18) Uani 1 1 d . . . H1A H -0.2335 0.6247 0.3021 0.048 Uiso 1 1 calc R . . H1B H -0.2293 0.6448 0.2389 0.048 Uiso 1 1 calc R . . O23 O 0.2160(2) 0.4751(4) 0.5829(3) 0.0432(13) Uani 1 1 d . . . O24 O 0.1963(3) 0.6026(7) 0.3401(6) 0.098(3) Uani 1 1 d . . . O25 O 0.2485(6) 0.6543(12) 0.4797(9) 0.170(6) Uani 1 1 d . . . 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 Sb1 0.01552(16) 0.01928(17) 0.02031(17) -0.00127(14) 0.01187(14) -0.00093(13) Sb2 0.01999(17) 0.01591(16) 0.01964(17) 0.00132(13) 0.01144(15) 0.00353(13) Zn1 0.0194(3) 0.0214(3) 0.0208(3) 0.0028(3) 0.0115(3) 0.0020(2) V1 0.0170(4) 0.0131(4) 0.0160(4) -0.0011(3) 0.0122(4) -0.0016(3) V2 0.0145(4) 0.0142(4) 0.0156(4) -0.0007(3) 0.0099(4) -0.0013(3) V3 0.0182(4) 0.0118(4) 0.0157(4) 0.0009(3) 0.0102(4) 0.0002(3) V4 0.0194(4) 0.0131(4) 0.0175(4) 0.0002(3) 0.0111(4) -0.0016(3) V5 0.0164(4) 0.0146(4) 0.0175(4) 0.0007(3) 0.0119(4) -0.0016(3) V6 0.0158(4) 0.0146(4) 0.0149(4) -0.0006(3) 0.0096(4) -0.0004(3) V7 0.0162(4) 0.0163(4) 0.0181(4) -0.0003(3) 0.0125(4) 0.0003(3) V8 0.0173(4) 0.0113(4) 0.0177(4) 0.0000(3) 0.0122(4) -0.0012(3) O1 0.0199(18) 0.0204(19) 0.0188(18) -0.0020(15) 0.0128(16) -0.0009(15) O2 0.0208(19) 0.0201(19) 0.0210(19) 0.0018(15) 0.0150(17) 0.0032(15) O3 0.0180(18) 0.0169(18) 0.0203(19) 0.0019(15) 0.0123(16) -0.0018(14) O4 0.0210(19) 0.0139(18) 0.034(2) -0.0094(16) 0.0199(18) -0.0056(14) O5 0.0196(18) 0.026(2) 0.0140(18) 0.0001(15) 0.0082(16) -0.0057(16) O6 0.0197(19) 0.0212(19) 0.0180(19) -0.0023(15) 0.0103(17) -0.0004(15) O7 0.028(2) 0.030(2) 0.022(2) 0.0032(17) 0.0131(19) 0.0010(18) O8 0.0216(19) 0.0206(19) 0.0204(19) 0.0004(15) 0.0164(17) 0.0010(15) O9 0.038(2) 0.0175(19) 0.022(2) 0.0045(16) 0.017(2) 0.0021(17) O10 0.0193(19) 0.0185(19) 0.030(2) 0.0032(17) 0.0121(18) 0.0022(15) O11 0.0182(18) 0.0202(19) 0.0185(18) -0.0001(15) 0.0099(16) -0.0015(15) O12 0.0228(19) 0.0120(17) 0.027(2) 0.0016(15) 0.0194(18) 0.0023(14) O13 0.022(2) 0.021(2) 0.026(2) -0.0027(16) 0.0125(18) -0.0051(16) O14 0.031(2) 0.022(2) 0.023(2) -0.0031(16) 0.0209(19) -0.0047(16) O15 0.035(2) 0.020(2) 0.033(2) 0.0000(17) 0.025(2) -0.0038(17) O17 0.0170(18) 0.0162(18) 0.030(2) -0.0037(16) 0.0153(17) -0.0044(14) O16 0.022(2) 0.037(2) 0.029(2) -0.0020(19) 0.0179(19) 0.0017(17) O18 0.026(2) 0.0132(17) 0.025(2) 0.0063(15) 0.0198(18) 0.0069(14) O19 0.0230(19) 0.0154(18) 0.0149(18) -0.0018(14) 0.0081(16) 0.0018(15) O20 0.027(2) 0.028(2) 0.033(2) 0.0017(18) 0.021(2) -0.0050(17) O21 0.032(2) 0.019(2) 0.034(2) -0.0024(18) 0.021(2) -0.0061(17) O22 0.24(2) 0.123(14) 0.129(14) 0.000 0.140(17) 0.000 N6 0.020(2) 0.017(2) 0.023(2) 0.0016(18) 0.013(2) 0.0002(17) N4 0.017(2) 0.026(3) 0.025(3) 0.003(2) 0.011(2) 0.0015(18) N8 0.037(3) 0.023(3) 0.024(3) 0.000(2) 0.018(2) -0.003(2) N3 0.025(3) 0.042(3) 0.022(2) 0.005(2) 0.015(2) 0.002(2) N2 0.028(3) 0.024(3) 0.025(3) -0.002(2) 0.014(2) 0.003(2) N5 0.020(2) 0.026(3) 0.026(3) 0.004(2) 0.012(2) 0.0054(19) N1 0.048(3) 0.021(3) 0.040(3) 0.005(2) 0.032(3) -0.003(2) C10 0.029(3) 0.024(3) 0.029(3) -0.002(2) 0.018(3) -0.007(2) N7 0.046(3) 0.034(3) 0.035(3) -0.003(2) 0.029(3) -0.005(3) C12 0.029(3) 0.021(3) 0.023(3) 0.002(2) 0.017(3) -0.003(2) C8 0.027(3) 0.023(3) 0.023(3) 0.000(2) 0.015(3) 0.004(2) C11 0.019(3) 0.019(3) 0.025(3) 0.006(2) 0.009(2) 0.004(2) C9 0.029(3) 0.034(3) 0.030(3) 0.003(3) 0.019(3) 0.001(3) C7 0.026(3) 0.024(3) 0.026(3) 0.002(2) 0.016(3) -0.001(2) C5 0.032(3) 0.033(3) 0.046(4) -0.004(3) 0.026(3) 0.004(3) C6 0.020(3) 0.033(3) 0.026(3) 0.006(3) 0.009(3) 0.001(2) C2 0.025(3) 0.049(4) 0.041(4) -0.001(3) 0.023(3) -0.008(3) C4 0.026(3) 0.034(4) 0.044(4) 0.002(3) 0.020(3) 0.008(3) C3 0.024(3) 0.047(4) 0.019(3) 0.010(3) 0.008(3) -0.003(3) C1 0.048(4) 0.031(4) 0.038(4) -0.004(3) 0.026(4) -0.019(3) O23 0.050(3) 0.031(3) 0.031(3) -0.011(2) 0.016(2) -0.006(2) O24 0.068(5) 0.083(6) 0.131(8) 0.026(6) 0.056(6) -0.015(4) O25 0.153(12) 0.203(15) 0.152(13) -0.002(12) 0.094(11) -0.037(11) _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 Sb1 O18 1.952(4) . ? Sb1 O10 1.960(4) . ? Sb1 O19 1.966(4) . ? Sb2 O10 1.947(4) . ? Sb2 O4 1.948(4) . ? Sb2 O5 1.952(4) . ? Zn1 N3 2.065(6) . ? Zn1 N2 2.091(5) . ? Zn1 N5 2.097(5) . ? Zn1 N1 2.102(5) . ? Zn1 N4 2.270(5) . ? V1 O14 1.638(4) . ? V1 O17 1.922(4) . ? V1 O3 1.941(4) . ? V1 O11 1.957(4) . ? V1 O12 1.971(4) . ? V1 V7 2.9459(13) . ? V1 V6 2.9472(13) . ? V2 O13 1.624(4) . ? V2 O12 1.932(4) . ? V2 O2 1.940(4) . ? V2 O8 1.962(4) . ? V2 O18 2.007(4) . ? V2 V8 2.9927(13) . ? V2 V6 3.0417(13) . ? V3 O9 1.608(4) . ? V3 O17 1.910(4) . ? V3 O6 1.932(4) . ? V3 O1 1.978(4) . ? V3 O4 2.004(4) . ? V3 V4 2.9631(13) . ? V3 V6 3.0064(12) . ? V4 O21 1.636(4) . ? V4 O1 1.921(4) 2 ? V4 O6 1.925(4) . ? V4 O1 1.946(4) . ? V4 O5 2.020(4) 2 ? V4 V4 2.729(2) 2 ? V4 V5 3.1014(13) . ? V5 O20 1.607(4) . ? V5 O6 1.939(4) . ? V5 O11 1.959(4) . ? V5 O19 2.012(4) 2 ? V5 O5 2.022(4) 2 ? V5 V7 3.0705(13) . ? V6 O7 1.630(4) . ? V6 O17 1.920(4) . ? V6 O12 1.943(4) . ? V6 O4 1.963(4) . ? V6 O18 1.970(4) . ? V7 O16 1.641(4) . ? V7 O3 1.923(4) . ? V7 O11 1.927(4) . ? V7 O8 1.963(4) 2 ? V7 O19 2.017(4) 2 ? V7 V8 2.9292(13) 2 ? V8 O15 1.645(4) . ? V8 O3 1.920(4) 2 ? V8 O2 1.941(4) . ? V8 O2 1.941(4) 2 ? V8 O8 1.989(4) . ? V8 V7 2.9292(13) 2 ? V8 V8 2.9667(19) 2 ? O1 V4 1.921(4) 2 ? O2 V8 1.941(4) 2 ? O3 V8 1.920(4) 2 ? O5 V4 2.020(4) 2 ? O5 V5 2.022(4) 2 ? O8 V7 1.963(4) 2 ? O19 V5 2.012(4) 2 ? O19 V7 2.017(4) 2 ? N6 C11 1.462(7) . ? N6 C10 1.468(8) . ? N6 C8 1.478(8) . ? N4 C4 1.472(9) . ? N4 C2 1.475(8) . ? N4 C6 1.483(9) . ? N8 C12 1.483(8) . ? N3 C3 1.480(8) . ? N2 C5 1.491(8) . ? N5 C7 1.479(8) . ? N1 C1 1.473(10) . ? C10 C9 1.510(10) . ? N7 C9 1.499(9) . ? C12 C11 1.532(8) . ? C8 C7 1.513(8) . ? C5 C4 1.529(10) . ? C6 C3 1.520(9) . ? C2 C1 1.533(11) . ? 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 O18 Sb1 O10 96.35(17) . . ? O18 Sb1 O19 93.73(17) . . ? O10 Sb1 O19 97.19(17) . . ? O10 Sb2 O4 94.33(17) . . ? O10 Sb2 O5 98.22(17) . . ? O4 Sb2 O5 96.59(18) . . ? N3 Zn1 N2 118.7(2) . . ? N3 Zn1 N5 103.0(2) . . ? N2 Zn1 N5 98.9(2) . . ? N3 Zn1 N1 107.2(2) . . ? N2 Zn1 N1 125.9(2) . . ? N5 Zn1 N1 97.0(2) . . ? N3 Zn1 N4 81.1(2) . . ? N2 Zn1 N4 80.4(2) . . ? N5 Zn1 N4 175.6(2) . . ? N1 Zn1 N4 80.1(2) . . ? O14 V1 O17 104.6(2) . . ? O14 V1 O3 109.3(2) . . ? O17 V1 O3 146.04(19) . . ? O14 V1 O11 110.30(19) . . ? O17 V1 O11 90.10(16) . . ? O3 V1 O11 80.10(16) . . ? O14 V1 O12 104.71(19) . . ? O17 V1 O12 80.09(16) . . ? O3 V1 O12 89.48(16) . . ? O11 V1 O12 144.98(18) . . ? O14 V1 V7 112.61(16) . . ? O17 V1 V7 125.24(12) . . ? O3 V1 V7 40.09(11) . . ? O11 V1 V7 40.28(12) . . ? O12 V1 V7 124.18(12) . . ? O14 V1 V6 104.01(16) . . ? O17 V1 V6 39.88(11) . . ? O3 V1 V6 126.06(12) . . ? O11 V1 V6 125.46(13) . . ? O12 V1 V6 40.80(11) . . ? V7 V1 V6 143.38(4) . . ? O13 V2 O12 110.1(2) . . ? O13 V2 O2 106.6(2) . . ? O12 V2 O2 92.00(17) . . ? O13 V2 O8 108.1(2) . . ? O12 V2 O8 141.67(17) . . ? O2 V2 O8 80.64(17) . . ? O13 V2 O18 105.18(19) . . ? O12 V2 O18 78.02(16) . . ? O2 V2 O18 148.24(17) . . ? O8 V2 O18 88.70(17) . . ? O13 V2 V8 112.28(16) . . ? O12 V2 V8 122.48(12) . . ? O2 V2 V8 39.56(12) . . ? O8 V2 V8 41.09(11) . . ? O18 V2 V8 123.90(13) . . ? O13 V2 V6 111.42(16) . . ? O12 V2 V6 38.41(11) . . ? O2 V2 V6 125.16(13) . . ? O8 V2 V6 120.84(12) . . ? O18 V2 V6 39.65(12) . . ? V8 V2 V6 136.29(4) . . ? O9 V3 O17 108.1(2) . . ? O9 V3 O6 107.8(2) . . ? O17 V3 O6 93.28(17) . . ? O9 V3 O1 110.6(2) . . ? O17 V3 O1 140.85(18) . . ? O6 V3 O1 79.94(17) . . ? O9 V3 O4 107.9(2) . . ? O17 V3 O4 78.36(16) . . ? O6 V3 O4 144.19(19) . . ? O1 V3 O4 85.00(17) . . ? O9 V3 V4 111.37(16) . . ? O17 V3 V4 125.60(13) . . ? O6 V3 V4 39.73(12) . . ? O1 V3 V4 40.55(11) . . ? O4 V3 V4 120.93(13) . . ? O9 V3 V6 110.06(16) . . ? O17 V3 V6 38.41(12) . . ? O6 V3 V6 125.74(12) . . ? O1 V3 V6 119.26(12) . . ? O4 V3 V6 40.21(11) . . ? V4 V3 V6 138.49(4) . . ? O21 V4 O1 107.3(2) . 2 ? O21 V4 O6 116.8(2) . . ? O1 V4 O6 135.91(18) 2 . ? O21 V4 O1 104.4(2) . . ? O1 V4 O1 89.37(17) 2 . ? O6 V4 O1 80.90(17) . . ? O21 V4 O5 109.4(2) . 2 ? O1 V4 O5 88.47(17) 2 2 ? O6 V4 O5 76.69(16) . 2 ? O1 V4 O5 145.11(17) . 2 ? O21 V4 V4 105.70(17) . 2 ? O1 V4 V4 45.48(12) 2 2 ? O6 V4 V4 117.93(13) . 2 ? O1 V4 V4 44.74(12) . 2 ? O5 V4 V4 128.80(13) 2 2 ? O21 V4 V3 113.44(17) . . ? O1 V4 V3 121.32(12) 2 . ? O6 V4 V3 39.88(12) . . ? O1 V4 V3 41.36(12) . . ? O5 V4 V3 114.06(12) 2 . ? V4 V4 V3 83.17(4) 2 . ? O21 V4 V5 119.73(17) . . ? O1 V4 V5 117.46(12) 2 . ? O6 V4 V5 36.79(12) . . ? O1 V4 V5 113.78(12) . . ? O5 V4 V5 39.90(11) 2 . ? V4 V4 V5 134.33(2) 2 . ? V3 V4 V5 75.31(3) . . ? O20 V5 O6 108.7(2) . . ? O20 V5 O11 109.4(2) . . ? O6 V5 O11 91.39(17) . . ? O20 V5 O19 108.3(2) . 2 ? O6 V5 O19 142.97(18) . 2 ? O11 V5 O19 77.68(16) . 2 ? O20 V5 O5 106.2(2) . 2 ? O6 V5 O5 76.34(16) . 2 ? O11 V5 O5 144.40(18) . 2 ? O19 V5 O5 92.14(16) 2 2 ? O20 V5 V7 111.85(17) . . ? O6 V5 V7 122.56(12) . . ? O11 V5 V7 37.42(12) . . ? O19 V5 V7 40.41(11) 2 . ? O5 V5 V7 125.97(13) 2 . ? O20 V5 V4 112.11(17) . . ? O6 V5 V4 36.48(12) . . ? O11 V5 V4 121.13(12) . . ? O19 V5 V4 123.58(13) 2 . ? O5 V5 V4 39.86(11) 2 . ? V7 V5 V4 135.95(4) . . ? O7 V6 O17 112.0(2) . . ? O7 V6 O12 111.0(2) . . ? O17 V6 O12 80.84(16) . . ? O7 V6 O4 108.4(2) . . ? O17 V6 O4 79.15(17) . . ? O12 V6 O4 140.17(18) . . ? O7 V6 O18 109.6(2) . . ? O17 V6 O18 137.95(18) . . ? O12 V6 O18 78.65(16) . . ? O4 V6 O18 93.96(17) . . ? O7 V6 V1 113.34(17) . . ? O17 V6 V1 39.92(12) . . ? O12 V6 V1 41.51(11) . . ? O4 V6 V1 114.91(12) . . ? O18 V6 V1 114.98(11) . . ? O7 V6 V3 113.15(17) . . ? O17 V6 V3 38.17(12) . . ? O12 V6 V3 114.12(12) . . ? O4 V6 V3 41.24(12) . . ? O18 V6 V3 125.46(13) . . ? V1 V6 V3 76.61(3) . . ? O7 V6 V2 115.07(17) . . ? O17 V6 V2 112.20(13) . . ? O12 V6 V2 38.15(12) . . ? O4 V6 V2 124.71(14) . . ? O18 V6 V2 40.55(11) . . ? V1 V6 V2 77.19(3) . . ? V3 V6 V2 131.02(4) . . ? O16 V7 O3 108.4(2) . . ? O16 V7 O11 113.2(2) . . ? O3 V7 O11 81.32(16) . . ? O16 V7 O8 109.4(2) . 2 ? O3 V7 O8 82.31(17) . 2 ? O11 V7 O8 137.28(18) . 2 ? O16 V7 O19 108.9(2) . 2 ? O3 V7 O19 142.07(18) . 2 ? O11 V7 O19 78.29(16) . 2 ? O8 V7 O19 91.43(16) 2 2 ? O16 V7 V8 110.51(17) . 2 ? O3 V7 V8 40.30(12) . 2 ? O11 V7 V8 115.32(12) . 2 ? O8 V7 V8 42.50(11) 2 2 ? O19 V7 V8 127.03(13) 2 2 ? O16 V7 V1 114.22(16) . . ? O3 V7 V1 40.54(12) . . ? O11 V7 V1 41.06(11) . . ? O8 V7 V1 115.65(12) 2 . ? O19 V7 V1 114.99(12) 2 . ? V8 V7 V1 78.32(3) 2 . ? O16 V7 V5 114.96(17) . . ? O3 V7 V5 114.94(12) . . ? O11 V7 V5 38.16(12) . . ? O8 V7 V5 122.06(12) 2 . ? O19 V7 V5 40.28(11) 2 . ? V8 V7 V5 134.03(4) 2 . ? V1 V7 V5 77.46(3) . . ? O15 V8 O3 113.9(2) . 2 ? O15 V8 O2 107.6(2) . . ? O3 V8 O2 138.35(17) 2 . ? O15 V8 O2 105.0(2) . 2 ? O3 V8 O2 91.95(17) 2 2 ? O2 V8 O2 80.16(18) . 2 ? O15 V8 O8 112.2(2) . . ? O3 V8 O8 81.70(16) 2 . ? O2 V8 O8 79.95(16) . . ? O2 V8 O8 141.58(17) 2 . ? O15 V8 V7 116.26(16) . 2 ? O3 V8 V7 40.37(11) 2 2 ? O2 V8 V7 115.94(12) . 2 ? O2 V8 V7 125.72(12) 2 2 ? O8 V8 V7 41.82(12) . 2 ? O15 V8 V8 108.71(16) . 2 ? O3 V8 V8 122.87(12) 2 2 ? O2 V8 V8 40.17(12) . 2 ? O2 V8 V8 40.16(12) 2 2 ? O8 V8 V8 115.11(12) . 2 ? V7 V8 V8 134.70(3) 2 2 ? O15 V8 V2 115.67(17) . . ? O3 V8 V2 113.95(12) 2 . ? O2 V8 V2 39.53(11) . . ? O2 V8 V2 113.59(13) 2 . ? O8 V8 V2 40.43(12) . . ? V7 V8 V2 79.07(3) 2 . ? V8 V8 V2 76.98(4) 2 . ? V4 O1 V4 89.78(17) 2 . ? V4 O1 V3 151.9(2) 2 . ? V4 O1 V3 98.08(18) . . ? V2 O2 V8 100.91(18) . . ? V2 O2 V8 145.8(2) . 2 ? V8 O2 V8 99.67(18) . 2 ? V8 O3 V7 99.33(18) 2 . ? V8 O3 V1 147.9(2) 2 . ? V7 O3 V1 99.37(17) . . ? Sb2 O4 V6 139.6(2) . . ? Sb2 O4 V3 121.86(19) . . ? V6 O4 V3 98.56(17) . . ? Sb2 O5 V4 117.3(2) . 2 ? Sb2 O5 V5 141.0(2) . 2 ? V4 O5 V5 100.24(17) 2 2 ? V4 O6 V3 100.39(19) . . ? V4 O6 V5 106.73(19) . . ? V3 O6 V5 146.5(2) . . ? V2 O8 V7 147.7(2) . 2 ? V2 O8 V8 98.48(17) . . ? V7 O8 V8 95.69(17) 2 . ? Sb2 O10 Sb1 131.2(2) . . ? V7 O11 V1 98.66(18) . . ? V7 O11 V5 104.41(18) . . ? V1 O11 V5 148.1(2) . . ? V2 O12 V6 103.44(18) . . ? V2 O12 V1 146.4(2) . . ? V6 O12 V1 97.69(17) . . ? V3 O17 V6 103.42(19) . . ? V3 O17 V1 148.8(2) . . ? V6 O17 V1 100.20(18) . . ? Sb1 O18 V6 136.7(2) . . ? Sb1 O18 V2 123.4(2) . . ? V6 O18 V2 99.80(18) . . ? Sb1 O19 V5 141.9(2) . 2 ? Sb1 O19 V7 118.64(19) . 2 ? V5 O19 V7 99.31(17) 2 2 ? C11 N6 C10 112.2(5) . . ? C11 N6 C8 111.1(5) . . ? C10 N6 C8 111.7(5) . . ? C4 N4 C2 112.0(6) . . ? C4 N4 C6 112.2(5) . . ? C2 N4 C6 112.9(5) . . ? C4 N4 Zn1 106.9(4) . . ? C2 N4 Zn1 106.1(4) . . ? C6 N4 Zn1 106.3(4) . . ? C3 N3 Zn1 109.0(4) . . ? C5 N2 Zn1 109.5(4) . . ? C7 N5 Zn1 118.1(4) . . ? C1 N1 Zn1 112.6(4) . . ? N6 C10 C9 111.4(5) . . ? N8 C12 C11 111.0(5) . . ? N6 C8 C7 113.2(5) . . ? N6 C11 C12 107.9(5) . . ? N7 C9 C10 109.4(5) . . ? N5 C7 C8 113.6(5) . . ? N2 C5 C4 108.2(6) . . ? N4 C6 C3 109.5(5) . . ? N4 C2 C1 109.9(6) . . ? N4 C4 C5 109.8(5) . . ? N3 C3 C6 109.5(5) . . ? N1 C1 C2 109.8(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8A O14 0.89 1.92 2.774(7) 161.3 . N8 H8C O23 0.89 2.17 3.044(9) 167.8 . N1 H1C O16 0.90 2.64 3.471(7) 154.6 . N7 H7C O15 0.89 2.11 2.977(8) 165.4 . N8 H8B O16 0.89 1.96 2.817(7) 162.5 5_566 N2 H2A O9 0.90 2.05 2.906(7) 158.1 5_566 N5 H5A O14 0.90 2.15 3.039(7) 170.6 5_566 N1 H1D O7 0.90 2.09 2.878(8) 145.1 5_566 N3 H3A O21 0.90 1.95 2.817(7) 162.0 1_565 N2 H2B O20 0.90 2.28 3.087(7) 149.5 1_565 N7 H7D O21 0.89 2.44 3.235(8) 148.1 1_565 N3 H3B O24 0.90 2.30 3.137(11) 154.2 2 N5 H5B O15 0.90 2.38 3.221(7) 156.0 2 N7 H7E O15 0.89 2.29 3.012(8) 137.9 2 N7 H7D O21 0.89 2.54 2.991(8) 111.9 2_565 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.831 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.170 # start Validation Reply Form _vrf_PLAT306_ea669r ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O22 RESPONSE: The O-H H atoms of the water molecule could not be located. ; # end Validation Reply Form