# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2303 data_global _publ_requested_journal 'J. Chem. Soc., Dalton, Trans.' _publ_contact_author_name ; Tomoji OZEKI ; _publ_contact_author_address ; Department of Chemistry and Materials Science Tokyo Institute of Technology 2-12-1 O-okayama, Meguro-ku Tokyo 152-8551 Japan ; _publ_contact_author_email ; tozeki@cms.titech.ac.jp ; _publ_contact_author_fax ; +81-3-5734-2442 ; _publ_section_title ; Hydrogen-bonded aggregates of protonated decavanadate anions in their tetraalkylammonium salts ; loop_ _publ_author_name _publ_author_address 'Setsuko NAKAMURA' ; Department of Chemistry and Materials Science Tokyo Institute of Technology 2-12-1 O-okayama, Meguro-ku Tokyo 152-8551 Japan ; 'Tomoji OZEKI' ; Department of Chemistry and Materials Science Tokyo Institute of Technology 2-12-1 O-okayama, Meguro-ku Tokyo 152-8551 Japan ; _publ_section_references ; Burnett, M. N. & Johnson, C. K. (1996) ORTEP-III. Report ORNL-6895. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. de Meulenaar, J. & Tompa, H. (1965) Acta Crystallogr. Sect. A 19, 1014-1018. Flack, H. D. (1983) Acta Crystallogr. Sect A 39, 876-881. Molecular Structure Corporation (1995) MSC/AFC Diffractometer control Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Molecular Structure Corporation (1993) teXsan. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Crsytallogr. Sect. A 24, 351-359. Sheldrick, G. M. (1990) Acta Crystallogr. Sect A 46, 467-473. Sheldrick, G. M. (1997a) SHELX-97. Programs for Crystal Structure Analysis. University of G\"ottingen, Germany. Sheldrick, G. M. (1997b) SADABS. Program for Scaling and Correction of Area-Detector Data. University of G\"ottingen, Germany. Siemens (1995) SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _publ_section_exptl_refinement ; Hydrogen atoms in the R~4~N^+^ cations were included using the riding model. For TMAh, TPAv, TBAh and TBAc, all the non-hydrogen atoms were refined with anisotropic displacement parameters. In the refinement of TPAc, V, O and N atoms were treated with anisotropic displacement parameters. In these five structures, H atoms attached to surface O atoms of decavanadate frameworks were found from difference Fourier syntheses and their positional and isotropic displacement parameters were refined. For the other two structures, protons on the decavanadate anions could not be located; protonation sites were therefore deduced from the bond valence sum calculations. For structure of TEAh, V and O atoms constituting the decavanadate framework were refined with anisotropic displacement parameters. For TPAh, only V atoms were refined anisotropically. ; data_TMAh _audit_creation_method SHELXL-97 _chemical_name_common ; Tetrakis(tetramethylammonium) dihydrogendecavanadate tetrahydrate ; _chemical_melting_point ? _chemical_formula_moiety ; (C4 H12 N +)4, (H2 V10 O28 4-), 3.8(H2 O) ; _chemical_formula_sum 'C16 H57.60 N4 O31.80 V10' _chemical_formula_weight 1324.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.645(3) _cell_length_b 15.695(4) _cell_length_c 12.627(3) _cell_angle_alpha 96.71(2) _cell_angle_beta 101.24(2) _cell_angle_gamma 68.140(18) _cell_volume 2278.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 14.29 _cell_measurement_theta_max 15.00 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 2.048 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'UltraX18 Rigaku Denki rotating Mo anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -5.284 _diffrn_reflns_number 10961 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.55 _reflns_number_total 10486 _reflns_number_gt 7011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control Software' _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_reduction 'teXsan PROCESS (Molecular Structure Corporation, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997a)' _refine_special_details ; H atoms attached to surface O atoms of decavanadate frameworks, H1 and H2, were found from difference Fourier syntheses and their positional and isotropic displacement parameters were refined. H atoms in the [(CH~3~)~4~N]^+^ cations were included in ideal positions and refined with the riding model. H atoms of water molecules were not included in refinement. ; _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^)+(0.0673P)^2^+4.4470P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10486 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1478 _refine_ls_wR_factor_gt 0.1288 _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 V2A V 0.49088(6) 0.34137(5) 0.48160(6) 0.02869(17) Uani 1 1 d . . . V1A V 0.63244(6) 0.34981(5) 0.31643(5) 0.02419(16) Uani 1 1 d . . . V2B' V 0.79765(7) 0.34792(6) 0.16458(6) 0.03312(18) Uani 1 1 d . . . V2A' V 0.98231(6) 0.16790(6) 0.25159(6) 0.03530(19) Uani 1 1 d . . . V1A' V 0.83488(6) 0.16362(5) 0.41718(6) 0.02656(16) Uani 1 1 d . . . V2B V 0.67549(7) 0.16544(5) 0.57446(6) 0.03142(18) Uani 1 1 d . . . V3B' V 0.57999(6) 0.17198(5) 0.32923(6) 0.03092(18) Uani 1 1 d . . . V3A' V 0.73180(6) 0.17552(5) 0.16780(6) 0.03218(18) Uani 1 1 d . . . V3A V 0.75386(6) 0.33135(5) 0.57945(6) 0.02614(16) Uani 1 1 d . . . V3B V 0.90262(6) 0.33780(5) 0.40953(6) 0.02884(17) Uani 1 1 d . . . OG1 O 0.3688(3) 0.4125(2) 0.5101(3) 0.0378(7) Uani 1 1 d . . . OG2' O 0.7803(3) 0.4161(3) 0.0726(3) 0.0473(9) Uani 1 1 d . . . OG1' O 1.1066(3) 0.1013(3) 0.2272(3) 0.0482(9) Uani 1 1 d . . . OG2 O 0.6900(3) 0.0982(2) 0.6669(3) 0.0432(8) Uani 1 1 d . . . OF2' O 0.5186(3) 0.1141(2) 0.2436(3) 0.0438(8) Uani 1 1 d . . . OF1' O 0.6726(3) 0.1162(2) 0.0813(3) 0.0445(8) Uani 1 1 d . . . OF1 O 0.8091(3) 0.3931(2) 0.6652(3) 0.0380(7) Uani 1 1 d . . . OF2 O 0.9601(3) 0.3990(2) 0.4945(3) 0.0391(8) Uani 1 1 d . . . OE1 O 0.5082(2) 0.41386(19) 0.3655(2) 0.0284(6) Uani 1 1 d . . . OE2' O 0.6430(2) 0.4115(2) 0.2217(2) 0.0309(7) Uani 1 1 d . . . OD1' O 0.9389(3) 0.2587(2) 0.1568(3) 0.0387(8) Uani 1 1 d . . . OE1' O 0.9618(2) 0.1064(2) 0.3760(2) 0.0332(7) Uani 1 1 d . . . OE2 O 0.8250(3) 0.1075(2) 0.5191(2) 0.0317(7) Uani 1 1 d . . . OD1 O 0.5365(3) 0.2558(2) 0.5848(2) 0.0331(7) Uani 1 1 d . . . OC2 O 0.7525(3) 0.2458(2) 0.6544(2) 0.0314(7) Uani 1 1 d . . . OC1 O 0.5916(3) 0.4019(3) 0.5768(3) 0.0310(7) Uani 1 1 d . . . OC4 O 0.8574(3) 0.4038(2) 0.2880(2) 0.0331(7) Uani 1 1 d . . . OC3 O 1.0211(2) 0.2475(2) 0.3653(2) 0.0340(7) Uani 1 1 d . . . OC2' O 0.7241(3) 0.2684(2) 0.0920(2) 0.0358(7) Uani 1 1 d . . . OC1' O 0.8847(3) 0.1134(2) 0.1689(2) 0.0364(7) Uani 1 1 d . . . OC4' O 0.6127(3) 0.1127(2) 0.4523(3) 0.0332(7) Uani 1 1 d . . . OC3' O 0.4527(2) 0.2669(2) 0.3753(3) 0.0320(7) Uani 1 1 d . . . OB2 O 0.8796(2) 0.25771(19) 0.5083(2) 0.0266(6) Uani 1 1 d . . . OB1 O 0.7327(3) 0.4019(2) 0.4388(2) 0.0262(6) Uani 1 1 d . . . OB2' O 0.5888(2) 0.2618(2) 0.2320(2) 0.0292(6) Uani 1 1 d . . . OB1' O 0.7393(2) 0.1190(2) 0.3055(2) 0.0303(6) Uani 1 1 d . . . OA1 O 0.6663(2) 0.26270(19) 0.4429(2) 0.0262(6) Uani 1 1 d . . . OA1' O 0.7985(2) 0.26112(19) 0.3040(2) 0.0266(6) Uani 1 1 d . . . N1 N 0.8222(4) 0.6252(3) 0.8047(4) 0.0477(11) Uani 1 1 d . . . C1 C 0.8398(5) 0.6045(5) 0.6905(5) 0.0625(17) Uani 1 1 d . . . H1A H 0.7680 0.6329 0.6437 0.094 Uiso 1 1 calc R . . H1B H 0.8666 0.5392 0.6757 0.094 Uiso 1 1 calc R . . H1C H 0.8961 0.6280 0.6780 0.094 Uiso 1 1 calc R . . C2 C 0.7338(6) 0.5891(5) 0.8232(5) 0.0646(17) Uani 1 1 d . . . H2A H 0.6623 0.6179 0.7764 0.097 Uiso 1 1 calc R . . H2B H 0.7221 0.6023 0.8971 0.097 Uiso 1 1 calc R . . H2C H 0.7602 0.5238 0.8082 0.097 Uiso 1 1 calc R . . C3 C 0.7813(7) 0.7266(5) 0.8273(7) 0.086(2) Uani 1 1 d . . . H3A H 0.7094 0.7552 0.7808 0.129 Uiso 1 1 calc R . . H3B H 0.8378 0.7497 0.8144 0.129 Uiso 1 1 calc R . . H3C H 0.7702 0.7402 0.9014 0.129 Uiso 1 1 calc R . . C4 C 0.9322(6) 0.5817(6) 0.8758(6) 0.089(3) Uani 1 1 d . . . H4A H 0.9211 0.5951 0.9499 0.133 Uiso 1 1 calc R . . H4B H 0.9883 0.6053 0.8631 0.133 Uiso 1 1 calc R . . H4C H 0.9590 0.5164 0.8610 0.133 Uiso 1 1 calc R . . N2 N 0.7059(3) 0.8624(3) 0.4555(3) 0.0370(9) Uani 1 1 d . . . C5 C 0.7461(5) 0.7606(3) 0.4443(5) 0.0576(16) Uani 1 1 d . . . H5A H 0.8153 0.7350 0.4953 0.086 Uiso 1 1 calc R . . H5B H 0.7616 0.7406 0.3723 0.086 Uiso 1 1 calc R . . H5C H 0.6872 0.7405 0.4582 0.086 Uiso 1 1 calc R . . C6 C 0.5994(5) 0.9018(4) 0.3769(6) 0.0639(18) Uani 1 1 d . . . H6A H 0.6150 0.8816 0.3050 0.096 Uiso 1 1 calc R . . H6B H 0.5734 0.9677 0.3839 0.096 Uiso 1 1 calc R . . H6C H 0.5406 0.8817 0.3909 0.096 Uiso 1 1 calc R . . C7 C 0.6812(6) 0.8941(5) 0.5663(5) 0.0662(17) Uani 1 1 d . . . H7A H 0.7501 0.8686 0.6177 0.099 Uiso 1 1 calc R . . H7B H 0.6221 0.8742 0.5800 0.099 Uiso 1 1 calc R . . H7C H 0.6553 0.9600 0.5731 0.099 Uiso 1 1 calc R . . C8 C 0.7976(5) 0.8943(4) 0.4368(5) 0.0530(14) Uani 1 1 d . . . H8A H 0.8663 0.8681 0.4883 0.079 Uiso 1 1 calc R . . H8B H 0.7715 0.9601 0.4452 0.079 Uiso 1 1 calc R . . H8C H 0.8142 0.8752 0.3649 0.079 Uiso 1 1 calc R . . N3 N 0.5053(3) 0.6570(3) 0.1345(3) 0.0405(10) Uani 1 1 d . . . C9 C 0.6087(5) 0.6311(4) 0.2221(4) 0.0500(13) Uani 1 1 d . . . H9A H 0.5848 0.6538 0.2908 0.075 Uiso 1 1 calc R . . H9B H 0.6625 0.6573 0.2098 0.075 Uiso 1 1 calc R . . H9C H 0.6450 0.5653 0.2217 0.075 Uiso 1 1 calc R . . C10 C 0.5427(5) 0.6214(5) 0.0277(4) 0.0611(17) Uani 1 1 d . . . H10A H 0.5790 0.5557 0.0276 0.092 Uiso 1 1 calc R . . H10B H 0.5965 0.6476 0.0155 0.092 Uiso 1 1 calc R . . H10C H 0.4766 0.6379 -0.0286 0.092 Uiso 1 1 calc R . . C11 C 0.4485(6) 0.7594(4) 0.1355(5) 0.0636(17) Uani 1 1 d . . . H11A H 0.4246 0.7819 0.2043 0.095 Uiso 1 1 calc R . . H11B H 0.3823 0.7762 0.0793 0.095 Uiso 1 1 calc R . . H11C H 0.5022 0.7859 0.1236 0.095 Uiso 1 1 calc R . . C12 C 0.4228(5) 0.6150(5) 0.1541(5) 0.0647(17) Uani 1 1 d . . . H12A H 0.3987 0.6379 0.2227 0.097 Uiso 1 1 calc R . . H12B H 0.4602 0.5494 0.1543 0.097 Uiso 1 1 calc R . . H12C H 0.3566 0.6307 0.0978 0.097 Uiso 1 1 calc R . . N4 N 0.9857(4) 0.1400(3) 0.8710(3) 0.0433(10) Uani 1 1 d . . . C13 C 0.9379(6) 0.2416(4) 0.8848(5) 0.0616(16) Uani 1 1 d . . . H13A H 0.9947 0.2661 0.8765 0.092 Uiso 1 1 calc R . . H13B H 0.9174 0.2590 0.9557 0.092 Uiso 1 1 calc R . . H13C H 0.8704 0.2656 0.8313 0.092 Uiso 1 1 calc R . . C14 C 1.0174(5) 0.1107(4) 0.7611(5) 0.0592(16) Uani 1 1 d . . . H14A H 1.0483 0.0448 0.7540 0.089 Uiso 1 1 calc R . . H14B H 1.0744 0.1346 0.7514 0.089 Uiso 1 1 calc R . . H14C H 0.9500 0.1338 0.7074 0.089 Uiso 1 1 calc R . . C15 C 0.8975(6) 0.1028(5) 0.8840(6) 0.0720(19) Uani 1 1 d . . . H15A H 0.9281 0.0369 0.8751 0.108 Uiso 1 1 calc R . . H15B H 0.8300 0.1269 0.8305 0.108 Uiso 1 1 calc R . . H15C H 0.8771 0.1203 0.9548 0.108 Uiso 1 1 calc R . . C16 C 1.0891(5) 0.1014(5) 0.9542(5) 0.0663(18) Uani 1 1 d . . . H16A H 1.1192 0.0356 0.9442 0.100 Uiso 1 1 calc R . . H16B H 1.0679 0.1181 1.0248 0.100 Uiso 1 1 calc R . . H16C H 1.1469 0.1254 0.9475 0.100 Uiso 1 1 calc R . . H1 H 0.572(4) 0.440(3) 0.591(4) 0.017(15) Uiso 1 1 d . . . H2 H 0.706(4) 0.451(3) 0.444(4) 0.030(14) Uiso 1 1 d . . . OW1 O 0.6496(11) 0.9970(9) -0.1363(10) 0.252(6) Uani 1 1 d . . . OW2A O 0.7830(12) 0.7247(10) 0.1133(8) 0.209(7) Uani 0.800(7) 1 d P A 1 OW4A O 0.6394(17) 0.9358(11) 0.1212(16) 0.324(12) Uani 0.800(7) 1 d P A 1 OW3A O 0.8798(4) 0.5723(3) 0.3236(5) 0.087(2) Uani 0.800(7) 1 d P A 1 OW4B O 0.587(2) 0.851(3) -0.0081(17) 0.131(16) Uani 0.200(7) 1 d P A 2 OW3B O 0.9458(13) 0.6581(14) 0.2342(16) 0.058(7) Uani 0.200(7) 1 d P A 2 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 V2A 0.0255(4) 0.0255(4) 0.0362(4) -0.0026(3) 0.0096(3) -0.0094(3) V1A 0.0216(3) 0.0249(4) 0.0245(3) -0.0011(3) 0.0027(3) -0.0077(3) V2B' 0.0311(4) 0.0411(5) 0.0265(4) 0.0014(3) 0.0068(3) -0.0113(3) V2A' 0.0262(4) 0.0421(5) 0.0315(4) -0.0053(3) 0.0079(3) -0.0059(3) V1A' 0.0245(3) 0.0251(4) 0.0259(4) -0.0029(3) 0.0018(3) -0.0065(3) V2B 0.0361(4) 0.0262(4) 0.0333(4) 0.0017(3) 0.0067(3) -0.0120(3) V3B' 0.0298(4) 0.0290(4) 0.0348(4) -0.0051(3) 0.0032(3) -0.0145(3) V3A' 0.0315(4) 0.0363(4) 0.0245(4) -0.0081(3) 0.0025(3) -0.0111(3) V3A 0.0285(4) 0.0256(4) 0.0234(3) -0.0032(3) 0.0039(3) -0.0101(3) V3B 0.0238(3) 0.0353(4) 0.0284(4) -0.0043(3) 0.0044(3) -0.0133(3) OG1 0.0300(16) 0.0338(17) 0.050(2) -0.0020(15) 0.0129(14) -0.0095(14) OG2' 0.049(2) 0.058(2) 0.0355(18) 0.0071(16) 0.0100(16) -0.0173(18) OG1' 0.0341(18) 0.056(2) 0.045(2) -0.0089(17) 0.0120(15) -0.0059(16) OG2 0.056(2) 0.0343(18) 0.0424(19) 0.0068(15) 0.0115(16) -0.0170(16) OF2' 0.045(2) 0.042(2) 0.047(2) -0.0115(16) 0.0019(16) -0.0259(16) OF1' 0.046(2) 0.047(2) 0.0361(18) -0.0099(15) -0.0004(15) -0.0186(17) OF1 0.0444(19) 0.0359(18) 0.0347(17) -0.0087(14) 0.0069(14) -0.0183(15) OF2 0.0362(17) 0.046(2) 0.0398(18) -0.0066(15) 0.0061(14) -0.0227(16) OE1 0.0238(14) 0.0247(15) 0.0346(16) -0.0011(12) 0.0043(12) -0.0075(12) OE2' 0.0312(15) 0.0309(16) 0.0292(15) 0.0003(12) 0.0060(12) -0.0093(13) OD1' 0.0309(16) 0.053(2) 0.0328(17) -0.0026(15) 0.0112(13) -0.0135(15) OE1' 0.0274(15) 0.0294(16) 0.0350(17) -0.0025(13) 0.0021(13) -0.0041(13) OE2 0.0327(16) 0.0268(16) 0.0319(16) 0.0003(12) 0.0033(13) -0.0079(13) OD1 0.0373(17) 0.0289(16) 0.0367(17) -0.0001(13) 0.0130(14) -0.0129(13) OC2 0.0376(17) 0.0310(16) 0.0248(15) -0.0015(12) 0.0054(13) -0.0121(13) OC1 0.0320(17) 0.0238(18) 0.0356(18) -0.0063(15) 0.0093(14) -0.0085(15) OC4 0.0302(16) 0.0381(18) 0.0338(17) -0.0013(14) 0.0068(13) -0.0155(14) OC3 0.0242(15) 0.0420(18) 0.0342(17) -0.0051(14) 0.0061(12) -0.0115(13) OC2' 0.0348(16) 0.0423(19) 0.0252(15) -0.0012(13) 0.0011(13) -0.0108(14) OC1' 0.0333(16) 0.0398(18) 0.0294(16) -0.0099(14) 0.0064(13) -0.0081(14) OC4' 0.0354(16) 0.0264(15) 0.0389(17) -0.0016(13) 0.0047(13) -0.0138(13) OC3' 0.0248(15) 0.0296(16) 0.0411(18) -0.0027(13) 0.0040(13) -0.0111(13) OB2 0.0250(14) 0.0270(15) 0.0246(14) -0.0025(11) 0.0006(11) -0.0084(12) OB1 0.0252(15) 0.0211(16) 0.0310(16) -0.0036(12) 0.0049(12) -0.0082(13) OB2' 0.0262(14) 0.0290(15) 0.0283(15) -0.0040(12) -0.0015(12) -0.0097(12) OB1' 0.0289(15) 0.0262(15) 0.0309(16) -0.0037(12) 0.0010(12) -0.0077(12) OA1 0.0253(14) 0.0260(15) 0.0265(15) -0.0014(12) 0.0041(11) -0.0091(12) OA1' 0.0257(14) 0.0280(15) 0.0237(14) -0.0036(12) 0.0030(11) -0.0089(12) N1 0.037(2) 0.061(3) 0.049(3) 0.004(2) 0.0032(19) -0.024(2) C1 0.056(4) 0.080(5) 0.058(4) 0.015(3) 0.016(3) -0.026(3) C2 0.064(4) 0.082(5) 0.063(4) 0.000(3) 0.022(3) -0.039(4) C3 0.089(5) 0.069(5) 0.104(6) -0.006(4) 0.006(5) -0.041(4) C4 0.055(4) 0.130(7) 0.074(5) 0.043(5) -0.013(4) -0.025(4) N2 0.0277(19) 0.031(2) 0.053(2) 0.0001(18) 0.0046(17) -0.0119(16) C5 0.051(3) 0.029(3) 0.087(5) -0.002(3) 0.000(3) -0.015(2) C6 0.038(3) 0.048(3) 0.099(5) 0.020(3) -0.016(3) -0.017(3) C7 0.066(4) 0.075(4) 0.067(4) -0.017(3) 0.028(3) -0.034(4) C8 0.044(3) 0.051(3) 0.073(4) 0.005(3) 0.018(3) -0.023(3) N3 0.039(2) 0.048(3) 0.028(2) -0.0027(17) 0.0046(16) -0.0094(19) C9 0.050(3) 0.055(3) 0.038(3) 0.003(2) -0.006(2) -0.017(3) C10 0.052(3) 0.083(5) 0.035(3) -0.011(3) 0.016(2) -0.009(3) C11 0.078(4) 0.046(3) 0.048(3) 0.004(3) 0.008(3) -0.002(3) C12 0.052(4) 0.085(5) 0.062(4) 0.000(3) 0.005(3) -0.034(3) N4 0.044(2) 0.049(3) 0.032(2) -0.0042(18) 0.0097(18) -0.010(2) C13 0.078(4) 0.050(3) 0.048(3) -0.005(3) 0.016(3) -0.012(3) C14 0.062(4) 0.064(4) 0.044(3) -0.004(3) 0.019(3) -0.011(3) C15 0.067(4) 0.094(5) 0.067(4) -0.008(4) 0.023(3) -0.040(4) C16 0.057(4) 0.081(5) 0.043(3) 0.001(3) -0.001(3) -0.009(3) OW1 0.258(14) 0.309(15) 0.223(12) -0.030(11) 0.047(10) -0.149(13) OW2A 0.307(16) 0.330(17) 0.134(9) -0.022(10) 0.089(9) -0.262(15) OW4A 0.46(3) 0.245(16) 0.43(3) -0.192(17) 0.35(2) -0.230(18) OW3A 0.053(3) 0.036(3) 0.128(5) -0.027(3) -0.039(3) -0.003(2) OW4B 0.089(18) 0.33(5) 0.040(12) -0.065(19) 0.034(12) -0.15(3) OW3B 0.023(8) 0.084(14) 0.084(14) 0.073(12) -0.027(8) -0.037(9) _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 V2A OG1 1.612(3) . ? V2A OC3' 1.789(3) . ? V2A OD1 1.836(3) . ? V2A OC1 2.002(4) . ? V2A OE1 2.047(3) . ? V2A OA1 2.219(3) . ? V2A V1A 3.0442(12) . ? V2A V2B 3.0559(14) . ? V2A V3B' 3.0753(14) . ? V1A OE2' 1.677(3) . ? V1A OE1 1.709(3) . ? V1A OB2' 1.829(3) . ? V1A OA1' 2.067(3) . ? V1A OB1 2.093(3) . ? V1A OA1 2.100(3) . ? V1A V2B' 3.0892(12) . ? V2B' OG2' 1.600(4) . ? V2B' OD1' 1.827(3) . ? V2B' OC4 1.866(3) . ? V2B' OC2' 1.878(3) . ? V2B' OE2' 2.066(3) . ? V2B' OA1' 2.344(3) . ? V2B' V2A' 3.0749(15) . ? V2B' V3B 3.1163(14) . ? V2B' V3A' 3.1197(13) . ? V2A' OG1' 1.596(3) . ? V2A' OD1' 1.823(4) . ? V2A' OC1' 1.849(3) . ? V2A' OC3 1.904(3) . ? V2A' OE1' 2.041(3) . ? V2A' OA1' 2.412(3) . ? V2A' V1A' 3.0817(13) . ? V2A' V3A' 3.0999(13) . ? V2A' V3B 3.1052(14) . ? V1A' OE1' 1.672(3) . ? V1A' OE2 1.691(3) . ? V1A' OB1' 1.917(3) . ? V1A' OB2 1.948(3) . ? V1A' OA1' 2.080(3) . ? V1A' OA1 2.180(3) . ? V1A' V2B 3.0840(13) . ? V1A' V3A 3.1187(13) . ? V2B OG2 1.603(3) . ? V2B OD1 1.819(3) . ? V2B OC4' 1.846(3) . ? V2B OC2 1.947(3) . ? V2B OE2 1.994(3) . ? V2B OA1 2.343(3) . ? V2B V3B' 3.0955(14) . ? V2B V3A 3.1025(12) . ? V3B' OF2' 1.601(3) . ? V3B' OC4' 1.804(3) . ? V3B' OC3' 1.878(3) . ? V3B' OB1' 1.941(3) . ? V3B' OB2' 2.020(3) . ? V3B' OA1 2.313(3) . ? V3B' V3A' 3.0780(13) . ? V3A' OF1' 1.607(3) . ? V3A' OC2' 1.799(3) . ? V3A' OC1' 1.810(3) . ? V3A' OB1' 2.013(3) . ? V3A' OB2' 2.061(3) . ? V3A' OA1' 2.283(3) . ? V3A OF1 1.601(3) . ? V3A OC2 1.737(3) . ? V3A OB2 1.901(3) . ? V3A OC1 1.931(4) . ? V3A OB1 2.122(3) . ? V3A OA1 2.252(3) . ? V3B OF2 1.605(3) . ? V3B OC3 1.768(3) . ? V3B OC4 1.829(3) . ? V3B OB2 2.000(3) . ? V3B OB1 2.092(3) . ? V3B OA1' 2.254(3) . ? N1 C4 1.469(7) . ? N1 C1 1.482(7) . ? N1 C3 1.491(8) . ? N1 C2 1.493(7) . ? N2 C6 1.477(6) . ? N2 C7 1.482(7) . ? N2 C5 1.484(6) . ? N2 C8 1.488(6) . ? N3 C10 1.493(6) . ? N3 C12 1.495(7) . ? N3 C11 1.496(7) . ? N3 C9 1.498(6) . ? N4 C15 1.481(7) . ? N4 C13 1.482(7) . ? N4 C16 1.484(7) . ? N4 C14 1.493(6) . ? 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 OE1 OC1 H1 3(5) 2_666 . ? OG1 OB1 H2 8(4) 2_666 . ? V1A OB1 H2 109(4) . . ? V3A OB1 H2 115(4) . . ? V3B OB1 H2 122(4) . . ? V2A OC1 H1 120(5) . . ? V3A OC1 H1 126(5) . . ? OG1 V2A OC3' 104.39(15) . . ? OG1 V2A OD1 103.10(16) . . ? OC3' V2A OD1 93.99(14) . . ? OG1 V2A OC1 97.36(16) . . ? OC3' V2A OC1 157.31(14) . . ? OD1 V2A OC1 87.21(15) . . ? OG1 V2A OE1 98.22(15) . . ? OC3' V2A OE1 87.96(13) . . ? OD1 V2A OE1 157.37(13) . . ? OC1 V2A OE1 82.57(13) . . ? OG1 V2A OA1 171.05(14) . . ? OC3' V2A OA1 81.93(12) . . ? OD1 V2A OA1 82.52(12) . . ? OC1 V2A OA1 75.76(13) . . ? OE1 V2A OA1 75.43(11) . . ? OG1 V2A V1A 130.48(13) . . ? OC3' V2A V1A 79.58(10) . . ? OD1 V2A V1A 126.12(10) . . ? OC1 V2A V1A 81.45(11) . . ? OE1 V2A V1A 32.29(8) . . ? OA1 V2A V1A 43.63(8) . . ? OG1 V2A V2B 136.18(13) . . ? OC3' V2A V2B 85.25(10) . . ? OD1 V2A V2B 33.08(10) . . ? OC1 V2A V2B 83.48(11) . . ? OE1 V2A V2B 125.11(9) . . ? OA1 V2A V2B 49.68(8) . . ? V1A V2A V2B 93.14(4) . . ? OG1 V2A V3B' 138.25(12) . . ? OC3' V2A V3B' 33.92(9) . . ? OD1 V2A V3B' 83.79(10) . . ? OC1 V2A V3B' 124.26(11) . . ? OE1 V2A V3B' 85.38(9) . . ? OA1 V2A V3B' 48.56(7) . . ? V1A V2A V3B' 61.47(3) . . ? V2B V2A V3B' 60.65(3) . . ? OE2' V1A OE1 106.34(15) . . ? OE2' V1A OB2' 100.80(14) . . ? OE1 V1A OB2' 101.36(14) . . ? OE2' V1A OA1' 87.92(13) . . ? OE1 V1A OA1' 163.00(13) . . ? OB2' V1A OA1' 84.55(12) . . ? OE2' V1A OB1 93.22(14) . . ? OE1 V1A OB1 92.20(13) . . ? OB2' V1A OB1 156.77(13) . . ? OA1' V1A OB1 77.49(12) . . ? OE2' V1A OA1 165.03(13) . . ? OE1 V1A OA1 85.98(13) . . ? OB2' V1A OA1 84.65(12) . . ? OA1' V1A OA1 78.66(11) . . ? OB1 V1A OA1 77.52(12) . . ? OE2' V1A V2A 146.11(11) . . ? OE1 V1A V2A 39.77(10) . . ? OB2' V1A V2A 89.31(10) . . ? OA1' V1A V2A 125.46(9) . . ? OB1 V1A V2A 89.23(9) . . ? OA1 V1A V2A 46.80(8) . . ? OE2' V1A V2B' 38.70(10) . . ? OE1 V1A V2B' 144.78(11) . . ? OB2' V1A V2B' 92.24(10) . . ? OA1' V1A V2B' 49.34(8) . . ? OB1 V1A V2B' 87.19(9) . . ? OA1 V1A V2B' 127.92(8) . . ? V2A V1A V2B' 174.31(3) . . ? OG2' V2B' OD1' 104.43(17) . . ? OG2' V2B' OC4 102.47(17) . . ? OD1' V2B' OC4 91.77(14) . . ? OG2' V2B' OC2' 102.33(17) . . ? OD1' V2B' OC2' 90.55(15) . . ? OC4 V2B' OC2' 153.66(14) . . ? OG2' V2B' OE2' 99.91(16) . . ? OD1' V2B' OE2' 155.62(14) . . ? OC4 V2B' OE2' 84.14(13) . . ? OC2' V2B' OE2' 83.00(13) . . ? OG2' V2B' OA1' 172.32(15) . . ? OD1' V2B' OA1' 83.25(13) . . ? OC4 V2B' OA1' 77.04(12) . . ? OC2' V2B' OA1' 77.19(12) . . ? OE2' V2B' OA1' 72.41(11) . . ? OG2' V2B' V2A' 136.98(14) . . ? OD1' V2B' V2A' 32.55(11) . . ? OC4 V2B' V2A' 85.03(10) . . ? OC2' V2B' V2A' 82.90(10) . . ? OE2' V2B' V2A' 123.08(9) . . ? OA1' V2B' V2A' 50.70(7) . . ? OG2' V2B' V1A 130.34(14) . . ? OD1' V2B' V1A 125.12(11) . . ? OC4 V2B' V1A 80.90(10) . . ? OC2' V2B' V1A 76.36(10) . . ? OE2' V2B' V1A 30.51(8) . . ? OA1' V2B' V1A 41.99(7) . . ? V2A' V2B' V1A 92.58(4) . . ? OG2' V2B' V3B 134.38(14) . . ? OD1' V2B' V3B 80.44(11) . . ? OC4 V2B' V3B 32.13(10) . . ? OC2' V2B' V3B 123.15(10) . . ? OE2' V2B' V3B 83.50(9) . . ? OA1' V2B' V3B 46.12(7) . . ? V2A' V2B' V3B 60.20(3) . . ? V1A V2B' V3B 64.93(3) . . ? OG2' V2B' V3A' 133.44(14) . . ? OD1' V2B' V3A' 81.13(11) . . ? OC4 V2B' V3A' 123.77(10) . . ? OC2' V2B' V3A' 31.18(10) . . ? OE2' V2B' V3A' 81.28(9) . . ? OA1' V2B' V3A' 46.78(7) . . ? V2A' V2B' V3A' 60.05(3) . . ? V1A V2B' V3A' 60.36(3) . . ? V3B V2B' V3A' 92.17(4) . . ? OG1' V2A' OD1' 103.85(18) . . ? OG1' V2A' OC1' 102.86(17) . . ? OD1' V2A' OC1' 91.98(15) . . ? OG1' V2A' OC3 101.92(16) . . ? OD1' V2A' OC3 89.99(15) . . ? OC1' V2A' OC3 153.89(14) . . ? OG1' V2A' OE1' 102.15(17) . . ? OD1' V2A' OE1' 153.93(13) . . ? OC1' V2A' OE1' 83.99(14) . . ? OC3 V2A' OE1' 82.88(13) . . ? OG1' V2A' OA1' 174.61(16) . . ? OD1' V2A' OA1' 81.38(12) . . ? OC1' V2A' OA1' 78.02(12) . . ? OC3 V2A' OA1' 76.55(11) . . ? OE1' V2A' OA1' 72.58(11) . . ? OG1' V2A' V2B' 136.48(15) . . ? OD1' V2A' V2B' 32.63(10) . . ? OC1' V2A' V2B' 84.40(11) . . ? OC3 V2A' V2B' 83.32(10) . . ? OE1' V2A' V2B' 121.34(9) . . ? OA1' V2A' V2B' 48.76(7) . . ? OG1' V2A' V1A' 132.40(15) . . ? OD1' V2A' V1A' 123.73(10) . . ? OC1' V2A' V1A' 78.63(10) . . ? OC3 V2A' V1A' 78.67(10) . . ? OE1' V2A' V1A' 30.25(8) . . ? OA1' V2A' V1A' 42.35(7) . . ? V2B' V2A' V1A' 91.11(4) . . ? OG1' V2A' V3A' 134.45(14) . . ? OD1' V2A' V3A' 81.76(10) . . ? OC1' V2A' V3A' 31.72(10) . . ? OC3 V2A' V3A' 123.45(9) . . ? OE1' V2A' V3A' 81.40(9) . . ? OA1' V2A' V3A' 46.91(7) . . ? V2B' V2A' V3A' 60.69(3) . . ? V1A' V2A' V3A' 61.55(3) . . ? OG1' V2A' V3B 132.76(14) . . ? OD1' V2A' V3B 80.80(11) . . ? OC1' V2A' V3B 124.15(10) . . ? OC3 V2A' V3B 30.94(9) . . ? OE1' V2A' V3B 80.28(9) . . ? OA1' V2A' V3B 46.13(7) . . ? V2B' V2A' V3B 60.56(3) . . ? V1A' V2A' V3B 61.66(3) . . ? V3A' V2A' V3B 92.76(3) . . ? OE1' V1A' OE2 108.52(15) . . ? OE1' V1A' OB1' 98.32(14) . . ? OE2 V1A' OB1' 96.88(14) . . ? OE1' V1A' OB2 97.33(14) . . ? OE2 V1A' OB2 96.31(13) . . ? OB1' V1A' OB2 155.13(12) . . ? OE1' V1A' OA1' 89.27(14) . . ? OE2 V1A' OA1' 162.16(13) . . ? OB1' V1A' OA1' 81.31(12) . . ? OB2 V1A' OA1' 79.69(12) . . ? OE1' V1A' OA1 165.83(14) . . ? OE2 V1A' OA1 85.58(13) . . ? OB1' V1A' OA1 80.93(12) . . ? OB2 V1A' OA1 79.17(11) . . ? OA1' V1A' OA1 76.60(11) . . ? OE1' V1A' V2A' 37.93(11) . . ? OE2 V1A' V2A' 146.45(11) . . ? OB1' V1A' V2A' 90.08(10) . . ? OB2 V1A' V2A' 90.48(9) . . ? OA1' V1A' V2A' 51.36(8) . . ? OA1 V1A' V2A' 127.97(8) . . ? OE1' V1A' V2B 144.89(11) . . ? OE2 V1A' V2B 36.40(10) . . ? OB1' V1A' V2B 87.97(10) . . ? OB2 V1A' V2B 90.26(9) . . ? OA1' V1A' V2B 125.84(8) . . ? OA1 V1A' V2B 49.26(8) . . ? V2A' V1A' V2B 176.87(3) . . ? OE1' V1A' V3A 132.57(11) . . ? OE2 V1A' V3A 81.48(10) . . ? OB1' V1A' V3A 127.15(9) . . ? OB2 V1A' V3A 35.39(8) . . ? OA1' V1A' V3A 85.52(8) . . ? OA1 V1A' V3A 46.21(7) . . ? V2A' V1A' V3A 119.62(4) . . ? V2B V1A' V3A 60.02(3) . . ? OG2 V2B OD1 103.12(17) . . ? OG2 V2B OC4' 102.86(16) . . ? OD1 V2B OC4' 91.66(14) . . ? OG2 V2B OC2 100.64(16) . . ? OD1 V2B OC2 89.45(13) . . ? OC4' V2B OC2 155.57(14) . . ? OG2 V2B OE2 102.31(16) . . ? OD1 V2B OE2 154.30(13) . . ? OC4' V2B OE2 86.20(13) . . ? OC2 V2B OE2 82.34(13) . . ? OG2 V2B OA1 176.47(15) . . ? OD1 V2B OA1 79.45(12) . . ? OC4' V2B OA1 79.37(12) . . ? OC2 V2B OA1 76.85(11) . . ? OE2 V2B OA1 74.99(11) . . ? OG2 V2B V2A 136.48(14) . . ? OD1 V2B V2A 33.44(10) . . ? OC4' V2B V2A 82.03(10) . . ? OC2 V2B V2A 85.57(9) . . ? OE2 V2B V2A 121.20(9) . . ? OA1 V2B V2A 46.24(7) . . ? OG2 V2B V1A' 132.52(13) . . ? OD1 V2B V1A' 124.28(10) . . ? OC4' V2B V1A' 80.15(10) . . ? OC2 V2B V1A' 79.10(9) . . ? OE2 V2B V1A' 30.21(9) . . ? OA1 V2B V1A' 44.83(7) . . ? V2A V2B V1A' 91.00(4) . . ? OG2 V2B V3B' 134.42(13) . . ? OD1 V2B V3B' 83.46(11) . . ? OC4' V2B V3B' 31.58(10) . . ? OC2 V2B V3B' 124.70(9) . . ? OE2 V2B V3B' 81.39(9) . . ? OA1 V2B V3B' 47.91(7) . . ? V2A V2B V3B' 59.99(3) . . ? V1A' V2B V3B' 61.43(3) . . ? OG2 V2B V3A 131.25(13) . . ? OD1 V2B V3A 82.59(10) . . ? OC4' V2B V3A 125.57(10) . . ? OC2 V2B V3A 30.61(9) . . ? OE2 V2B V3A 77.97(9) . . ? OA1 V2B V3A 46.29(7) . . ? V2A V2B V3A 64.04(3) . . ? V1A' V2B V3A 60.54(3) . . ? V3B' V2B V3A 94.20(3) . . ? OF2' V3B' OC4' 103.14(17) . . ? OF2' V3B' OC3' 101.92(16) . . ? OC4' V3B' OC3' 92.16(14) . . ? OF2' V3B' OB1' 102.67(16) . . ? OC4' V3B' OB1' 92.50(14) . . ? OC3' V3B' OB1' 153.20(13) . . ? OF2' V3B' OB2' 100.67(16) . . ? OC4' V3B' OB2' 155.66(13) . . ? OC3' V3B' OB2' 87.83(13) . . ? OB1' V3B' OB2' 77.31(13) . . ? OF2' V3B' OA1 175.83(16) . . ? OC4' V3B' OA1 81.03(12) . . ? OC3' V3B' OA1 77.60(12) . . ? OB1' V3B' OA1 77.09(11) . . ? OB2' V3B' OA1 75.19(11) . . ? OF2' V3B' V2A 133.89(13) . . ? OC4' V3B' V2A 82.09(10) . . ? OC3' V3B' V2A 32.11(9) . . ? OB1' V3B' V2A 123.05(9) . . ? OB2' V3B' V2A 85.11(9) . . ? OA1 V3B' V2A 46.00(7) . . ? OF2' V3B' V3A' 91.34(14) . . ? OC4' V3B' V3A' 132.24(11) . . ? OC3' V3B' V3A' 129.37(10) . . ? OB1' V3B' V3A' 39.74(9) . . ? OB2' V3B' V3A' 41.56(8) . . ? OA1 V3B' V3A' 85.86(8) . . ? V2A V3B' V3A' 119.12(4) . . ? OF2' V3B' V2B 135.42(14) . . ? OC4' V3B' V2B 32.42(9) . . ? OC3' V3B' V2B 82.71(10) . . ? OB1' V3B' V2B 87.22(9) . . ? OB2' V3B' V2B 123.89(8) . . ? OA1 V3B' V2B 48.73(7) . . ? V2A V3B' V2B 59.37(3) . . ? V3A' V3B' V2B 120.05(3) . . ? OF1' V3A' OC2' 103.84(17) . . ? OF1' V3A' OC1' 103.19(16) . . ? OC2' V3A' OC1' 95.09(15) . . ? OF1' V3A' OB1' 100.29(16) . . ? OC2' V3A' OB1' 153.05(13) . . ? OC1' V3A' OB1' 90.90(14) . . ? OF1' V3A' OB2' 99.50(15) . . ? OC2' V3A' OB2' 89.44(13) . . ? OC1' V3A' OB2' 155.04(13) . . ? OB1' V3A' OB2' 74.81(12) . . ? OF1' V3A' OA1' 172.57(16) . . ? OC2' V3A' OA1' 80.35(12) . . ? OC1' V3A' OA1' 82.35(12) . . ? OB1' V3A' OA1' 74.44(11) . . ? OB2' V3A' OA1' 74.22(11) . . ? OF1' V3A' V3B' 89.43(14) . . ? OC2' V3A' V3B' 129.97(11) . . ? OC1' V3A' V3B' 128.96(11) . . ? OB1' V3A' V3B' 38.06(8) . . ? OB2' V3A' V3B' 40.55(9) . . ? OA1' V3A' V3B' 83.21(8) . . ? OF1' V3A' V2A' 135.49(13) . . ? OC2' V3A' V2A' 83.36(10) . . ? OC1' V3A' V2A' 32.49(10) . . ? OB1' V3A' V2A' 87.83(9) . . ? OB2' V3A' V2A' 124.71(8) . . ? OA1' V3A' V2A' 50.51(7) . . ? V3B' V3A' V2A' 119.68(4) . . ? OF1' V3A' V2B' 136.38(14) . . ? OC2' V3A' V2B' 32.72(10) . . ? OC1' V3A' V2B' 83.67(11) . . ? OB1' V3A' V2B' 122.87(9) . . ? OB2' V3A' V2B' 87.09(9) . . ? OA1' V3A' V2B' 48.44(8) . . ? V3B' V3A' V2B' 119.81(3) . . ? V2A' V3A' V2B' 59.26(3) . . ? OF1 V3A OC2 104.74(16) . . ? OF1 V3A OB2 102.79(15) . . ? OC2 V3A OB2 97.34(13) . . ? OF1 V3A OC1 100.21(16) . . ? OC2 V3A OC1 93.66(15) . . ? OB2 V3A OC1 150.98(14) . . ? OF1 V3A OB1 98.19(15) . . ? OC2 V3A OB1 156.96(13) . . ? OB2 V3A OB1 75.06(12) . . ? OC1 V3A OB1 84.39(14) . . ? OF1 V3A OA1 171.36(15) . . ? OC2 V3A OA1 83.51(12) . . ? OB2 V3A OA1 78.32(11) . . ? OC1 V3A OA1 76.35(13) . . ? OB1 V3A OA1 73.71(11) . . ? OF1 V3A V2B 139.30(13) . . ? OC2 V3A V2B 34.80(10) . . ? OB2 V3A V2B 90.58(9) . . ? OC1 V3A V2B 83.30(11) . . ? OB1 V3A V2B 122.47(9) . . ? OA1 V3A V2B 48.77(8) . . ? OF1 V3A V1A' 138.51(12) . . ? OC2 V3A V1A' 80.90(10) . . ? OB2 V3A V1A' 36.39(8) . . ? OC1 V3A V1A' 120.68(11) . . ? OB1 V3A V1A' 80.43(9) . . ? OA1 V3A V1A' 44.34(7) . . ? V2B V3A V1A' 59.43(3) . . ? OF2 V3B OC3 104.55(16) . . ? OF2 V3B OC4 102.06(16) . . ? OC3 V3B OC4 96.92(15) . . ? OF2 V3B OB2 101.18(15) . . ? OC3 V3B OB2 92.75(14) . . ? OC4 V3B OB2 151.64(12) . . ? OF2 V3B OB1 97.96(15) . . ? OC3 V3B OB1 155.69(14) . . ? OC4 V3B OB1 87.09(13) . . ? OB2 V3B OB1 73.76(12) . . ? OF2 V3B OA1' 171.16(14) . . ? OC3 V3B OA1' 83.53(12) . . ? OC4 V3B OA1' 80.17(12) . . ? OB2 V3B OA1' 74.51(11) . . ? OB1 V3B OA1' 73.51(11) . . ? OF2 V3B V2A' 137.91(12) . . ? OC3 V3B V2A' 33.61(10) . . ? OC4 V3B V2A' 84.74(10) . . ? OB2 V3B V2A' 88.84(9) . . ? OB1 V3B V2A' 124.00(9) . . ? OA1' V3B V2A' 50.50(7) . . ? OF2 V3B V2B' 134.73(13) . . ? OC3 V3B V2B' 84.17(11) . . ? OC4 V3B V2B' 32.88(10) . . ? OB2 V3B V2B' 123.02(8) . . ? OB1 V3B V2B' 86.49(9) . . ? OA1' V3B V2B' 48.56(8) . . ? V2A' V3B V2B' 59.24(3) . . ? V1A OE1 V2A 107.94(14) . . ? V1A OE2' V2B' 110.79(15) . . ? V2A' OD1' V2B' 114.82(17) . . ? V1A' OE1' V2A' 111.82(16) . . ? V1A' OE2 V2B 113.39(15) . . ? V2B OD1 V2A 113.47(16) . . ? V3A OC2 V2B 114.59(15) . . ? V3A OC1 V2A 112.27(18) . . ? V3B OC4 V2B' 114.99(16) . . ? V3B OC3 V2A' 115.45(15) . . ? V3A' OC2' V2B' 116.10(16) . . ? V3A' OC1' V2A' 115.79(16) . . ? V3B' OC4' V2B 116.01(16) . . ? V2A OC3' V3B' 113.97(15) . . ? V3A OB2 V1A' 108.22(14) . . ? V3A OB2 V3B 107.60(14) . . ? V1A' OB2 V3B 106.83(13) . . ? V3B OB1 V1A 105.51(14) . . ? V3B OB1 V3A 96.71(13) . . ? V1A OB1 V3A 106.32(13) . . ? V1A OB2' V3B' 108.58(14) . . ? V1A OB2' V3A' 106.55(14) . . ? V3B' OB2' V3A' 97.89(13) . . ? V1A' OB1' V3B' 109.77(14) . . ? V1A' OB1' V3A' 107.15(14) . . ? V3B' OB1' V3A' 102.20(13) . . ? V1A OA1 V1A' 99.91(12) . . ? V1A OA1 V2A 89.58(11) . . ? V1A' OA1 V2A 169.14(15) . . ? V1A OA1 V3A 101.57(12) . . ? V1A' OA1 V3A 89.45(10) . . ? V2A OA1 V3A 93.85(11) . . ? V1A OA1 V3B' 90.13(10) . . ? V1A' OA1 V3B' 89.22(10) . . ? V2A OA1 V3B' 85.45(10) . . ? V3A OA1 V3B' 168.28(14) . . ? V1A OA1 V2B 171.23(14) . . ? V1A' OA1 V2B 85.91(10) . . ? V2A OA1 V2B 84.08(10) . . ? V3A OA1 V2B 84.93(10) . . ? V3B' OA1 V2B 83.36(10) . . ? V1A OA1' V1A' 104.39(13) . . ? V1A OA1' V3B 100.79(12) . . ? V1A' OA1' V3B 93.96(11) . . ? V1A OA1' V3A' 91.56(11) . . ? V1A' OA1' V3A' 92.81(11) . . ? V3B OA1' V3A' 163.97(14) . . ? V1A OA1' V2B' 88.67(11) . . ? V1A' OA1' V2B' 166.80(15) . . ? V3B OA1' V2B' 85.32(10) . . ? V3A' OA1' V2B' 84.78(10) . . ? V1A OA1' V2A' 168.12(14) . . ? V1A' OA1' V2A' 86.29(10) . . ? V3B OA1' V2A' 83.37(9) . . ? V3A' OA1' V2A' 82.59(9) . . ? V2B' OA1' V2A' 80.54(10) . . ? C4 N1 C1 109.3(5) . . ? C4 N1 C3 109.3(6) . . ? C1 N1 C3 109.2(5) . . ? C4 N1 C2 110.2(5) . . ? C1 N1 C2 109.1(5) . . ? C3 N1 C2 109.7(5) . . ? C6 N2 C7 109.1(5) . . ? C6 N2 C5 109.4(4) . . ? C7 N2 C5 109.8(5) . . ? C6 N2 C8 110.4(4) . . ? C7 N2 C8 108.1(4) . . ? C5 N2 C8 109.9(4) . . ? C10 N3 C12 109.4(5) . . ? C10 N3 C11 109.9(4) . . ? C12 N3 C11 110.0(5) . . ? C10 N3 C9 109.3(4) . . ? C12 N3 C9 108.9(4) . . ? C11 N3 C9 109.4(4) . . ? C15 N4 C13 109.2(5) . . ? C15 N4 C16 108.4(5) . . ? C13 N4 C16 110.4(5) . . ? C15 N4 C14 108.5(5) . . ? C13 N4 C14 110.9(5) . . ? C16 N4 C14 109.5(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag OC1 H1 OE1 2_666 0.57(4) 2.19(5) 2.763(5) 176(7) ? OB1 H2 OG1 2_666 0.72(5) 2.06(5) 2.766(5) 169(5) ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.755 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.103 #===END data_TEAh _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Tris(tetraethylammonium) trihydrogendecavanadate dihydrate ; _chemical_melting_point ? _chemical_formula_moiety '(C8 H20 N +)3, (H3 V10 O28 3-), 2(H2 O)' _chemical_formula_sum 'C24 H67 N3 O30 V10' _chemical_formula_weight 1387.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/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 33.4919(9) _cell_length_b 21.5128(5) _cell_length_c 13.9059(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.5520(10) _cell_angle_gamma 90.00 _cell_volume 9907.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 28.39 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5616 _exptl_absorpt_coefficient_mu 1.886 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'UltraX18 Rigaku Denki rotating Mo anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD SMART Area Detector System' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.005 _diffrn_reflns_number 39819 _diffrn_reflns_av_R_equivalents 0.0767 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 28.39 _reflns_number_total 12329 _reflns_number_gt 6615 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART program' _computing_cell_refinement 'Siemens SAINT program' _computing_data_reduction 'Siemens SAINT program' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997a)' _refine_special_details ; H atoms in the [(C~2~H~5~)~4~N]^+^ cations were included in ideal positions and refined with the riding model. H atoms attached to surface O atoms of decavanadate frameworks and H atoms of water molecules were not included in refinement. Distances between the following atom pairs were restrained to 1.54\%A with estimated standard deviation 0.01: N2 and C15A, N4 and C25B, C15A and C16, C11A and C12A, C13A and C14A, C13B and C14B, N2 and C13A, C11B and C12B, C31B and C32B, C15B and C16, C21 and C22. ; _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^)+(0.1037P)^2^+1.1961P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12329 _refine_ls_number_parameters 545 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1976 _refine_ls_wR_factor_gt 0.1609 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 V2B' V 0.13240(3) 0.15835(4) 0.39433(7) 0.0443(2) Uani 1 1 d . . . V1A V 0.17708(2) 0.26518(3) 0.50955(6) 0.02996(19) Uani 1 1 d . . . V2A V 0.21853(3) 0.36990(4) 0.63500(7) 0.0375(2) Uani 1 1 d . . . V2B V 0.17870(3) 0.33275(4) 0.81252(7) 0.0438(2) Uani 1 1 d . . . V1A' V 0.13464(2) 0.22353(4) 0.69520(6) 0.0331(2) Uani 1 1 d . . . V2A' V 0.09087(3) 0.11834(4) 0.56841(7) 0.0470(3) Uani 1 1 d . . . V3A' V 0.08274(3) 0.25439(4) 0.49137(7) 0.0412(2) Uani 1 1 d . . . V3B' V 0.12606(3) 0.36045(4) 0.61328(7) 0.0394(2) Uani 1 1 d . . . V3B V 0.18452(3) 0.12185(4) 0.60637(6) 0.0368(2) Uani 1 1 d . . . V3A V 0.22911(2) 0.23027(4) 0.72966(6) 0.0338(2) Uani 1 1 d . . . OG2' O 0.13252(12) 0.1345(2) 0.2863(3) 0.0649(12) Uani 1 1 d . . . OG1 O 0.25198(11) 0.41839(15) 0.6111(3) 0.0489(10) Uani 1 1 d . . . OG2 O 0.17845(13) 0.3570(2) 0.9201(3) 0.0640(12) Uani 1 1 d . . . OG1' O 0.05944(13) 0.06663(19) 0.5898(3) 0.0673(12) Uani 1 1 d . . . OF1' O 0.04664(11) 0.30077(19) 0.4529(3) 0.0580(11) Uani 1 1 d . . . OF2' O 0.08961(12) 0.40597(17) 0.5744(3) 0.0557(11) Uani 1 1 d . . . OF2 O 0.22206(11) 0.07743(16) 0.6402(3) 0.0520(10) Uani 1 1 d . . . OF1 O 0.26640(11) 0.18589(17) 0.7635(3) 0.0483(9) Uani 1 1 d . . . OE2' O 0.17530(10) 0.22597(15) 0.4023(2) 0.0376(8) Uani 1 1 d . . . OE1 O 0.21359(9) 0.31955(14) 0.5081(2) 0.0338(7) Uani 1 1 d . . . OD1 O 0.21389(11) 0.38329(16) 0.7645(3) 0.0435(9) Uani 1 1 d . . . OE2 O 0.14037(10) 0.25870(15) 0.8045(2) 0.0403(8) Uani 1 1 d . . . OE1' O 0.10173(10) 0.16477(15) 0.6980(3) 0.0429(9) Uani 1 1 d . . . OD1' O 0.09937(11) 0.10313(16) 0.4454(3) 0.0501(10) Uani 1 1 d . . . OC2' O 0.09485(11) 0.21846(18) 0.3786(3) 0.0489(9) Uani 1 1 d . . . OB2' O 0.13157(10) 0.31199(14) 0.4879(2) 0.0357(8) Uani 1 1 d . . . OC3' O 0.17123(10) 0.40536(14) 0.5903(3) 0.0436(9) Uani 1 1 d . . . OC4' O 0.13428(11) 0.37361(15) 0.7414(3) 0.0463(9) Uani 1 1 d . . . OB1' O 0.09788(9) 0.28239(15) 0.6267(2) 0.0352(8) Uani 1 1 d . . . OC1' O 0.05819(10) 0.18673(16) 0.5283(3) 0.0458(9) Uani 1 1 d . . . OC4 O 0.17886(10) 0.10992(15) 0.4655(2) 0.0421(8) Uani 1 1 d . . . OB1 O 0.21913(9) 0.20144(13) 0.5808(2) 0.0296(7) Uani 1 1 d . . . OC1 O 0.25712(10) 0.30046(14) 0.6827(2) 0.0362(8) Uani 1 1 d . . . OC2 O 0.21842(10) 0.26716(16) 0.8329(2) 0.0426(8) Uani 1 1 d . . . OB2 O 0.18365(9) 0.17374(14) 0.7198(2) 0.0338(7) Uani 1 1 d . . . OC3 O 0.14182(11) 0.07970(15) 0.6196(3) 0.0469(9) Uani 1 1 d . . . OA1' O 0.14016(9) 0.19686(14) 0.5522(2) 0.0329(7) Uani 1 1 d . . . OA1 O 0.17772(9) 0.28813(13) 0.6544(2) 0.0308(7) Uani 1 1 d . . . N1 N 0.18543(16) 0.0978(2) 1.0004(4) 0.0608(13) Uiso 1 1 d . . . C1 C 0.1655(2) 0.0694(3) 1.0812(5) 0.0643(17) Uiso 1 1 d . . . H1A H 0.1420 0.0941 1.0891 0.077 Uiso 1 1 calc R . . H1B H 0.1562 0.0281 1.0613 0.077 Uiso 1 1 calc R . . C2 C 0.1916(2) 0.0649(3) 1.1764(5) 0.0700(19) Uiso 1 1 d . . . H2A H 0.1766 0.0465 1.2229 0.105 Uiso 1 1 calc R . . H2B H 0.2005 0.1056 1.1979 0.105 Uiso 1 1 calc R . . H2C H 0.2146 0.0394 1.1701 0.105 Uiso 1 1 calc R . . C3 C 0.2020(2) 0.1619(3) 1.0249(6) 0.079(2) Uiso 1 1 d . . . H3A H 0.2247 0.1579 1.0769 0.095 Uiso 1 1 calc R . . H3B H 0.2126 0.1779 0.9685 0.095 Uiso 1 1 calc R . . C4 C 0.1746(3) 0.2077(4) 1.0542(6) 0.100(3) Uiso 1 1 d . . . H4A H 0.1886 0.2464 1.0681 0.150 Uiso 1 1 calc R . . H4B H 0.1644 0.1935 1.1114 0.150 Uiso 1 1 calc R . . H4C H 0.1525 0.2138 1.0027 0.150 Uiso 1 1 calc R . . C5 C 0.2219(2) 0.0566(4) 0.9890(6) 0.090(2) Uiso 1 1 d . . . H5A H 0.2404 0.0576 1.0497 0.109 Uiso 1 1 calc R . . H5B H 0.2124 0.0141 0.9791 0.109 Uiso 1 1 calc R . . C6 C 0.2456(3) 0.0732(4) 0.9069(7) 0.111(3) Uiso 1 1 d . . . H6A H 0.2676 0.0447 0.9071 0.166 Uiso 1 1 calc R . . H6B H 0.2559 0.1148 0.9164 0.166 Uiso 1 1 calc R . . H6C H 0.2281 0.0708 0.8457 0.166 Uiso 1 1 calc R . . C7 C 0.1571(3) 0.1016(4) 0.9084(6) 0.089(2) Uiso 1 1 d . . . H7A H 0.1706 0.1225 0.8606 0.106 Uiso 1 1 calc R . . H7B H 0.1344 0.1275 0.9194 0.106 Uiso 1 1 calc R . . C8 C 0.1404(3) 0.0397(5) 0.8650(8) 0.143(4) Uiso 1 1 d . . . H8A H 0.1222 0.0475 0.8061 0.214 Uiso 1 1 calc R . . H8B H 0.1262 0.0188 0.9107 0.214 Uiso 1 1 calc R . . H8C H 0.1623 0.0142 0.8509 0.214 Uiso 1 1 calc R . . N2 N 0.0000 0.2965(4) 0.7500 0.073(2) Uiso 1 2 d SD . . C9 C 0.0234(6) 0.3467(8) 0.7028(14) 0.096(5) Uiso 0.50 1 d P A . H9A H 0.0265 0.3352 0.6369 0.116 Uiso 0.50 1 calc PR . . H9B H 0.0500 0.3531 0.7401 0.116 Uiso 0.50 1 calc PR . . C10 C -0.0044(11) 0.4095(12) 0.704(2) 0.209(14) Uiso 0.50 1 d P . . H10A H 0.0091 0.4439 0.6785 0.314 Uiso 0.50 1 calc PR A . H10B H -0.0086 0.4184 0.7689 0.314 Uiso 0.50 1 calc PR . . H10C H -0.0300 0.4029 0.6636 0.314 Uiso 0.50 1 calc PR . . C11A C 0.0113(8) 0.2390(9) 0.6956(18) 0.040(7) Uiso 0.220(15) 1 d PD A 1 H11A H 0.0400 0.2391 0.6924 0.048 Uiso 0.220(15) 1 calc PR A 1 H11B H -0.0031 0.2391 0.6297 0.048 Uiso 0.220(15) 1 calc PR A 1 C12A C 0.0000 0.1804(11) 0.7500 0.112(13) Uiso 0.44(3) 2 d SPD A 1 H12A H 0.0062 0.1440 0.7153 0.167 Uiso 0.220(15) 1 calc PR A 1 H12B H -0.0284 0.1811 0.7542 0.167 Uiso 0.220(15) 1 calc PR A 1 H12C H 0.0151 0.1799 0.8143 0.167 Uiso 0.220(15) 1 calc PR A 1 C11B C 0.0302(11) 0.2446(13) 0.758(3) 0.098(11) Uiso 0.280(15) 1 d PD A 2 H11C H 0.0567 0.2631 0.7758 0.117 Uiso 0.280(15) 1 calc PR A 2 H11D H 0.0295 0.2273 0.6933 0.117 Uiso 0.280(15) 1 calc PR A 2 C12B C 0.0274(12) 0.1900(14) 0.827(3) 0.127(15) Uiso 0.280(15) 1 d PD A 2 H12D H 0.0479 0.1599 0.8192 0.191 Uiso 0.280(15) 1 calc PR A 2 H12E H 0.0013 0.1710 0.8127 0.191 Uiso 0.280(15) 1 calc PR A 2 H12F H 0.0314 0.2048 0.8931 0.191 Uiso 0.280(15) 1 calc PR A 2 C13A C 0.0012(9) 0.273(3) 0.8547(16) 0.088(13) Uiso 0.23(2) 1 d PD A 1 H13A H -0.0167 0.2373 0.8543 0.105 Uiso 0.23(2) 1 calc PR A 1 H13B H -0.0087 0.3052 0.8936 0.105 Uiso 0.23(2) 1 calc PR A 1 C14A C 0.0440(9) 0.254(2) 0.902(3) 0.082(13) Uiso 0.23(2) 1 d PD A 1 H14A H 0.0427 0.2350 0.9645 0.124 Uiso 0.23(2) 1 calc PR A 1 H14B H 0.0611 0.2897 0.9108 0.124 Uiso 0.23(2) 1 calc PR A 1 H14C H 0.0550 0.2242 0.8613 0.124 Uiso 0.23(2) 1 calc PR A 1 C13B C 0.0012(7) 0.3118(16) 0.8593(17) 0.063(9) Uiso 0.27(2) 1 d PD A 2 H13C H -0.0202 0.2894 0.8842 0.076 Uiso 0.27(2) 1 calc PR A 2 H13D H -0.0034 0.3560 0.8667 0.076 Uiso 0.27(2) 1 calc PR A 2 C14B C 0.0426(9) 0.294(3) 0.919(3) 0.121(15) Uiso 0.27(2) 1 d PD A 2 H14D H 0.0409 0.2968 0.9875 0.181 Uiso 0.27(2) 1 calc PR A 2 H14E H 0.0631 0.3216 0.9037 0.181 Uiso 0.27(2) 1 calc PR A 2 H14F H 0.0493 0.2520 0.9039 0.181 Uiso 0.27(2) 1 calc PR A 2 C15A C -0.0410(7) 0.329(2) 0.7169(16) 0.074(12) Uiso 0.27(3) 1 d PD A 1 H15A H -0.0628 0.3046 0.7360 0.089 Uiso 0.27(3) 1 calc PR A 1 H15B H -0.0412 0.3696 0.7484 0.089 Uiso 0.27(3) 1 calc PR A 1 C15B C -0.0463(9) 0.296(2) 0.694(3) 0.067(13) Uiso 0.23(3) 1 d PD A 2 H15C H -0.0544 0.2542 0.6748 0.081 Uiso 0.23(3) 1 calc PR A 2 H15D H -0.0644 0.3117 0.7372 0.081 Uiso 0.23(3) 1 calc PR A 2 C16 C -0.0479(9) 0.3380(13) 0.6052(15) 0.193(13) Uiso 0.50 1 d PD . . H16A H -0.0732 0.3586 0.5856 0.290 Uiso 0.27(3) 1 calc PR A 1 H16B H -0.0483 0.2981 0.5742 0.290 Uiso 0.27(3) 1 calc PR A 1 H16C H -0.0264 0.3627 0.5865 0.290 Uiso 0.27(3) 1 calc PR A 1 H16D H -0.0741 0.3570 0.5914 0.290 Uiso 0.23(3) 1 calc PR A 2 H16E H -0.0430 0.3136 0.5503 0.290 Uiso 0.23(3) 1 calc PR A 2 H16F H -0.0276 0.3697 0.6177 0.290 Uiso 0.23(3) 1 calc PR A 2 N3 N 0.0000 0.0857(5) 0.2500 0.093(3) Uiso 1 2 d S . . C17 C -0.0040(7) 0.0916(10) 0.1459(15) 0.121(7) Uiso 0.50 1 d P . . H17A H -0.0183 0.1301 0.1285 0.145 Uiso 0.50 1 calc PR . . H17B H -0.0214 0.0581 0.1181 0.145 Uiso 0.50 1 calc PR . . C18 C 0.0339(6) 0.0913(9) 0.0932(14) 0.103(5) Uiso 0.50 1 d P . . H18A H 0.0256 0.0945 0.0243 0.155 Uiso 0.50 1 calc PR . . H18B H 0.0486 0.0532 0.1076 0.155 Uiso 0.50 1 calc PR . . H18C H 0.0510 0.1259 0.1153 0.155 Uiso 0.50 1 calc PR . . C19 C 0.0185(8) 0.1463(12) 0.2980(19) 0.170(10) Uiso 0.50 1 d P . . H19A H 0.0473 0.1459 0.2957 0.205 Uiso 0.50 1 calc PR . . H19B H 0.0149 0.1459 0.3660 0.205 Uiso 0.50 1 calc PR . . C20 C 0.0000 0.2116(11) 0.2500 0.229(11) Uiso 1 2 d S . . H20A H 0.0116 0.2458 0.2887 0.344 Uiso 0.50 1 calc PR . . H20B H -0.0288 0.2118 0.2480 0.344 Uiso 0.50 1 calc PR . . H20C H 0.0063 0.2154 0.1852 0.344 Uiso 0.50 1 calc PR . . C21 C -0.0379(9) 0.0845(14) 0.294(2) 0.182(11) Uiso 0.50 1 d PD . . H21A H -0.0384 0.0494 0.3376 0.219 Uiso 0.50 1 calc PR . . H21B H -0.0615 0.0832 0.2445 0.219 Uiso 0.50 1 calc PR . . C22 C -0.0349(18) 0.1462(18) 0.349(4) 0.40(3) Uiso 0.50 1 d PD . . H22A H -0.0580 0.1507 0.3824 0.598 Uiso 0.50 1 calc PR . . H22B H -0.0343 0.1799 0.3044 0.598 Uiso 0.50 1 calc PR . . H22C H -0.0107 0.1467 0.3960 0.598 Uiso 0.50 1 calc PR . . C23 C 0.0331(5) 0.0382(8) 0.2839(13) 0.096(5) Uiso 0.50 1 d P . . H23A H 0.0513 0.0371 0.2358 0.115 Uiso 0.50 1 calc PR . . H23B H 0.0485 0.0535 0.3439 0.115 Uiso 0.50 1 calc PR . . C24 C 0.0219(7) -0.0206(11) 0.2993(18) 0.164(10) Uiso 0.50 1 d P . . H24A H 0.0455 -0.0459 0.3165 0.246 Uiso 0.50 1 calc PR . . H24B H 0.0062 -0.0366 0.2412 0.246 Uiso 0.50 1 calc PR . . H24C H 0.0059 -0.0213 0.3513 0.246 Uiso 0.50 1 calc PR . . N4 N 0.13253(17) 0.4214(3) 0.2475(4) 0.0658(14) Uiso 1 1 d D . . C25A C 0.1688(3) 0.4173(4) 0.3315(7) 0.057(3) Uiso 0.683(9) 1 d P B 1 H25A H 0.1596 0.3967 0.3863 0.069 Uiso 0.683(9) 1 calc PR B 1 H25B H 0.1894 0.3910 0.3101 0.069 Uiso 0.683(9) 1 calc PR B 1 C27A C 0.1042(4) 0.4666(6) 0.2603(9) 0.091(4) Uiso 0.683(9) 1 d P B 1 H27A H 0.0823 0.4645 0.2062 0.109 Uiso 0.683(9) 1 calc PR B 1 H27B H 0.1168 0.5071 0.2585 0.109 Uiso 0.683(9) 1 calc PR B 1 C28A C 0.0869(5) 0.4609(9) 0.3536(13) 0.129(6) Uiso 0.683(9) 1 d P B 1 H28A H 0.0677 0.4936 0.3572 0.194 Uiso 0.683(9) 1 calc PR B 1 H28B H 0.1082 0.4641 0.4078 0.194 Uiso 0.683(9) 1 calc PR B 1 H28C H 0.0737 0.4213 0.3555 0.194 Uiso 0.683(9) 1 calc PR B 1 C29A C 0.1516(4) 0.4380(6) 0.1576(9) 0.099(4) Uiso 0.683(9) 1 d P B 1 H29A H 0.1633 0.4792 0.1671 0.118 Uiso 0.683(9) 1 calc PR B 1 H29B H 0.1736 0.4092 0.1536 0.118 Uiso 0.683(9) 1 calc PR B 1 C31A C 0.1100(6) 0.3617(7) 0.2403(13) 0.132(6) Uiso 0.683(9) 1 d P B 1 H31A H 0.1042 0.3521 0.3050 0.158 Uiso 0.683(9) 1 calc PR B 1 H31B H 0.0842 0.3694 0.2002 0.158 Uiso 0.683(9) 1 calc PR B 1 C32A C 0.1255(5) 0.3086(6) 0.2055(12) 0.104(4) Uiso 0.683(9) 1 d P B 1 H32A H 0.1064 0.2753 0.2057 0.156 Uiso 0.683(9) 1 calc PR B 1 H32B H 0.1502 0.2978 0.2462 0.156 Uiso 0.683(9) 1 calc PR B 1 H32C H 0.1306 0.3156 0.1403 0.156 Uiso 0.683(9) 1 calc PR B 1 C25B C 0.1660(6) 0.4709(10) 0.270(2) 0.094(9) Uiso 0.317(9) 1 d PD B 2 H25C H 0.1857 0.4637 0.2266 0.112 Uiso 0.317(9) 1 calc PR B 2 H25D H 0.1539 0.5112 0.2534 0.112 Uiso 0.317(9) 1 calc PR B 2 C27B C 0.0948(7) 0.4264(12) 0.3201(19) 0.077(7) Uiso 0.317(9) 1 d P B 2 H27C H 0.0705 0.4060 0.2884 0.092 Uiso 0.317(9) 1 calc PR B 2 H27D H 0.1034 0.4059 0.3819 0.092 Uiso 0.317(9) 1 calc PR B 2 C28B C 0.0860(8) 0.4962(12) 0.337(2) 0.082(8) Uiso 0.317(9) 1 d P B 2 H28D H 0.0651 0.4996 0.3773 0.122 Uiso 0.317(9) 1 calc PR B 2 H28E H 0.0774 0.5161 0.2758 0.122 Uiso 0.317(9) 1 calc PR B 2 H28F H 0.1101 0.5160 0.3691 0.122 Uiso 0.317(9) 1 calc PR B 2 C29B C 0.1059(9) 0.4412(14) 0.149(2) 0.103(10) Uiso 0.317(9) 1 d P B 2 H29C H 0.0820 0.4151 0.1391 0.124 Uiso 0.317(9) 1 calc PR B 2 H29D H 0.0970 0.4837 0.1558 0.124 Uiso 0.317(9) 1 calc PR B 2 C31B C 0.1374(8) 0.3512(12) 0.2396(18) 0.079(7) Uiso 0.317(9) 1 d PD B 2 H31C H 0.1411 0.3333 0.3043 0.095 Uiso 0.317(9) 1 calc PR B 2 H31D H 0.1615 0.3424 0.2109 0.095 Uiso 0.317(9) 1 calc PR B 2 C32B C 0.1008(11) 0.320(2) 0.178(3) 0.173(19) Uiso 0.317(9) 1 d PD B 2 H32D H 0.1054 0.2759 0.1752 0.260 Uiso 0.317(9) 1 calc PR B 2 H32E H 0.0974 0.3366 0.1130 0.260 Uiso 0.317(9) 1 calc PR B 2 H32F H 0.0770 0.3276 0.2065 0.260 Uiso 0.317(9) 1 calc PR B 2 C26 C 0.1874(3) 0.4755(4) 0.3653(6) 0.104(3) Uiso 1 1 d . . . H26A H 0.2094 0.4676 0.4166 0.156 Uiso 0.683(9) 1 calc PR B 1 H26B H 0.1678 0.5015 0.3893 0.156 Uiso 0.683(9) 1 calc PR B 1 H26C H 0.1975 0.4960 0.3124 0.156 Uiso 0.683(9) 1 calc PR B 1 H26D H 0.2121 0.4523 0.3695 0.156 Uiso 0.317(9) 1 calc PR B 2 H26E H 0.1712 0.4590 0.4107 0.156 Uiso 0.317(9) 1 calc PR B 2 H26F H 0.1935 0.5183 0.3804 0.156 Uiso 0.317(9) 1 calc PR B 2 C30 C 0.1256(4) 0.4373(5) 0.0666(9) 0.145(4) Uiso 1 1 d . . . H30A H 0.1409 0.4473 0.0154 0.217 Uiso 0.683(9) 1 calc PR B 1 H30B H 0.1045 0.4674 0.0676 0.217 Uiso 0.683(9) 1 calc PR B 1 H30C H 0.1139 0.3967 0.0554 0.217 Uiso 0.683(9) 1 calc PR B 1 H30D H 0.1381 0.4764 0.0565 0.217 Uiso 0.317(9) 1 calc PR B 2 H30E H 0.1063 0.4274 0.0106 0.217 Uiso 0.317(9) 1 calc PR B 2 H30F H 0.1459 0.4054 0.0764 0.217 Uiso 0.317(9) 1 calc PR B 2 OW1A O -0.0057(5) 0.3845(8) 0.3169(16) 0.132(7) Uiso 0.48(2) 1 d P C 1 OW2A O 0.0042(7) 0.4302(12) 0.471(2) 0.219(14) Uiso 0.48(2) 1 d P C 1 OW1B O -0.0079(4) 0.3978(6) 0.3741(13) 0.107(5) Uiso 0.52(2) 1 d P C 2 OW2B O 0.0140(6) 0.4754(10) 0.5373(15) 0.190(11) Uiso 0.52(2) 1 d P . 2 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 V2B' 0.0346(5) 0.0523(6) 0.0479(5) -0.0113(4) 0.0123(4) -0.0024(4) V1A 0.0277(4) 0.0294(4) 0.0357(4) 0.0031(3) 0.0142(3) 0.0040(3) V2A 0.0372(5) 0.0277(4) 0.0520(5) -0.0019(4) 0.0206(4) 0.0007(3) V2B 0.0480(6) 0.0441(5) 0.0435(5) -0.0079(4) 0.0208(4) 0.0001(4) V1A' 0.0308(5) 0.0329(4) 0.0394(5) 0.0050(3) 0.0175(4) 0.0033(3) V2A' 0.0384(5) 0.0425(5) 0.0634(6) -0.0014(4) 0.0189(5) -0.0088(4) V3A' 0.0281(5) 0.0495(6) 0.0476(5) 0.0026(4) 0.0114(4) 0.0053(4) V3B' 0.0362(5) 0.0303(5) 0.0557(6) 0.0038(4) 0.0203(4) 0.0091(4) V3B 0.0366(5) 0.0261(4) 0.0510(5) 0.0023(4) 0.0173(4) 0.0032(3) V3A 0.0318(5) 0.0342(5) 0.0370(5) 0.0035(3) 0.0108(4) 0.0030(3) OG2' 0.055(3) 0.086(3) 0.056(3) -0.027(2) 0.015(2) -0.005(2) OG1 0.051(2) 0.0328(19) 0.069(3) -0.0030(17) 0.028(2) -0.0056(16) OG2 0.073(3) 0.075(3) 0.049(2) -0.021(2) 0.027(2) -0.002(2) OG1' 0.057(3) 0.057(3) 0.095(3) -0.003(2) 0.034(2) -0.020(2) OF1' 0.035(2) 0.072(3) 0.067(3) 0.009(2) 0.0078(19) 0.0151(19) OF2' 0.047(2) 0.042(2) 0.082(3) 0.0087(19) 0.024(2) 0.0177(17) OF2 0.050(2) 0.034(2) 0.075(3) 0.0062(17) 0.019(2) 0.0129(17) OF1 0.037(2) 0.048(2) 0.061(2) 0.0115(17) 0.0087(18) 0.0078(16) OE2' 0.0315(19) 0.049(2) 0.0341(18) 0.0009(15) 0.0113(14) 0.0011(15) OE1 0.0322(18) 0.0286(17) 0.0445(19) 0.0049(14) 0.0179(15) 0.0016(13) OD1 0.042(2) 0.0370(19) 0.056(2) -0.0104(16) 0.0217(17) -0.0023(15) OE2 0.041(2) 0.043(2) 0.040(2) 0.0015(15) 0.0188(16) 0.0041(16) OE1' 0.039(2) 0.039(2) 0.056(2) 0.0032(16) 0.0241(17) -0.0007(15) OD1' 0.039(2) 0.049(2) 0.064(3) -0.0137(18) 0.0140(19) -0.0102(17) OC2' 0.036(2) 0.068(3) 0.042(2) -0.0011(18) 0.0044(16) 0.0022(18) OB2' 0.0317(19) 0.0360(18) 0.0411(19) 0.0078(14) 0.0106(15) 0.0085(14) OC3' 0.043(2) 0.0266(18) 0.067(2) 0.0057(16) 0.0258(19) 0.0071(15) OC4' 0.047(2) 0.036(2) 0.061(2) -0.0048(16) 0.0281(19) 0.0051(16) OB1' 0.0292(18) 0.0356(18) 0.045(2) 0.0047(14) 0.0199(15) 0.0050(13) OC1' 0.030(2) 0.053(2) 0.057(2) -0.0021(17) 0.0150(17) -0.0029(16) OC4 0.041(2) 0.0358(19) 0.052(2) -0.0106(16) 0.0134(17) 0.0010(15) OB1 0.0274(17) 0.0252(16) 0.0377(18) 0.0018(13) 0.0102(14) 0.0004(12) OC1 0.0322(19) 0.0356(19) 0.044(2) -0.0032(14) 0.0148(15) -0.0029(14) OC2 0.041(2) 0.050(2) 0.039(2) -0.0013(16) 0.0127(16) 0.0000(16) OB2 0.0320(18) 0.0346(18) 0.0372(18) 0.0068(14) 0.0125(14) 0.0028(14) OC3 0.046(2) 0.0314(19) 0.068(3) 0.0043(16) 0.0260(19) -0.0028(16) OA1' 0.0286(17) 0.0308(17) 0.0416(19) 0.0027(13) 0.0130(14) 0.0025(13) OA1 0.0303(18) 0.0279(17) 0.0373(18) -0.0007(13) 0.0155(14) 0.0025(13) _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 OW1A OF1' 2.98(2) . ? OW1B OF1' 2.88(1) . ? OW2B OF2' 2.92(2) . ? OC4 OG1 2.758(5) 7_556 ? OB1 OE1 2.764(4) 7_556 ? OC1 OE2' 2.764(4) 7_556 ? V2B' OG2' 1.589(4) . ? V2B' OC2' 1.794(4) . ? V2B' OD1' 1.836(4) . ? V2B' OC4 2.007(4) . ? V2B' OE2' 2.036(3) . ? V2B' OA1' 2.325(3) . ? V2B' V1A 3.0619(12) . ? V2B' V3A' 3.0859(12) . ? V2B' V2A' 3.0881(13) . ? V1A OE1 1.694(3) . ? V1A OE2' 1.707(3) . ? V1A OB2' 1.814(3) . ? V1A OA1' 2.064(3) . ? V1A OA1 2.071(3) . ? V1A OB1 2.105(3) . ? V1A V2A 3.0537(12) . ? V2A OG1 1.602(3) . ? V2A OC3' 1.785(4) . ? V2A OD1 1.852(3) . ? V2A OC1 2.022(3) . ? V2A OE1 2.056(3) . ? V2A OA1 2.268(3) . ? V2A V3B' 3.0734(12) . ? V2A V2B 3.0807(12) . ? V2B OG2 1.586(4) . ? V2B OD1 1.803(3) . ? V2B OC4' 1.878(4) . ? V2B OC2 1.931(4) . ? V2B OE2 2.039(3) . ? V2B OA1 2.395(3) . ? V2B V3A 3.1010(11) . ? V2B V1A' 3.1056(12) . ? V2B V3B' 3.1123(13) . ? V1A' OE1' 1.681(3) . ? V1A' OE2 1.684(3) . ? V1A' OB1' 1.917(3) . ? V1A' OB2 1.947(3) . ? V1A' OA1' 2.104(3) . ? V1A' OA1 2.140(3) . ? V1A' V2A' 3.0998(13) . ? V1A' V3B 3.1171(11) . ? V2A' OG1' 1.590(4) . ? V2A' OD1' 1.806(4) . ? V2A' OC1' 1.869(4) . ? V2A' OC3 1.936(4) . ? V2A' OE1' 2.045(4) . ? V2A' OA1' 2.396(3) . ? V2A' V3B 3.1033(12) . ? V2A' V3A' 3.1146(13) . ? V3A' OF1' 1.597(4) . ? V3A' OC1' 1.784(4) . ? V3A' OC2' 1.846(4) . ? V3A' OB1' 1.970(3) . ? V3A' OB2' 2.058(3) . ? V3A' OA1' 2.337(3) . ? V3A' V3B' 3.0747(13) . ? V3B' OF2' 1.595(4) . ? V3B' OC4' 1.785(4) . ? V3B' OC3' 1.862(3) . ? V3B' OB1' 1.949(3) . ? V3B' OB2' 2.063(3) . ? V3B' OA1 2.334(3) . ? V3B OF2 1.594(4) . ? V3B OC3 1.726(3) . ? V3B OB2 1.936(3) . ? V3B OC4 1.956(3) . ? V3B OB1 2.127(3) . ? V3B OA1' 2.246(3) . ? V3A OF1 1.587(3) . ? V3A OC2 1.724(3) . ? V3A OB2 1.938(3) . ? V3A OC1 1.941(3) . ? V3A OB1 2.139(3) . ? V3A OA1 2.252(3) . ? N1 C7 1.478(9) . ? N1 C3 1.506(8) . ? N1 C1 1.517(8) . ? N1 C5 1.536(9) . ? C1 C2 1.476(9) . ? C3 C4 1.448(10) . ? C5 C6 1.526(11) . ? C7 C8 1.532(12) . ? N2 C11B 1.50(3) 2_556 ? N2 C11B 1.50(3) . ? N2 C11A 1.53(2) . ? N2 C11A 1.53(2) 2_556 ? N2 C13A 1.538(10) 2_556 ? N2 C13A 1.538(10) . ? N2 C9 1.538(17) . ? N2 C9 1.538(17) 2_556 ? N2 C13B 1.55(2) . ? N2 C13B 1.55(2) 2_556 ? N2 C15A 1.553(10) 2_556 ? N2 C15A 1.553(10) . ? C9 C10 1.64(3) . ? C11A C12A 1.545(10) . ? C11B C12B 1.530(10) . ? C13A C14A 1.543(10) . ? C13B C14B 1.556(10) . ? C15A C16 1.548(10) . ? C15B C16 1.528(10) . ? N3 C17 1.44(2) 2 ? N3 C17 1.44(2) . ? N3 C21 1.49(3) 2 ? N3 C21 1.49(3) . ? N3 C23 1.529(17) 2 ? N3 C23 1.529(17) . ? N3 C19 1.55(2) . ? N3 C19 1.55(2) 2 ? C17 C18 1.56(3) . ? C19 C20 1.64(3) . ? C21 C22 1.531(10) . ? C23 C24 1.35(2) . ? C24 C24 1.85(5) 2 ? N4 C27A 1.388(12) . ? N4 C31A 1.487(17) . ? N4 C31B 1.53(3) . ? N4 C29A 1.528(13) . ? N4 C25B 1.546(10) . ? N4 C25A 1.559(10) . ? N4 C29B 1.57(3) . ? N4 C27B 1.73(3) . ? C25A C26 1.446(11) . ? C27A C28A 1.50(2) . ? C29A C30 1.426(15) . ? C31A C32A 1.371(18) . ? C25B C26 1.41(2) . ? C27B C28B 1.55(4) . ? C29B C30 1.41(3) . ? C31B C32B 1.543(10) . ? 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 OG2' V2B' OC2' 102.6(2) . . ? OG2' V2B' OD1' 104.1(2) . . ? OC2' V2B' OD1' 93.53(17) . . ? OG2' V2B' OC4 100.82(19) . . ? OC2' V2B' OC4 155.78(16) . . ? OD1' V2B' OC4 86.61(16) . . ? OG2' V2B' OE2' 100.47(18) . . ? OC2' V2B' OE2' 88.16(15) . . ? OD1' V2B' OE2' 154.40(16) . . ? OC4 V2B' OE2' 81.66(14) . . ? OG2' V2B' OA1' 173.16(17) . . ? OC2' V2B' OA1' 80.56(14) . . ? OD1' V2B' OA1' 81.65(14) . . ? OC4 V2B' OA1' 75.50(12) . . ? OE2' V2B' OA1' 73.44(12) . . ? OG2' V2B' V1A 131.91(16) . . ? OC2' V2B' V1A 78.57(12) . . ? OD1' V2B' V1A 123.98(12) . . ? OC4 V2B' V1A 81.30(10) . . ? OE2' V2B' V1A 31.70(9) . . ? OA1' V2B' V1A 42.35(8) . . ? OG2' V2B' V3A' 135.04(17) . . ? OC2' V2B' V3A' 32.56(12) . . ? OD1' V2B' V3A' 82.49(11) . . ? OC4 V2B' V3A' 124.09(10) . . ? OE2' V2B' V3A' 85.39(9) . . ? OA1' V2B' V3A' 48.72(8) . . ? V1A V2B' V3A' 61.44(3) . . ? OG2' V2B' V2A' 135.73(16) . . ? OC2' V2B' V2A' 84.66(12) . . ? OD1' V2B' V2A' 31.71(11) . . ? OC4 V2B' V2A' 82.83(10) . . ? OE2' V2B' V2A' 123.56(10) . . ? OA1' V2B' V2A' 50.15(8) . . ? V1A V2B' V2A' 92.35(3) . . ? V3A' V2B' V2A' 60.59(3) . . ? OE1 V1A OE2' 105.22(16) . . ? OE1 V1A OB2' 101.82(15) . . ? OE2' V1A OB2' 102.11(16) . . ? OE1 V1A OA1' 163.59(15) . . ? OE2' V1A OA1' 87.39(14) . . ? OB2' V1A OA1' 85.33(13) . . ? OE1 V1A OA1 86.77(14) . . ? OE2' V1A OA1 164.09(14) . . ? OB2' V1A OA1 85.19(14) . . ? OA1' V1A OA1 79.05(12) . . ? OE1 V1A OB1 91.25(13) . . ? OE2' V1A OB1 91.33(14) . . ? OB2' V1A OB1 157.91(13) . . ? OA1' V1A OB1 77.78(12) . . ? OA1 V1A OB1 77.77(12) . . ? OE1 V1A V2A 39.63(11) . . ? OE2' V1A V2A 144.86(11) . . ? OB2' V1A V2A 89.12(11) . . ? OA1' V1A V2A 127.02(9) . . ? OA1 V1A V2A 47.96(8) . . ? OB1 V1A V2A 89.79(9) . . ? OE1 V1A V2B' 144.04(11) . . ? OE2' V1A V2B' 38.82(11) . . ? OB2' V1A V2B' 89.80(11) . . ? OA1' V1A V2B' 49.37(9) . . ? OA1 V1A V2B' 128.42(9) . . ? OB1 V1A V2B' 89.88(9) . . ? V2A V1A V2B' 176.32(4) . . ? OG1 V2A OC3' 105.15(18) . . ? OG1 V2A OD1 105.24(17) . . ? OC3' V2A OD1 94.21(16) . . ? OG1 V2A OC1 96.70(16) . . ? OC3' V2A OC1 157.10(14) . . ? OD1 V2A OC1 86.43(15) . . ? OG1 V2A OE1 97.73(16) . . ? OC3' V2A OE1 88.43(15) . . ? OD1 V2A OE1 155.27(14) . . ? OC1 V2A OE1 81.85(13) . . ? OG1 V2A OA1 169.23(15) . . ? OC3' V2A OA1 81.57(13) . . ? OD1 V2A OA1 82.29(13) . . ? OC1 V2A OA1 75.82(12) . . ? OE1 V2A OA1 73.77(11) . . ? OG1 V2A V1A 129.38(14) . . ? OC3' V2A V1A 79.16(12) . . ? OD1 V2A V1A 124.98(11) . . ? OC1 V2A V1A 81.75(9) . . ? OE1 V2A V1A 31.72(8) . . ? OA1 V2A V1A 42.70(8) . . ? OG1 V2A V3B' 138.45(14) . . ? OC3' V2A V3B' 33.35(10) . . ? OD1 V2A V3B' 82.93(11) . . ? OC1 V2A V3B' 124.69(9) . . ? OE1 V2A V3B' 85.96(9) . . ? OA1 V2A V3B' 49.02(8) . . ? V1A V2A V3B' 61.92(3) . . ? OG1 V2A V2B 137.31(14) . . ? OC3' V2A V2B 85.53(11) . . ? OD1 V2A V2B 32.08(11) . . ? OC1 V2A V2B 82.95(9) . . ? OE1 V2A V2B 124.18(9) . . ? OA1 V2A V2B 50.44(8) . . ? V1A V2A V2B 92.99(3) . . ? V3B' V2A V2B 60.76(3) . . ? OG2 V2B OD1 104.3(2) . . ? OG2 V2B OC4' 103.1(2) . . ? OD1 V2B OC4' 91.90(16) . . ? OG2 V2B OC2 101.7(2) . . ? OD1 V2B OC2 91.20(15) . . ? OC4' V2B OC2 153.37(16) . . ? OG2 V2B OE2 102.54(19) . . ? OD1 V2B OE2 153.13(15) . . ? OC4' V2B OE2 83.91(15) . . ? OC2 V2B OE2 81.46(14) . . ? OG2 V2B OA1 175.48(18) . . ? OD1 V2B OA1 79.75(13) . . ? OC4' V2B OA1 78.63(13) . . ? OC2 V2B OA1 75.93(13) . . ? OE2 V2B OA1 73.40(12) . . ? OG2 V2B V2A 137.23(16) . . ? OD1 V2B V2A 33.07(11) . . ? OC4' V2B V2A 81.98(11) . . ? OC2 V2B V2A 86.34(10) . . ? OE2 V2B V2A 120.22(10) . . ? OA1 V2B V2A 46.91(7) . . ? OG2 V2B V3A 131.63(17) . . ? OD1 V2B V3A 82.47(11) . . ? OC4' V2B V3A 124.74(11) . . ? OC2 V2B V3A 29.98(10) . . ? OE2 V2B V3A 78.32(9) . . ? OA1 V2B V3A 46.20(7) . . ? V2A V2B V3A 64.03(3) . . ? OG2 V2B V1A' 132.54(16) . . ? OD1 V2B V1A' 123.18(11) . . ? OC4' V2B V1A' 78.48(11) . . ? OC2 V2B V1A' 77.72(11) . . ? OE2 V2B V1A' 30.00(9) . . ? OA1 V2B V1A' 43.44(7) . . ? V2A V2B V1A' 90.22(3) . . ? V3A V2B V1A' 60.62(3) . . ? OG2 V2B V3B' 134.02(17) . . ? OD1 V2B V3B' 82.51(12) . . ? OC4' V2B V3B' 30.93(10) . . ? OC2 V2B V3B' 123.86(11) . . ? OE2 V2B V3B' 80.35(10) . . ? OA1 V2B V3B' 48.00(7) . . ? V2A V2B V3B' 59.50(3) . . ? V3A V2B V3B' 94.19(3) . . ? V1A' V2B V3B' 61.00(3) . . ? OE1' V1A' OE2 107.70(17) . . ? OE1' V1A' OB1' 97.67(15) . . ? OE2 V1A' OB1' 97.48(16) . . ? OE1' V1A' OB2 96.94(15) . . ? OE2 V1A' OB2 96.24(15) . . ? OB1' V1A' OB2 155.87(13) . . ? OE1' V1A' OA1' 88.12(15) . . ? OE2 V1A' OA1' 164.11(15) . . ? OB1' V1A' OA1' 81.43(13) . . ? OB2 V1A' OA1' 79.95(13) . . ? OE1' V1A' OA1 164.73(15) . . ? OE2 V1A' OA1 87.51(14) . . ? OB1' V1A' OA1 81.25(13) . . ? OB2 V1A' OA1 79.61(12) . . ? OA1' V1A' OA1 76.65(12) . . ? OE1' V1A' V2A' 37.66(12) . . ? OE2 V1A' V2A' 145.34(12) . . ? OB1' V1A' V2A' 89.16(10) . . ? OB2 V1A' V2A' 90.76(10) . . ? OA1' V1A' V2A' 50.51(9) . . ? OA1 V1A' V2A' 127.15(9) . . ? OE1' V1A' V2B 144.94(12) . . ? OE2 V1A' V2B 37.25(11) . . ? OB1' V1A' V2B 88.91(10) . . ? OB2 V1A' V2B 90.09(10) . . ? OA1' V1A' V2B 126.94(9) . . ? OA1 V1A' V2B 50.30(8) . . ? V2A' V1A' V2B 177.06(4) . . ? OE1' V1A' V3B 82.73(11) . . ? OE2 V1A' V3B 132.64(12) . . ? OB1' V1A' V3B 127.52(10) . . ? OB2 V1A' V3B 36.49(10) . . ? OA1' V1A' V3B 46.09(9) . . ? OA1 V1A' V3B 85.90(8) . . ? V2A' V1A' V3B 59.89(3) . . ? V2B V1A' V3B 119.88(3) . . ? OG1' V2A' OD1' 104.6(2) . . ? OG1' V2A' OC1' 103.4(2) . . ? OD1' V2A' OC1' 91.60(17) . . ? OG1' V2A' OC3 101.7(2) . . ? OD1' V2A' OC3 90.90(17) . . ? OC1' V2A' OC3 153.24(15) . . ? OG1' V2A' OE1' 102.30(19) . . ? OD1' V2A' OE1' 153.01(15) . . ? OC1' V2A' OE1' 84.15(15) . . ? OC3 V2A' OE1' 81.63(15) . . ? OG1' V2A' OA1' 174.7(2) . . ? OD1' V2A' OA1' 80.26(13) . . ? OC1' V2A' OA1' 78.35(13) . . ? OC3 V2A' OA1' 75.83(12) . . ? OE1' V2A' OA1' 72.77(12) . . ? OG1' V2A' V2B' 136.84(17) . . ? OD1' V2A' V2B' 32.32(11) . . ? OC1' V2A' V2B' 81.88(11) . . ? OC3 V2A' V2B' 86.13(11) . . ? OE1' V2A' V2B' 120.85(10) . . ? OA1' V2A' V2B' 48.15(8) . . ? OG1' V2A' V1A' 132.44(17) . . ? OD1' V2A' V1A' 122.92(11) . . ? OC1' V2A' V1A' 78.55(11) . . ? OC3 V2A' V1A' 77.77(11) . . ? OE1' V2A' V1A' 30.14(9) . . ? OA1' V2A' V1A' 42.66(8) . . ? V2B' V2A' V1A' 90.71(3) . . ? OG1' V2A' V3B 131.75(18) . . ? OD1' V2A' V3B 82.41(12) . . ? OC1' V2A' V3B 124.33(11) . . ? OC3 V2A' V3B 30.07(10) . . ? OE1' V2A' V3B 78.20(10) . . ? OA1' V2A' V3B 46.03(8) . . ? V2B' V2A' V3B 64.21(3) . . ? V1A' V2A' V3B 60.33(3) . . ? OG1' V2A' V3A' 134.06(17) . . ? OD1' V2A' V3A' 82.10(12) . . ? OC1' V2A' V3A' 30.70(10) . . ? OC3 V2A' V3A' 123.85(10) . . ? OE1' V2A' V3A' 80.75(10) . . ? OA1' V2A' V3A' 48.04(8) . . ? V2B' V2A' V3A' 59.67(3) . . ? V1A' V2A' V3A' 61.28(3) . . ? V3B V2A' V3A' 94.02(3) . . ? OF1' V3A' OC1' 104.34(19) . . ? OF1' V3A' OC2' 103.18(19) . . ? OC1' V3A' OC2' 94.11(17) . . ? OF1' V3A' OB1' 101.74(18) . . ? OC1' V3A' OB1' 92.20(15) . . ? OC2' V3A' OB1' 151.85(15) . . ? OF1' V3A' OB2' 100.40(18) . . ? OC1' V3A' OB2' 154.12(15) . . ? OC2' V3A' OB2' 87.51(15) . . ? OB1' V3A' OB2' 75.28(13) . . ? OF1' V3A' OA1' 173.31(18) . . ? OC1' V3A' OA1' 81.57(14) . . ? OC2' V3A' OA1' 79.22(14) . . ? OB1' V3A' OA1' 74.63(12) . . ? OB2' V3A' OA1' 73.35(11) . . ? OF1' V3A' V3B' 89.58(16) . . ? OC1' V3A' V3B' 130.27(13) . . ? OC2' V3A' V3B' 129.32(12) . . ? OB1' V3A' V3B' 38.07(9) . . ? OB2' V3A' V3B' 41.82(9) . . ? OA1' V3A' V3B' 84.14(8) . . ? OF1' V3A' V2B' 134.60(16) . . ? OC1' V3A' V2B' 83.17(11) . . ? OC2' V3A' V2B' 31.53(12) . . ? OB1' V3A' V2B' 122.94(9) . . ? OB2' V3A' V2B' 84.90(9) . . ? OA1' V3A' V2B' 48.38(8) . . ? V3B' V3A' V2B' 119.81(3) . . ? OF1' V3A' V2A' 136.49(15) . . ? OC1' V3A' V2A' 32.32(11) . . ? OC2' V3A' V2A' 83.09(12) . . ? OB1' V3A' V2A' 87.81(10) . . ? OB2' V3A' V2A' 123.01(9) . . ? OA1' V3A' V2A' 49.67(8) . . ? V3B' V3A' V2A' 119.85(4) . . ? V2B' V3A' V2A' 59.74(3) . . ? OF2' V3B' OC4' 103.76(19) . . ? OF2' V3B' OC3' 102.93(18) . . ? OC4' V3B' OC3' 94.60(17) . . ? OF2' V3B' OB1' 101.79(17) . . ? OC4' V3B' OB1' 92.62(15) . . ? OC3' V3B' OB1' 151.74(14) . . ? OF2' V3B' OB2' 100.58(18) . . ? OC4' V3B' OB2' 154.70(14) . . ? OC3' V3B' OB2' 86.58(14) . . ? OB1' V3B' OB2' 75.60(13) . . ? OF2' V3B' OA1 173.84(18) . . ? OC4' V3B' OA1 82.09(14) . . ? OC3' V3B' OA1 78.25(13) . . ? OB1' V3B' OA1 75.76(12) . . ? OB2' V3B' OA1 73.39(12) . . ? OF2' V3B' V2A 134.57(14) . . ? OC4' V3B' V2A 83.56(12) . . ? OC3' V3B' V2A 31.79(10) . . ? OB1' V3B' V2A 122.87(10) . . ? OB2' V3B' V2A 84.32(9) . . ? OA1 V3B' V2A 47.20(7) . . ? OF2' V3B' V3A' 89.65(16) . . ? OC4' V3B' V3A' 131.17(12) . . ? OC3' V3B' V3A' 128.27(12) . . ? OB1' V3B' V3A' 38.56(10) . . ? OB2' V3B' V3A' 41.69(9) . . ? OA1 V3B' V3A' 84.96(8) . . ? V2A V3B' V3A' 119.29(3) . . ? OF2' V3B' V2B 136.30(16) . . ? OC4' V3B' V2B 32.73(11) . . ? OC3' V3B' V2B 83.38(12) . . ? OB1' V3B' V2B 88.16(10) . . ? OB2' V3B' V2B 123.07(9) . . ? OA1 V3B' V2B 49.69(8) . . ? V2A V3B' V2B 59.74(3) . . ? V3A' V3B' V2B 120.47(3) . . ? OF2 V3B OC3 106.46(18) . . ? OF2 V3B OB2 102.24(18) . . ? OC3 V3B OB2 95.92(16) . . ? OF2 V3B OC4 99.90(18) . . ? OC3 V3B OC4 94.53(17) . . ? OB2 V3B OC4 151.67(14) . . ? OF2 V3B OB1 96.12(16) . . ? OC3 V3B OB1 157.12(15) . . ? OB2 V3B OB1 75.33(12) . . ? OC4 V3B OB1 84.97(13) . . ? OF2 V3B OA1' 169.51(16) . . ? OC3 V3B OA1' 84.02(14) . . ? OB2 V3B OA1' 76.67(12) . . ? OC4 V3B OA1' 78.34(13) . . ? OB1 V3B OA1' 73.46(11) . . ? OF2 V3B V2A' 140.24(14) . . ? OC3 V3B V2A' 34.19(12) . . ? OB2 V3B V2A' 90.87(10) . . ? OC4 V3B V2A' 83.19(11) . . ? OB1 V3B V2A' 123.59(9) . . ? OA1' V3B V2A' 50.14(8) . . ? OF2 V3B V1A' 138.55(15) . . ? OC3 V3B V1A' 79.92(12) . . ? OB2 V3B V1A' 36.73(9) . . ? OC4 V3B V1A' 120.73(10) . . ? OB1 V3B V1A' 80.73(8) . . ? OA1' V3B V1A' 42.43(8) . . ? V2A' V3B V1A' 59.78(3) . . ? OF1 V3A OC2 106.34(19) . . ? OF1 V3A OB2 102.65(17) . . ? OC2 V3A OB2 95.15(15) . . ? OF1 V3A OC1 99.76(16) . . ? OC2 V3A OC1 95.31(15) . . ? OB2 V3A OC1 151.44(14) . . ? OF1 V3A OB1 96.65(16) . . ? OC2 V3A OB1 156.56(15) . . ? OB2 V3A OB1 75.01(12) . . ? OC1 V3A OB1 85.06(13) . . ? OF1 V3A OA1 169.71(16) . . ? OC2 V3A OA1 83.88(14) . . ? OB2 V3A OA1 77.04(12) . . ? OC1 V3A OA1 77.76(13) . . ? OB1 V3A OA1 73.26(11) . . ? OF1 V3A V2B 139.93(14) . . ? OC2 V3A V2B 34.04(12) . . ? OB2 V3A V2B 90.40(10) . . ? OC1 V3A V2B 83.62(9) . . ? OB1 V3A V2B 123.39(9) . . ? OA1 V3A V2B 50.13(8) . . ? V1A OE2' V2B' 109.49(16) . . ? V1A OE1 V2A 108.65(15) . . ? V2B OD1 V2A 114.85(18) . . ? V1A' OE2 V2B 112.75(17) . . ? V1A' OE1' V2A' 112.20(17) . . ? V2A' OD1' V2B' 115.97(18) . . ? V2B' OC2' V3A' 115.9(2) . . ? V1A OB2' V3A' 108.22(15) . . ? V1A OB2' V3B' 108.57(16) . . ? V3A' OB2' V3B' 96.49(13) . . ? V2A OC3' V3B' 114.86(17) . . ? V3B' OC4' V2B 116.34(17) . . ? V1A' OB1' V3B' 109.42(16) . . ? V1A' OB1' V3A' 109.12(15) . . ? V3B' OB1' V3A' 103.37(14) . . ? V3A' OC1' V2A' 116.97(18) . . ? V3B OC4 V2B' 112.23(15) . . ? V1A OB1 V3B 105.08(13) . . ? V1A OB1 V3A 105.30(13) . . ? V3B OB1 V3A 94.71(12) . . ? V3A OC1 V2A 111.58(15) . . ? V3A OC2 V2B 115.98(19) . . ? V3B OB2 V3A 108.22(14) . . ? V3B OB2 V1A' 106.78(16) . . ? V3A OB2 V1A' 107.48(15) . . ? V3B OC3 V2A' 115.75(18) . . ? V1A OA1' V1A' 102.60(14) . . ? V1A OA1' V3B 102.31(13) . . ? V1A' OA1' V3B 91.48(12) . . ? V1A OA1' V2B' 88.28(11) . . ? V1A' OA1' V2B' 167.56(16) . . ? V3B OA1' V2B' 92.07(11) . . ? V1A OA1' V3A' 90.85(12) . . ? V1A' OA1' V3A' 90.83(11) . . ? V3B OA1' V3A' 165.79(15) . . ? V2B' OA1' V3A' 82.90(11) . . ? V1A OA1' V2A' 168.47(17) . . ? V1A' OA1' V2A' 86.83(11) . . ? V3B OA1' V2A' 83.84(10) . . ? V2B' OA1' V2A' 81.70(11) . . ? V3A' OA1' V2A' 82.30(10) . . ? V1A OA1 V1A' 101.13(13) . . ? V1A OA1 V3A 102.52(12) . . ? V1A' OA1 V3A 90.96(11) . . ? V1A OA1 V2A 89.33(11) . . ? V1A' OA1 V2A 167.76(15) . . ? V3A OA1 V2A 92.95(12) . . ? V1A OA1 V3B' 91.18(12) . . ? V1A' OA1 V3B' 89.62(11) . . ? V3A OA1 V3B' 165.91(15) . . ? V2A OA1 V3B' 83.79(10) . . ? V1A OA1 V2B 170.16(15) . . ? V1A' OA1 V2B 86.26(10) . . ? V3A OA1 V2B 83.67(11) . . ? V2A OA1 V2B 82.66(10) . . ? V3B' OA1 V2B 82.32(10) . . ? C7 N1 C3 108.3(5) . . ? C7 N1 C1 111.5(5) . . ? C3 N1 C1 112.9(5) . . ? C7 N1 C5 111.1(6) . . ? C3 N1 C5 106.2(5) . . ? C1 N1 C5 106.7(5) . . ? C2 C1 N1 115.1(6) . . ? C4 C3 N1 117.3(7) . . ? C6 C5 N1 116.9(7) . . ? N1 C7 C8 116.3(7) . . ? C11B N2 C11B 84(3) 2_556 . ? C11B N2 C11A 64.7(14) 2_556 . ? C11B N2 C11A 38.7(15) . . ? C11B N2 C11A 38.7(15) 2_556 2_556 ? C11B N2 C11A 64.7(14) . 2_556 ? C11A N2 C11A 71.7(15) . 2_556 ? C11B N2 C13A 76(2) 2_556 2_556 ? C11B N2 C13A 75(2) . 2_556 ? C11A N2 C13A 40(2) . 2_556 ? C11A N2 C13A 103(2) 2_556 2_556 ? C11B N2 C13A 75(2) 2_556 . ? C11B N2 C13A 76(2) . . ? C11A N2 C13A 103(2) . . ? C11A N2 C13A 40(2) 2_556 . ? C13A N2 C13A 141(4) 2_556 . ? C11B N2 C9 150.7(16) 2_556 . ? C11B N2 C9 99.9(13) . . ? C11A N2 C9 100.3(10) . . ? C11A N2 C9 163.7(12) 2_556 . ? C13A N2 C9 77(2) 2_556 . ? C13A N2 C9 134(2) . . ? C11B N2 C9 99.9(13) 2_556 2_556 ? C11B N2 C9 150.7(16) . 2_556 ? C11A N2 C9 163.7(12) . 2_556 ? C11A N2 C9 100.3(10) 2_556 2_556 ? C13A N2 C9 134(2) 2_556 2_556 ? C13A N2 C9 77(2) . 2_556 ? C9 N2 C9 90.9(14) . 2_556 ? C11B N2 C13B 98.6(17) 2_556 . ? C11B N2 C13B 99.6(18) . . ? C11A N2 C13B 133.3(16) . . ? C11A N2 C13B 70.1(15) 2_556 . ? C13A N2 C13B 173(3) 2_556 . ? C13A N2 C13B 31.7(17) . . ? C9 N2 C13B 109.2(15) . . ? C9 N2 C13B 51.2(12) 2_556 . ? C11B N2 C13B 99.6(18) 2_556 2_556 ? C11B N2 C13B 98.6(17) . 2_556 ? C11A N2 C13B 70.1(15) . 2_556 ? C11A N2 C13B 133.3(16) 2_556 2_556 ? C13A N2 C13B 31.7(17) 2_556 2_556 ? C13A N2 C13B 173(3) . 2_556 ? C9 N2 C13B 51.2(12) . 2_556 ? C9 N2 C13B 109.2(15) 2_556 2_556 ? C13B N2 C13B 155(3) . 2_556 ? C11B N2 C15A 157(2) 2_556 2_556 ? C11B N2 C15A 76(2) . 2_556 ? C11A N2 C15A 104.0(18) . 2_556 ? C11A N2 C15A 119.7(18) 2_556 2_556 ? C13A N2 C15A 109.2(15) 2_556 2_556 ? C13A N2 C15A 88.4(18) . 2_556 ? C9 N2 C15A 47.3(15) . 2_556 ? C9 N2 C15A 92.3(16) 2_556 2_556 ? C13B N2 C15A 73.7(13) . 2_556 ? C13B N2 C15A 95.0(14) 2_556 2_556 ? C11B N2 C15A 76(2) 2_556 . ? C11B N2 C15A 157(2) . . ? C11A N2 C15A 119.7(18) . . ? C11A N2 C15A 104.0(18) 2_556 . ? C13A N2 C15A 88.4(18) 2_556 . ? C13A N2 C15A 109.2(15) . . ? C9 N2 C15A 92.3(16) . . ? C9 N2 C15A 47.3(15) 2_556 . ? C13B N2 C15A 95.0(14) . . ? C13B N2 C15A 73.7(13) 2_556 . ? C15A N2 C15A 126(4) 2_556 . ? N2 C9 C10 104.4(16) . . ? N2 C11A C12A 108.8(16) . . ? N2 C11B C12B 121(3) . . ? N2 C13A C14A 113(2) . . ? N2 C13B C14B 111(2) . . ? C16 C15A N2 110.2(15) . . ? C16 C15B N2 107(2) . . ? C15B C16 C15A 29.7(14) . . ? C17 N3 C17 169.8(18) 2 . ? C17 N3 C21 117.2(14) 2 2 ? C17 N3 C21 63.0(14) . 2 ? C17 N3 C21 63.0(14) 2 . ? C17 N3 C21 117.2(14) . . ? C21 N3 C21 178(3) 2 . ? C17 N3 C23 108.9(11) 2 2 ? C17 N3 C23 78.2(11) . 2 ? C21 N3 C23 119.1(16) 2 2 ? C21 N3 C23 59.5(12) . 2 ? C17 N3 C23 78.2(11) 2 . ? C17 N3 C23 108.9(11) . . ? C21 N3 C23 59.5(12) 2 . ? C21 N3 C23 119.1(16) . . ? C23 N3 C23 96.2(15) 2 . ? C17 N3 C19 61.4(12) 2 . ? C17 N3 C19 109.2(15) . . ? C21 N3 C19 83.2(16) 2 . ? C21 N3 C19 98.4(17) . . ? C23 N3 C19 156.7(13) 2 . ? C23 N3 C19 101.8(12) . . ? C17 N3 C19 109.2(15) 2 2 ? C17 N3 C19 61.4(12) . 2 ? C21 N3 C19 98.4(17) 2 2 ? C21 N3 C19 83.2(16) . 2 ? C23 N3 C19 101.8(12) 2 2 ? C23 N3 C19 156.7(13) . 2 ? C19 N3 C19 65.5(19) . 2 ? N3 C17 C18 120.8(17) . . ? N3 C19 C20 116.3(17) . . ? N3 C21 C22 101(3) . . ? C24 C23 N3 118.0(17) . . ? C23 C24 C24 95.2(14) . 2 ? C27A N4 C31A 105.3(10) . . ? C27A N4 C31B 141.8(12) . . ? C31A N4 C31B 36.7(10) . . ? C27A N4 C29A 108.5(8) . . ? C31A N4 C29A 114.7(9) . . ? C31B N4 C29A 96.3(12) . . ? C27A N4 C25B 88.8(12) . . ? C31A N4 C25B 162.9(13) . . ? C31B N4 C25B 128.0(14) . . ? C29A N4 C25B 68.1(11) . . ? C27A N4 C25A 114.5(7) . . ? C31A N4 C25A 109.4(9) . . ? C31B N4 C25A 85.3(10) . . ? C29A N4 C25A 104.6(7) . . ? C25B N4 C25A 54.9(10) . . ? C27A N4 C29B 67.1(11) . . ? C31A N4 C29B 87.7(14) . . ? C31B N4 C29B 105.0(15) . . ? C29A N4 C29B 58.7(11) . . ? C25B N4 C29B 106.9(15) . . ? C25A N4 C29B 160.7(12) . . ? C27A N4 C27B 46.5(9) . . ? C31A N4 C27B 71.7(10) . . ? C31B N4 C27B 101.5(14) . . ? C29A N4 C27B 153.1(10) . . ? C25B N4 C27B 114.0(14) . . ? C25A N4 C27B 96.9(10) . . ? C29B N4 C27B 96.8(14) . . ? C26 C25A N4 116.4(7) . . ? N4 C27A C28A 114.3(12) . . ? C30 C29A N4 116.7(11) . . ? C32A C31A N4 121.8(16) . . ? C26 C25B N4 119.5(17) . . ? C28B C27B N4 108.7(17) . . ? C30 C29B N4 115(2) . . ? N4 C31B C32B 113(3) . . ? C25B C26 C25A 60.1(9) . . ? C29B C30 C29A 64.8(14) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.112 _refine_diff_density_min -0.892 _refine_diff_density_rms 0.261 #==END data_TPAc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Bis(tetra-n-propylammonium) tetrahydrogendecavanadate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H60 N2 O28 V10' _chemical_formula_weight 1334.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_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 8.55680(10) _cell_length_b 13.1873(2) _cell_length_c 20.1901(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.6530(10) _cell_angle_gamma 90.00 _cell_volume 2275.83(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 4769 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 28.29 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.947 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997b)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'UltraX18 Rigaku Denki rotating Mo anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD SMART Area Detector System' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 135 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 16898 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.34 _reflns_number_total 5664 _reflns_number_gt 3395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART program' _computing_cell_refinement 'Siemens SAINT program' _computing_data_reduction 'Siemens SAINT program' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997a)' _refine_special_details ; H atoms attached to surface O atoms of decavanadate frameworks, H1 and H2, were found from difference Fourier syntheses and their positional and isotropic displacement parameters were refined. H atoms in the [(C~3~H~7~)~4~N]^+^ cations were included in ideal positions and refined with the riding model. The 1,3-distance between C4 and C7B was restrained to 2.50\%A with estimated standard deviation 0.02. ; _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^)+(0.0559P)^2^+0.2174P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5664 _refine_ls_number_parameters 284 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.985 _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 V2B V 0.51179(9) 0.42811(6) 0.66340(3) 0.03323(19) Uani 1 1 d . . . V1A V 0.43710(7) 0.41313(5) 0.44679(3) 0.02372(16) Uani 1 1 d . . . V2A V 0.37122(8) 0.27239(5) 0.56401(4) 0.03101(18) Uani 1 1 d . . . V3A V 0.23299(8) 0.50153(5) 0.57093(3) 0.02596(17) Uani 1 1 d . . . V3B V 0.29427(8) 0.64941(5) 0.45146(3) 0.02878(18) Uani 1 1 d . . . OG2 O 0.5370(4) 0.4338(3) 0.74149(14) 0.0494(9) Uani 1 1 d . . . OG1 O 0.2930(4) 0.1641(2) 0.56665(16) 0.0451(8) Uani 1 1 d . . . OF1 O 0.0575(3) 0.5438(2) 0.57392(14) 0.0347(7) Uani 1 1 d . . . OF2 O 0.1208(3) 0.6930(2) 0.45603(15) 0.0405(7) Uani 1 1 d . . . OE2 O 0.5805(3) 0.5671(2) 0.63541(13) 0.0319(7) Uani 1 1 d . . . OE1 O 0.3599(3) 0.30013(19) 0.46185(13) 0.0299(6) Uani 1 1 d . . . OD1 O 0.4122(3) 0.3055(2) 0.64851(14) 0.0357(7) Uani 1 1 d . . . OC2 O 0.3025(3) 0.4932(2) 0.65107(13) 0.0339(7) Uani 1 1 d . . . OC1 O 0.1857(4) 0.3593(2) 0.56053(16) 0.0312(7) Uani 1 1 d . . . OB2 O 0.3486(3) 0.62033(19) 0.54592(13) 0.0264(6) Uani 1 1 d . . . OB1 O 0.2426(3) 0.4965(2) 0.46486(13) 0.0253(6) Uani 1 1 d . . . OC3 O 0.4197(3) 0.7557(2) 0.45057(14) 0.0343(7) Uani 1 1 d . . . OC4 O 0.3049(3) 0.6200(2) 0.36305(13) 0.0338(7) Uani 1 1 d . . . OA1 O 0.4669(3) 0.43613(19) 0.54719(12) 0.0246(6) Uani 1 1 d . . . H2 H 0.168(5) 0.476(3) 0.449(2) 0.032(13) Uiso 1 1 d . . . H1 H 0.113(6) 0.343(4) 0.556(3) 0.06(2) Uiso 1 1 d . . . N1 N -0.0132(6) 0.5816(3) 0.1889(2) 0.0592(12) Uani 1 1 d . . . C1 C 0.0359(8) 0.6815(5) 0.2226(3) 0.0749(18) Uani 1 1 d . A . H1A H 0.1430 0.6745 0.2399 0.090 Uiso 1 1 calc R . . H1B H 0.0347 0.7343 0.1891 0.090 Uiso 1 1 calc R . . C2 C -0.0617(9) 0.7160(5) 0.2777(3) 0.086(2) Uani 1 1 d . . . H2A H -0.0560 0.6663 0.3131 0.103 Uiso 1 1 calc R A . H2B H -0.1700 0.7213 0.2616 0.103 Uiso 1 1 calc R . . C3 C -0.0063(10) 0.8179(5) 0.3043(4) 0.104(3) Uani 1 1 d . A . H3A H -0.0710 0.8386 0.3395 0.155 Uiso 1 1 calc R . . H3B H -0.0131 0.8673 0.2693 0.155 Uiso 1 1 calc R . . H3C H 0.1003 0.8123 0.3209 0.155 Uiso 1 1 calc R . . C4 C -0.1861(9) 0.5841(5) 0.1641(3) 0.081(2) Uani 1 1 d D A . H4A H -0.2095 0.5219 0.1399 0.098 Uiso 1 1 calc R . . H4B H -0.2510 0.5853 0.2022 0.098 Uiso 1 1 calc R . . C5 C -0.2289(11) 0.6693(6) 0.1218(4) 0.102(3) Uani 1 1 d . . . H5A H -0.1595 0.6728 0.0852 0.122 Uiso 1 1 calc R A . H5B H -0.2188 0.7319 0.1468 0.122 Uiso 1 1 calc R . . C6 C -0.4004(9) 0.6561(6) 0.0947(4) 0.099(2) Uani 1 1 d . A . H6A H -0.4287 0.7121 0.0662 0.148 Uiso 1 1 calc R . . H6B H -0.4688 0.6542 0.1311 0.148 Uiso 1 1 calc R . . H6C H -0.4099 0.5940 0.0701 0.148 Uiso 1 1 calc R . . C7A C 0.0270(12) 0.5086(7) 0.2466(5) 0.035(2) Uiso 0.497(10) 1 d P A 1 H7A1 H -0.0390 0.5234 0.2832 0.043 Uiso 0.497(10) 1 calc PR A 1 H7A2 H 0.1350 0.5187 0.2620 0.043 Uiso 0.497(10) 1 calc PR A 1 C8A C 0.0024(14) 0.3943(8) 0.2244(5) 0.051(3) Uiso 0.497(10) 1 d P A 1 H8A1 H -0.1064 0.3810 0.2117 0.062 Uiso 0.497(10) 1 calc PR A 1 H8A2 H 0.0666 0.3776 0.1875 0.062 Uiso 0.497(10) 1 calc PR A 1 C7B C -0.0333(17) 0.4766(11) 0.2276(7) 0.082(4) Uiso 0.503(10) 1 d PD A 2 H7B1 H -0.1168 0.4841 0.2581 0.098 Uiso 0.503(10) 1 calc PR A 2 H7B2 H -0.0647 0.4246 0.1958 0.098 Uiso 0.503(10) 1 calc PR A 2 C8B C 0.095(2) 0.4458(13) 0.2614(8) 0.104(6) Uiso 0.503(10) 1 d P A 2 H8B1 H 0.1198 0.4909 0.2983 0.125 Uiso 0.503(10) 1 calc PR A 2 H8B2 H 0.1834 0.4439 0.2330 0.125 Uiso 0.503(10) 1 calc PR A 2 C9 C 0.0547(8) 0.3334(5) 0.2876(3) 0.0773(19) Uiso 1 1 d . . . H9A H 0.0444 0.2621 0.2788 0.116 Uiso 0.497(10) 1 calc PR A 1 H9B H -0.0098 0.3517 0.3233 0.116 Uiso 0.497(10) 1 calc PR A 1 H9C H 0.1620 0.3489 0.2996 0.116 Uiso 0.497(10) 1 calc PR A 1 H9D H 0.1431 0.3070 0.3130 0.116 Uiso 0.503(10) 1 calc PR A 2 H9E H 0.0311 0.2898 0.2504 0.116 Uiso 0.503(10) 1 calc PR A 2 H9F H -0.0340 0.3367 0.3149 0.116 Uiso 0.503(10) 1 calc PR A 2 C10A C 0.1241(13) 0.5783(8) 0.1438(5) 0.042(3) Uiso 0.503(10) 1 d P A 1 H10A H 0.2203 0.5687 0.1703 0.050 Uiso 0.503(10) 1 calc PR A 1 H10B H 0.1313 0.6425 0.1206 0.050 Uiso 0.503(10) 1 calc PR A 1 C11A C 0.1053(15) 0.4920(9) 0.0930(6) 0.065(4) Uiso 0.503(10) 1 d P A 1 H11A H 0.0216 0.5069 0.0604 0.078 Uiso 0.503(10) 1 calc PR A 1 H11B H 0.0823 0.4285 0.1147 0.078 Uiso 0.503(10) 1 calc PR A 1 C10B C 0.0573(17) 0.5538(11) 0.1225(6) 0.066(4) Uiso 0.497(10) 1 d P A 2 H10C H 0.0098 0.4916 0.1057 0.079 Uiso 0.497(10) 1 calc PR A 2 H10D H 0.0337 0.6071 0.0905 0.079 Uiso 0.497(10) 1 calc PR A 2 C11B C 0.228(2) 0.5402(12) 0.1299(7) 0.092(5) Uiso 0.497(10) 1 d P A 2 H11C H 0.2567 0.4969 0.1673 0.111 Uiso 0.497(10) 1 calc PR A 2 H11D H 0.2814 0.6048 0.1353 0.111 Uiso 0.497(10) 1 calc PR A 2 C12 C 0.2677(9) 0.4859(5) 0.0591(3) 0.088(2) Uiso 1 1 d . . . H12A H 0.2642 0.4327 0.0266 0.132 Uiso 0.497(10) 1 calc PR A 1 H12B H 0.3490 0.4719 0.0922 0.132 Uiso 0.497(10) 1 calc PR A 1 H12C H 0.2885 0.5494 0.0380 0.132 Uiso 0.497(10) 1 calc PR A 1 H12D H 0.3779 0.4728 0.0584 0.132 Uiso 0.503(10) 1 calc PR A 2 H12E H 0.2369 0.5301 0.0231 0.132 Uiso 0.503(10) 1 calc PR A 2 H12F H 0.2112 0.4232 0.0547 0.132 Uiso 0.503(10) 1 calc PR A 2 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 V2B 0.0283(4) 0.0430(4) 0.0281(4) 0.0042(3) -0.0022(3) -0.0037(3) V1A 0.0174(3) 0.0245(4) 0.0291(4) -0.0043(3) -0.0003(3) -0.0005(3) V2A 0.0215(4) 0.0263(4) 0.0451(4) 0.0056(3) -0.0002(3) -0.0028(3) V3A 0.0172(3) 0.0298(4) 0.0311(4) -0.0028(3) 0.0030(3) -0.0006(3) V3B 0.0174(4) 0.0263(4) 0.0424(4) 0.0045(3) -0.0014(3) 0.0015(3) OG2 0.048(2) 0.069(2) 0.0304(17) 0.0055(15) -0.0065(15) -0.0073(17) OG1 0.0365(19) 0.0312(17) 0.067(2) 0.0074(15) 0.0019(16) -0.0092(14) OF1 0.0208(16) 0.0381(17) 0.0454(17) -0.0079(13) 0.0038(13) 0.0015(13) OF2 0.0232(17) 0.0345(17) 0.064(2) 0.0053(15) -0.0014(14) 0.0040(13) OE2 0.0280(16) 0.0382(17) 0.0291(15) -0.0055(12) -0.0018(12) -0.0028(12) OE1 0.0252(16) 0.0225(14) 0.0418(16) -0.0039(12) 0.0007(12) -0.0027(11) OD1 0.0271(16) 0.0389(17) 0.0411(17) 0.0096(13) 0.0014(13) -0.0044(13) OC2 0.0258(16) 0.0436(18) 0.0328(15) -0.0028(13) 0.0054(12) -0.0023(13) OC1 0.0173(16) 0.0299(16) 0.0465(19) 0.0030(13) 0.0016(14) -0.0013(13) OB2 0.0174(14) 0.0241(14) 0.0377(15) -0.0050(11) 0.0016(11) 0.0002(11) OB1 0.0147(14) 0.0271(15) 0.0337(16) -0.0011(12) -0.0024(12) -0.0025(12) OC3 0.0246(16) 0.0251(15) 0.0527(18) 0.0062(13) -0.0017(13) 0.0030(11) OC4 0.0233(16) 0.0390(17) 0.0385(16) 0.0076(13) -0.0056(12) -0.0025(12) OA1 0.0173(14) 0.0261(14) 0.0304(14) -0.0012(11) 0.0004(11) 0.0008(10) N1 0.065(3) 0.052(3) 0.062(3) 0.004(2) 0.021(2) 0.007(2) C1 0.059(4) 0.072(4) 0.094(5) -0.002(4) 0.007(4) 0.005(3) C2 0.098(6) 0.087(5) 0.074(4) -0.001(4) 0.021(4) 0.013(4) C3 0.136(8) 0.070(5) 0.105(6) -0.022(4) 0.008(5) -0.013(5) C4 0.114(7) 0.053(4) 0.079(4) -0.007(3) 0.020(4) -0.010(4) C5 0.141(8) 0.086(6) 0.077(5) 0.010(4) -0.002(5) 0.003(5) C6 0.095(6) 0.119(6) 0.081(5) -0.013(4) -0.012(4) 0.013(5) _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 OB1 H2 0.75(4) . ? H2 OF1 1.98(5) 2_566 ? OB1 OF1 2.702(4) 2_566 ? OC1 H1 0.66(5) . ? H1 OF2 2.06(5) 2_566 ? OC1 OF2 2.717(4) 2_566 ? V2B OG2 1.583(3) . ? V2B OC4 1.796(3) 3_666 ? V2B OD1 1.846(3) . ? V2B OC2 1.991(3) . ? V2B OE2 2.014(3) . ? V2B OA1 2.362(3) . ? V2B V2A 3.0770(10) . ? V2B V3B 3.0876(10) 3_666 ? V2B V1A 3.1008(10) 3_666 ? V2B V3A 3.1149(10) . ? V1A OE1 1.664(3) . ? V1A OE2 1.680(3) 3_666 ? V1A OB2 1.885(3) 3_666 ? V1A OB1 2.042(3) . ? V1A OA1 2.054(2) . ? V1A OA1 2.152(3) 3_666 ? V1A V3A 3.0753(9) 3_666 ? V1A V2A 3.0801(10) . ? V1A V2B 3.1008(10) 3_666 ? V2A OG1 1.579(3) . ? V2A OD1 1.780(3) . ? V2A OC3 1.863(3) 3_666 ? V2A OC1 1.957(3) . ? V2A OE1 2.093(3) . ? V2A OA1 2.340(3) . ? V2A V3B 3.0720(10) 3_666 ? V3A OF1 1.606(3) . ? V3A OC2 1.701(3) . ? V3A OC1 1.928(3) . ? V3A OB2 1.933(3) . ? V3A OB1 2.148(3) . ? V3A OA1 2.251(3) . ? V3A V1A 3.0752(9) 3_666 ? V3B OF2 1.598(3) . ? V3B OC3 1.766(3) . ? V3B OC4 1.833(3) . ? V3B OB2 1.980(3) . ? V3B OB1 2.085(3) . ? V3B OA1 2.333(3) 3_666 ? V3B V2A 3.0720(10) 3_666 ? V3B V2B 3.0876(10) 3_666 ? OE2 V1A 1.680(3) 3_666 ? OB2 V1A 1.885(3) 3_666 ? OC3 V2A 1.863(3) 3_666 ? OC4 V2B 1.796(3) 3_666 ? OA1 V1A 2.152(3) 3_666 ? OA1 V3B 2.333(3) 3_666 ? N1 C10A 1.521(11) . ? N1 C7A 1.538(10) . ? N1 C1 1.532(7) . ? N1 C4 1.541(8) . ? N1 C10B 1.540(13) . ? N1 C7B 1.603(14) . ? C1 C2 1.491(8) . ? C2 C3 1.514(9) . ? C4 C5 1.448(8) . ? C5 C6 1.552(10) . ? C7A C8A 1.585(15) . ? C8A C9 1.556(11) . ? C7B C8B 1.33(2) . ? C8B C9 1.616(17) . ? C10A C11A 1.536(16) . ? C11A C12 1.578(14) . ? C10B C11B 1.47(2) . ? C11B C12 1.648(15) . ? 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 OF1 OB1 H2 14(3) 2_566 . ? OF2 OC1 H1 5(5) 2_566 . ? V1A OB1 H2 114(3) . . ? V3A OB1 H2 111(3) . . ? V3B OB1 H2 118(3) . . ? V2A OC1 H1 125(5) . . ? V3A OC1 H1 122(5) . . ? OG2 V2B OC4 103.42(16) . 3_666 ? OG2 V2B OD1 104.13(16) . . ? OC4 V2B OD1 92.58(13) 3_666 . ? OG2 V2B OC2 100.64(15) . . ? OC4 V2B OC2 155.21(12) 3_666 . ? OD1 V2B OC2 87.24(13) . . ? OG2 V2B OE2 102.04(15) . . ? OC4 V2B OE2 88.14(13) 3_666 . ? OD1 V2B OE2 152.89(12) . . ? OC2 V2B OE2 81.07(12) . . ? OG2 V2B OA1 174.52(15) . . ? OC4 V2B OA1 79.89(11) 3_666 . ? OD1 V2B OA1 79.91(11) . . ? OC2 V2B OA1 75.67(10) . . ? OE2 V2B OA1 73.53(10) . . ? OG2 V2B V2A 135.41(13) . . ? OC4 V2B V2A 83.73(9) 3_666 . ? OD1 V2B V2A 31.30(9) . . ? OC2 V2B V2A 83.35(8) . . ? OE2 V2B V2A 122.33(8) . . ? OA1 V2B V2A 48.81(6) . . ? OG2 V2B V3B 135.26(13) . 3_666 ? OC4 V2B V3B 32.06(9) 3_666 3_666 ? OD1 V2B V3B 81.24(9) . 3_666 ? OC2 V2B V3B 124.08(8) . 3_666 ? OE2 V2B V3B 85.21(8) . 3_666 ? OA1 V2B V3B 48.48(6) . 3_666 ? V2A V2B V3B 59.78(2) . 3_666 ? OG2 V2B V1A 131.72(13) . 3_666 ? OC4 V2B V1A 82.58(9) 3_666 3_666 ? OD1 V2B V1A 123.64(9) . 3_666 ? OC2 V2B V1A 76.99(8) . 3_666 ? OE2 V2B V1A 29.70(7) . 3_666 ? OA1 V2B V1A 43.86(6) . 3_666 ? V2A V2B V1A 92.67(2) . 3_666 ? V3B V2B V1A 65.55(2) 3_666 3_666 ? OG2 V2B V3A 130.37(13) . . ? OC4 V2B V3A 125.92(9) 3_666 . ? OD1 V2B V3A 80.78(9) . . ? OC2 V2B V3A 29.73(8) . . ? OE2 V2B V3A 76.95(8) . . ? OA1 V2B V3A 46.05(6) . . ? V2A V2B V3A 63.32(2) . . ? V3B V2B V3A 94.36(2) 3_666 . ? V1A V2B V3A 59.31(2) 3_666 . ? OE1 V1A OE2 107.55(13) . 3_666 ? OE1 V1A OB2 99.74(13) . 3_666 ? OE2 V1A OB2 98.97(13) 3_666 3_666 ? OE1 V1A OB1 96.63(13) . . ? OE2 V1A OB1 93.23(13) 3_666 . ? OB2 V1A OB1 155.54(12) 3_666 . ? OE1 V1A OA1 89.10(12) . . ? OE2 V1A OA1 162.45(12) 3_666 . ? OB2 V1A OA1 83.20(11) 3_666 . ? OB1 V1A OA1 79.00(11) . . ? OE1 V1A OA1 166.10(12) . 3_666 ? OE2 V1A OA1 85.91(12) 3_666 3_666 ? OB2 V1A OA1 81.06(10) 3_666 3_666 ? OB1 V1A OA1 78.75(11) . 3_666 ? OA1 V1A OA1 77.19(11) . 3_666 ? OE1 V1A V3A 136.35(10) . 3_666 ? OE2 V1A V3A 82.47(10) 3_666 3_666 ? OB2 V1A V3A 36.87(8) 3_666 3_666 ? OB1 V1A V3A 125.75(9) . 3_666 ? OA1 V1A V3A 89.31(7) . 3_666 ? OA1 V1A V3A 47.04(7) 3_666 3_666 ? OE1 V1A V2A 39.79(9) . . ? OE2 V1A V2A 147.30(10) 3_666 . ? OB2 V1A V2A 90.63(8) 3_666 . ? OB1 V1A V2A 90.42(8) . . ? OA1 V1A V2A 49.42(7) . . ? OA1 V1A V2A 126.59(7) 3_666 . ? V3A V1A V2A 120.77(3) 3_666 . ? OE1 V1A V2B 143.73(10) . 3_666 ? OE2 V1A V2B 36.43(10) 3_666 3_666 ? OB2 V1A V2B 92.59(8) 3_666 3_666 ? OB1 V1A V2B 84.72(8) . 3_666 ? OA1 V1A V2B 126.39(8) . 3_666 ? OA1 V1A V2B 49.51(7) 3_666 3_666 ? V3A V1A V2B 60.57(2) 3_666 3_666 ? V2A V1A V2B 174.32(3) . 3_666 ? OG1 V2A OD1 104.74(15) . . ? OG1 V2A OC3 103.74(15) . 3_666 ? OD1 V2A OC3 92.97(13) . 3_666 ? OG1 V2A OC1 100.72(15) . . ? OD1 V2A OC1 90.83(14) . . ? OC3 V2A OC1 153.37(13) 3_666 . ? OG1 V2A OE1 101.01(14) . . ? OD1 V2A OE1 154.14(12) . . ? OC3 V2A OE1 83.12(12) 3_666 . ? OC1 V2A OE1 82.05(12) . . ? OG1 V2A OA1 172.42(14) . . ? OD1 V2A OA1 81.84(11) . . ? OC3 V2A OA1 79.36(10) 3_666 . ? OC1 V2A OA1 75.11(11) . . ? OE1 V2A OA1 72.32(9) . . ? OG1 V2A V3B 134.89(12) . 3_666 ? OD1 V2A V3B 82.63(9) . 3_666 ? OC3 V2A V3B 31.22(8) 3_666 3_666 ? OC1 V2A V3B 123.92(10) . 3_666 ? OE1 V2A V3B 80.91(8) . 3_666 ? OA1 V2A V3B 48.81(6) . 3_666 ? OG1 V2A V2B 137.31(12) . . ? OD1 V2A V2B 32.60(9) . . ? OC3 V2A V2B 83.48(9) 3_666 . ? OC1 V2A V2B 85.67(10) . . ? OE1 V2A V2B 121.67(8) . . ? OA1 V2A V2B 49.45(6) . . ? V3B V2A V2B 60.28(2) 3_666 . ? OG1 V2A V1A 131.59(12) . . ? OD1 V2A V1A 123.62(9) . . ? OC3 V2A V1A 77.71(9) 3_666 . ? OC1 V2A V1A 78.26(9) . . ? OE1 V2A V1A 30.58(7) . . ? OA1 V2A V1A 41.81(6) . . ? V3B V2A V1A 60.99(2) 3_666 . ? V2B V2A V1A 91.09(3) . . ? OF1 V3A OC2 105.84(14) . . ? OF1 V3A OC1 98.63(14) . . ? OC2 V3A OC1 95.93(14) . . ? OF1 V3A OB2 102.66(13) . . ? OC2 V3A OB2 98.04(13) . . ? OC1 V3A OB2 150.18(13) . . ? OF1 V3A OB1 97.31(13) . . ? OC2 V3A OB1 156.69(13) . . ? OC1 V3A OB1 83.03(12) . . ? OB2 V3A OB1 73.81(11) . . ? OF1 V3A OA1 169.52(12) . . ? OC2 V3A OA1 84.41(12) . . ? OC1 V3A OA1 77.78(11) . . ? OB2 V3A OA1 77.52(10) . . ? OB1 V3A OA1 72.58(10) . . ? OF1 V3A V1A 137.93(11) . 3_666 ? OC2 V3A V1A 81.48(10) . 3_666 ? OC1 V3A V1A 122.17(10) . 3_666 ? OB2 V3A V1A 35.81(8) . 3_666 ? OB1 V3A V1A 79.50(8) . 3_666 ? OA1 V3A V1A 44.40(7) . 3_666 ? OF1 V3A V2B 140.99(11) . . ? OC2 V3A V2B 35.47(10) . . ? OC1 V3A V2B 85.06(10) . . ? OB2 V3A V2B 91.23(8) . . ? OB1 V3A V2B 121.63(8) . . ? OA1 V3A V2B 49.06(6) . . ? V1A V3A V2B 60.12(2) 3_666 . ? OF2 V3B OC3 106.36(14) . . ? OF2 V3B OC4 102.74(14) . . ? OC3 V3B OC4 95.76(13) . . ? OF2 V3B OB2 101.04(14) . . ? OC3 V3B OB2 92.74(12) . . ? OC4 V3B OB2 151.30(12) . . ? OF2 V3B OB1 97.89(14) . . ? OC3 V3B OB1 154.38(12) . . ? OC4 V3B OB1 86.67(12) . . ? OB2 V3B OB1 74.30(11) . . ? OF2 V3B OA1 171.25(13) . 3_666 ? OC3 V3B OA1 81.45(11) . 3_666 ? OC4 V3B OA1 79.98(11) . 3_666 ? OB2 V3B OA1 74.25(10) . 3_666 ? OB1 V3B OA1 73.85(10) . 3_666 ? OF2 V3B V2A 139.22(11) . 3_666 ? OC3 V3B V2A 33.16(9) . 3_666 ? OC4 V3B V2A 83.31(9) . 3_666 ? OB2 V3B V2A 89.11(8) . 3_666 ? OB1 V3B V2A 122.83(8) . 3_666 ? OA1 V3B V2A 48.99(6) 3_666 3_666 ? OF2 V3B V2B 134.05(12) . 3_666 ? OC3 V3B V2B 84.66(10) . 3_666 ? OC4 V3B V2B 31.33(9) . 3_666 ? OB2 V3B V2B 123.30(8) . 3_666 ? OB1 V3B V2B 84.37(8) . 3_666 ? OA1 V3B V2B 49.29(6) 3_666 3_666 ? V2A V3B V2B 59.94(2) 3_666 3_666 ? V1A OE2 V2B 113.88(14) 3_666 . ? V1A OE1 V2A 109.63(13) . . ? V2A OD1 V2B 116.10(15) . . ? V3A OC2 V2B 114.80(15) . . ? V3A OC1 V2A 113.58(16) . . ? V1A OB2 V3A 107.32(12) 3_666 . ? V1A OB2 V3B 107.75(13) 3_666 . ? V3A OB2 V3B 107.96(12) . . ? V1A OB1 V3B 108.53(13) . . ? V1A OB1 V3A 105.30(12) . . ? V3B OB1 V3A 96.74(12) . . ? V3B OC3 V2A 115.63(14) . 3_666 ? V2B OC4 V3B 116.61(14) 3_666 . ? V1A OA1 V1A 102.81(11) . 3_666 ? V1A OA1 V3A 101.28(10) . . ? V1A OA1 V3A 88.56(9) 3_666 . ? V1A OA1 V3B 90.50(10) . 3_666 ? V1A OA1 V3B 96.55(10) 3_666 3_666 ? V3A OA1 V3B 165.82(13) . 3_666 ? V1A OA1 V2A 88.77(9) . . ? V1A OA1 V2A 168.37(13) 3_666 . ? V3A OA1 V2A 90.12(9) . . ? V3B OA1 V2A 82.20(8) 3_666 . ? V1A OA1 V2B 168.73(13) . . ? V1A OA1 V2B 86.63(9) 3_666 . ? V3A OA1 V2B 84.89(9) . . ? V3B OA1 V2B 82.23(8) 3_666 . ? V2A OA1 V2B 81.75(8) . . ? C10A N1 C7A 106.5(6) . . ? C10A N1 C1 95.0(6) . . ? C7A N1 C1 98.9(5) . . ? C10A N1 C4 124.2(6) . . ? C7A N1 C4 116.0(5) . . ? C1 N1 C4 111.5(4) . . ? C10A N1 C10B 29.1(5) . . ? C7A N1 C10B 115.3(7) . . ? C1 N1 C10B 118.7(7) . . ? C4 N1 C10B 97.5(7) . . ? C10A N1 C7B 111.8(7) . . ? C7A N1 C7B 27.8(5) . . ? C1 N1 C7B 124.0(7) . . ? C4 N1 C7B 93.1(6) . . ? C10B N1 C7B 105.9(8) . . ? C2 C1 N1 116.2(6) . . ? C1 C2 C3 111.0(6) . . ? C5 C4 N1 114.9(6) . . ? C4 C5 C6 109.3(7) . . ? N1 C7A C8A 111.0(7) . . ? C9 C8A C7A 103.2(7) . . ? C8B C7B N1 114.2(14) . . ? C7B C8B C9 105.4(14) . . ? C8A C9 C8B 46.9(6) . . ? N1 C10A C11A 111.2(9) . . ? C10A C11A C12 105.1(9) . . ? C11B C10B N1 111.6(11) . . ? C10B C11B C12 102.0(10) . . ? C11A C12 C11B 51.8(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag OB1 H2 OF1 2_666 0.75(4) 1.98(5) 2.702(4) 161(5) ? OC1 H1 OF2 2_666 0.66(5) 2.06(5) 2.717(4) 174(7) ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.543 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.105 #==END data_TPAv _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Tris(tetra-n-propylammonium) trihydrogendecavanadate ; _chemical_melting_point ? _chemical_formula_moiety '(C12 H28 N +)3, (H3 V10 O28 3-)' _chemical_formula_sum 'C36 H87 N3 O28 V10' _chemical_formula_weight 1519.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.3026(13) _cell_length_b 14.0097(13) _cell_length_c 21.9911(18) _cell_angle_alpha 90.00 _cell_angle_beta 110.996(5) _cell_angle_gamma 90.00 _cell_volume 5839.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 14.88 _cell_measurement_theta_max 14.96 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3112 _exptl_absorpt_coefficient_mu 1.605 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC 7R' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.20 _diffrn_reflns_number 13743 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.49 _reflns_number_total 13371 _reflns_number_gt 9478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control Software' _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_reduction 'teXsan PROCESS (Molecular Structure Corporation, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997a)' _refine_special_details ; H atoms attached to surface O atoms of decavanadate frameworks, H1, H2, and H3, were found from difference Fourier syntheses and their positional and isotropic displacement parameters were refined. H atoms in the [(C~3~H~7~)~4~N]^+^ cations were included in ideal positions and refined with the riding model. ; _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^)+(0.0573P)^2^+0.9482P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13371 _refine_ls_number_parameters 736 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V2B' V 0.60913(3) 0.45088(4) 0.74274(2) 0.02887(12) Uani 1 1 d . . . V1A V 0.65496(2) 0.58477(3) 0.65536(2) 0.02197(11) Uani 1 1 d . . . V2A V 0.70649(3) 0.70907(4) 0.56695(3) 0.03388(13) Uani 1 1 d . . . V2B V 0.79591(3) 0.54548(4) 0.54398(3) 0.03477(13) Uani 1 1 d . . . V1A' V 0.74706(2) 0.40988(3) 0.62998(2) 0.02391(11) Uani 1 1 d . . . V2A' V 0.69901(3) 0.28601(4) 0.72236(3) 0.03101(13) Uani 1 1 d . . . V3A' V 0.76794(3) 0.48188(4) 0.77278(2) 0.02858(12) Uani 1 1 d . . . V3B' V 0.81743(3) 0.60776(4) 0.68490(3) 0.03210(13) Uani 1 1 d . . . V3B V 0.58600(3) 0.37082(3) 0.59687(2) 0.02593(11) Uani 1 1 d . . . V3A V 0.63563(3) 0.50285(4) 0.50707(2) 0.02672(12) Uani 1 1 d . . . OG2' O 0.55657(12) 0.46812(16) 0.78054(11) 0.0381(5) Uani 1 1 d . . . OG1 O 0.68780(13) 0.81628(17) 0.54297(13) 0.0481(6) Uani 1 1 d . . . OG2 O 0.84589(13) 0.53067(19) 0.50303(12) 0.0496(7) Uani 1 1 d . . . OG1' O 0.71679(13) 0.17794(17) 0.74532(12) 0.0461(6) Uani 1 1 d . . . OF1' O 0.83375(12) 0.51538(17) 0.83415(10) 0.0415(6) Uani 1 1 d . . . OF2' O 0.88320(12) 0.64383(18) 0.74570(12) 0.0463(6) Uani 1 1 d . . . OF2 O 0.51857(11) 0.33866(16) 0.53475(11) 0.0395(5) Uani 1 1 d . . . OF1 O 0.56624(11) 0.47272(17) 0.44569(10) 0.0376(5) Uani 1 1 d . . . OE2' O 0.60047(10) 0.57911(14) 0.69752(9) 0.0258(4) Uani 1 1 d . . . OE1 O 0.64355(11) 0.69298(14) 0.61971(10) 0.0298(5) Uani 1 1 d . . . OD1 O 0.76267(12) 0.66653(17) 0.52358(11) 0.0394(5) Uani 1 1 d . . . OE2 O 0.79574(11) 0.41341(15) 0.58221(10) 0.0312(5) Uani 1 1 d . . . OE1' O 0.75255(11) 0.29905(14) 0.66103(10) 0.0300(5) Uani 1 1 d . . . OD1' O 0.63489(11) 0.32607(15) 0.75757(10) 0.0338(5) Uani 1 1 d . . . OC2' O 0.69358(11) 0.49426(15) 0.79999(9) 0.0317(5) Uani 1 1 d . . . OB2' O 0.74086(10) 0.60400(14) 0.72275(9) 0.0270(4) Uani 1 1 d . . . OC3' O 0.77900(12) 0.72000(15) 0.64355(11) 0.0373(5) Uani 1 1 d . . . OC4' O 0.85651(11) 0.57871(16) 0.62482(11) 0.0357(5) Uani 1 1 d . . . OB1' O 0.81163(10) 0.47127(14) 0.70460(9) 0.0271(4) Uani 1 1 d . . . OC1' O 0.77059(11) 0.35217(15) 0.78091(10) 0.0320(5) Uani 1 1 d . . . OC4 O 0.53874(12) 0.41127(17) 0.65597(11) 0.0300(5) Uani 1 1 d . . . OB1 O 0.58242(11) 0.51955(15) 0.57403(10) 0.0240(4) Uani 1 1 d . . . OC1 O 0.62682(12) 0.64109(16) 0.49926(11) 0.0315(5) Uani 1 1 d . . . OC2 O 0.70466(11) 0.49765(17) 0.48052(10) 0.0358(5) Uani 1 1 d . . . OB2 O 0.65614(10) 0.38749(14) 0.55747(9) 0.0259(4) Uani 1 1 d . . . OC3 O 0.61924(11) 0.26946(14) 0.63829(10) 0.0321(5) Uani 1 1 d . . . OA1' O 0.67512(10) 0.44030(13) 0.67678(9) 0.0234(4) Uani 1 1 d . . . OA1 O 0.71663(10) 0.55047(14) 0.60060(9) 0.0251(4) Uani 1 1 d . . . N1 N 0.66908(14) 0.12477(18) 0.47242(12) 0.0316(6) Uani 1 1 d . . . C1 C 0.60259(17) 0.1340(2) 0.41327(15) 0.0360(7) Uani 1 1 d . . . H1A H 0.5757 0.0756 0.4089 0.043 Uiso 1 1 calc R . . H1B H 0.6158 0.1390 0.3752 0.043 Uiso 1 1 calc R . . C2 C 0.5547(2) 0.2173(3) 0.41266(19) 0.0532(10) Uani 1 1 d . . . H2A H 0.5366 0.2106 0.4477 0.064 Uiso 1 1 calc R . . H2B H 0.5808 0.2767 0.4188 0.064 Uiso 1 1 calc R . . C3 C 0.4944(2) 0.2179(3) 0.3475(2) 0.0586(11) Uani 1 1 d . . . H3A H 0.4634 0.2703 0.3461 0.088 Uiso 1 1 calc R . . H3B H 0.4688 0.1590 0.3419 0.088 Uiso 1 1 calc R . . H3C H 0.5129 0.2249 0.3132 0.088 Uiso 1 1 calc R . . C4 C 0.71604(18) 0.2119(2) 0.47755(16) 0.0358(7) Uani 1 1 d . . . H4A H 0.6914 0.2681 0.4840 0.043 Uiso 1 1 calc R . . H4B H 0.7585 0.2048 0.5158 0.043 Uiso 1 1 calc R . . C5 C 0.7371(2) 0.2281(3) 0.41900(18) 0.0468(9) Uani 1 1 d . . . H5A H 0.6951 0.2366 0.3804 0.056 Uiso 1 1 calc R . . H5B H 0.7623 0.1727 0.4123 0.056 Uiso 1 1 calc R . . C6 C 0.7835(2) 0.3158(3) 0.4291(2) 0.0589(11) Uani 1 1 d . . . H6A H 0.7965 0.3252 0.3916 0.088 Uiso 1 1 calc R . . H6B H 0.8254 0.3069 0.4669 0.088 Uiso 1 1 calc R . . H6C H 0.7583 0.3706 0.4352 0.088 Uiso 1 1 calc R . . C7 C 0.70490(17) 0.0341(2) 0.46255(15) 0.0361(7) Uani 1 1 d . . . H7A H 0.6740 -0.0193 0.4612 0.043 Uiso 1 1 calc R . . H7B H 0.7098 0.0377 0.4203 0.043 Uiso 1 1 calc R . . C8 C 0.77630(19) 0.0130(3) 0.51292(17) 0.0446(9) Uani 1 1 d . . . H8A H 0.7718 0.0018 0.5548 0.053 Uiso 1 1 calc R . . H8B H 0.8073 0.0673 0.5172 0.053 Uiso 1 1 calc R . . C9 C 0.8078(2) -0.0747(3) 0.4929(2) 0.0569(11) Uani 1 1 d . . . H9A H 0.8533 -0.0878 0.5251 0.085 Uiso 1 1 calc R . . H9B H 0.8126 -0.0631 0.4516 0.085 Uiso 1 1 calc R . . H9C H 0.7773 -0.1285 0.4891 0.085 Uiso 1 1 calc R . . C10 C 0.65295(18) 0.1203(2) 0.53485(15) 0.0364(7) Uani 1 1 d . . . H10A H 0.6971 0.1138 0.5713 0.044 Uiso 1 1 calc R . . H10B H 0.6319 0.1805 0.5400 0.044 Uiso 1 1 calc R . . C11 C 0.6044(2) 0.0404(3) 0.53835(18) 0.0496(9) Uani 1 1 d . . . H11A H 0.5618 0.0422 0.4998 0.059 Uiso 1 1 calc R . . H11B H 0.6275 -0.0203 0.5388 0.059 Uiso 1 1 calc R . . C12 C 0.5850(3) 0.0481(3) 0.5980(2) 0.0658(13) Uani 1 1 d . . . H12A H 0.5544 -0.0038 0.5986 0.099 Uiso 1 1 calc R . . H12B H 0.5612 0.1075 0.5971 0.099 Uiso 1 1 calc R . . H12C H 0.6270 0.0454 0.6362 0.099 Uiso 1 1 calc R . . N2 N 0.71249(14) 0.64254(19) 0.31374(12) 0.0346(6) Uani 1 1 d . . . C13 C 0.68493(18) 0.5483(2) 0.33019(17) 0.0415(8) Uani 1 1 d . . . H13A H 0.7188 0.4987 0.3317 0.050 Uiso 1 1 calc R . . H13B H 0.6830 0.5537 0.3735 0.050 Uiso 1 1 calc R . . C14 C 0.6137(2) 0.5168(3) 0.28450(19) 0.0529(10) Uani 1 1 d . . . H14A H 0.6140 0.5129 0.2406 0.063 Uiso 1 1 calc R . . H14B H 0.5784 0.5633 0.2847 0.063 Uiso 1 1 calc R . . C15 C 0.5951(2) 0.4204(3) 0.3047(2) 0.0516(10) Uani 1 1 d . . . H15A H 0.5495 0.4012 0.2751 0.077 Uiso 1 1 calc R . . H15B H 0.5941 0.4245 0.3480 0.077 Uiso 1 1 calc R . . H15C H 0.6297 0.3743 0.3039 0.077 Uiso 1 1 calc R . . C16 C 0.78122(18) 0.6642(3) 0.36907(16) 0.0414(8) Uani 1 1 d . . . H16A H 0.7713 0.6716 0.4088 0.050 Uiso 1 1 calc R . . H16B H 0.8123 0.6097 0.3749 0.050 Uiso 1 1 calc R . . C17 C 0.8194(2) 0.7512(3) 0.3601(2) 0.0622(12) Uani 1 1 d . . . H17A H 0.7910 0.8075 0.3588 0.075 Uiso 1 1 calc R . . H17B H 0.8268 0.7471 0.3190 0.075 Uiso 1 1 calc R . . C18 C 0.8897(2) 0.7602(3) 0.4152(3) 0.0807(16) Uani 1 1 d . . . H18A H 0.9137 0.8163 0.4089 0.121 Uiso 1 1 calc R . . H18B H 0.9179 0.7049 0.4160 0.121 Uiso 1 1 calc R . . H18C H 0.8822 0.7652 0.4558 0.121 Uiso 1 1 calc R . . C19 C 0.72373(19) 0.6341(3) 0.24934(15) 0.0394(8) Uani 1 1 d . . . H19A H 0.6792 0.6172 0.2158 0.047 Uiso 1 1 calc R . . H19B H 0.7374 0.6962 0.2382 0.047 Uiso 1 1 calc R . . C20 C 0.7785(2) 0.5621(3) 0.24853(19) 0.0593(11) Uani 1 1 d . . . H20A H 0.8239 0.5813 0.2797 0.071 Uiso 1 1 calc R . . H20B H 0.7666 0.5007 0.2622 0.071 Uiso 1 1 calc R . . C21 C 0.7844(3) 0.5515(4) 0.1832(2) 0.0778(15) Uani 1 1 d . . . H21A H 0.8199 0.5048 0.1856 0.117 Uiso 1 1 calc R . . H21B H 0.7972 0.6117 0.1698 0.117 Uiso 1 1 calc R . . H21C H 0.7399 0.5311 0.1522 0.117 Uiso 1 1 calc R . . C22 C 0.65986(19) 0.7227(2) 0.30678(16) 0.0408(8) Uani 1 1 d . . . H22A H 0.6792 0.7811 0.2963 0.049 Uiso 1 1 calc R . . H22B H 0.6170 0.7081 0.2703 0.049 Uiso 1 1 calc R . . C23 C 0.6408(2) 0.7405(3) 0.3663(2) 0.0636(12) Uani 1 1 d . . . H23A H 0.6282 0.6804 0.3812 0.076 Uiso 1 1 calc R . . H23B H 0.6815 0.7660 0.4010 0.076 Uiso 1 1 calc R . . C24 C 0.5804(3) 0.8090(4) 0.3525(2) 0.0772(15) Uani 1 1 d . . . H24A H 0.5700 0.8187 0.3913 0.116 Uiso 1 1 calc R . . H24B H 0.5396 0.7832 0.3190 0.116 Uiso 1 1 calc R . . H24C H 0.5928 0.8688 0.3382 0.116 Uiso 1 1 calc R . . N3 N 0.96625(15) 0.2594(2) 0.82855(16) 0.0463(7) Uani 1 1 d . A . C25 C 0.92916(19) 0.3089(3) 0.86841(19) 0.0524(10) Uani 1 1 d . . . H25A H 0.9134 0.3710 0.8493 0.063 Uiso 1 1 calc R . . H25B H 0.8875 0.2722 0.8651 0.063 Uiso 1 1 calc R . . C26 C 0.9723(3) 0.3224(5) 0.9390(2) 0.0854(17) Uani 1 1 d . . . H26A H 1.0165 0.3531 0.9431 0.102 Uiso 1 1 calc R . . H26B H 0.9830 0.2606 0.9601 0.102 Uiso 1 1 calc R . . C27 C 0.9343(3) 0.3820(5) 0.9724(2) 0.0940(19) Uani 1 1 d . . . H27A H 0.9634 0.3896 1.0174 0.141 Uiso 1 1 calc R . . H27B H 0.8910 0.3511 0.9693 0.141 Uiso 1 1 calc R . . H27C H 0.9240 0.4435 0.9519 0.141 Uiso 1 1 calc R . . C28 C 0.9123(2) 0.2475(3) 0.76017(19) 0.0594(11) Uani 1 1 d . . . H28A H 0.8696 0.2205 0.7631 0.071 Uiso 0.69(2) 1 calc PR A 1 H28B H 0.9006 0.3101 0.7403 0.071 Uiso 0.69(2) 1 calc PR A 1 H28C H 0.8791 0.3001 0.7510 0.071 Uiso 0.31(2) 1 calc PR A 2 H28D H 0.8862 0.1890 0.7583 0.071 Uiso 0.31(2) 1 calc PR A 2 C29A C 0.9362(5) 0.1861(12) 0.7174(5) 0.075(4) Uani 0.69(2) 1 d P A 1 H29A H 0.9354 0.1200 0.7301 0.090 Uiso 0.69(2) 1 calc PR A 1 H29B H 0.9845 0.2023 0.7230 0.090 Uiso 0.69(2) 1 calc PR A 1 C29B C 0.9489(10) 0.244(2) 0.7009(11) 0.071(7) Uani 0.31(2) 1 d P A 2 H29C H 0.9595 0.3075 0.6893 0.085 Uiso 0.31(2) 1 calc PR A 2 H29D H 0.9914 0.2055 0.7142 0.085 Uiso 0.31(2) 1 calc PR A 2 C30 C 0.8897(3) 0.1979(6) 0.6461(3) 0.135(3) Uani 1 1 d . . . H30A H 0.9061 0.1564 0.6198 0.202 Uiso 0.69(2) 1 calc PR A 1 H30B H 0.8918 0.2629 0.6331 0.202 Uiso 0.69(2) 1 calc PR A 1 H30C H 0.8419 0.1819 0.6404 0.202 Uiso 0.69(2) 1 calc PR A 1 H30D H 0.9091 0.1572 0.6216 0.202 Uiso 0.31(2) 1 calc PR A 2 H30E H 0.8613 0.2465 0.6181 0.202 Uiso 0.31(2) 1 calc PR A 2 H30F H 0.8611 0.1607 0.6638 0.202 Uiso 0.31(2) 1 calc PR A 2 C31 C 0.9952(2) 0.1638(3) 0.8584(2) 0.0644(12) Uani 1 1 d . . . H31A H 1.0307 0.1750 0.9011 0.077 Uiso 1 1 calc R A . H31B H 1.0186 0.1341 0.8318 0.077 Uiso 1 1 calc R . . C32 C 0.9414(3) 0.0942(4) 0.8658(4) 0.115(2) Uani 1 1 d . A . H32A H 0.9150 0.0671 0.8234 0.138 Uiso 0.64(4) 1 calc PR B 1 H32B H 0.9084 0.1288 0.8803 0.138 Uiso 0.64(4) 1 calc PR B 1 H32C H 0.8995 0.0917 0.8266 0.138 Uiso 0.36(4) 1 calc PR B 2 H32D H 0.9279 0.1106 0.9026 0.138 Uiso 0.36(4) 1 calc PR B 2 C33A C 0.9744(9) 0.0109(12) 0.9147(17) 0.125(10) Uani 0.64(4) 1 d P A 1 H33A H 0.9374 -0.0294 0.9177 0.187 Uiso 0.64(4) 1 calc PR B 1 H33B H 1.0006 0.0370 0.9569 0.187 Uiso 0.64(4) 1 calc PR B 1 H33C H 1.0054 -0.0258 0.8996 0.187 Uiso 0.64(4) 1 calc PR B 1 C33B C 0.9829(11) -0.0026(13) 0.8775(14) 0.070(6) Uani 0.36(4) 1 d P A 2 H33D H 0.9535 -0.0529 0.8831 0.105 Uiso 0.36(4) 1 calc PR B 2 H33E H 1.0246 0.0024 0.9158 0.105 Uiso 0.36(4) 1 calc PR B 2 H33F H 0.9961 -0.0165 0.8406 0.105 Uiso 0.36(4) 1 calc PR B 2 C34 C 1.0289(2) 0.3169(3) 0.8280(2) 0.0635(12) Uani 1 1 d . . . H34A H 1.0513 0.2832 0.8022 0.076 Uiso 1 1 calc R A . H34B H 1.0627 0.3207 0.8722 0.076 Uiso 1 1 calc R . . C35 C 1.0110(4) 0.4198(5) 0.8008(3) 0.104(2) Uani 1 1 d . A . H35A H 0.9635 0.4203 0.7686 0.125 Uiso 0.510(10) 1 calc PR C 1 H35B H 1.0430 0.4374 0.7788 0.125 Uiso 0.510(10) 1 calc PR C 1 H35C H 0.9668 0.4411 0.8037 0.125 Uiso 0.490(10) 1 calc PR C 2 H35D H 1.0480 0.4639 0.8248 0.125 Uiso 0.490(10) 1 calc PR C 2 C36A C 1.0162(6) 0.4975(7) 0.8550(6) 0.101(5) Uani 0.510(10) 1 d P A 1 H36A H 1.0033 0.5589 0.8348 0.152 Uiso 0.510(10) 1 calc PR C 1 H36B H 1.0637 0.4999 0.8858 0.152 Uiso 0.510(10) 1 calc PR C 1 H36C H 0.9847 0.4806 0.8770 0.152 Uiso 0.510(10) 1 calc PR C 1 C36B C 1.0054(10) 0.4137(12) 0.7297(9) 0.174(10) Uani 0.490(10) 1 d P A 2 H36D H 0.9934 0.4752 0.7096 0.261 Uiso 0.490(10) 1 calc PR C 2 H36E H 0.9694 0.3684 0.7070 0.261 Uiso 0.490(10) 1 calc PR C 2 H36F H 1.0498 0.3934 0.7278 0.261 Uiso 0.490(10) 1 calc PR C 2 H1 H 0.589(2) 0.657(3) 0.487(2) 0.060(14) Uiso 1 1 d . D 2 H2 H 0.5468(18) 0.535(2) 0.5618(16) 0.030(10) Uiso 1 1 d . E 2 H3 H 0.5123(17) 0.441(2) 0.6416(15) 0.019(9) Uiso 1 1 d . F 2 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 V2B' 0.0284(3) 0.0326(3) 0.0284(3) 0.0062(2) 0.0137(2) 0.0055(2) V1A 0.0202(2) 0.0208(2) 0.0236(2) -0.00059(18) 0.00635(19) 0.00168(19) V2A 0.0330(3) 0.0277(3) 0.0424(3) 0.0088(2) 0.0151(2) 0.0002(2) V2B 0.0282(3) 0.0439(3) 0.0367(3) 0.0070(2) 0.0171(2) 0.0039(2) V1A' 0.0197(2) 0.0256(2) 0.0257(2) 0.0006(2) 0.0073(2) 0.00429(19) V2A' 0.0315(3) 0.0248(3) 0.0370(3) 0.0071(2) 0.0126(2) 0.0049(2) V3A' 0.0252(3) 0.0327(3) 0.0236(2) 0.0014(2) 0.0036(2) 0.0030(2) V3B' 0.0223(3) 0.0348(3) 0.0361(3) -0.0003(2) 0.0068(2) -0.0062(2) V3B 0.0214(2) 0.0234(2) 0.0316(3) -0.0038(2) 0.0078(2) -0.0005(2) V3A 0.0242(3) 0.0330(3) 0.0220(2) 0.0005(2) 0.0070(2) 0.0058(2) OG2' 0.0385(13) 0.0440(13) 0.0388(12) 0.0113(10) 0.0223(11) 0.0095(11) OG1 0.0501(15) 0.0325(13) 0.0640(16) 0.0155(12) 0.0232(13) 0.0022(11) OG2 0.0424(14) 0.0675(17) 0.0495(15) 0.0131(13) 0.0293(12) 0.0099(13) OG1' 0.0480(15) 0.0326(13) 0.0596(16) 0.0144(11) 0.0216(13) 0.0096(11) OF1' 0.0356(13) 0.0474(14) 0.0311(11) -0.0013(10) -0.0005(10) 0.0049(11) OF2' 0.0285(12) 0.0518(15) 0.0501(14) -0.0062(12) 0.0039(11) -0.0103(11) OF2 0.0249(11) 0.0409(13) 0.0471(13) -0.0120(11) 0.0062(10) -0.0030(10) OF1 0.0314(12) 0.0477(14) 0.0274(11) -0.0040(10) 0.0028(9) 0.0086(10) OE2' 0.0270(11) 0.0257(10) 0.0263(10) -0.0006(8) 0.0115(8) 0.0055(8) OE1 0.0323(11) 0.0241(10) 0.0331(11) 0.0032(9) 0.0121(9) 0.0032(9) OD1 0.0354(13) 0.0440(13) 0.0437(13) 0.0135(11) 0.0202(11) 0.0018(11) OE2 0.0256(11) 0.0377(12) 0.0326(11) 0.0029(9) 0.0133(9) 0.0063(9) OE1' 0.0283(11) 0.0271(11) 0.0336(11) 0.0005(9) 0.0099(9) 0.0066(9) OD1' 0.0333(12) 0.0303(11) 0.0407(12) 0.0109(10) 0.0167(10) 0.0050(9) OC2' 0.0320(12) 0.0373(12) 0.0247(10) 0.0027(9) 0.0088(9) 0.0073(10) OB2' 0.0213(10) 0.0275(10) 0.0278(10) -0.0015(8) 0.0036(8) -0.0003(8) OC3' 0.0339(12) 0.0305(11) 0.0461(13) 0.0003(10) 0.0127(10) -0.0077(10) OC4' 0.0228(11) 0.0410(13) 0.0444(13) 0.0051(10) 0.0135(10) -0.0008(10) OB1' 0.0193(10) 0.0314(11) 0.0286(10) -0.0009(9) 0.0061(8) 0.0017(8) OC1' 0.0324(12) 0.0315(11) 0.0307(11) 0.0070(9) 0.0097(9) 0.0089(9) OC4 0.0233(12) 0.0303(12) 0.0365(12) 0.0029(10) 0.0107(10) 0.0023(10) OB1 0.0178(11) 0.0254(10) 0.0256(10) -0.0017(8) 0.0040(9) 0.0041(9) OC1 0.0283(12) 0.0332(12) 0.0325(11) 0.0082(9) 0.0103(10) 0.0059(10) OC2 0.0328(12) 0.0481(14) 0.0276(11) 0.0040(10) 0.0124(9) 0.0086(10) OB2 0.0227(10) 0.0272(10) 0.0260(10) -0.0040(8) 0.0066(8) 0.0036(8) OC3 0.0296(11) 0.0243(10) 0.0411(12) -0.0015(9) 0.0110(10) -0.0002(9) OA1' 0.0221(10) 0.0228(10) 0.0250(10) 0.0010(8) 0.0079(8) 0.0026(8) OA1 0.0225(10) 0.0264(10) 0.0261(10) 0.0006(8) 0.0083(8) 0.0020(8) N1 0.0321(14) 0.0308(14) 0.0276(13) -0.0062(11) 0.0058(11) 0.0027(11) C1 0.0349(18) 0.0339(17) 0.0337(17) -0.0049(14) 0.0057(14) 0.0029(14) C2 0.055(2) 0.048(2) 0.050(2) -0.0049(18) 0.0113(19) 0.0193(19) C3 0.046(2) 0.053(2) 0.065(3) -0.001(2) 0.005(2) 0.0167(19) C4 0.0386(18) 0.0321(17) 0.0358(17) -0.0069(14) 0.0120(14) -0.0015(14) C5 0.054(2) 0.048(2) 0.0428(19) -0.0041(17) 0.0226(18) -0.0044(18) C6 0.061(3) 0.052(2) 0.076(3) -0.001(2) 0.039(2) -0.005(2) C7 0.0378(18) 0.0304(16) 0.0356(17) -0.0054(13) 0.0078(14) 0.0056(14) C8 0.040(2) 0.047(2) 0.0417(19) 0.0014(16) 0.0083(16) 0.0092(17) C9 0.049(2) 0.048(2) 0.073(3) 0.009(2) 0.021(2) 0.0137(19) C10 0.0418(19) 0.0384(18) 0.0296(16) -0.0055(14) 0.0136(14) -0.0002(15) C11 0.060(2) 0.044(2) 0.045(2) -0.0054(17) 0.0196(19) -0.0103(19) C12 0.082(3) 0.061(3) 0.069(3) -0.006(2) 0.044(3) -0.021(2) N2 0.0352(15) 0.0353(14) 0.0284(13) 0.0077(11) 0.0051(11) 0.0017(12) C13 0.043(2) 0.0393(19) 0.0406(18) 0.0136(15) 0.0125(16) 0.0009(16) C14 0.045(2) 0.054(2) 0.052(2) 0.0127(19) 0.0081(18) -0.0079(19) C15 0.052(2) 0.042(2) 0.066(3) 0.0013(19) 0.027(2) -0.0041(18) C16 0.0387(19) 0.045(2) 0.0298(16) 0.0029(15) -0.0009(14) 0.0015(16) C17 0.056(3) 0.060(3) 0.054(2) -0.003(2) -0.001(2) -0.015(2) C18 0.052(3) 0.066(3) 0.097(4) -0.018(3) -0.006(3) -0.007(2) C19 0.046(2) 0.0417(19) 0.0301(16) 0.0008(14) 0.0129(15) -0.0043(16) C20 0.075(3) 0.055(2) 0.048(2) 0.0029(19) 0.023(2) 0.014(2) C21 0.093(4) 0.081(3) 0.064(3) -0.001(3) 0.034(3) 0.023(3) C22 0.042(2) 0.0395(19) 0.0359(18) 0.0076(15) 0.0082(15) 0.0060(16) C23 0.071(3) 0.072(3) 0.052(2) 0.011(2) 0.027(2) 0.022(2) C24 0.088(4) 0.073(3) 0.081(3) 0.012(3) 0.042(3) 0.035(3) N3 0.0271(15) 0.0449(17) 0.0588(19) -0.0085(15) 0.0056(14) 0.0057(13) C25 0.0331(19) 0.060(3) 0.059(2) -0.005(2) 0.0102(17) 0.0127(18) C26 0.054(3) 0.137(5) 0.054(3) -0.006(3) 0.006(2) 0.028(3) C27 0.064(3) 0.148(6) 0.064(3) -0.027(3) 0.015(3) 0.022(4) C28 0.041(2) 0.066(3) 0.059(2) -0.019(2) 0.0019(19) 0.014(2) C29A 0.069(5) 0.080(8) 0.068(5) -0.033(5) 0.015(4) 0.016(5) C29B 0.044(9) 0.065(14) 0.091(13) -0.014(11) 0.009(8) 0.023(9) C30 0.108(5) 0.180(7) 0.093(4) -0.061(5) 0.007(4) 0.066(5) C31 0.032(2) 0.047(2) 0.095(3) -0.001(2) -0.001(2) 0.0119(18) C32 0.057(3) 0.065(4) 0.192(7) 0.028(4) 0.008(4) -0.003(3) C33A 0.120(10) 0.074(8) 0.15(2) 0.042(11) 0.019(12) -0.006(7) C33B 0.084(11) 0.057(8) 0.061(11) 0.017(8) 0.016(9) 0.008(8) C34 0.045(2) 0.074(3) 0.072(3) -0.009(2) 0.022(2) -0.010(2) C35 0.101(5) 0.104(5) 0.098(5) 0.017(4) 0.024(4) -0.028(4) C36A 0.093(9) 0.051(6) 0.123(10) 0.016(6) -0.006(7) -0.015(6) C36B 0.21(2) 0.135(15) 0.21(2) 0.060(14) 0.105(18) -0.026(14) _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 V2B' OG2' 1.589(2) . ? V2B' OD1' 1.821(2) . ? V2B' OC2' 1.830(2) . ? V2B' OC4 2.009(2) . ? V2B' OE2' 2.030(2) . ? V2B' OA1' 2.3053(19) . ? V2B' V1A 3.0591(7) . ? V2B' V2A' 3.0744(7) . ? V2B' V3A' 3.0814(8) . ? V1A OE2' 1.6806(19) . ? V1A OE1 1.684(2) . ? V1A OB2' 1.8597(19) . ? V1A OB1 2.077(2) . ? V1A OA1 2.0807(19) . ? V1A OA1' 2.0851(19) . ? V1A V2A 3.0601(7) . ? V2A OG1 1.592(2) . ? V2A OC3' 1.803(2) . ? V2A OD1 1.829(2) . ? V2A OC1 2.003(2) . ? V2A OE1 2.023(2) . ? V2A OA1 2.328(2) . ? V2A V2B 3.0758(8) . ? V2A V3B' 3.1030(8) . ? V2B OG2 1.593(2) . ? V2B OD1 1.821(2) . ? V2B OC4' 1.823(2) . ? V2B OC2 1.994(2) . ? V2B OE2 2.033(2) . ? V2B OA1 2.363(2) . ? V2B V1A' 3.0843(7) . ? V2B V3B' 3.0961(8) . ? V2B V3A 3.1164(8) . ? V1A' OE2 1.681(2) . ? V1A' OE1' 1.684(2) . ? V1A' OB1' 1.900(2) . ? V1A' OB2 1.985(2) . ? V1A' OA1 2.096(2) . ? V1A' OA1' 2.1098(19) . ? V1A' V2A' 3.0840(7) . ? V2A' OG1' 1.596(2) . ? V2A' OC1' 1.813(2) . ? V2A' OD1' 1.825(2) . ? V2A' OC3 1.987(2) . ? V2A' OE1' 2.021(2) . ? V2A' OA1' 2.3588(19) . ? V2A' V3A' 3.0993(8) . ? V3A' OF1' 1.592(2) . ? V3A' OC2' 1.821(2) . ? V3A' OC1' 1.825(2) . ? V3A' OB2' 2.002(2) . ? V3A' OB1' 2.002(2) . ? V3A' OA1' 2.3445(19) . ? V3A' V3B' 3.0406(8) . ? V3B' OF2' 1.596(2) . ? V3B' OC4' 1.815(2) . ? V3B' OC3' 1.844(2) . ? V3B' OB1' 1.973(2) . ? V3B' OB2' 2.010(2) . ? V3B' OA1 2.356(2) . ? V3B OF2 1.613(2) . ? V3B OC3 1.691(2) . ? V3B OB2 1.928(2) . ? V3B OC4 1.956(2) . ? V3B OB1 2.139(2) . ? V3B OA1' 2.2430(19) . ? V3A OF1 1.619(2) . ? V3A OC2 1.702(2) . ? V3A OB2 1.919(2) . ? V3A OC1 1.947(2) . ? V3A OB1 2.128(2) . ? V3A OA1 2.226(2) . ? N1 C1 1.508(4) . ? N1 C7 1.517(4) . ? N1 C10 1.523(4) . ? N1 C4 1.528(4) . ? C1 C2 1.516(5) . ? C2 C3 1.515(5) . ? C4 C5 1.512(5) . ? C5 C6 1.515(5) . ? C7 C8 1.505(4) . ? C8 C9 1.521(5) . ? C10 C11 1.511(5) . ? C11 C12 1.502(5) . ? N2 C16 1.518(4) . ? N2 C19 1.518(4) . ? N2 C22 1.520(4) . ? N2 C13 1.527(4) . ? C13 C14 1.501(5) . ? C14 C15 1.512(5) . ? C16 C17 1.495(5) . ? C17 C18 1.512(5) . ? C19 C20 1.506(5) . ? C20 C21 1.491(5) . ? C22 C23 1.513(5) . ? C23 C24 1.500(6) . ? N3 C34 1.509(5) . ? N3 C25 1.513(5) . ? N3 C31 1.514(5) . ? N3 C28 1.519(5) . ? C25 C26 1.496(5) . ? C26 C27 1.496(6) . ? C28 C29A 1.478(8) . ? C28 C29B 1.72(3) . ? C29A C30 1.523(11) . ? C29B C30 1.51(2) . ? C31 C32 1.515(7) . ? C32 C33A 1.566(16) . ? C32 C33B 1.568(19) . ? C34 C35 1.554(7) . ? C35 C36B 1.528(17) . ? C35 C36A 1.589(12) . ? 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 OF2 OC1 H1 13(3) 3_666 . ? OF1 OB1 H2 21(3) 3_666 . ? OF2 OB1 H2 40(3) 3_666 . ? OF1 OC4 H3 19(3) 3_666 . ? V1A OB1 H2 120(3) . . ? V3B OB1 H2 110(3) . . ? V3A OB1 H2 118(3) . . ? V2B' OC4 H3 117(3) . . ? V3B OC4 H3 112(3) . . ? V2A OC1 H1 125(3) . . ? V3A OC1 H1 112(3) . . ? OG2' V2B' OD1' 104.83(11) . . ? OG2' V2B' OC2' 103.24(11) . . ? OD1' V2B' OC2' 93.30(10) . . ? OG2' V2B' OC4 98.99(11) . . ? OD1' V2B' OC4 88.03(10) . . ? OC2' V2B' OC4 156.57(9) . . ? OG2' V2B' OE2' 99.52(10) . . ? OD1' V2B' OE2' 155.01(9) . . ? OC2' V2B' OE2' 86.47(9) . . ? OC4 V2B' OE2' 82.64(9) . . ? OG2' V2B' OA1' 171.84(9) . . ? OD1' V2B' OA1' 81.75(8) . . ? OC2' V2B' OA1' 80.89(8) . . ? OC4 V2B' OA1' 76.15(8) . . ? OE2' V2B' OA1' 73.53(7) . . ? OG2' V2B' V1A 130.39(8) . . ? OD1' V2B' V1A 124.67(7) . . ? OC2' V2B' V1A 78.90(7) . . ? OC4 V2B' V1A 81.13(7) . . ? OE2' V2B' V1A 30.93(5) . . ? OA1' V2B' V1A 42.94(5) . . ? OG2' V2B' V2A' 137.36(8) . . ? OD1' V2B' V2A' 32.56(7) . . ? OC2' V2B' V2A' 83.75(7) . . ? OC4 V2B' V2A' 84.92(7) . . ? OE2' V2B' V2A' 123.03(6) . . ? OA1' V2B' V2A' 49.52(5) . . ? V1A V2B' V2A' 92.239(19) . . ? OG2' V2B' V3A' 135.55(9) . . ? OD1' V2B' V3A' 83.43(7) . . ? OC2' V2B' V3A' 32.33(6) . . ? OC4 V2B' V3A' 125.17(7) . . ? OE2' V2B' V3A' 83.14(6) . . ? OA1' V2B' V3A' 49.04(5) . . ? V1A V2B' V3A' 61.170(17) . . ? V2A' V2B' V3A' 60.461(17) . . ? OE2' V1A OE1 106.94(10) . . ? OE2' V1A OB2' 100.48(9) . . ? OE1 V1A OB2' 100.01(10) . . ? OE2' V1A OB1 92.90(9) . . ? OE1 V1A OB1 93.34(9) . . ? OB2' V1A OB1 157.37(9) . . ? OE2' V1A OA1 163.72(9) . . ? OE1 V1A OA1 87.10(9) . . ? OB2' V1A OA1 84.70(8) . . ? OB1 V1A OA1 77.77(8) . . ? OE2' V1A OA1' 86.81(9) . . ? OE1 V1A OA1' 164.16(9) . . ? OB2' V1A OA1' 84.75(8) . . ? OB1 V1A OA1' 77.81(8) . . ? OA1 V1A OA1' 78.25(8) . . ? OE2' V1A V2B' 38.38(7) . . ? OE1 V1A V2B' 145.32(7) . . ? OB2' V1A V2B' 89.87(6) . . ? OB1 V1A V2B' 89.42(6) . . ? OA1 V1A V2B' 127.12(6) . . ? OA1' V1A V2B' 48.87(5) . . ? OE2' V1A V2A 145.06(7) . . ? OE1 V1A V2A 38.12(7) . . ? OB2' V1A V2A 89.27(6) . . ? OB1 V1A V2A 90.09(6) . . ? OA1 V1A V2A 49.47(5) . . ? OA1' V1A V2A 127.72(6) . . ? V2B' V1A V2A 176.56(2) . . ? OG1 V2A OC3' 104.31(12) . . ? OG1 V2A OD1 104.70(12) . . ? OC3' V2A OD1 93.55(11) . . ? OG1 V2A OC1 99.74(12) . . ? OC3' V2A OC1 154.97(10) . . ? OD1 V2A OC1 86.90(10) . . ? OG1 V2A OE1 99.82(11) . . ? OC3' V2A OE1 86.89(9) . . ? OD1 V2A OE1 154.54(9) . . ? OC1 V2A OE1 82.27(9) . . ? OG1 V2A OA1 171.63(11) . . ? OC3' V2A OA1 80.47(8) . . ? OD1 V2A OA1 81.61(9) . . ? OC1 V2A OA1 74.83(8) . . ? OE1 V2A OA1 73.35(7) . . ? OG1 V2A V1A 130.71(10) . . ? OC3' V2A V1A 78.77(7) . . ? OD1 V2A V1A 124.40(7) . . ? OC1 V2A V1A 80.37(6) . . ? OE1 V2A V1A 30.93(6) . . ? OA1 V2A V1A 42.80(5) . . ? OG1 V2A V2B 137.15(10) . . ? OC3' V2A V2B 83.36(8) . . ? OD1 V2A V2B 32.49(7) . . ? OC1 V2A V2B 83.72(7) . . ? OE1 V2A V2B 122.86(6) . . ? OA1 V2A V2B 49.51(5) . . ? V1A V2A V2B 92.10(2) . . ? OG1 V2A V3B' 136.37(10) . . ? OC3' V2A V3B' 32.09(7) . . ? OD1 V2A V3B' 83.42(7) . . ? OC1 V2A V3B' 123.69(7) . . ? OE1 V2A V3B' 83.58(6) . . ? OA1 V2A V3B' 48.90(5) . . ? V1A V2A V3B' 61.291(17) . . ? V2B V2A V3B' 60.141(18) . . ? OG2 V2B OD1 103.71(12) . . ? OG2 V2B OC4' 103.91(12) . . ? OD1 V2B OC4' 93.64(11) . . ? OG2 V2B OC2 100.41(12) . . ? OD1 V2B OC2 88.35(10) . . ? OC4' V2B OC2 154.36(9) . . ? OG2 V2B OE2 102.18(11) . . ? OD1 V2B OE2 153.40(9) . . ? OC4' V2B OE2 85.97(9) . . ? OC2 V2B OE2 81.07(9) . . ? OG2 V2B OA1 173.63(12) . . ? OD1 V2B OA1 80.79(8) . . ? OC4' V2B OA1 80.08(8) . . ? OC2 V2B OA1 75.00(8) . . ? OE2 V2B OA1 72.93(7) . . ? OG2 V2B V2A 136.29(10) . . ? OD1 V2B V2A 32.65(7) . . ? OC4' V2B V2A 83.19(7) . . ? OC2 V2B V2A 84.85(7) . . ? OE2 V2B V2A 121.44(6) . . ? OA1 V2B V2A 48.53(5) . . ? OG2 V2B V1A' 132.54(10) . . ? OD1 V2B V1A' 123.54(7) . . ? OC4' V2B V1A' 79.18(7) . . ? OC2 V2B V1A' 78.46(6) . . ? OE2 V2B V1A' 30.37(6) . . ? OA1 V2B V1A' 42.75(5) . . ? V2A V2B V1A' 91.14(2) . . ? OG2 V2B V3B' 135.44(10) . . ? OD1 V2B V3B' 83.75(8) . . ? OC4' V2B V3B' 31.58(7) . . ? OC2 V2B V3B' 123.90(6) . . ? OE2 V2B V3B' 82.13(6) . . ? OA1 V2B V3B' 48.90(5) . . ? V2A V2B V3B' 60.365(18) . . ? V1A' V2B V3B' 61.376(17) . . ? OG2 V2B V3A 130.15(10) . . ? OD1 V2B V3A 81.61(7) . . ? OC4' V2B V3A 125.44(7) . . ? OC2 V2B V3A 29.74(6) . . ? OE2 V2B V3A 77.11(6) . . ? OA1 V2B V3A 45.41(5) . . ? V2A V2B V3A 64.082(18) . . ? V1A' V2B V3A 60.427(16) . . ? V3B' V2B V3A 94.27(2) . . ? OE2 V1A' OE1' 108.19(10) . . ? OE2 V1A' OB1' 98.52(10) . . ? OE1' V1A' OB1' 98.17(10) . . ? OE2 V1A' OB2 95.07(9) . . ? OE1' V1A' OB2 95.02(9) . . ? OB1' V1A' OB2 157.04(8) . . ? OE2 V1A' OA1 87.37(9) . . ? OE1' V1A' OA1 163.95(9) . . ? OB1' V1A' OA1 82.92(8) . . ? OB2 V1A' OA1 79.30(8) . . ? OE2 V1A' OA1' 164.47(9) . . ? OE1' V1A' OA1' 86.86(9) . . ? OB1' V1A' OA1' 82.60(8) . . ? OB2 V1A' OA1' 79.44(8) . . ? OA1 V1A' OA1' 77.37(7) . . ? OE2 V1A' V2A' 145.46(8) . . ? OE1' V1A' V2A' 37.30(7) . . ? OB1' V1A' V2A' 88.22(6) . . ? OB2 V1A' V2A' 91.02(6) . . ? OA1 V1A' V2A' 127.16(6) . . ? OA1' V1A' V2A' 49.81(5) . . ? OE2 V1A' V2B 37.69(7) . . ? OE1' V1A' V2B 145.85(7) . . ? OB1' V1A' V2B 88.67(6) . . ? OB2 V1A' V2B 90.89(6) . . ? OA1 V1A' V2B 49.92(5) . . ? OA1' V1A' V2B 127.27(6) . . ? V2A' V1A' V2B 176.04(2) . . ? OG1' V2A' OC1' 103.15(12) . . ? OG1' V2A' OD1' 105.81(11) . . ? OC1' V2A' OD1' 93.08(10) . . ? OG1' V2A' OC3 101.55(11) . . ? OC1' V2A' OC3 154.01(9) . . ? OD1' V2A' OC3 87.89(9) . . ? OG1' V2A' OE1' 100.49(11) . . ? OC1' V2A' OE1' 86.66(9) . . ? OD1' V2A' OE1' 153.02(9) . . ? OC3 V2A' OE1' 81.00(9) . . ? OG1' V2A' OA1' 173.01(11) . . ? OC1' V2A' OA1' 79.85(8) . . ? OD1' V2A' OA1' 80.17(8) . . ? OC3 V2A' OA1' 74.73(8) . . ? OE1' V2A' OA1' 73.23(7) . . ? OG1' V2A' V2B' 138.20(9) . . ? OC1' V2A' V2B' 83.05(7) . . ? OD1' V2A' V2B' 32.47(7) . . ? OC3 V2A' V2B' 83.97(6) . . ? OE1' V2A' V2B' 121.24(6) . . ? OA1' V2A' V2B' 48.02(5) . . ? OG1' V2A' V1A' 130.78(9) . . ? OC1' V2A' V1A' 79.51(7) . . ? OD1' V2A' V1A' 123.26(7) . . ? OC3 V2A' V1A' 78.31(6) . . ? OE1' V2A' V1A' 30.32(6) . . ? OA1' V2A' V1A' 43.10(5) . . ? V2B' V2A' V1A' 91.013(19) . . ? OG1' V2A' V3A' 134.82(10) . . ? OC1' V2A' V3A' 31.69(6) . . ? OD1' V2A' V3A' 82.84(7) . . ? OC3 V2A' V3A' 123.31(6) . . ? OE1' V2A' V3A' 82.92(6) . . ? OA1' V2A' V3A' 48.58(5) . . ? V2B' V2A' V3A' 59.881(18) . . ? V1A' V2A' V3A' 61.874(17) . . ? OF1' V3A' OC2' 103.66(11) . . ? OF1' V3A' OC1' 102.95(11) . . ? OC2' V3A' OC1' 93.52(10) . . ? OF1' V3A' OB2' 101.29(11) . . ? OC2' V3A' OB2' 90.14(9) . . ? OC1' V3A' OB2' 153.85(9) . . ? OF1' V3A' OB1' 101.21(11) . . ? OC2' V3A' OB1' 153.52(9) . . ? OC1' V3A' OB1' 89.66(9) . . ? OB2' V3A' OB1' 76.11(8) . . ? OF1' V3A' OA1' 175.03(11) . . ? OC2' V3A' OA1' 79.98(8) . . ? OC1' V3A' OA1' 80.02(8) . . ? OB2' V3A' OA1' 75.14(7) . . ? OB1' V3A' OA1' 74.70(7) . . ? OF1' V3A' V3B' 89.99(9) . . ? OC2' V3A' V3B' 130.95(7) . . ? OC1' V3A' V3B' 129.42(7) . . ? OB2' V3A' V3B' 40.81(6) . . ? OB1' V3A' V3B' 39.76(6) . . ? OA1' V3A' V3B' 85.06(5) . . ? OF1' V3A' V2B' 135.98(9) . . ? OC2' V3A' V2B' 32.51(7) . . ? OC1' V3A' V2B' 82.67(7) . . ? OB2' V3A' V2B' 86.70(6) . . ? OB1' V3A' V2B' 122.63(6) . . ? OA1' V3A' V2B' 47.95(5) . . ? V3B' V3A' V2B' 120.28(2) . . ? OF1' V3A' V2A' 134.30(9) . . ? OC2' V3A' V2A' 83.14(7) . . ? OC1' V3A' V2A' 31.47(7) . . ? OB2' V3A' V2A' 124.08(6) . . ? OB1' V3A' V2A' 86.03(6) . . ? OA1' V3A' V2A' 48.98(5) . . ? V3B' V3A' V2A' 119.73(2) . . ? V2B' V3A' V2A' 59.658(17) . . ? OF2' V3B' OC4' 103.18(12) . . ? OF2' V3B' OC3' 102.85(12) . . ? OC4' V3B' OC3' 92.89(10) . . ? OF2' V3B' OB1' 102.75(11) . . ? OC4' V3B' OB1' 91.06(9) . . ? OC3' V3B' OB1' 152.45(9) . . ? OF2' V3B' OB2' 101.57(11) . . ? OC4' V3B' OB2' 154.24(9) . . ? OC3' V3B' OB2' 88.46(9) . . ? OB1' V3B' OB2' 76.58(8) . . ? OF2' V3B' OA1 175.81(11) . . ? OC4' V3B' OA1 80.43(8) . . ? OC3' V3B' OA1 78.91(8) . . ? OB1' V3B' OA1 74.89(8) . . ? OB2' V3B' OA1 74.59(7) . . ? OF2' V3B' V3A' 91.09(9) . . ? OC4' V3B' V3A' 131.53(8) . . ? OC3' V3B' V3A' 129.07(7) . . ? OB1' V3B' V3A' 40.47(6) . . ? OB2' V3B' V3A' 40.61(6) . . ? OA1 V3B' V3A' 84.89(5) . . ? OF2' V3B' V2B 134.70(9) . . ? OC4' V3B' V2B 31.75(7) . . ? OC3' V3B' V2B 82.16(7) . . ? OB1' V3B' V2B 87.05(6) . . ? OB2' V3B' V2B 123.67(6) . . ? OA1 V3B' V2B 49.09(5) . . ? V3A' V3B' V2B 120.83(2) . . ? OF2' V3B' V2A 133.98(10) . . ? OC4' V3B' V2A 82.52(7) . . ? OC3' V3B' V2A 31.30(7) . . ? OB1' V3B' V2A 122.96(6) . . ? OB2' V3B' V2A 85.45(6) . . ? OA1 V3B' V2A 48.11(5) . . ? V3A' V3B' V2A 119.37(2) . . ? V2B V3B' V2A 59.494(18) . . ? OF2 V3B OC3 105.98(11) . . ? OF2 V3B OB2 101.10(10) . . ? OC3 V3B OB2 97.31(9) . . ? OF2 V3B OC4 100.03(11) . . ? OC3 V3B OC4 94.68(10) . . ? OB2 V3B OC4 151.74(9) . . ? OF2 V3B OB1 97.24(10) . . ? OC3 V3B OB1 156.62(10) . . ? OB2 V3B OB1 75.22(8) . . ? OC4 V3B OB1 83.70(9) . . ? OF2 V3B OA1' 170.44(10) . . ? OC3 V3B OA1' 83.58(9) . . ? OB2 V3B OA1' 77.36(8) . . ? OC4 V3B OA1' 78.68(8) . . ? OB1 V3B OA1' 73.21(7) . . ? OF1 V3A OC2 106.27(11) . . ? OF1 V3A OB2 101.88(11) . . ? OC2 V3A OB2 97.31(10) . . ? OF1 V3A OC1 99.25(11) . . ? OC2 V3A OC1 94.20(11) . . ? OB2 V3A OC1 151.98(9) . . ? OF1 V3A OB1 95.72(10) . . ? OC2 V3A OB1 157.90(9) . . ? OB2 V3A OB1 75.64(8) . . ? OC1 V3A OB1 84.16(9) . . ? OF1 V3A OA1 169.20(10) . . ? OC2 V3A OA1 84.45(9) . . ? OB2 V3A OA1 77.48(8) . . ? OC1 V3A OA1 78.32(9) . . ? OB1 V3A OA1 73.62(8) . . ? OF1 V3A V2B 141.49(8) . . ? OC2 V3A V2B 35.54(7) . . ? OB2 V3A V2B 91.19(6) . . ? OC1 V3A V2B 83.49(7) . . ? OB1 V3A V2B 122.70(6) . . ? OA1 V3A V2B 49.09(5) . . ? V1A OE2' V2B' 110.69(10) . . ? V1A OE1 V2A 110.94(10) . . ? V2B OD1 V2A 114.86(11) . . ? V1A' OE2 V2B 111.95(11) . . ? V1A' OE1' V2A' 112.38(10) . . ? V2B' OD1' V2A' 114.97(11) . . ? V3A' OC2' V2B' 115.16(11) . . ? V1A OB2' V3A' 107.97(10) . . ? V1A OB2' V3B' 108.51(9) . . ? V3A' OB2' V3B' 98.58(9) . . ? V2A OC3' V3B' 116.61(12) . . ? V3B' OC4' V2B 116.67(11) . . ? V1A' OB1' V3B' 109.03(10) . . ? V1A' OB1' V3A' 109.07(9) . . ? V3B' OB1' V3A' 99.77(9) . . ? V2A' OC1' V3A' 116.84(11) . . ? V3B OC4 V2B' 111.09(11) . . ? V1A OB1 V3A 105.37(9) . . ? V1A OB1 V3B 105.80(9) . . ? V3A OB1 V3B 94.15(8) . . ? V3A OC1 V2A 112.53(11) . . ? V3A OC2 V2B 114.72(11) . . ? V3A OB2 V3B 108.61(9) . . ? V3A OB2 V1A' 106.13(10) . . ? V3B OB2 V1A' 106.39(9) . . ? V3B OC3 V2A' 115.97(11) . . ? V1A OA1' V1A' 101.54(8) . . ? V1A OA1' V3B 101.91(8) . . ? V1A' OA1' V3B 92.02(7) . . ? V1A OA1' V2B' 88.19(7) . . ? V1A' OA1' V2B' 168.51(10) . . ? V3B OA1' V2B' 91.91(7) . . ? V1A OA1' V3A' 89.52(7) . . ? V1A' OA1' V3A' 90.91(7) . . ? V3B OA1' V3A' 167.38(9) . . ? V2B' OA1' V3A' 83.01(6) . . ? V1A OA1' V2A' 168.33(10) . . ? V1A' OA1' V2A' 87.10(7) . . ? V3B OA1' V2A' 85.45(7) . . ? V2B' OA1' V2A' 82.46(6) . . ? V3A' OA1' V2A' 82.44(6) . . ? V1A OA1 V1A' 102.16(8) . . ? V1A OA1 V3A 101.85(8) . . ? V1A' OA1 V3A 92.39(8) . . ? V1A OA1 V2A 87.74(7) . . ? V1A' OA1 V2A 167.92(10) . . ? V3A OA1 V2A 92.32(7) . . ? V1A OA1 V3B' 89.94(7) . . ? V1A' OA1 V3B' 90.04(7) . . ? V3A OA1 V3B' 167.15(10) . . ? V2A OA1 V3B' 82.98(7) . . ? V1A OA1 V2B 167.61(10) . . ? V1A' OA1 V2B 87.33(7) . . ? V3A OA1 V2B 85.50(7) . . ? V2A OA1 V2B 81.96(6) . . ? V3B' OA1 V2B 82.01(6) . . ? C1 N1 C7 106.0(2) . . ? C1 N1 C10 111.5(2) . . ? C7 N1 C10 111.3(2) . . ? C1 N1 C4 109.7(2) . . ? C7 N1 C4 111.2(2) . . ? C10 N1 C4 107.2(2) . . ? N1 C1 C2 116.5(3) . . ? C3 C2 C1 108.1(3) . . ? C5 C4 N1 114.6(3) . . ? C4 C5 C6 110.4(3) . . ? C8 C7 N1 116.4(3) . . ? C7 C8 C9 109.8(3) . . ? C11 C10 N1 115.5(3) . . ? C12 C11 C10 111.8(3) . . ? C16 N2 C19 111.2(3) . . ? C16 N2 C22 110.1(3) . . ? C19 N2 C22 107.4(2) . . ? C16 N2 C13 107.0(2) . . ? C19 N2 C13 110.2(3) . . ? C22 N2 C13 111.0(3) . . ? C14 C13 N2 116.3(3) . . ? C13 C14 C15 110.4(3) . . ? C17 C16 N2 115.4(3) . . ? C16 C17 C18 110.3(4) . . ? C20 C19 N2 114.9(3) . . ? C21 C20 C19 113.1(3) . . ? C23 C22 N2 115.0(3) . . ? C24 C23 C22 111.9(3) . . ? C34 N3 C25 110.8(3) . . ? C34 N3 C31 106.2(3) . . ? C25 N3 C31 110.5(3) . . ? C34 N3 C28 111.2(3) . . ? C25 N3 C28 106.9(3) . . ? C31 N3 C28 111.3(3) . . ? C26 C25 N3 115.6(3) . . ? C25 C26 C27 111.6(4) . . ? C29A C28 N3 114.1(4) . . ? C29A C28 C29B 34.0(6) . . ? N3 C28 C29B 113.5(7) . . ? C28 C29A C30 111.6(7) . . ? C30 C29B C28 100.4(16) . . ? C29B C30 C29A 36.9(9) . . ? N3 C31 C32 115.7(3) . . ? C31 C32 C33A 113.9(7) . . ? C31 C32 C33B 102.0(10) . . ? C33A C32 C33B 34.0(8) . . ? N3 C34 C35 114.7(4) . . ? C36B C35 C34 105.3(8) . . ? C36B C35 C36A 140.0(9) . . ? C34 C35 C36A 113.7(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag OC1 H1 OF2 2_666 0.75(4) 2.06(4) 2.787(3) 162(4) ? OB1 H2 OF1 2_666 0.71(3) 2.24(3) 2.893(3) 153(4) ? OC4 H3 OF1 2_666 0.67(3) 2.34(3) 2.961(3) 155(4) ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.564 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.082 #===END data_TPAh _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Tris(tetra-n-propylammonium) trihydrogendecavanadate monohydrate ; _chemical_melting_point ? _chemical_formula_moiety '(C12 H28 N +)3, (H3 V10 O28 3-), 0.5(H2 O)' _chemical_formula_sum 'C36 H88 N3 O28.50 V10' _chemical_formula_weight 1528.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 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' _cell_length_a 27.994(4) _cell_length_b 24.643(4) _cell_length_c 17.9049(15) _cell_angle_alpha 90.00 _cell_angle_beta 95.448(9) _cell_angle_gamma 90.00 _cell_volume 12296(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 14.855 _cell_measurement_theta_max 14.995 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6264 _exptl_absorpt_coefficient_mu 1.526 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.928 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'UltraX18 Rigaku Denki rotating Mo anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.084 _diffrn_reflns_number 16466 _diffrn_reflns_av_R_equivalents 0.0859 _diffrn_reflns_av_sigmaI/netI 0.1189 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.59 _reflns_number_total 8347 _reflns_number_gt 3612 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control Software' _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_reduction 'teXsan PROCESS (Molecular Structure Corporation, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997a)' _refine_special_details ; H atoms in the [(C~3~H~7~)~4~N]^+^ cations were included in ideal positions and refined with the riding model. H atoms attached to surface O atoms of decavanadate frameworks and H atoms of water molecules were not included in refinement. Distances between the following atom pairs were restrained to 1.53\%A with estimated standard deviation 0.02: N3 and C31, C55 and C57, C41 and C42, C47 and C48, C44 and C45. The 1,3-distance between N4 and C47 was restrained to 2.70\%A with estimated standard deviation 0.04. ; _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^)+(0.1090P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.09(7) _refine_ls_number_reflns 8347 _refine_ls_number_parameters 689 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1797 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1972 _refine_ls_wR_factor_gt 0.1432 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 V2AA V -0.1149(2) 0.2244(2) -0.0751(3) 0.0457(18) Uani 1 1 d . . . V1AA V -0.0489(2) 0.1829(2) 0.0587(3) 0.0316(15) Uani 1 1 d . . . V2B'A V 0.0124(2) 0.1420(2) 0.1994(3) 0.0362(15) Uani 1 1 d . . . V2A'A V -0.0661(2) 0.1660(2) 0.3019(3) 0.0389(17) Uani 1 1 d . . . V1A'A V -0.1335(2) 0.2095(2) 0.1653(3) 0.0337(16) Uani 1 1 d . . . V2BA V -0.1955(2) 0.2487(2) 0.0242(3) 0.0445(18) Uani 1 1 d . . . V3B'A V -0.1512(2) 0.1337(2) 0.0243(3) 0.0406(17) Uani 1 1 d . . . V3A'A V -0.0871(2) 0.0931(2) 0.1613(3) 0.0354(16) Uani 1 1 d . . . V3AA V -0.0993(2) 0.3052(2) 0.0702(3) 0.0331(15) Uani 1 1 d . . . V3BA V -0.0347(2) 0.2644(2) 0.2100(3) 0.0373(16) Uani 1 1 d . . . OG1A O -0.1076(6) 0.2375(6) -0.1617(10) 0.041(4) Uiso 1 1 d . . . OG2'A O 0.0671(11) 0.1205(10) 0.2089(17) 0.074(8) Uiso 1 1 d . . . OG1'A O -0.0710(6) 0.1553(6) 0.3860(10) 0.043(4) Uiso 1 1 d . . . OG2A O -0.2492(8) 0.2723(8) 0.0146(12) 0.047(5) Uiso 1 1 d . . . OF2'A O -0.1672(9) 0.0741(9) 0.0052(14) 0.062(6) Uiso 1 1 d . . . OF1'A O -0.1043(8) 0.0330(8) 0.1472(13) 0.051(6) Uiso 1 1 d . . . OF1A O -0.0754(8) 0.3643(9) 0.0872(13) 0.054(6) Uiso 1 1 d . . . OF2A O -0.0105(10) 0.3228(9) 0.2238(15) 0.056(6) Uiso 1 1 d . . . OE1A O -0.0462(9) 0.2004(9) -0.0315(14) 0.047(6) Uiso 1 1 d . . . OE2'A O 0.0076(6) 0.1659(6) 0.0866(9) 0.027(4) Uiso 1 1 d . . . OD1'A O -0.0055(8) 0.1424(8) 0.2905(12) 0.047(5) Uiso 1 1 d . . . OE1'A O -0.1321(8) 0.1968(8) 0.2571(12) 0.037(5) Uiso 1 1 d . . . OE2A O -0.1875(7) 0.2377(7) 0.1373(11) 0.035(5) Uiso 1 1 d . . . OD1A O -0.1726(7) 0.2558(7) -0.0673(11) 0.037(4) Uiso 1 1 d . . . OC3'A O -0.1329(6) 0.1600(6) -0.0718(9) 0.034(4) Uiso 1 1 d . . . OB2'A O -0.0794(7) 0.1165(7) 0.0563(10) 0.030(4) Uiso 1 1 d . . . OC2'A O -0.0216(8) 0.0834(7) 0.1738(12) 0.038(5) Uiso 1 1 d . . . OC1'A O -0.0900(8) 0.1039(8) 0.2628(12) 0.043(5) Uiso 1 1 d . . . OB1'A O -0.1450(7) 0.1341(7) 0.1318(11) 0.038(5) Uiso 1 1 d . . . OC4'A O -0.2031(8) 0.1715(8) 0.0179(13) 0.048(6) Uiso 1 1 d . . . OC1A O -0.0869(9) 0.2959(8) -0.0351(14) 0.048(6) Uiso 1 1 d . . . OB1A O -0.0332(9) 0.2623(8) 0.0927(13) 0.044(6) Uiso 1 1 d . . . OC4A O 0.0237(7) 0.2232(7) 0.2121(11) 0.033(5) Uiso 1 1 d . . . OC3A O -0.0450(7) 0.2386(7) 0.2977(11) 0.039(5) Uiso 1 1 d . . . OB2A O -0.0980(8) 0.2778(8) 0.1682(13) 0.048(6) Uiso 1 1 d . . . OC2A O -0.1580(7) 0.3152(8) 0.0566(11) 0.041(5) Uiso 1 1 d . . . OA1A O -0.1167(7) 0.2190(7) 0.0548(11) 0.035(5) Uiso 1 1 d . . . OA1'A O -0.0617(8) 0.1816(8) 0.1735(12) 0.036(5) Uiso 1 1 d . . . V2AB V 0.11442(19) 0.2764(2) 0.0748(3) 0.0360(15) Uani 1 1 d . . . V1AB V 0.04850(19) 0.3178(2) -0.0584(3) 0.0327(15) Uani 1 1 d . . . V2B'B V -0.0118(2) 0.3572(2) -0.1972(3) 0.0420(17) Uani 1 1 d . . . V2A'B V 0.0683(2) 0.3337(2) -0.2995(3) 0.0407(17) Uani 1 1 d . . . V1A'B V 0.1337(2) 0.2904(2) -0.1647(3) 0.0346(16) Uani 1 1 d . . . V2BB V 0.1971(2) 0.2516(2) -0.0221(3) 0.0391(16) Uani 1 1 d . . . V3B'B V 0.15232(19) 0.3664(2) -0.0226(3) 0.0365(15) Uani 1 1 d . . . V3A'B V 0.0890(2) 0.4076(2) -0.1601(3) 0.0387(17) Uani 1 1 d . . . V3AB V 0.1002(2) 0.1940(2) -0.0700(4) 0.0414(17) Uani 1 1 d . . . V3BB V 0.0347(2) 0.2361(2) -0.2095(3) 0.0363(16) Uani 1 1 d . . . OG1B O 0.1003(6) 0.2726(6) 0.1589(10) 0.042(4) Uiso 1 1 d . . . OG2'B O -0.0661(8) 0.3770(7) -0.2099(12) 0.042(5) Uiso 1 1 d . . . OG1'B O 0.0812(6) 0.3351(6) -0.3855(10) 0.045(4) Uiso 1 1 d . . . OG2B O 0.2512(9) 0.2276(10) -0.0073(14) 0.062(7) Uiso 1 1 d . . . OF2'B O 0.1744(7) 0.4266(7) -0.0073(12) 0.045(5) Uiso 1 1 d . . . OF1'B O 0.1111(8) 0.4675(8) -0.1442(12) 0.047(5) Uiso 1 1 d . . . OF1B O 0.0822(8) 0.1340(8) -0.0822(12) 0.048(5) Uiso 1 1 d . . . OF2B O 0.0130(8) 0.1769(8) -0.2222(13) 0.044(5) Uiso 1 1 d . . . OE1B O 0.0490(7) 0.3019(7) 0.0352(11) 0.029(4) Uiso 1 1 d . . . OE2'B O -0.0086(7) 0.3424(7) -0.0876(12) 0.046(5) Uiso 1 1 d . . . OD1'B O 0.0089(7) 0.3545(7) -0.2957(11) 0.039(5) Uiso 1 1 d . . . OE1'B O 0.1313(8) 0.3004(8) -0.2585(13) 0.038(5) Uiso 1 1 d . . . OE2B O 0.1889(8) 0.2668(8) -0.1349(12) 0.042(5) Uiso 1 1 d . . . OD1B O 0.1760(9) 0.2516(8) 0.0704(14) 0.058(6) Uiso 1 1 d . . . OC3'B O 0.1340(7) 0.3490(7) 0.0672(11) 0.046(5) Uiso 1 1 d . . . OB2'B O 0.0812(7) 0.3797(7) -0.0502(11) 0.036(5) Uiso 1 1 d . . . OC2'B O 0.0213(8) 0.4167(8) -0.1705(13) 0.044(6) Uiso 1 1 d . . . OC1'B O 0.0956(7) 0.3989(7) -0.2552(11) 0.039(5) Uiso 1 1 d . . . OB1'B O 0.1468(7) 0.3621(7) -0.1361(10) 0.030(4) Uiso 1 1 d . . . OC4'B O 0.2052(7) 0.3236(7) -0.0141(11) 0.036(5) Uiso 1 1 d . . . OC1B O 0.0915(8) 0.2045(7) 0.0366(12) 0.036(5) Uiso 1 1 d . . . OB1B O 0.0341(7) 0.2374(7) -0.0899(11) 0.026(4) Uiso 1 1 d . . . OC4B O -0.0233(8) 0.2788(8) -0.2079(12) 0.042(5) Uiso 1 1 d . . . OC3B O 0.0512(7) 0.2553(7) -0.2942(11) 0.038(5) Uiso 1 1 d . . . OB2B O 0.1020(6) 0.2205(6) -0.1725(9) 0.023(4) Uiso 1 1 d . . . OC2B O 0.1636(8) 0.1877(8) -0.0490(11) 0.043(5) Uiso 1 1 d . . . OA1B O 0.1164(7) 0.2845(6) -0.0485(10) 0.029(4) Uiso 1 1 d . . . OA1'B O 0.0620(8) 0.3182(8) -0.1687(12) 0.036(5) Uiso 1 1 d . . . N1 N 0.0291(9) 0.4807(10) 0.1116(14) 0.046(6) Uiso 1 1 d . . . C1 C -0.0094(11) 0.5011(13) 0.1651(18) 0.059(8) Uiso 1 1 d . . . H1A H 0.0079 0.5238 0.2029 0.071 Uiso 1 1 calc R . . H1B H -0.0311 0.5249 0.1351 0.071 Uiso 1 1 calc R . . C2 C 0.0597(10) 0.5258(9) 0.0950(15) 0.053(6) Uiso 1 1 d . . . H2A H 0.0782 0.5369 0.1411 0.063 Uiso 1 1 calc R . . H2B H 0.0396 0.5562 0.0776 0.063 Uiso 1 1 calc R . . C3 C -0.0111(12) 0.4581(12) 0.0408(18) 0.054(9) Uiso 1 1 d . . . H3A H 0.0070 0.4408 0.0038 0.065 Uiso 1 1 calc R . . H3B H -0.0303 0.4301 0.0613 0.065 Uiso 1 1 calc R . . C4 C 0.0617(8) 0.4362(8) 0.1377(13) 0.036(4) Uiso 1 1 d . . . H4A H 0.0832 0.4296 0.0993 0.043 Uiso 1 1 calc R . . H4B H 0.0426 0.4037 0.1416 0.043 Uiso 1 1 calc R . . C5 C -0.0405(11) 0.4634(11) 0.2069(18) 0.062(7) Uiso 1 1 d . . . H5A H -0.0647 0.4479 0.1707 0.074 Uiso 1 1 calc R . . H5B H -0.0205 0.4338 0.2273 0.074 Uiso 1 1 calc R . . C6 C 0.0938(14) 0.5134(13) 0.037(2) 0.095(9) Uiso 1 1 d . . . H6A H 0.1185 0.4892 0.0593 0.114 Uiso 1 1 calc R . . H6B H 0.0763 0.4941 -0.0041 0.114 Uiso 1 1 calc R . . C7 C -0.0459(19) 0.4991(18) -0.001(3) 0.118(15) Uiso 1 1 d . . . H7A H -0.0624 0.5206 0.0339 0.142 Uiso 1 1 calc R . . H7B H -0.0290 0.5232 -0.0324 0.142 Uiso 1 1 calc R . . C8 C 0.092(2) 0.444(2) 0.213(4) 0.15(2) Uiso 1 1 d . . . H8A H 0.1203 0.4662 0.2054 0.182 Uiso 1 1 calc R . . H8B H 0.0738 0.4629 0.2481 0.182 Uiso 1 1 calc R . . C9 C -0.0810(14) 0.4624(13) -0.049(2) 0.081(9) Uiso 1 1 d . . . H9A H -0.1055 0.4843 -0.0751 0.122 Uiso 1 1 calc R . . H9B H -0.0955 0.4373 -0.0166 0.122 Uiso 1 1 calc R . . H9C H -0.0640 0.4428 -0.0841 0.122 Uiso 1 1 calc R . . C10 C 0.1075(17) 0.3936(16) 0.243(3) 0.126(14) Uiso 1 1 d . . . H10A H 0.1299 0.3991 0.2865 0.189 Uiso 1 1 calc R . . H10B H 0.1228 0.3734 0.2061 0.189 Uiso 1 1 calc R . . H10C H 0.0802 0.3737 0.2570 0.189 Uiso 1 1 calc R . . C11 C 0.1160(13) 0.5587(12) 0.0079(19) 0.081(8) Uiso 1 1 d . . . H11A H 0.1355 0.5471 -0.0305 0.121 Uiso 1 1 calc R . . H11B H 0.1358 0.5764 0.0473 0.121 Uiso 1 1 calc R . . H11C H 0.0919 0.5835 -0.0132 0.121 Uiso 1 1 calc R . . C12 C -0.0632(18) 0.4851(17) 0.263(3) 0.109(15) Uiso 1 1 d . . . H12A H -0.0803 0.4571 0.2871 0.163 Uiso 1 1 calc R . . H12B H -0.0854 0.5124 0.2437 0.163 Uiso 1 1 calc R . . H12C H -0.0400 0.5012 0.2997 0.163 Uiso 1 1 calc R . . N2 N -0.0200(10) 0.0206(11) -0.1055(16) 0.054(7) Uiso 1 1 d . . . C13 C 0.0040(12) 0.0441(12) -0.0490(18) 0.053(8) Uiso 1 1 d . . . H13A H -0.0175 0.0537 -0.0117 0.063 Uiso 1 1 calc R . . H13B H 0.0185 0.0772 -0.0656 0.063 Uiso 1 1 calc R . . C14 C 0.0002(11) -0.0033(12) -0.1746(17) 0.052(7) Uiso 1 1 d . . . H14A H 0.0208 -0.0341 -0.1608 0.063 Uiso 1 1 calc R . . H14B H -0.0255 -0.0152 -0.2110 0.063 Uiso 1 1 calc R . . C15 C -0.0492(17) 0.0689(16) -0.143(3) 0.112(14) Uiso 1 1 d . . . H15A H -0.0288 0.0897 -0.1734 0.135 Uiso 1 1 calc R . . H15B H -0.0595 0.0927 -0.1046 0.135 Uiso 1 1 calc R . . C16 C -0.0466(9) -0.0288(8) -0.0713(13) 0.041(5) Uiso 1 1 d . . . H16A H -0.0687 -0.0443 -0.1107 0.049 Uiso 1 1 calc R . . H16B H -0.0229 -0.0564 -0.0562 0.049 Uiso 1 1 calc R . . C17 C -0.0974(18) 0.0469(17) -0.197(3) 0.119(14) Uiso 1 1 d . . . H17A H -0.0876 0.0213 -0.2341 0.143 Uiso 1 1 calc R . . H17B H -0.1193 0.0286 -0.1668 0.143 Uiso 1 1 calc R . . C18 C 0.0290(11) 0.0422(10) -0.2071(17) 0.059(7) Uiso 1 1 d . . . H18A H 0.0074 0.0698 -0.2294 0.070 Uiso 1 1 calc R . . H18B H 0.0501 0.0589 -0.1676 0.070 Uiso 1 1 calc R . . C19 C 0.0424(12) 0.0070(12) -0.0149(18) 0.064(8) Uiso 1 1 d . . . H19A H 0.0273 -0.0263 0.0000 0.077 Uiso 1 1 calc R . . H19B H 0.0633 -0.0024 -0.0531 0.077 Uiso 1 1 calc R . . C20 C -0.0742(8) -0.0164(8) -0.0054(12) 0.043(4) Uiso 1 1 d . . . H20A H -0.0520 -0.0028 0.0353 0.052 Uiso 1 1 calc R . . H20B H -0.0971 0.0122 -0.0194 0.052 Uiso 1 1 calc R . . C21 C 0.0721(16) 0.0287(15) 0.051(3) 0.102(13) Uiso 1 1 d . . . H21A H 0.0929 0.0007 0.0723 0.154 Uiso 1 1 calc R . . H21B H 0.0517 0.0412 0.0874 0.154 Uiso 1 1 calc R . . H21C H 0.0910 0.0585 0.0354 0.154 Uiso 1 1 calc R . . C22 C 0.0573(14) 0.0191(14) -0.264(2) 0.084(11) Uiso 1 1 d . . . H22A H 0.0767 0.0471 -0.2835 0.126 Uiso 1 1 calc R . . H22B H 0.0360 0.0044 -0.3045 0.126 Uiso 1 1 calc R . . H22C H 0.0776 -0.0091 -0.2423 0.126 Uiso 1 1 calc R . . C23 C -0.1236(14) 0.0981(13) -0.239(2) 0.101(10) Uiso 1 1 d . . . H23A H -0.1478 0.0855 -0.2765 0.152 Uiso 1 1 calc R . . H23B H -0.1004 0.1194 -0.2622 0.152 Uiso 1 1 calc R . . H23C H -0.1382 0.1199 -0.2029 0.152 Uiso 1 1 calc R . . C24 C -0.1003(14) -0.0635(14) 0.022(2) 0.096(10) Uiso 1 1 d . . . H24A H -0.1167 -0.0527 0.0645 0.144 Uiso 1 1 calc R . . H24B H -0.0779 -0.0919 0.0370 0.144 Uiso 1 1 calc R . . H24C H -0.1232 -0.0764 -0.0170 0.144 Uiso 1 1 calc R . . N3 N -0.2496(8) 0.0632(5) 0.2630(8) 0.045(4) Uiso 1 1 d D . . C25 C -0.2140(11) 0.1009(9) 0.2759(16) 0.065(7) Uiso 1 1 d . . . H25A H -0.2073 0.1186 0.2297 0.078 Uiso 1 1 calc R . . H25B H -0.1848 0.0844 0.2990 0.078 Uiso 1 1 calc R . . C26 C -0.2352(12) 0.1418(11) 0.3303(18) 0.079(7) Uiso 1 1 d . . . H26A H -0.2632 0.1257 0.3495 0.095 Uiso 1 1 calc R . . H26B H -0.2455 0.1742 0.3025 0.095 Uiso 1 1 calc R . . C27 C -0.1926(10) 0.1610(10) 0.4087(15) 0.060(6) Uiso 1 1 d . . . H27A H -0.2082 0.1841 0.4422 0.090 Uiso 1 1 calc R . . H27B H -0.1662 0.1801 0.3904 0.090 Uiso 1 1 calc R . . H27C H -0.1809 0.1290 0.4350 0.090 Uiso 1 1 calc R . . C28 C -0.2733(9) 0.0257(9) 0.3129(14) 0.044(5) Uiso 1 1 d . . . H28A H -0.2940 0.0472 0.3419 0.052 Uiso 1 1 calc R . . H28B H -0.2939 0.0016 0.2815 0.052 Uiso 1 1 calc R . . C29 C -0.2429(12) -0.0074(13) 0.365(2) 0.078(9) Uiso 1 1 d . . . H29A H -0.2207 -0.0285 0.3383 0.093 Uiso 1 1 calc R . . H29B H -0.2245 0.0153 0.4015 0.093 Uiso 1 1 calc R . . C30 C -0.2735(18) -0.0419(17) 0.401(3) 0.100(15) Uiso 1 1 d . . . H30A H -0.2546 -0.0657 0.4344 0.150 Uiso 1 1 calc R . . H30B H -0.2925 -0.0629 0.3641 0.150 Uiso 1 1 calc R . . H30C H -0.2942 -0.0205 0.4291 0.150 Uiso 1 1 calc R . . C31 C -0.2857(7) 0.0932(7) 0.1975(10) 0.038(4) Uiso 1 1 d D . . H31A H -0.3065 0.0650 0.1752 0.046 Uiso 1 1 calc R . . H31B H -0.3059 0.1171 0.2238 0.046 Uiso 1 1 calc R . . C32 C -0.2688(9) 0.1283(8) 0.1281(14) 0.059(5) Uiso 1 1 d . . . H32A H -0.2355 0.1391 0.1384 0.071 Uiso 1 1 calc R . . H32B H -0.2719 0.1069 0.0825 0.071 Uiso 1 1 calc R . . C33 C -0.2966(13) 0.1713(12) 0.121(2) 0.090(9) Uiso 1 1 d . . . H33A H -0.2860 0.1946 0.0824 0.135 Uiso 1 1 calc R . . H33B H -0.2951 0.1906 0.1673 0.135 Uiso 1 1 calc R . . H33C H -0.3291 0.1601 0.1065 0.135 Uiso 1 1 calc R . . C34 C -0.2209(14) 0.0307(13) 0.2079(19) 0.084(10) Uiso 1 1 d . . . H34A H -0.1945 0.0124 0.2367 0.101 Uiso 1 1 calc R . . H34B H -0.2071 0.0562 0.1747 0.101 Uiso 1 1 calc R . . C35 C -0.2502(14) -0.0126(14) 0.159(2) 0.084(10) Uiso 1 1 d . . . H35A H -0.2795 0.0045 0.1369 0.101 Uiso 1 1 calc R . . H35B H -0.2595 -0.0412 0.1918 0.101 Uiso 1 1 calc R . . C36 C -0.2232(15) -0.0405(14) 0.091(2) 0.078(11) Uiso 1 1 d . . . H36A H -0.2453 -0.0640 0.0622 0.116 Uiso 1 1 calc R . . H36B H -0.1962 -0.0613 0.1122 0.116 Uiso 1 1 calc R . . H36C H -0.2124 -0.0127 0.0592 0.116 Uiso 1 1 calc R . . N4 N -0.2255(12) 0.3615(11) 0.2562(19) 0.103(8) Uiso 1 1 d D . . C37 C -0.1948(16) 0.3158(17) 0.313(3) 0.118(11) Uiso 1 1 d . . . H37A H -0.2118 0.3079 0.3561 0.141 Uiso 1 1 calc R . . H37B H -0.1904 0.2822 0.2859 0.141 Uiso 1 1 calc R . . C38 C -0.1485(19) 0.3409(19) 0.336(3) 0.142(15) Uiso 1 1 d . . . H38A H -0.1532 0.3783 0.3505 0.170 Uiso 1 1 calc R . . H38B H -0.1287 0.3409 0.2941 0.170 Uiso 1 1 calc R . . C39 C -0.119(2) 0.3023(19) 0.415(3) 0.164(17) Uiso 1 1 d . . . H39A H -0.0882 0.3184 0.4304 0.246 Uiso 1 1 calc R . . H39B H -0.1143 0.2655 0.3999 0.246 Uiso 1 1 calc R . . H39C H -0.1385 0.3030 0.4562 0.246 Uiso 1 1 calc R . . C40 C -0.2535(19) 0.4048(17) 0.283(3) 0.140(16) Uiso 1 1 d . . . H40A H -0.2797 0.4130 0.2456 0.168 Uiso 1 1 calc R . . H40B H -0.2336 0.4369 0.2899 0.168 Uiso 1 1 calc R . . C41 C -0.2747(19) 0.3925(17) 0.358(3) 0.136(13) Uiso 1 1 d D . . H41A H -0.2948 0.3606 0.3500 0.163 Uiso 1 1 calc R . . H41B H -0.2481 0.3823 0.3941 0.163 Uiso 1 1 calc R . . C42 C -0.304(3) 0.435(2) 0.397(5) 0.27(4) Uiso 1 1 d D . . H42A H -0.3178 0.4190 0.4386 0.405 Uiso 1 1 calc R . . H42B H -0.3296 0.4485 0.3615 0.405 Uiso 1 1 calc R . . H42C H -0.2838 0.4648 0.4140 0.405 Uiso 1 1 calc R . . C43 C -0.2669(19) 0.3186(19) 0.216(3) 0.149(15) Uiso 1 1 d . . . H43A H -0.2587 0.3064 0.1671 0.179 Uiso 1 1 calc R . . H43B H -0.2712 0.2873 0.2474 0.179 Uiso 1 1 calc R . . C44 C -0.301(3) 0.346(3) 0.210(5) 0.24(3) Uiso 1 1 d D . . H44A H -0.2916 0.3829 0.1991 0.286 Uiso 1 1 calc R . . H44B H -0.3150 0.3465 0.2578 0.286 Uiso 1 1 calc R . . C45 C -0.338(3) 0.325(4) 0.148(5) 0.28(5) Uiso 1 1 d D . . H45A H -0.3641 0.3505 0.1408 0.425 Uiso 1 1 calc R . . H45B H -0.3498 0.2905 0.1619 0.425 Uiso 1 1 calc R . . H45C H -0.3231 0.3217 0.1020 0.425 Uiso 1 1 calc R . . C46 C -0.195(2) 0.3846(19) 0.197(3) 0.161(17) Uiso 1 1 d . . . H46A H -0.1869 0.3557 0.1638 0.193 Uiso 1 1 calc R . . H46B H -0.1649 0.3984 0.2223 0.193 Uiso 1 1 calc R . . C47 C -0.224(3) 0.436(3) 0.147(4) 0.30(4) Uiso 1 1 d D . . H47A H -0.2564 0.4254 0.1306 0.361 Uiso 1 1 calc R . . H47B H -0.2237 0.4686 0.1760 0.361 Uiso 1 1 calc R . . C48 C -0.195(3) 0.444(2) 0.079(4) 0.19(2) Uiso 1 1 d D . . H48A H -0.2070 0.4748 0.0516 0.287 Uiso 1 1 calc R . . H48B H -0.1986 0.4120 0.0478 0.287 Uiso 1 1 calc R . . H48C H -0.1619 0.4488 0.0963 0.287 Uiso 1 1 calc R . . N5 N 0.0870(10) 0.2334(10) -0.5642(15) 0.089(6) Uiso 1 1 d . . . C49 C 0.0705(16) 0.2109(14) -0.488(2) 0.121(11) Uiso 1 1 d . . . H49A H 0.0980 0.1945 -0.4591 0.145 Uiso 1 1 calc R . . H49B H 0.0601 0.2412 -0.4586 0.145 Uiso 1 1 calc R . . C50 C 0.0945(14) 0.1807(13) -0.617(2) 0.107(10) Uiso 1 1 d . . . H50A H 0.0650 0.1599 -0.6205 0.129 Uiso 1 1 calc R . . H50B H 0.0992 0.1936 -0.6665 0.129 Uiso 1 1 calc R . . C51 C 0.1357(16) 0.2675(15) -0.540(2) 0.125(12) Uiso 1 1 d . . . H51A H 0.1297 0.2974 -0.5070 0.149 Uiso 1 1 calc R . . H51B H 0.1606 0.2444 -0.5158 0.149 Uiso 1 1 calc R . . C52 C 0.0540(17) 0.2715(15) -0.604(3) 0.125(12) Uiso 1 1 d . . . H52A H 0.0278 0.2510 -0.6292 0.150 Uiso 1 1 calc R . . H52B H 0.0707 0.2895 -0.6418 0.150 Uiso 1 1 calc R . . C53 C 0.133(2) 0.144(2) -0.593(4) 0.19(2) Uiso 1 1 d . . . H53A H 0.1599 0.1672 -0.5747 0.229 Uiso 1 1 calc R . . H53B H 0.1234 0.1251 -0.5501 0.229 Uiso 1 1 calc R . . C54 C 0.1497(19) 0.2886(18) -0.617(3) 0.151(15) Uiso 1 1 d . . . H54A H 0.1630 0.2596 -0.6457 0.181 Uiso 1 1 calc R . . H54B H 0.1222 0.3039 -0.6470 0.181 Uiso 1 1 calc R . . C55 C 0.034(2) 0.313(2) -0.558(3) 0.21(2) Uiso 1 1 d D . . H55A H 0.0596 0.3325 -0.5294 0.250 Uiso 1 1 calc R . . H55B H 0.0146 0.2958 -0.5221 0.250 Uiso 1 1 calc R . . C58 C 0.1523(11) 0.1061(10) -0.6359(17) 0.081(7) Uiso 1 1 d . . . H58A H 0.1768 0.0865 -0.6059 0.121 Uiso 1 1 calc R . . H58B H 0.1661 0.1232 -0.6770 0.121 Uiso 1 1 calc R . . H58C H 0.1276 0.0814 -0.6551 0.121 Uiso 1 1 calc R . . C57 C 0.002(2) 0.355(2) -0.603(3) 0.19(2) Uiso 1 1 d D . . H57A H -0.0081 0.3829 -0.5705 0.284 Uiso 1 1 calc R . . H57B H -0.0263 0.3372 -0.6271 0.284 Uiso 1 1 calc R . . H57C H 0.0194 0.3712 -0.6410 0.284 Uiso 1 1 calc R . . C56 C 0.0310(18) 0.1702(15) -0.497(3) 0.132(13) Uiso 1 1 d . . . H56A H 0.0023 0.1855 -0.5230 0.158 Uiso 1 1 calc R . . H56B H 0.0406 0.1384 -0.5233 0.158 Uiso 1 1 calc R . . C59 C 0.184(2) 0.3285(17) -0.598(3) 0.164(16) Uiso 1 1 d . . . H59A H 0.2000 0.3386 -0.6410 0.247 Uiso 1 1 calc R . . H59B H 0.2077 0.3145 -0.5597 0.247 Uiso 1 1 calc R . . H59C H 0.1691 0.3598 -0.5785 0.247 Uiso 1 1 calc R . . C60 C 0.0234(17) 0.1569(15) -0.419(3) 0.128(13) Uiso 1 1 d . . . H60A H -0.0050 0.1351 -0.4183 0.192 Uiso 1 1 calc R . . H60B H 0.0196 0.1898 -0.3914 0.192 Uiso 1 1 calc R . . H60C H 0.0505 0.1371 -0.3963 0.192 Uiso 1 1 calc R . . N6 N -0.1829(9) 0.3020(9) -0.3046(14) 0.082(6) Uiso 1 1 d . . . C61 C -0.1820(5) 0.3257(5) -0.2236(7) 0.093(8) Uiso 1 1 d . . . H61A H -0.1747 0.2955 -0.1897 0.112 Uiso 1 1 calc R . . H61B H -0.1546 0.3499 -0.2174 0.112 Uiso 1 1 calc R . . C62 C -0.2277(5) 0.2654(5) -0.3150(7) 0.080(7) Uiso 1 1 d R . . H62A H -0.2354 0.2573 -0.3678 0.096 Uiso 1 1 calc R . . H62B H -0.2549 0.2838 -0.2968 0.096 Uiso 1 1 calc R . . C63 C -0.1987(5) 0.3512(5) -0.3658(7) 0.137(13) Uiso 1 1 d R . . H63A H -0.1995 0.3370 -0.4165 0.164 Uiso 1 1 calc R . . H63B H -0.2307 0.3639 -0.3582 0.164 Uiso 1 1 calc R . . C64 C -0.1409(5) 0.2836(5) -0.3218(7) 0.077(7) Uiso 1 1 d R . . H64A H -0.1330 0.2535 -0.2877 0.092 Uiso 1 1 calc R . . H64B H -0.1179 0.3120 -0.3071 0.092 Uiso 1 1 calc R . . C65 C -0.2172(5) 0.2112(5) -0.2700(7) 0.151(15) Uiso 1 1 d R . . H65A H -0.1841 0.2007 -0.2741 0.182 Uiso 1 1 calc R . . H65B H -0.2206 0.2180 -0.2174 0.182 Uiso 1 1 calc R . . C66 C -0.2177(5) 0.3519(5) -0.1975(7) 0.131(12) Uiso 1 1 d R . . H66A H -0.2426 0.3264 -0.1867 0.157 Uiso 1 1 calc R . . H66B H -0.2314 0.3774 -0.2348 0.157 Uiso 1 1 calc R . . C67 C -0.1686(5) 0.3916(5) -0.3579(7) 0.63(12) Uiso 1 1 d R . . H67A H -0.1361 0.3777 -0.3490 0.751 Uiso 1 1 calc R . . H67B H -0.1752 0.4132 -0.3148 0.751 Uiso 1 1 calc R . . C68 C -0.1281(5) 0.2637(5) -0.4001(7) 0.179(19) Uiso 1 1 d R . . H68A H -0.1551 0.2425 -0.4217 0.215 Uiso 1 1 calc R . . H68B H -0.1264 0.2957 -0.4313 0.215 Uiso 1 1 calc R . . C69 C -0.1729(5) 0.4292(5) -0.4318(7) 0.27(3) Uiso 1 1 d R . . H69A H -0.1504 0.4587 -0.4250 0.411 Uiso 1 1 calc R . . H69B H -0.2048 0.4434 -0.4402 0.411 Uiso 1 1 calc R . . H69C H -0.1658 0.4080 -0.4744 0.411 Uiso 1 1 calc R . . C70 C -0.2481(5) 0.1664(5) -0.2950(7) 0.144(13) Uiso 1 1 d R . . H70A H -0.2396 0.1350 -0.2650 0.216 Uiso 1 1 calc R . . H70B H -0.2444 0.1586 -0.3466 0.216 Uiso 1 1 calc R . . H70C H -0.2809 0.1759 -0.2898 0.216 Uiso 1 1 calc R . . C71 C -0.1975(5) 0.3856(5) -0.1179(7) 0.162(16) Uiso 1 1 d R . . H71A H -0.2236 0.4047 -0.0989 0.242 Uiso 1 1 calc R . . H71B H -0.1731 0.4110 -0.1290 0.242 Uiso 1 1 calc R . . H71C H -0.1842 0.3601 -0.0810 0.242 Uiso 1 1 calc R . . C72 C -0.0895(5) 0.2354(5) -0.4075(7) 0.136(13) Uiso 1 1 d R . . H72A H -0.0878 0.2270 -0.4595 0.203 Uiso 1 1 calc R . . H72B H -0.0906 0.2023 -0.3794 0.203 Uiso 1 1 calc R . . H72C H -0.0617 0.2559 -0.3890 0.203 Uiso 1 1 calc R . . OW1 O 0.1717(18) 0.1376(17) 0.152(3) 0.250(18) Uiso 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 V2AA 0.046(4) 0.058(4) 0.033(3) 0.001(3) 0.006(3) -0.012(3) V1AA 0.027(3) 0.035(3) 0.031(3) -0.003(3) -0.005(3) -0.005(3) V2B'A 0.031(4) 0.039(3) 0.037(3) 0.004(3) -0.004(3) -0.001(3) V2A'A 0.052(4) 0.043(4) 0.020(2) -0.001(3) -0.002(3) -0.014(3) V1A'A 0.037(4) 0.034(3) 0.030(3) -0.007(3) 0.005(3) -0.011(3) V2BA 0.041(4) 0.045(4) 0.048(4) 0.007(3) 0.001(4) 0.008(3) V3B'A 0.040(4) 0.041(3) 0.041(3) -0.003(3) 0.006(3) 0.005(3) V3A'A 0.041(4) 0.025(3) 0.038(3) 0.005(3) -0.005(3) 0.000(3) V3AA 0.037(4) 0.035(3) 0.025(3) 0.002(3) -0.005(3) 0.003(3) V3BA 0.035(4) 0.044(4) 0.031(3) -0.004(3) -0.003(3) -0.015(3) V2AB 0.027(3) 0.050(4) 0.029(3) -0.002(3) -0.011(3) -0.004(3) V1AB 0.031(4) 0.038(3) 0.029(3) -0.002(3) 0.005(3) 0.000(3) V2B'B 0.035(4) 0.045(4) 0.045(3) 0.005(3) -0.001(4) 0.000(3) V2A'B 0.035(4) 0.048(4) 0.039(3) 0.011(3) 0.001(4) 0.005(3) V1A'B 0.030(4) 0.040(3) 0.033(3) 0.006(3) 0.004(3) 0.006(3) V2BB 0.026(4) 0.052(4) 0.037(3) 0.004(3) -0.006(3) -0.001(3) V3B'B 0.030(3) 0.042(4) 0.035(3) -0.006(3) -0.013(3) -0.017(3) V3A'B 0.035(4) 0.042(3) 0.039(3) 0.001(3) 0.004(3) -0.009(3) V3AB 0.038(4) 0.035(3) 0.051(3) 0.003(3) 0.004(4) -0.007(3) V3BB 0.045(4) 0.033(3) 0.030(3) 0.001(3) 0.000(3) 0.002(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 V2AA OG1A 1.616(17) . ? V2AA OC3'A 1.665(16) . ? V2AA OD1A 1.808(19) . ? V2AA OC1A 2.03(2) . ? V2AA OE1A 2.09(3) . ? V2AA OA1A 2.335(18) . ? V2AA V1AA 3.059(9) . ? V2AA V2BA 3.059(7) . ? V2AA V3B'A 3.087(7) . ? V1AA OE2'A 1.668(19) . ? V1AA OE1A 1.68(2) . ? V1AA OB2'A 1.844(17) . ? V1AA OB1A 2.08(2) . ? V1AA OA1A 2.09(2) . ? V1AA OA1'A 2.120(19) . ? V1AA V2B'A 3.081(9) . ? V1AA V3B'A 3.116(8) . ? V2B'A OG2'A 1.61(3) . ? V2B'A OD1'A 1.753(19) . ? V2B'A OC2'A 1.77(2) . ? V2B'A OC4A 2.036(18) . ? V2B'A OE2'A 2.096(16) . ? V2B'A OA1'A 2.30(2) . ? V2B'A V2A'A 3.051(6) . ? V2B'A V3A'A 3.052(9) . ? V2A'A OG1'A 1.547(18) . ? V2A'A OC1'A 1.79(2) . ? V2A'A OD1'A 1.82(2) . ? V2A'A OC3A 1.888(18) . ? V2A'A OE1'A 2.09(3) . ? V2A'A OA1'A 2.35(2) . ? V2A'A V3A'A 3.102(8) . ? V2A'A V3BA 3.105(7) . ? V1A'A OE1'A 1.67(2) . ? V1A'A OE2A 1.70(2) . ? V1A'A OB2A 1.95(2) . ? V1A'A OB1'A 1.969(19) . ? V1A'A OA1A 2.090(17) . ? V1A'A OA1'A 2.11(2) . ? V1A'A V2BA 3.082(9) . ? V1A'A V3AA 3.113(7) . ? V1A'A V3BA 3.115(8) . ? V2BA OG2A 1.61(2) . ? V2BA OD1A 1.822(17) . ? V2BA OC4'A 1.92(2) . ? V2BA OC2A 2.00(2) . ? V2BA OE2A 2.03(2) . ? V2BA OA1A 2.34(2) . ? V2BA V3AA 3.073(9) . ? V2BA V3B'A 3.093(8) . ? V3B'A OF2'A 1.56(2) . ? V3B'A OC4'A 1.72(2) . ? V3B'A OB1'A 1.92(2) . ? V3B'A OC3'A 1.952(15) . ? V3B'A OB2'A 2.08(2) . ? V3B'A OA1A 2.357(19) . ? V3B'A V3A'A 3.067(9) . ? V3A'A OF1'A 1.57(2) . ? V3A'A OC2'A 1.84(2) . ? V3A'A OC1'A 1.85(2) . ? V3A'A OB1'A 1.94(2) . ? V3A'A OB2'A 1.998(17) . ? V3A'A OA1'A 2.30(2) . ? V3AA OF1A 1.62(2) . ? V3AA OC2A 1.66(2) . ? V3AA OB2A 1.88(2) . ? V3AA OC1A 1.96(2) . ? V3AA OB1A 2.13(3) . ? V3AA OA1A 2.189(18) . ? V3AA V3BA 3.112(9) . ? V3BA OF2A 1.60(2) . ? V3BA OC3A 1.744(19) . ? V3BA OB2A 1.89(3) . ? V3BA OC4A 1.92(2) . ? V3BA OB1A 2.11(2) . ? V3BA OA1'A 2.25(2) . ? V2AB OG1B 1.596(16) . ? V2AB OD1B 1.84(2) . ? V2AB OC3'B 1.881(18) . ? V2AB OC1B 1.98(2) . ? V2AB OE1B 2.00(2) . ? V2AB OA1B 2.222(17) . ? V2AB V1AB 3.049(9) . ? V2AB V3B'B 3.072(7) . ? V2AB V2BB 3.082(6) . ? V1AB OE1B 1.72(2) . ? V1AB OE2'B 1.74(2) . ? V1AB OB2'B 1.779(19) . ? V1AB OA1'B 2.045(19) . ? V1AB OA1B 2.063(19) . ? V1AB OB1B 2.089(18) . ? V1AB V2B'B 3.029(9) . ? V2B'B OG2'B 1.59(2) . ? V2B'B OC2'B 1.77(2) . ? V2B'B OD1'B 1.909(18) . ? V2B'B OC4B 1.96(2) . ? V2B'B OE2'B 1.99(2) . ? V2B'B OA1'B 2.29(2) . ? V2B'B V2A'B 3.080(7) . ? V2B'B V3A'B 3.097(9) . ? V2A'B OG1'B 1.615(17) . ? V2A'B OD1'B 1.75(2) . ? V2A'B OC1'B 1.92(2) . ? V2A'B OC3B 1.996(17) . ? V2A'B OE1'B 2.02(3) . ? V2A'B OA1'B 2.40(2) . ? V2A'B V1A'B 3.079(9) . ? V2A'B V3BB 3.092(7) . ? V2A'B V3A'B 3.099(9) . ? V1A'B OE1'B 1.69(2) . ? V1A'B OE2B 1.69(2) . ? V1A'B OB1'B 1.865(18) . ? V1A'B OB2B 1.937(16) . ? V1A'B OA1'B 2.11(2) . ? V1A'B OA1B 2.184(16) . ? V1A'B V3BB 3.112(9) . ? V1A'B V3AB 3.114(7) . ? V1A'B V2BB 3.119(9) . ? V2BB OG2B 1.62(3) . ? V2BB OC4'B 1.793(18) . ? V2BB OD1B 1.81(2) . ? V2BB OC2B 1.87(2) . ? V2BB OE2B 2.05(2) . ? V2BB OA1B 2.40(2) . ? V2BB V3B'B 3.095(8) . ? V2BB V3AB 3.109(9) . ? V3B'B OF2'B 1.620(19) . ? V3B'B OC3'B 1.785(17) . ? V3B'B OC4'B 1.81(2) . ? V3B'B OB1'B 2.026(18) . ? V3B'B OB2'B 2.03(2) . ? V3B'B OA1B 2.283(18) . ? V3B'B V3A'B 3.068(9) . ? V3A'B OF1'B 1.61(2) . ? V3A'B OC1'B 1.743(19) . ? V3A'B OC2'B 1.90(2) . ? V3A'B OB1'B 1.982(19) . ? V3A'B OB2'B 2.117(18) . ? V3A'B OA1'B 2.33(2) . ? V3AB OF1B 1.57(2) . ? V3AB OC2B 1.79(2) . ? V3AB OB2B 1.953(17) . ? V3AB OC1B 1.964(19) . ? V3AB OB1B 2.14(2) . ? V3AB OA1B 2.300(17) . ? V3BB OF2B 1.59(2) . ? V3BB OC3B 1.695(18) . ? V3BB OC4B 1.94(2) . ? V3BB OB2B 1.972(19) . ? V3BB OB1B 2.142(18) . ? V3BB OA1'B 2.26(2) . ? N1 C2 1.45(3) . ? N1 C4 1.47(3) . ? N1 C1 1.59(3) . ? N1 C3 1.71(4) . ? C1 C5 1.52(3) . ? C2 C6 1.51(3) . ? C3 C7 1.55(6) . ? C4 C8 1.54(8) . ? C5 C12 1.36(4) . ? C6 C11 1.40(4) . ? C7 C9 1.53(6) . ? C8 C10 1.40(6) . ? N2 C13 1.30(5) . ? N2 C14 1.53(3) . ? N2 C15 1.56(5) . ? N2 C16 1.58(3) . ? C13 C19 1.50(5) . ? C14 C18 1.53(3) . ? C15 C17 1.68(7) . ? C16 C20 1.50(2) . ? C17 C23 1.61(6) . ? C18 C22 1.47(3) . ? C19 C21 1.48(6) . ? C20 C24 1.48(4) . ? N3 C25 1.37(3) . ? N3 C28 1.48(2) . ? N3 C34 1.55(3) . ? N3 C31 1.649(17) . ? C25 C26 1.56(3) . ? C26 C27 1.82(5) . ? C28 C29 1.45(4) . ? C29 C30 1.41(4) . ? C31 C32 1.62(3) . ? C32 C33 1.32(4) . ? C34 C35 1.56(5) . ? C35 C36 1.64(4) . ? N4 C40 1.44(4) . ? N4 C46 1.53(4) . ? N4 C43 1.68(6) . ? N4 C37 1.69(6) . ? C37 C38 1.46(7) . ? C38 C39 1.84(9) . ? C40 C41 1.55(4) . ? C41 C42 1.54(2) . ? C43 C44 1.16(8) . ? C44 C45 1.54(2) . ? C46 C47 1.71(8) . ? C47 C48 1.51(2) . ? N5 C52 1.45(5) . ? N5 C49 1.59(4) . ? N5 C51 1.63(5) . ? N5 C50 1.63(4) . ? C49 C56 1.49(5) . ? C50 C53 1.44(7) . ? C51 C54 1.56(5) . ? C52 C55 1.47(6) . ? C53 C58 1.35(5) . ? C54 C59 1.40(6) . ? C55 C57 1.55(2) . ? C56 C60 1.46(5) . ? N6 C64 1.32(2) . ? N6 C62 1.54(3) . ? N6 C61 1.56(3) . ? N6 C63 1.67(3) . ? C61 C66 1.3125 . ? C62 C65 1.5722 . ? C63 C67 1.3056 . ? C64 C68 1.5581 . ? C65 C70 1.4476 . ? C66 C71 1.6995 . ? C67 C69 1.6104 . ? C68 C72 1.3029 . ? 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 OG1A V2AA OC3'A 106.9(8) . . ? OG1A V2AA OD1A 100.6(10) . . ? OC3'A V2AA OD1A 97.6(8) . . ? OG1A V2AA OC1A 94.8(8) . . ? OC3'A V2AA OC1A 157.1(10) . . ? OD1A V2AA OC1A 85.3(9) . . ? OG1A V2AA OE1A 102.6(9) . . ? OC3'A V2AA OE1A 89.3(9) . . ? OD1A V2AA OE1A 152.7(9) . . ? OC1A V2AA OE1A 78.6(10) . . ? OG1A V2AA OA1A 169.6(8) . . ? OC3'A V2AA OA1A 82.9(7) . . ? OD1A V2AA OA1A 81.0(8) . . ? OC1A V2AA OA1A 75.0(8) . . ? OE1A V2AA OA1A 73.6(8) . . ? OG1A V2AA V1AA 134.1(7) . . ? OC3'A V2AA V1AA 79.4(7) . . ? OD1A V2AA V1AA 124.0(7) . . ? OC1A V2AA V1AA 80.2(8) . . ? OE1A V2AA V1AA 31.5(5) . . ? OA1A V2AA V1AA 43.0(5) . . ? OG1A V2AA V2BA 133.3(8) . . ? OC3'A V2AA V2BA 85.7(5) . . ? OD1A V2AA V2BA 32.7(6) . . ? OC1A V2AA V2BA 84.7(5) . . ? OE1A V2AA V2BA 122.7(6) . . ? OA1A V2AA V2BA 49.2(5) . . ? V1AA V2AA V2BA 92.0(2) . . ? OG1A V2AA V3B'A 141.0(6) . . ? OC3'A V2AA V3B'A 34.3(5) . . ? OD1A V2AA V3B'A 85.5(5) . . ? OC1A V2AA V3B'A 124.2(7) . . ? OE1A V2AA V3B'A 85.5(6) . . ? OA1A V2AA V3B'A 49.2(5) . . ? V1AA V2AA V3B'A 60.94(19) . . ? V2BA V2AA V3B'A 60.43(16) . . ? OE2'A V1AA OE1A 102.9(10) . . ? OE2'A V1AA OB2'A 102.0(8) . . ? OE1A V1AA OB2'A 105.5(10) . . ? OE2'A V1AA OB1A 88.9(9) . . ? OE1A V1AA OB1A 90.7(10) . . ? OB2'A V1AA OB1A 157.6(7) . . ? OE2'A V1AA OA1A 161.7(8) . . ? OE1A V1AA OA1A 89.0(11) . . ? OB2'A V1AA OA1A 87.8(8) . . ? OB1A V1AA OA1A 77.0(9) . . ? OE2'A V1AA OA1'A 87.1(8) . . ? OE1A V1AA OA1'A 164.4(9) . . ? OB2'A V1AA OA1'A 83.6(8) . . ? OB1A V1AA OA1'A 77.4(8) . . ? OA1A V1AA OA1'A 78.6(8) . . ? OE2'A V1AA V2AA 143.5(5) . . ? OE1A V1AA V2AA 40.6(9) . . ? OB2'A V1AA V2AA 92.0(7) . . ? OB1A V1AA V2AA 90.6(8) . . ? OA1A V1AA V2AA 49.7(5) . . ? OA1'A V1AA V2AA 128.3(6) . . ? OE2'A V1AA V2B'A 39.9(5) . . ? OE1A V1AA V2B'A 142.9(9) . . ? OB2'A V1AA V2B'A 87.1(7) . . ? OB1A V1AA V2B'A 89.0(8) . . ? OA1A V1AA V2B'A 126.9(5) . . ? OA1'A V1AA V2B'A 48.3(6) . . ? V2AA V1AA V2B'A 176.5(2) . . ? OE2'A V1AA V3B'A 142.1(6) . . ? OE1A V1AA V3B'A 91.9(9) . . ? OB2'A V1AA V3B'A 40.2(6) . . ? OB1A V1AA V3B'A 126.0(7) . . ? OA1A V1AA V3B'A 49.1(5) . . ? OA1'A V1AA V3B'A 87.1(6) . . ? V2AA V1AA V3B'A 59.98(18) . . ? V2B'A V1AA V3B'A 117.7(2) . . ? OG2'A V2B'A OD1'A 104.8(14) . . ? OG2'A V2B'A OC2'A 104.0(12) . . ? OD1'A V2B'A OC2'A 92.9(9) . . ? OG2'A V2B'A OC4A 100.1(12) . . ? OD1'A V2B'A OC4A 86.9(8) . . ? OC2'A V2B'A OC4A 155.1(10) . . ? OG2'A V2B'A OE2'A 99.7(11) . . ? OD1'A V2B'A OE2'A 153.9(9) . . ? OC2'A V2B'A OE2'A 89.8(8) . . ? OC4A V2B'A OE2'A 80.0(7) . . ? OG2'A V2B'A OA1'A 171.6(11) . . ? OD1'A V2B'A OA1'A 81.5(9) . . ? OC2'A V2B'A OA1'A 80.8(9) . . ? OC4A V2B'A OA1'A 74.5(8) . . ? OE2'A V2B'A OA1'A 73.3(6) . . ? OG2'A V2B'A V2A'A 136.9(11) . . ? OD1'A V2B'A V2A'A 32.1(8) . . ? OC2'A V2B'A V2A'A 85.0(6) . . ? OC4A V2B'A V2A'A 81.7(5) . . ? OE2'A V2B'A V2A'A 122.8(5) . . ? OA1'A V2B'A V2A'A 49.6(5) . . ? OG2'A V2B'A V3A'A 136.9(10) . . ? OD1'A V2B'A V3A'A 82.8(8) . . ? OC2'A V2B'A V3A'A 33.0(7) . . ? OC4A V2B'A V3A'A 122.8(6) . . ? OE2'A V2B'A V3A'A 85.5(5) . . ? OA1'A V2B'A V3A'A 48.4(5) . . ? V2A'A V2B'A V3A'A 61.10(17) . . ? OG2'A V2B'A V1AA 130.1(10) . . ? OD1'A V2B'A V1AA 124.9(8) . . ? OC2'A V2B'A V1AA 79.1(8) . . ? OC4A V2B'A V1AA 80.7(7) . . ? OE2'A V2B'A V1AA 30.7(4) . . ? OA1'A V2B'A V1AA 43.4(5) . . ? V2A'A V2B'A V1AA 92.9(2) . . ? V3A'A V2B'A V1AA 61.35(18) . . ? OG1'A V2A'A OC1'A 99.8(9) . . ? OG1'A V2A'A OD1'A 102.9(10) . . ? OC1'A V2A'A OD1'A 90.1(10) . . ? OG1'A V2A'A OC3A 104.9(9) . . ? OC1'A V2A'A OC3A 154.6(10) . . ? OD1'A V2A'A OC3A 90.0(8) . . ? OG1'A V2A'A OE1'A 106.2(9) . . ? OC1'A V2A'A OE1'A 82.8(10) . . ? OD1'A V2A'A OE1'A 150.8(9) . . ? OC3A V2A'A OE1'A 84.8(9) . . ? OG1'A V2A'A OA1'A 177.9(9) . . ? OC1'A V2A'A OA1'A 79.0(8) . . ? OD1'A V2A'A OA1'A 78.9(9) . . ? OC3A V2A'A OA1'A 76.1(8) . . ? OE1'A V2A'A OA1'A 71.9(8) . . ? OG1'A V2A'A V2B'A 133.5(8) . . ? OC1'A V2A'A V2B'A 82.2(5) . . ? OD1'A V2A'A V2B'A 30.7(7) . . ? OC3A V2A'A V2B'A 85.1(5) . . ? OE1'A V2A'A V2B'A 120.1(6) . . ? OA1'A V2A'A V2B'A 48.3(5) . . ? OG1'A V2A'A V3A'A 131.6(6) . . ? OC1'A V2A'A V3A'A 31.9(6) . . ? OD1'A V2A'A V3A'A 80.3(7) . . ? OC3A V2A'A V3A'A 123.5(6) . . ? OE1'A V2A'A V3A'A 78.8(6) . . ? OA1'A V2A'A V3A'A 47.4(5) . . ? V2B'A V2A'A V3A'A 59.47(18) . . ? OG1'A V2A'A V3BA 134.8(6) . . ? OC1'A V2A'A V3BA 125.2(7) . . ? OD1'A V2A'A V3BA 82.9(6) . . ? OC3A V2A'A V3BA 29.9(6) . . ? OE1'A V2A'A V3BA 78.3(5) . . ? OA1'A V2A'A V3BA 46.3(5) . . ? V2B'A V2A'A V3BA 64.94(16) . . ? V3A'A V2A'A V3BA 93.66(19) . . ? OE1'A V1A'A OE2A 107.7(10) . . ? OE1'A V1A'A OB2A 99.9(10) . . ? OE2A V1A'A OB2A 95.2(10) . . ? OE1'A V1A'A OB1'A 96.3(9) . . ? OE2A V1A'A OB1'A 100.4(10) . . ? OB2A V1A'A OB1'A 152.8(7) . . ? OE1'A V1A'A OA1A 165.2(11) . . ? OE2A V1A'A OA1A 87.0(9) . . ? OB2A V1A'A OA1A 76.6(8) . . ? OB1'A V1A'A OA1A 82.2(7) . . ? OE1'A V1A'A OA1'A 86.5(10) . . ? OE2A V1A'A OA1'A 165.4(9) . . ? OB2A V1A'A OA1'A 78.5(9) . . ? OB1'A V1A'A OA1'A 80.9(8) . . ? OA1A V1A'A OA1'A 78.7(8) . . ? OE1'A V1A'A V2BA 145.5(8) . . ? OE2A V1A'A V2BA 38.0(6) . . ? OB2A V1A'A V2BA 89.8(8) . . ? OB1'A V1A'A V2BA 89.0(7) . . ? OA1A V1A'A V2BA 49.3(6) . . ? OA1'A V1A'A V2BA 128.0(6) . . ? OE1'A V1A'A V3AA 134.5(7) . . ? OE2A V1A'A V3AA 80.7(6) . . ? OB2A V1A'A V3AA 34.8(7) . . ? OB1'A V1A'A V3AA 126.7(5) . . ? OA1A V1A'A V3AA 44.6(5) . . ? OA1'A V1A'A V3AA 86.8(5) . . ? V2BA V1A'A V3AA 59.47(19) . . ? OE1'A V1A'A V3BA 83.8(8) . . ? OE2A V1A'A V3BA 130.0(7) . . ? OB2A V1A'A V3BA 35.1(7) . . ? OB1'A V1A'A V3BA 127.2(6) . . ? OA1A V1A'A V3BA 85.4(6) . . ? OA1'A V1A'A V3BA 46.3(6) . . ? V2BA V1A'A V3BA 119.4(2) . . ? V3AA V1A'A V3BA 59.96(18) . . ? OG2A V2BA OD1A 105.9(10) . . ? OG2A V2BA OC4'A 104.8(11) . . ? OD1A V2BA OC4'A 95.2(8) . . ? OG2A V2BA OC2A 101.2(10) . . ? OD1A V2BA OC2A 87.9(8) . . ? OC4'A V2BA OC2A 151.9(11) . . ? OG2A V2BA OE2A 99.6(9) . . ? OD1A V2BA OE2A 153.2(10) . . ? OC4'A V2BA OE2A 85.8(9) . . ? OC2A V2BA OE2A 79.4(8) . . ? OG2A V2BA OA1A 172.2(10) . . ? OD1A V2BA OA1A 80.6(8) . . ? OC4'A V2BA OA1A 78.5(9) . . ? OC2A V2BA OA1A 74.4(8) . . ? OE2A V2BA OA1A 73.3(7) . . ? OG2A V2BA V2AA 138.0(8) . . ? OD1A V2BA V2AA 32.4(7) . . ? OC4'A V2BA V2AA 81.7(5) . . ? OC2A V2BA V2AA 86.3(5) . . ? OE2A V2BA V2AA 122.4(7) . . ? OA1A V2BA V2AA 49.1(4) . . ? OG2A V2BA V3AA 130.7(8) . . ? OD1A V2BA V3AA 79.8(7) . . ? OC4'A V2BA V3AA 123.7(8) . . ? OC2A V2BA V3AA 29.6(6) . . ? OE2A V2BA V3AA 77.5(6) . . ? OA1A V2BA V3AA 45.2(4) . . ? V2AA V2BA V3AA 64.51(18) . . ? OG2A V2BA V1A'A 130.5(8) . . ? OD1A V2BA V1A'A 123.3(7) . . ? OC4'A V2BA V1A'A 77.7(8) . . ? OC2A V2BA V1A'A 77.3(7) . . ? OE2A V2BA V1A'A 30.9(6) . . ? OA1A V2BA V1A'A 42.7(4) . . ? V2AA V2BA V1A'A 91.5(2) . . ? V3AA V2BA V1A'A 60.75(19) . . ? OG2A V2BA V3B'A 134.6(8) . . ? OD1A V2BA V3B'A 85.1(6) . . ? OC4'A V2BA V3B'A 29.9(7) . . ? OC2A V2BA V3B'A 123.5(7) . . ? OE2A V2BA V3B'A 82.6(6) . . ? OA1A V2BA V3B'A 49.1(5) . . ? V2AA V2BA V3B'A 60.23(17) . . ? V3AA V2BA V3B'A 94.2(2) . . ? V1A'A V2BA V3B'A 61.17(19) . . ? OF2'A V3B'A OC4'A 105.8(12) . . ? OF2'A V3B'A OB1'A 102.7(11) . . ? OC4'A V3B'A OB1'A 93.4(10) . . ? OF2'A V3B'A OC3'A 102.3(10) . . ? OC4'A V3B'A OC3'A 93.0(9) . . ? OB1'A V3B'A OC3'A 151.3(8) . . ? OF2'A V3B'A OB2'A 96.7(11) . . ? OC4'A V3B'A OB2'A 156.3(10) . . ? OB1'A V3B'A OB2'A 74.4(8) . . ? OC3'A V3B'A OB2'A 89.0(7) . . ? OF2'A V3B'A OA1A 172.4(11) . . ? OC4'A V3B'A OA1A 81.8(9) . . ? OB1'A V3B'A OA1A 76.5(7) . . ? OC3'A V3B'A OA1A 76.8(7) . . ? OB2'A V3B'A OA1A 75.7(7) . . ? OF2'A V3B'A V3A'A 90.1(11) . . ? OC4'A V3B'A V3A'A 131.0(8) . . ? OB1'A V3B'A V3A'A 37.6(6) . . ? OC3'A V3B'A V3A'A 129.1(6) . . ? OB2'A V3B'A V3A'A 40.2(5) . . ? OA1A V3B'A V3A'A 84.8(6) . . ? OF2'A V3B'A V2AA 131.1(9) . . ? OC4'A V3B'A V2AA 83.7(7) . . ? OB1'A V3B'A V2AA 124.9(6) . . ? OC3'A V3B'A V2AA 28.7(5) . . ? OB2'A V3B'A V2AA 86.8(5) . . ? OA1A V3B'A V2AA 48.6(4) . . ? V3A'A V3B'A V2AA 119.9(3) . . ? OF2'A V3B'A V2BA 139.0(10) . . ? OC4'A V3B'A V2BA 33.7(7) . . ? OB1'A V3B'A V2BA 89.7(6) . . ? OC3'A V3B'A V2BA 80.4(5) . . ? OB2'A V3B'A V2BA 124.3(5) . . ? OA1A V3B'A V2BA 48.5(5) . . ? V3A'A V3B'A V2BA 120.2(2) . . ? V2AA V3B'A V2BA 59.34(17) . . ? OF2'A V3B'A V1AA 130.3(9) . . ? OC4'A V3B'A V1AA 123.8(7) . . ? OB1'A V3B'A V1AA 78.8(6) . . ? OC3'A V3B'A V1AA 74.4(6) . . ? OB2'A V3B'A V1AA 34.9(5) . . ? OA1A V3B'A V1AA 42.1(5) . . ? V3A'A V3B'A V1AA 60.80(18) . . ? V2AA V3B'A V1AA 59.08(19) . . ? V2BA V3B'A V1AA 90.2(2) . . ? OF1'A V3A'A OC2'A 100.6(11) . . ? OF1'A V3A'A OC1'A 104.7(10) . . ? OC2'A V3A'A OC1'A 92.1(10) . . ? OF1'A V3A'A OB1'A 102.2(11) . . ? OC2'A V3A'A OB1'A 153.8(8) . . ? OC1'A V3A'A OB1'A 94.5(9) . . ? OF1'A V3A'A OB2'A 100.3(10) . . ? OC2'A V3A'A OB2'A 87.5(8) . . ? OC1'A V3A'A OB2'A 154.6(8) . . ? OB1'A V3A'A OB2'A 75.9(8) . . ? OF1'A V3A'A OA1'A 176.2(9) . . ? OC2'A V3A'A OA1'A 79.4(8) . . ? OC1'A V3A'A OA1'A 79.2(8) . . ? OB1'A V3A'A OA1'A 77.0(8) . . ? OB2'A V3A'A OA1'A 75.8(7) . . ? OF1'A V3A'A V2B'A 131.9(9) . . ? OC2'A V3A'A V2B'A 31.5(6) . . ? OC1'A V3A'A V2B'A 81.3(7) . . ? OB1'A V3A'A V2B'A 125.2(6) . . ? OB2'A V3A'A V2B'A 85.3(6) . . ? OA1'A V3A'A V2B'A 48.4(6) . . ? OF1'A V3A'A V3B'A 91.8(10) . . ? OC2'A V3A'A V3B'A 129.8(7) . . ? OC1'A V3A'A V3B'A 131.5(7) . . ? OB1'A V3A'A V3B'A 37.1(5) . . ? OB2'A V3A'A V3B'A 42.3(6) . . ? OA1'A V3A'A V3B'A 85.3(6) . . ? V2B'A V3A'A V3B'A 120.1(2) . . ? OF1'A V3A'A V2A'A 135.1(8) . . ? OC2'A V3A'A V2A'A 82.3(7) . . ? OC1'A V3A'A V2A'A 30.8(6) . . ? OB1'A V3A'A V2A'A 90.5(6) . . ? OB2'A V3A'A V2A'A 124.6(5) . . ? OA1'A V3A'A V2A'A 48.7(5) . . ? V2B'A V3A'A V2A'A 59.43(18) . . ? V3B'A V3A'A V2A'A 120.8(2) . . ? OF1A V3AA OC2A 106.2(11) . . ? OF1A V3AA OB2A 100.2(11) . . ? OC2A V3AA OB2A 97.0(9) . . ? OF1A V3AA OC1A 100.2(10) . . ? OC2A V3AA OC1A 98.1(11) . . ? OB2A V3AA OC1A 150.1(9) . . ? OF1A V3AA OB1A 94.3(11) . . ? OC2A V3AA OB1A 158.6(9) . . ? OB2A V3AA OB1A 72.9(9) . . ? OC1A V3AA OB1A 83.9(9) . . ? OF1A V3AA OA1A 168.1(11) . . ? OC2A V3AA OA1A 85.5(9) . . ? OB2A V3AA OA1A 75.7(8) . . ? OC1A V3AA OA1A 79.9(8) . . ? OB1A V3AA OA1A 73.9(8) . . ? OF1A V3AA V2BA 142.5(9) . . ? OC2A V3AA V2BA 36.6(7) . . ? OB2A V3AA V2BA 91.6(7) . . ? OC1A V3AA V2BA 85.4(8) . . ? OB1A V3AA V2BA 123.2(6) . . ? OA1A V3AA V2BA 49.4(6) . . ? OF1A V3AA V3BA 86.6(10) . . ? OC2A V3AA V3BA 131.2(7) . . ? OB2A V3AA V3BA 34.3(7) . . ? OC1A V3AA V3BA 126.3(8) . . ? OB1A V3AA V3BA 42.4(6) . . ? OA1A V3AA V3BA 83.9(6) . . ? V2BA V3AA V3BA 119.8(2) . . ? OF1A V3AA V1A'A 136.2(8) . . ? OC2A V3AA V1A'A 80.9(7) . . ? OB2A V3AA V1A'A 36.5(7) . . ? OC1A V3AA V1A'A 122.0(6) . . ? OB1A V3AA V1A'A 80.1(5) . . ? OA1A V3AA V1A'A 42.1(5) . . ? V2BA V3AA V1A'A 59.78(19) . . ? V3BA V3AA V1A'A 60.06(18) . . ? OF2A V3BA OC3A 107.0(11) . . ? OF2A V3BA OB2A 105.8(13) . . ? OC3A V3BA OB2A 101.0(9) . . ? OF2A V3BA OC4A 97.2(11) . . ? OC3A V3BA OC4A 90.2(9) . . ? OB2A V3BA OC4A 150.0(10) . . ? OF2A V3BA OB1A 97.4(11) . . ? OC3A V3BA OB1A 155.5(9) . . ? OB2A V3BA OB1A 73.4(9) . . ? OC4A V3BA OB1A 84.8(9) . . ? OF2A V3BA OA1'A 170.3(9) . . ? OC3A V3BA OA1'A 81.4(8) . . ? OB2A V3BA OA1'A 76.5(9) . . ? OC4A V3BA OA1'A 77.8(8) . . ? OB1A V3BA OA1'A 74.1(8) . . ? OF2A V3BA V2A'A 139.3(10) . . ? OC3A V3BA V2A'A 32.7(6) . . ? OB2A V3BA V2A'A 92.5(6) . . ? OC4A V3BA V2A'A 81.9(5) . . ? OB1A V3BA V2A'A 122.9(6) . . ? OA1'A V3BA V2A'A 48.8(5) . . ? OF2A V3BA V3AA 92.2(11) . . ? OC3A V3BA V3AA 135.1(8) . . ? OB2A V3BA V3AA 34.1(6) . . ? OC4A V3BA V3AA 127.9(6) . . ? OB1A V3BA V3AA 43.1(7) . . ? OA1'A V3BA V3AA 84.6(7) . . ? V2A'A V3BA V3AA 120.4(2) . . ? OF2A V3BA V1A'A 141.6(10) . . ? OC3A V3BA V1A'A 81.6(7) . . ? OB2A V3BA V1A'A 36.5(6) . . ? OC4A V3BA V1A'A 120.5(6) . . ? OB1A V3BA V1A'A 80.4(7) . . ? OA1'A V3BA V1A'A 42.7(6) . . ? V2A'A V3BA V1A'A 60.48(18) . . ? V3AA V3BA V1A'A 59.98(19) . . ? V1AA OE1A V2AA 107.9(10) . . ? V1AA OE2'A V2B'A 109.4(6) . . ? V2B'A OD1'A V2A'A 117.2(14) . . ? V1A'A OE1'A V2A'A 112.5(9) . . ? V1A'A OE2A V2BA 111.0(8) . . ? V2AA OD1A V2BA 114.9(12) . . ? V2AA OC3'A V3B'A 116.9(9) . . ? V1AA OB2'A V3A'A 109.0(9) . . ? V1AA OB2'A V3B'A 104.9(9) . . ? V3A'A OB2'A V3B'A 97.5(7) . . ? V2B'A OC2'A V3A'A 115.6(10) . . ? V2A'A OC1'A V3A'A 117.3(10) . . ? V3B'A OB1'A V3A'A 105.3(8) . . ? V3B'A OB1'A V1A'A 107.9(9) . . ? V3A'A OB1'A V1A'A 107.4(11) . . ? V3B'A OC4'A V2BA 116.5(12) . . ? V3AA OC1A V2AA 109.9(9) . . ? V1AA OB1A V3BA 106.9(9) . . ? V1AA OB1A V3AA 104.7(12) . . ? V3BA OB1A V3AA 94.4(7) . . ? V3BA OC4A V2B'A 113.2(10) . . ? V3BA OC3A V2A'A 117.4(11) . . ? V3AA OB2A V3BA 111.6(9) . . ? V3AA OB2A V1A'A 108.7(12) . . ? V3BA OB2A V1A'A 108.4(11) . . ? V3AA OC2A V2BA 113.9(10) . . ? V1A'A OA1A V1AA 101.9(9) . . ? V1A'A OA1A V3AA 93.3(7) . . ? V1AA OA1A V3AA 102.6(8) . . ? V1A'A OA1A V2AA 167.7(11) . . ? V1AA OA1A V2AA 87.3(6) . . ? V3AA OA1A V2AA 92.6(7) . . ? V1A'A OA1A V2BA 88.0(6) . . ? V1AA OA1A V2BA 166.7(10) . . ? V3AA OA1A V2BA 85.4(7) . . ? V2AA OA1A V2BA 81.8(7) . . ? V1A'A OA1A V3B'A 89.7(6) . . ? V1AA OA1A V3B'A 88.8(6) . . ? V3AA OA1A V3B'A 167.3(11) . . ? V2AA OA1A V3B'A 82.3(6) . . ? V2BA OA1A V3B'A 82.4(7) . . ? V1A'A OA1'A V1AA 100.1(10) . . ? V1A'A OA1'A V3BA 91.0(7) . . ? V1AA OA1'A V3BA 100.6(7) . . ? V1A'A OA1'A V3A'A 91.1(8) . . ? V1AA OA1'A V3A'A 90.1(7) . . ? V3BA OA1'A V3A'A 168.6(11) . . ? V1A'A OA1'A V2B'A 169.9(9) . . ? V1AA OA1'A V2B'A 88.3(6) . . ? V3BA OA1'A V2B'A 93.1(9) . . ? V3A'A OA1'A V2B'A 83.2(7) . . ? V1A'A OA1'A V2A'A 89.1(6) . . ? V1AA OA1'A V2A'A 169.2(11) . . ? V3BA OA1'A V2A'A 84.9(7) . . ? V3A'A OA1'A V2A'A 83.8(6) . . ? V2B'A OA1'A V2A'A 82.1(8) . . ? OG1B V2AB OD1B 109.8(11) . . ? OG1B V2AB OC3'B 102.9(8) . . ? OD1B V2AB OC3'B 91.8(9) . . ? OG1B V2AB OC1B 99.9(7) . . ? OD1B V2AB OC1B 87.8(9) . . ? OC3'B V2AB OC1B 155.8(9) . . ? OG1B V2AB OE1B 93.0(8) . . ? OD1B V2AB OE1B 156.9(10) . . ? OC3'B V2AB OE1B 86.4(9) . . ? OC1B V2AB OE1B 84.5(9) . . ? OG1B V2AB OA1B 167.1(9) . . ? OD1B V2AB OA1B 82.8(9) . . ? OC3'B V2AB OA1B 78.9(7) . . ? OC1B V2AB OA1B 77.1(7) . . ? OE1B V2AB OA1B 74.3(7) . . ? OG1B V2AB V1AB 124.9(7) . . ? OD1B V2AB V1AB 125.3(8) . . ? OC3'B V2AB V1AB 77.5(7) . . ? OC1B V2AB V1AB 83.0(7) . . ? OE1B V2AB V1AB 32.1(5) . . ? OA1B V2AB V1AB 42.6(5) . . ? OG1B V2AB V3B'B 135.0(6) . . ? OD1B V2AB V3B'B 80.8(7) . . ? OC3'B V2AB V3B'B 32.1(5) . . ? OC1B V2AB V3B'B 124.6(6) . . ? OE1B V2AB V3B'B 85.7(5) . . ? OA1B V2AB V3B'B 47.8(5) . . ? V1AB V2AB V3B'B 62.01(18) . . ? OG1B V2AB V2BB 141.8(8) . . ? OD1B V2AB V2BB 32.1(8) . . ? OC3'B V2AB V2BB 84.8(5) . . ? OC1B V2AB V2BB 82.2(5) . . ? OE1B V2AB V2BB 125.0(5) . . ? OA1B V2AB V2BB 50.8(5) . . ? V1AB V2AB V2BB 93.3(2) . . ? V3B'B V2AB V2BB 60.39(17) . . ? OE1B V1AB OE2'B 107.0(9) . . ? OE1B V1AB OB2'B 99.1(10) . . ? OE2'B V1AB OB2'B 100.1(9) . . ? OE1B V1AB OA1'B 163.2(9) . . ? OE2'B V1AB OA1'B 87.5(9) . . ? OB2'B V1AB OA1'B 86.2(8) . . ? OE1B V1AB OA1B 84.5(9) . . ? OE2'B V1AB OA1B 167.4(9) . . ? OB2'B V1AB OA1B 82.6(8) . . ? OA1'B V1AB OA1B 80.3(8) . . ? OE1B V1AB OB1B 91.8(8) . . ? OE2'B V1AB OB1B 95.8(9) . . ? OB2'B V1AB OB1B 157.1(7) . . ? OA1'B V1AB OB1B 78.1(7) . . ? OA1B V1AB OB1B 78.4(8) . . ? OE1B V1AB V2B'B 145.6(7) . . ? OE2'B V1AB V2B'B 38.6(6) . . ? OB2'B V1AB V2B'B 92.0(8) . . ? OA1'B V1AB V2B'B 49.1(7) . . ? OA1B V1AB V2B'B 129.4(5) . . ? OB1B V1AB V2B'B 90.2(7) . . ? OE1B V1AB V2AB 38.2(7) . . ? OE2'B V1AB V2AB 145.2(6) . . ? OB2'B V1AB V2AB 87.3(8) . . ? OA1'B V1AB V2AB 127.1(7) . . ? OA1B V1AB V2AB 46.8(5) . . ? OB1B V1AB V2AB 88.9(6) . . ? V2B'B V1AB V2AB 176.2(2) . . ? OG2'B V2B'B OC2'B 104.6(11) . . ? OG2'B V2B'B OD1'B 104.4(11) . . ? OC2'B V2B'B OD1'B 94.7(8) . . ? OG2'B V2B'B OC4B 98.1(10) . . ? OC2'B V2B'B OC4B 156.2(11) . . ? OD1'B V2B'B OC4B 86.4(8) . . ? OG2'B V2B'B OE2'B 98.6(10) . . ? OC2'B V2B'B OE2'B 84.9(9) . . ? OD1'B V2B'B OE2'B 156.3(9) . . ? OC4B V2B'B OE2'B 84.7(8) . . ? OG2'B V2B'B OA1'B 171.3(9) . . ? OC2'B V2B'B OA1'B 81.4(9) . . ? OD1'B V2B'B OA1'B 81.1(8) . . ? OC4B V2B'B OA1'B 75.3(9) . . ? OE2'B V2B'B OA1'B 75.4(8) . . ? OG2'B V2B'B V1AB 131.7(8) . . ? OC2'B V2B'B V1AB 78.9(8) . . ? OD1'B V2B'B V1AB 123.5(7) . . ? OC4B V2B'B V1AB 80.7(8) . . ? OE2'B V2B'B V1AB 33.1(6) . . ? OA1'B V2B'B V1AB 42.4(5) . . ? OG2'B V2B'B V2A'B 135.4(8) . . ? OC2'B V2B'B V2A'B 85.7(6) . . ? OD1'B V2B'B V2A'B 31.0(7) . . ? OC4B V2B'B V2A'B 83.1(5) . . ? OE2'B V2B'B V2A'B 125.8(7) . . ? OA1'B V2B'B V2A'B 50.4(5) . . ? V1AB V2B'B V2A'B 92.7(2) . . ? OG2'B V2B'B V3A'B 138.2(7) . . ? OC2'B V2B'B V3A'B 33.9(7) . . ? OD1'B V2B'B V3A'B 82.0(7) . . ? OC4B V2B'B V3A'B 123.6(7) . . ? OE2'B V2B'B V3A'B 84.7(6) . . ? OA1'B V2B'B V3A'B 48.4(5) . . ? V1AB V2B'B V3A'B 61.81(19) . . ? V2A'B V2B'B V3A'B 60.23(18) . . ? OG1'B V2A'B OD1'B 109.3(10) . . ? OG1'B V2A'B OC1'B 105.1(8) . . ? OD1'B V2A'B OC1'B 94.7(9) . . ? OG1'B V2A'B OC3B 98.1(8) . . ? OD1'B V2A'B OC3B 92.9(8) . . ? OC1'B V2A'B OC3B 151.6(9) . . ? OG1'B V2A'B OE1'B 95.1(9) . . ? OD1'B V2A'B OE1'B 155.0(9) . . ? OC1'B V2A'B OE1'B 83.7(9) . . ? OC3B V2A'B OE1'B 78.1(9) . . ? OG1'B V2A'B OA1'B 168.3(9) . . ? OD1'B V2A'B OA1'B 81.4(8) . . ? OC1'B V2A'B OA1'B 78.0(7) . . ? OC3B V2A'B OA1'B 76.1(7) . . ? OE1'B V2A'B OA1'B 73.9(8) . . ? OG1'B V2A'B V1A'B 125.8(7) . . ? OD1'B V2A'B V1A'B 124.6(7) . . ? OC1'B V2A'B V1A'B 77.4(7) . . ? OC3B V2A'B V1A'B 75.7(7) . . ? OE1'B V2A'B V1A'B 30.7(5) . . ? OA1'B V2A'B V1A'B 43.2(5) . . ? OG1'B V2A'B V2B'B 143.5(8) . . ? OD1'B V2A'B V2B'B 34.2(7) . . ? OC1'B V2A'B V2B'B 83.1(5) . . ? OC3B V2A'B V2B'B 87.9(4) . . ? OE1'B V2A'B V2B'B 121.3(6) . . ? OA1'B V2A'B V2B'B 47.5(5) . . ? V1A'B V2A'B V2B'B 90.6(2) . . ? OG1'B V2A'B V3BB 128.3(6) . . ? OD1'B V2A'B V3BB 82.6(6) . . ? OC1'B V2A'B V3BB 124.4(6) . . ? OC3B V2A'B V3BB 30.2(5) . . ? OE1'B V2A'B V3BB 78.0(5) . . ? OA1'B V2A'B V3BB 46.5(5) . . ? V1A'B V2A'B V3BB 60.57(19) . . ? V2B'B V2A'B V3BB 64.03(17) . . ? OG1'B V2A'B V3A'B 135.5(6) . . ? OD1'B V2A'B V3A'B 84.4(7) . . ? OC1'B V2A'B V3A'B 30.5(5) . . ? OC3B V2A'B V3A'B 123.9(6) . . ? OE1'B V2A'B V3A'B 81.7(7) . . ? OA1'B V2A'B V3A'B 48.1(5) . . ? V1A'B V2A'B V3A'B 61.3(2) . . ? V2B'B V2A'B V3A'B 60.15(18) . . ? V3BB V2A'B V3A'B 94.6(2) . . ? OE1'B V1A'B OE2B 108.1(10) . . ? OE1'B V1A'B OB1'B 97.1(9) . . ? OE2B V1A'B OB1'B 95.2(10) . . ? OE1'B V1A'B OB2B 94.8(9) . . ? OE2B V1A'B OB2B 96.6(9) . . ? OB1'B V1A'B OB2B 159.8(6) . . ? OE1'B V1A'B OA1'B 88.4(11) . . ? OE2B V1A'B OA1'B 163.5(9) . . ? OB1'B V1A'B OA1'B 82.2(8) . . ? OB2B V1A'B OA1'B 81.9(7) . . ? OE1'B V1A'B OA1B 164.4(10) . . ? OE2B V1A'B OA1B 87.4(8) . . ? OB1'B V1A'B OA1B 81.8(6) . . ? OB2B V1A'B OA1B 82.4(6) . . ? OA1'B V1A'B OA1B 76.1(8) . . ? OE1'B V1A'B V2A'B 37.5(8) . . ? OE2B V1A'B V2A'B 145.5(7) . . ? OB1'B V1A'B V2A'B 88.5(7) . . ? OB2B V1A'B V2A'B 91.0(6) . . ? OA1'B V1A'B V2A'B 50.9(6) . . ? OA1B V1A'B V2A'B 127.0(5) . . ? OE1'B V1A'B V3BB 81.8(8) . . ? OE2B V1A'B V3BB 134.2(7) . . ? OB1'B V1A'B V3BB 128.7(6) . . ? OB2B V1A'B V3BB 37.6(5) . . ? OA1'B V1A'B V3BB 46.6(6) . . ? OA1B V1A'B V3BB 86.8(5) . . ? V2A'B V1A'B V3BB 59.93(19) . . ? OE1'B V1A'B V3AB 131.7(8) . . ? OE2B V1A'B V3AB 83.1(6) . . ? OB1'B V1A'B V3AB 129.4(5) . . ? OB2B V1A'B V3AB 37.0(5) . . ? OA1'B V1A'B V3AB 86.1(5) . . ? OA1B V1A'B V3AB 47.6(4) . . ? V2A'B V1A'B V3AB 120.3(3) . . ? V3BB V1A'B V3AB 60.36(19) . . ? OE1'B V1A'B V2BB 145.4(9) . . ? OE2B V1A'B V2BB 37.2(6) . . ? OB1'B V1A'B V2BB 89.1(7) . . ? OB2B V1A'B V2BB 90.4(6) . . ? OA1'B V1A'B V2BB 126.3(6) . . ? OA1B V1A'B V2BB 50.2(5) . . ? V2A'B V1A'B V2BB 176.6(2) . . ? V3BB V1A'B V2BB 120.2(2) . . ? V3AB V1A'B V2BB 59.8(2) . . ? OG2B V2BB OC4'B 103.7(11) . . ? OG2B V2BB OD1B 103.4(12) . . ? OC4'B V2BB OD1B 88.6(8) . . ? OG2B V2BB OC2B 100.0(11) . . ? OC4'B V2BB OC2B 155.4(11) . . ? OD1B V2BB OC2B 92.2(9) . . ? OG2B V2BB OE2B 104.0(10) . . ? OC4'B V2BB OE2B 84.2(9) . . ? OD1B V2BB OE2B 152.6(11) . . ? OC2B V2BB OE2B 83.8(9) . . ? OG2B V2BB OA1B 177.6(10) . . ? OC4'B V2BB OA1B 77.9(8) . . ? OD1B V2BB OA1B 78.4(10) . . ? OC2B V2BB OA1B 78.2(8) . . ? OE2B V2BB OA1B 74.3(7) . . ? OG2B V2BB V2AB 136.0(9) . . ? OC4'B V2BB V2AB 81.6(5) . . ? OD1B V2BB V2AB 32.6(9) . . ? OC2B V2BB V2AB 85.9(5) . . ? OE2B V2BB V2AB 120.0(7) . . ? OA1B V2BB V2AB 45.8(4) . . ? OG2B V2BB V3B'B 134.7(9) . . ? OC4'B V2BB V3B'B 31.0(6) . . ? OD1B V2BB V3B'B 80.5(7) . . ? OC2B V2BB V3B'B 125.2(7) . . ? OE2B V2BB V3B'B 79.8(6) . . ? OA1B V2BB V3B'B 47.0(4) . . ? V2AB V2BB V3B'B 59.65(16) . . ? OG2B V2BB V3AB 131.0(9) . . ? OC4'B V2BB V3AB 125.0(7) . . ? OD1B V2BB V3AB 84.3(8) . . ? OC2B V2BB V3AB 31.0(7) . . ? OE2B V2BB V3AB 78.3(6) . . ? OA1B V2BB V3AB 47.2(4) . . ? V2AB V2BB V3AB 64.12(17) . . ? V3B'B V2BB V3AB 94.2(2) . . ? OG2B V2BB V1A'B 134.0(8) . . ? OC4'B V2BB V1A'B 79.6(7) . . ? OD1B V2BB V1A'B 122.6(9) . . ? OC2B V2BB V1A'B 79.3(7) . . ? OE2B V2BB V1A'B 30.0(6) . . ? OA1B V2BB V1A'B 44.3(4) . . ? V2AB V2BB V1A'B 90.0(2) . . ? V3B'B V2BB V1A'B 61.18(18) . . ? V3AB V2BB V1A'B 59.99(19) . . ? OF2'B V3B'B OC3'B 101.9(9) . . ? OF2'B V3B'B OC4'B 103.0(10) . . ? OC3'B V3B'B OC4'B 95.0(9) . . ? OF2'B V3B'B OB1'B 102.1(9) . . ? OC3'B V3B'B OB1'B 152.8(9) . . ? OC4'B V3B'B OB1'B 92.2(8) . . ? OF2'B V3B'B OB2'B 104.0(9) . . ? OC3'B V3B'B OB2'B 84.2(9) . . ? OC4'B V3B'B OB2'B 152.6(8) . . ? OB1'B V3B'B OB2'B 77.5(7) . . ? OF2'B V3B'B OA1B 175.8(10) . . ? OC3'B V3B'B OA1B 79.2(7) . . ? OC4'B V3B'B OA1B 80.9(8) . . ? OB1'B V3B'B OA1B 76.0(7) . . ? OB2'B V3B'B OA1B 72.0(7) . . ? OF2'B V3B'B V3A'B 90.8(8) . . ? OC3'B V3B'B V3A'B 127.5(8) . . ? OC4'B V3B'B V3A'B 131.7(6) . . ? OB1'B V3B'B V3A'B 39.5(5) . . ? OB2'B V3B'B V3A'B 43.4(5) . . ? OA1B V3B'B V3A'B 85.4(5) . . ? OF2'B V3B'B V2AB 135.4(7) . . ? OC3'B V3B'B V2AB 34.0(6) . . ? OC4'B V3B'B V2AB 81.6(5) . . ? OB1'B V3B'B V2AB 122.2(5) . . ? OB2'B V3B'B V2AB 82.6(5) . . ? OA1B V3B'B V2AB 46.2(4) . . ? V3A'B V3B'B V2AB 119.4(2) . . ? OF2'B V3B'B V2BB 133.6(8) . . ? OC3'B V3B'B V2BB 85.9(6) . . ? OC4'B V3B'B V2BB 30.7(6) . . ? OB1'B V3B'B V2BB 87.0(5) . . ? OB2'B V3B'B V2BB 122.4(5) . . ? OA1B V3B'B V2BB 50.4(5) . . ? V3A'B V3B'B V2BB 120.5(2) . . ? V2AB V3B'B V2BB 59.96(16) . . ? OF1'B V3A'B OC1'B 102.2(10) . . ? OF1'B V3A'B OC2'B 105.7(10) . . ? OC1'B V3A'B OC2'B 96.6(11) . . ? OF1'B V3A'B OB1'B 100.9(10) . . ? OC1'B V3A'B OB1'B 89.0(9) . . ? OC2'B V3A'B OB1'B 150.9(8) . . ? OF1'B V3A'B OB2'B 101.8(9) . . ? OC1'B V3A'B OB2'B 153.9(8) . . ? OC2'B V3A'B OB2'B 86.5(8) . . ? OB1'B V3A'B OB2'B 76.5(7) . . ? OF1'B V3A'B OA1'B 172.8(11) . . ? OC1'B V3A'B OA1'B 83.3(8) . . ? OC2'B V3A'B OA1'B 77.9(8) . . ? OB1'B V3A'B OA1'B 74.4(8) . . ? OB2'B V3A'B OA1'B 72.0(7) . . ? OF1'B V3A'B V3B'B 88.8(9) . . ? OC1'B V3A'B V3B'B 129.6(7) . . ? OC2'B V3A'B V3B'B 127.7(7) . . ? OB1'B V3A'B V3B'B 40.6(5) . . ? OB2'B V3A'B V3B'B 41.2(6) . . ? OA1'B V3A'B V3B'B 84.2(6) . . ? OF1'B V3A'B V2B'B 136.9(8) . . ? OC1'B V3A'B V2B'B 85.4(8) . . ? OC2'B V3A'B V2B'B 31.4(6) . . ? OB1'B V3A'B V2B'B 121.8(5) . . ? OB2'B V3A'B V2B'B 84.1(6) . . ? OA1'B V3A'B V2B'B 47.4(6) . . ? V3B'B V3A'B V2B'B 119.0(2) . . ? OF1'B V3A'B V2A'B 135.9(7) . . ? OC1'B V3A'B V2A'B 33.9(6) . . ? OC2'B V3A'B V2A'B 83.2(7) . . ? OB1'B V3A'B V2A'B 85.9(6) . . ? OB2'B V3A'B V2A'B 122.0(6) . . ? OA1'B V3A'B V2A'B 50.0(5) . . ? V3B'B V3A'B V2A'B 120.1(2) . . ? V2B'B V3A'B V2A'B 59.62(18) . . ? OF1B V3AB OC2B 104.2(11) . . ? OF1B V3AB OB2B 102.7(9) . . ? OC2B V3AB OB2B 96.5(8) . . ? OF1B V3AB OC1B 101.0(9) . . ? OC2B V3AB OC1B 91.1(10) . . ? OB2B V3AB OC1B 152.4(7) . . ? OF1B V3AB OB1B 100.8(10) . . ? OC2B V3AB OB1B 155.0(9) . . ? OB2B V3AB OB1B 77.0(7) . . ? OC1B V3AB OB1B 84.9(8) . . ? OF1B V3AB OA1B 172.5(9) . . ? OC2B V3AB OA1B 82.7(8) . . ? OB2B V3AB OA1B 79.1(6) . . ? OC1B V3AB OA1B 75.6(7) . . ? OB1B V3AB OA1B 72.4(7) . . ? OF1B V3AB V2BB 136.6(9) . . ? OC2B V3AB V2BB 32.7(6) . . ? OB2B V3AB V2BB 90.4(5) . . ? OC1B V3AB V2BB 81.8(7) . . ? OB1B V3AB V2BB 122.5(5) . . ? OA1B V3AB V2BB 50.1(5) . . ? OF1B V3AB V1A'B 138.7(8) . . ? OC2B V3AB V1A'B 80.6(6) . . ? OB2B V3AB V1A'B 36.6(5) . . ? OC1B V3AB V1A'B 120.0(6) . . ? OB1B V3AB V1A'B 80.1(4) . . ? OA1B V3AB V1A'B 44.5(4) . . ? V2BB V3AB V1A'B 60.17(19) . . ? OF2B V3BB OC3B 105.2(10) . . ? OF2B V3BB OC4B 101.0(10) . . ? OC3B V3BB OC4B 99.3(10) . . ? OF2B V3BB OB2B 102.2(10) . . ? OC3B V3BB OB2B 91.3(8) . . ? OC4B V3BB OB2B 151.0(9) . . ? OF2B V3BB OB1B 96.7(9) . . ? OC3B V3BB OB1B 156.8(9) . . ? OC4B V3BB OB1B 83.7(8) . . ? OB2B V3BB OB1B 76.5(7) . . ? OF2B V3BB OA1'B 169.0(9) . . ? OC3B V3BB OA1'B 85.8(8) . . ? OC4B V3BB OA1'B 76.5(9) . . ? OB2B V3BB OA1'B 77.5(8) . . ? OB1B V3BB OA1'B 72.4(7) . . ? OF2B V3BB V2A'B 140.5(8) . . ? OC3B V3BB V2A'B 36.3(6) . . ? OC4B V3BB V2A'B 83.1(6) . . ? OB2B V3BB V2A'B 89.9(5) . . ? OB1B V3BB V2A'B 122.8(5) . . ? OA1'B V3BB V2A'B 50.3(5) . . ? OF2B V3BB V1A'B 138.8(9) . . ? OC3B V3BB V1A'B 78.4(8) . . ? OC4B V3BB V1A'B 119.2(7) . . ? OB2B V3BB V1A'B 36.8(5) . . ? OB1B V3BB V1A'B 80.1(6) . . ? OA1'B V3BB V1A'B 42.8(6) . . ? V2A'B V3BB V1A'B 59.50(18) . . ? V1AB OE1B V2AB 109.8(8) . . ? V1AB OE2'B V2B'B 108.3(8) . . ? V2A'B OD1'B V2B'B 114.8(12) . . ? V1A'B OE1'B V2A'B 111.8(10) . . ? V1A'B OE2B V2BB 112.8(9) . . ? V2BB OD1B V2AB 115.3(15) . . ? V3B'B OC3'B V2AB 113.8(9) . . ? V1AB OB2'B V3B'B 111.5(10) . . ? V1AB OB2'B V3A'B 107.4(10) . . ? V3B'B OB2'B V3A'B 95.4(7) . . ? V2B'B OC2'B V3A'B 114.8(10) . . ? V3A'B OC1'B V2A'B 115.6(9) . . ? V1A'B OB1'B V3A'B 110.0(10) . . ? V1A'B OB1'B V3B'B 108.6(8) . . ? V3A'B OB1'B V3B'B 99.9(7) . . ? V2BB OC4'B V3B'B 118.3(11) . . ? V3AB OC1B V2AB 112.7(8) . . ? V1AB OB1B V3AB 106.7(10) . . ? V1AB OB1B V3BB 105.3(7) . . ? V3AB OB1B V3BB 94.0(6) . . ? V3BB OC4B V2B'B 113.9(11) . . ? V3BB OC3B V2A'B 113.6(10) . . ? V1A'B OB2B V3AB 106.4(8) . . ? V1A'B OB2B V3BB 105.5(8) . . ? V3AB OB2B V3BB 105.8(7) . . ? V3AB OC2B V2BB 116.3(11) . . ? V1AB OA1B V1A'B 100.2(9) . . ? V1AB OA1B V2AB 90.6(6) . . ? V1A'B OA1B V2AB 168.7(10) . . ? V1AB OA1B V3B'B 92.9(6) . . ? V1A'B OA1B V3B'B 90.1(6) . . ? V2AB OA1B V3B'B 86.0(7) . . ? V1AB OA1B V3AB 101.8(8) . . ? V1A'B OA1B V3AB 87.9(6) . . ? V2AB OA1B V3AB 93.2(6) . . ? V3B'B OA1B V3AB 165.3(10) . . ? V1AB OA1B V2BB 172.8(9) . . ? V1A'B OA1B V2BB 85.5(5) . . ? V2AB OA1B V2BB 83.4(7) . . ? V3B'B OA1B V2BB 82.6(7) . . ? V3AB OA1B V2BB 82.7(6) . . ? V1AB OA1'B V1A'B 103.2(11) . . ? V1AB OA1'B V3BB 102.7(7) . . ? V1A'B OA1'B V3BB 90.6(7) . . ? V1AB OA1'B V2B'B 88.4(7) . . ? V1A'B OA1'B V2B'B 167.3(10) . . ? V3BB OA1'B V2B'B 91.9(9) . . ? V1AB OA1'B V3A'B 91.8(8) . . ? V1A'B OA1'B V3A'B 90.2(8) . . ? V3BB OA1'B V3A'B 165.0(10) . . ? V2B'B OA1'B V3A'B 84.2(7) . . ? V1AB OA1'B V2A'B 169.1(11) . . ? V1A'B OA1'B V2A'B 85.8(6) . . ? V3BB OA1'B V2A'B 83.1(7) . . ? V2B'B OA1'B V2A'B 82.1(8) . . ? V3A'B OA1'B V2A'B 81.9(6) . . ? C2 N1 C4 106(2) . . ? C2 N1 C1 109(2) . . ? C4 N1 C1 119(2) . . ? C2 N1 C3 117(2) . . ? C4 N1 C3 110(2) . . ? C1 N1 C3 97(2) . . ? C5 C1 N1 124(2) . . ? N1 C2 C6 114(2) . . ? C7 C3 N1 119(3) . . ? N1 C4 C8 117(3) . . ? C12 C5 C1 117(3) . . ? C11 C6 C2 115(3) . . ? C9 C7 C3 103(3) . . ? C10 C8 C4 110(4) . . ? C13 N2 C14 127(3) . . ? C13 N2 C15 102(3) . . ? C14 N2 C15 99(3) . . ? C13 N2 C16 106(2) . . ? C14 N2 C16 104(2) . . ? C15 N2 C16 120(3) . . ? N2 C13 C19 110(3) . . ? C18 C14 N2 106(2) . . ? N2 C15 C17 111(3) . . ? C20 C16 N2 116.3(18) . . ? C23 C17 C15 109(3) . . ? C22 C18 C14 109(2) . . ? C21 C19 C13 116(3) . . ? C24 C20 C16 114(2) . . ? C25 N3 C28 133(2) . . ? C25 N3 C34 92.6(19) . . ? C28 N3 C34 110.5(13) . . ? C25 N3 C31 101.6(15) . . ? C28 N3 C31 115.3(18) . . ? C34 N3 C31 95.7(18) . . ? N3 C25 C26 103.4(19) . . ? C25 C26 C27 113(2) . . ? C29 C28 N3 118(2) . . ? C30 C29 C28 107(3) . . ? C32 C31 N3 125.5(16) . . ? C33 C32 C31 107.1(18) . . ? N3 C34 C35 116(3) . . ? C34 C35 C36 117(3) . . ? C40 N4 C46 109(3) . . ? C40 N4 C43 104(3) . . ? C46 N4 C43 110(3) . . ? C40 N4 C37 124(3) . . ? C46 N4 C37 112(3) . . ? C43 N4 C37 97(3) . . ? C38 C37 N4 106(3) . . ? C37 C38 C39 109(4) . . ? N4 C40 C41 114(3) . . ? C42 C41 C40 121(4) . . ? C44 C43 N4 101(6) . . ? C43 C44 C45 111(8) . . ? N4 C46 C47 112(4) . . ? C48 C47 C46 105(5) . . ? C52 N5 C49 115(2) . . ? C52 N5 C51 106(3) . . ? C49 N5 C51 105(3) . . ? C52 N5 C50 110(3) . . ? C49 N5 C50 106(2) . . ? C51 N5 C50 114(2) . . ? C56 C49 N5 115(4) . . ? C53 C50 N5 118(4) . . ? C54 C51 N5 102(4) . . ? N5 C52 C55 116(4) . . ? C58 C53 C50 127(6) . . ? C59 C54 C51 104(4) . . ? C52 C55 C57 114(5) . . ? C60 C56 C49 103(4) . . ? C64 N6 C62 120.1(16) . . ? C64 N6 C61 114(2) . . ? C62 N6 C61 105.7(11) . . ? C64 N6 C63 106.5(12) . . ? C62 N6 C63 100.6(18) . . ? C61 N6 C63 108.6(13) . . ? C66 C61 N6 124.7(11) . . ? N6 C62 C65 108.9(11) . . ? C67 C63 N6 110.8(10) . . ? N6 C64 C68 127.0(13) . . ? C70 C65 C62 114.3 . . ? C61 C66 C71 109.5 . . ? C63 C67 C69 110.7 . . ? C72 C68 C64 121.6 . . ? _diffrn_measured_fraction_theta_max 0.585 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.585 _refine_diff_density_max 0.527 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.087 #===END data_TBAc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Bis(tetra-n-butylammonium) tetrahydrogendecavanadate ; _chemical_melting_point ? _chemical_formula_moiety '(C16 H36 N +)2, (H4 V10 O28 2-)' _chemical_formula_sum 'C32 H76 N2 O28 V10' _chemical_formula_weight 1446.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_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 8.5633(9) _cell_length_b 21.048(3) _cell_length_c 15.435(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.375(10) _cell_angle_gamma 90.00 _cell_volume 2764.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.93 _cell_measurement_theta_max 15.00 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 1.690 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.794 _exptl_absorpt_process_details 'de Meulenaar & Tompa (1965)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w--2q\ _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.568 _diffrn_reflns_number 6330 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6330 _reflns_number_gt 4518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control Software' _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_reduction 'teXsan PROCESS (Molecular Structure Corporation, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997a)' _refine_special_details ; H atoms attached to surface O atoms of decavanadate frameworks, H1 and H2, were found from difference Fourier syntheses and their positional and isotropic displacement parameters were refined. H atoms in the [(C~4~H~9~)~4~N]^+^ cations were included in ideal positions and refined with the riding model. ; _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^)+(0.0835P)^2^+0.6566P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6330 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V2B V 0.54192(7) 0.57165(3) 0.70094(4) 0.02899(15) Uani 1 1 d . . . V1A V 0.54244(6) 0.54408(3) 0.41839(4) 0.02161(14) Uani 1 1 d . . . V2A V 0.64607(7) 0.65005(3) 0.54923(4) 0.02623(15) Uani 1 1 d . . . V3A V 0.79319(6) 0.51003(3) 0.59432(4) 0.02399(14) Uani 1 1 d . . . V3B V 0.69369(6) 0.39887(3) 0.46161(4) 0.02582(15) Uani 1 1 d . . . OG2 O 0.5426(3) 0.58136(14) 0.80263(18) 0.0430(7) Uani 1 1 d . . . OG1 O 0.7245(3) 0.71674(12) 0.53310(18) 0.0371(6) Uani 1 1 d . . . OF1 O 0.9712(3) 0.48411(13) 0.60585(17) 0.0323(6) Uani 1 1 d . . . OF2 O 0.8698(3) 0.37102(12) 0.47495(19) 0.0363(6) Uani 1 1 d . . . OE2 O 0.4649(3) 0.48195(11) 0.68521(15) 0.0275(5) Uani 1 1 d . . . OE1 O 0.6245(3) 0.61635(11) 0.42247(16) 0.0268(5) Uani 1 1 d . . . OD1 O 0.6351(3) 0.64522(12) 0.66364(16) 0.0314(5) Uani 1 1 d . . . OC2 O 0.7481(3) 0.52961(12) 0.69597(16) 0.0295(5) Uani 1 1 d . . . OB2 O 0.6704(2) 0.43269(11) 0.57936(15) 0.0246(5) Uani 1 1 d . . . OC3 O 0.5689(3) 0.33384(11) 0.47526(17) 0.0296(5) Uani 1 1 d . . . OC4 O 0.6524(3) 0.40231(12) 0.34287(17) 0.0309(5) Uani 1 1 d . . . OB1 O 0.7473(3) 0.49567(11) 0.45623(16) 0.0226(5) Uani 1 1 d . . . OC1 O 0.8335(4) 0.59640(15) 0.5601(2) 0.0293(6) Uani 1 1 d . . . OA1 O 0.5482(2) 0.54729(10) 0.55197(14) 0.0231(5) Uani 1 1 d . . . N1 N 0.5303(4) 0.78538(17) 0.2988(2) 0.0395(8) Uani 1 1 d . . . C1 C 0.4561(5) 0.7790(2) 0.3831(3) 0.0444(10) Uani 1 1 d . . . H1A H 0.5318 0.7932 0.4306 0.053 Uiso 1 1 calc R . . H1B H 0.4359 0.7344 0.3926 0.053 Uiso 1 1 calc R . . C2 C 0.3040(6) 0.8154(3) 0.3880(4) 0.0622(14) Uani 1 1 d . . . H2A H 0.3205 0.8601 0.3770 0.075 Uiso 1 1 calc R . . H2B H 0.2238 0.7997 0.3439 0.075 Uiso 1 1 calc R . . C3 C 0.2502(9) 0.8070(4) 0.4775(5) 0.106(3) Uani 1 1 d . . . H3A H 0.2378 0.7619 0.4877 0.127 Uiso 1 1 calc R . . H3B H 0.3329 0.8223 0.5205 0.127 Uiso 1 1 calc R . . C4 C 0.1042(10) 0.8388(5) 0.4927(6) 0.125(3) Uani 1 1 d . . . H4A H 0.0816 0.8305 0.5512 0.188 Uiso 1 1 calc R . . H4B H 0.0199 0.8231 0.4522 0.188 Uiso 1 1 calc R . . H4C H 0.1153 0.8838 0.4847 0.188 Uiso 1 1 calc R . . C5 C 0.4271(5) 0.7535(2) 0.2243(3) 0.0456(10) Uani 1 1 d . . . H5A H 0.3242 0.7733 0.2198 0.055 Uiso 1 1 calc R . . H5B H 0.4717 0.7625 0.1705 0.055 Uiso 1 1 calc R . . C6 C 0.4048(6) 0.6824(2) 0.2304(4) 0.0584(13) Uani 1 1 d . . . H6A H 0.3590 0.6723 0.2834 0.070 Uiso 1 1 calc R . . H6B H 0.5061 0.6614 0.2328 0.070 Uiso 1 1 calc R . . C7 C 0.2982(6) 0.6582(2) 0.1521(4) 0.0580(13) Uani 1 1 d . . . H7A H 0.1951 0.6773 0.1523 0.070 Uiso 1 1 calc R . . H7B H 0.3403 0.6716 0.0992 0.070 Uiso 1 1 calc R . . C8 C 0.2813(10) 0.5875(3) 0.1512(5) 0.096(2) Uani 1 1 d . . . H8A H 0.2133 0.5749 0.1005 0.143 Uiso 1 1 calc R . . H8B H 0.2372 0.5740 0.2027 0.143 Uiso 1 1 calc R . . H8C H 0.3827 0.5683 0.1498 0.143 Uiso 1 1 calc R . . C9 C 0.6893(5) 0.7535(2) 0.3144(3) 0.0444(10) Uani 1 1 d . . . H9A H 0.7519 0.7761 0.3608 0.053 Uiso 1 1 calc R . . H9B H 0.6741 0.7106 0.3349 0.053 Uiso 1 1 calc R . . C10 C 0.7817(6) 0.7500(3) 0.2367(4) 0.0668(16) Uani 1 1 d . . . H10A H 0.7243 0.7248 0.1912 0.080 Uiso 1 1 calc R . . H10B H 0.7945 0.7924 0.2139 0.080 Uiso 1 1 calc R . . C11 C 0.9404(7) 0.7209(3) 0.2618(6) 0.094(2) Uani 1 1 d . . . H11A H 0.9973 0.7220 0.2109 0.113 Uiso 1 1 calc R . . H11B H 0.9966 0.7480 0.3055 0.113 Uiso 1 1 calc R . . C12 C 0.9477(9) 0.6581(4) 0.2944(7) 0.133(4) Uani 1 1 d . . . H12A H 1.0556 0.6461 0.3091 0.200 Uiso 1 1 calc R . . H12B H 0.8991 0.6297 0.2508 0.200 Uiso 1 1 calc R . . H12C H 0.8935 0.6558 0.3455 0.200 Uiso 1 1 calc R . . C13 C 0.5459(5) 0.8552(2) 0.2739(3) 0.0436(10) Uani 1 1 d . . . H13A H 0.5946 0.8572 0.2201 0.052 Uiso 1 1 calc R . . H13B H 0.4414 0.8732 0.2623 0.052 Uiso 1 1 calc R . . C14 C 0.6404(6) 0.8961(2) 0.3415(4) 0.0588(13) Uani 1 1 d . . . H14A H 0.6024 0.8897 0.3978 0.071 Uiso 1 1 calc R . . H14B H 0.7498 0.8832 0.3464 0.071 Uiso 1 1 calc R . . C15 C 0.6282(7) 0.9658(2) 0.3177(4) 0.0658(14) Uani 1 1 d . . . H15A H 0.6672 0.9721 0.2617 0.079 Uiso 1 1 calc R . . H15B H 0.5185 0.9783 0.3118 0.079 Uiso 1 1 calc R . . C16 C 0.7189(10) 1.0078(3) 0.3842(5) 0.103(3) Uani 1 1 d . . . H16A H 0.7076 1.0513 0.3660 0.155 Uiso 1 1 calc R . . H16B H 0.8280 0.9962 0.3895 0.155 Uiso 1 1 calc R . . H16C H 0.6791 1.0026 0.4395 0.155 Uiso 1 1 calc R . . H2 H 0.814(4) 0.4985(17) 0.430(2) 0.013(9) Uiso 1 1 d . . . H1 H 0.877(6) 0.606(3) 0.547(4) 0.037(19) Uiso 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 V2B 0.0272(3) 0.0342(3) 0.0264(3) -0.0050(2) 0.0068(2) -0.0043(2) V1A 0.0171(3) 0.0247(3) 0.0235(3) 0.0024(2) 0.0043(2) -0.0011(2) V2A 0.0218(3) 0.0243(3) 0.0329(3) -0.0018(2) 0.0044(2) -0.0033(2) V3A 0.0161(3) 0.0289(3) 0.0268(3) 0.0017(2) 0.0016(2) -0.0017(2) V3B 0.0177(3) 0.0251(3) 0.0354(3) -0.0012(2) 0.0062(2) 0.0009(2) OG2 0.0448(16) 0.0546(18) 0.0307(14) -0.0077(13) 0.0101(12) -0.0103(14) OG1 0.0356(14) 0.0300(14) 0.0454(16) 0.0011(12) 0.0035(12) -0.0081(11) OF1 0.0194(11) 0.0401(14) 0.0371(14) 0.0035(11) 0.0020(10) 0.0000(10) OF2 0.0231(12) 0.0328(13) 0.0541(17) 0.0008(12) 0.0092(11) 0.0037(10) OE2 0.0252(12) 0.0329(13) 0.0247(12) 0.0016(10) 0.0043(9) -0.0029(10) OE1 0.0239(11) 0.0255(12) 0.0318(13) 0.0027(10) 0.0063(10) -0.0035(9) OD1 0.0271(12) 0.0344(13) 0.0332(14) -0.0075(11) 0.0057(10) -0.0070(10) OC2 0.0251(12) 0.0363(13) 0.0268(12) 0.0003(10) 0.0011(10) -0.0044(10) OB2 0.0178(10) 0.0261(12) 0.0301(12) 0.0037(9) 0.0038(9) 0.0001(9) OC3 0.0242(12) 0.0249(12) 0.0400(14) -0.0005(10) 0.0055(10) 0.0011(9) OC4 0.0280(12) 0.0318(13) 0.0347(13) -0.0062(11) 0.0116(10) -0.0005(10) OB1 0.0158(11) 0.0252(12) 0.0281(12) 0.0006(9) 0.0075(9) 0.0006(9) OC1 0.0186(13) 0.0316(14) 0.0384(16) 0.0034(11) 0.0061(11) -0.0037(11) OA1 0.0198(11) 0.0249(11) 0.0250(11) -0.0004(9) 0.0042(9) -0.0005(9) N1 0.0349(17) 0.0446(19) 0.0402(18) 0.0156(15) 0.0091(14) 0.0070(14) C1 0.040(2) 0.055(3) 0.040(2) 0.015(2) 0.0128(18) 0.0072(19) C2 0.041(2) 0.080(4) 0.070(3) 0.016(3) 0.023(2) 0.017(2) C3 0.100(5) 0.121(6) 0.110(6) 0.063(5) 0.074(5) 0.064(5) C4 0.101(6) 0.185(9) 0.099(6) 0.038(6) 0.053(5) 0.051(6) C5 0.041(2) 0.050(2) 0.046(2) 0.014(2) 0.0055(19) 0.0095(19) C6 0.057(3) 0.050(3) 0.067(3) 0.022(2) 0.002(2) 0.002(2) C7 0.056(3) 0.054(3) 0.064(3) 0.011(2) 0.007(2) 0.002(2) C8 0.122(6) 0.058(4) 0.100(5) 0.012(3) -0.021(4) -0.013(4) C9 0.033(2) 0.048(2) 0.053(3) 0.017(2) 0.0107(18) 0.0088(17) C10 0.056(3) 0.066(3) 0.086(4) 0.035(3) 0.039(3) 0.023(2) C11 0.058(4) 0.091(5) 0.144(7) 0.015(5) 0.055(4) 0.018(3) C12 0.098(6) 0.123(7) 0.192(10) 0.086(7) 0.078(6) 0.068(5) C13 0.045(2) 0.044(2) 0.043(2) 0.0161(19) 0.0111(18) 0.0116(18) C14 0.049(3) 0.067(3) 0.060(3) 0.018(3) 0.002(2) -0.002(2) C15 0.072(4) 0.052(3) 0.072(4) -0.001(3) 0.000(3) 0.009(3) C16 0.118(7) 0.072(4) 0.113(6) -0.016(4) -0.019(5) -0.009(4) _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 OB1 H2 0.74(4) . ? H2 OF1 2.01(4) 2_766 ? OB1 OF1 2.725(3) 2_766 ? OC1 H1 0.48(5) . ? H1 OF2 2.29(5) 2_766 ? OC1 OF2 2.742(4) 2_766 ? V2B OG2 1.582(3) . ? V2B OC4 1.810(3) 3_666 ? V2B OD1 1.862(3) . ? V2B OC2 1.984(3) . ? V2B OE2 2.006(2) . ? V2B OA1 2.362(2) . ? V2B V2A 3.0766(9) . ? V2B V1A 3.0908(9) 3_666 ? V2B V3B 3.1027(9) 3_666 ? V1A OE1 1.674(2) . ? V1A OE2 1.685(2) 3_666 ? V1A OB2 1.891(2) 3_666 ? V1A OB1 2.056(2) . ? V1A OA1 2.058(2) . ? V1A OA1 2.142(2) 3_666 ? V1A V2A 3.0729(9) . ? V1A V3A 3.0774(8) 3_666 ? V1A V2B 3.0908(9) 3_666 ? V2A OG1 1.588(3) . ? V2A OD1 1.782(3) . ? V2A OC3 1.869(2) 3_666 ? V2A OC1 1.955(3) . ? V2A OE1 2.070(3) . ? V2A OA1 2.322(2) . ? V2A V3B 3.0732(8) 3_666 ? V3A OF1 1.610(2) . ? V3A OC2 1.707(3) . ? V3A OC1 1.935(3) . ? V3A OB2 1.938(2) . ? V3A OB1 2.145(3) . ? V3A OA1 2.267(2) . ? V3A V1A 3.0774(8) 3_666 ? V3B OF2 1.610(2) . ? V3B OC3 1.763(2) . ? V3B OC4 1.829(3) . ? V3B OB2 1.982(2) . ? V3B OB1 2.092(2) . ? V3B OA1 2.350(2) 3_666 ? V3B V2A 3.0732(8) 3_666 ? V3B V2B 3.1028(9) 3_666 ? OE2 V1A 1.685(2) 3_666 ? OB2 V1A 1.891(2) 3_666 ? OC3 V2A 1.869(2) 3_666 ? OC4 V2B 1.810(3) 3_666 ? OA1 V1A 2.142(2) 3_666 ? OA1 V3B 2.350(2) 3_666 ? N1 C9 1.513(5) . ? N1 C1 1.516(5) . ? N1 C5 1.526(6) . ? N1 C13 1.528(5) . ? C1 C2 1.519(6) . ? C2 C3 1.514(7) . ? C3 C4 1.459(9) . ? C5 C6 1.514(6) . ? C6 C7 1.519(7) . ? C7 C8 1.495(8) . ? C9 C10 1.510(6) . ? C10 C11 1.502(8) . ? C11 C12 1.414(9) . ? C13 C14 1.516(7) . ? C14 C15 1.513(7) . ? C15 C16 1.504(8) . ? 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 OB1 H2 OF1 162(4) . 2_766 ? OF1 OB1 H2 13(3) 2_766 . ? OC1 H1 OF2 160(8) . 2_766 ? OF2 OC1 H1 17(7) 2_766 . ? V1A OB1 H2 120(3) . . ? V3A OB1 H2 118(3) . . ? V3B OB1 H2 107(3) . . ? V2A OC1 H1 114(7) . . ? V3A OC1 H1 131(7) . . ? OG2 V2B OC4 103.50(14) . 3_666 ? OG2 V2B OD1 104.17(13) . . ? OC4 V2B OD1 92.30(11) 3_666 . ? OG2 V2B OC2 101.00(14) . . ? OC4 V2B OC2 154.91(11) 3_666 . ? OD1 V2B OC2 86.86(11) . . ? OG2 V2B OE2 101.93(13) . . ? OC4 V2B OE2 87.92(11) 3_666 . ? OD1 V2B OE2 153.08(11) . . ? OC2 V2B OE2 81.80(10) . . ? OG2 V2B OA1 174.67(13) . . ? OC4 V2B OA1 79.70(10) 3_666 . ? OD1 V2B OA1 79.79(9) . . ? OC2 V2B OA1 75.47(9) . . ? OE2 V2B OA1 73.77(9) . . ? OG2 V2B V2A 135.76(11) . . ? OC4 V2B V2A 83.41(8) 3_666 . ? OD1 V2B V2A 31.61(8) . . ? OC2 V2B V2A 82.84(7) . . ? OE2 V2B V2A 122.13(7) . . ? OA1 V2B V2A 48.37(6) . . ? OG2 V2B V1A 131.90(11) . 3_666 ? OC4 V2B V1A 82.63(8) 3_666 3_666 ? OD1 V2B V1A 123.43(8) . 3_666 ? OC2 V2B V1A 77.03(7) . 3_666 ? OE2 V2B V1A 30.00(7) . 3_666 ? OA1 V2B V1A 43.77(6) . 3_666 ? V2A V2B V1A 92.14(2) . 3_666 ? OG2 V2B V3B 134.97(12) . 3_666 ? OC4 V2B V3B 31.69(8) 3_666 3_666 ? OD1 V2B V3B 81.15(8) . 3_666 ? OC2 V2B V3B 124.02(7) . 3_666 ? OE2 V2B V3B 85.12(7) . 3_666 ? OA1 V2B V3B 48.64(6) . 3_666 ? V2A V2B V3B 59.64(2) . 3_666 ? V1A V2B V3B 65.65(2) 3_666 3_666 ? OE1 V1A OE2 107.61(12) . 3_666 ? OE1 V1A OB2 99.54(11) . 3_666 ? OE2 V1A OB2 99.60(11) 3_666 3_666 ? OE1 V1A OB1 95.65(11) . . ? OE2 V1A OB1 92.83(11) 3_666 . ? OB2 V1A OB1 156.40(10) 3_666 . ? OE1 V1A OA1 88.24(11) . . ? OE2 V1A OA1 162.88(11) 3_666 . ? OB2 V1A OA1 83.62(9) 3_666 . ? OB1 V1A OA1 78.88(9) . . ? OE1 V1A OA1 165.55(11) . 3_666 ? OE2 V1A OA1 86.24(10) 3_666 3_666 ? OB2 V1A OA1 81.70(9) 3_666 3_666 ? OB1 V1A OA1 79.17(9) . 3_666 ? OA1 V1A OA1 77.55(10) . 3_666 ? OE1 V1A V2A 39.31(8) . . ? OE2 V1A V2A 146.87(8) 3_666 . ? OB2 V1A V2A 90.51(7) 3_666 . ? OB1 V1A V2A 89.89(7) . . ? OA1 V1A V2A 49.06(6) . . ? OA1 V1A V2A 126.61(6) 3_666 . ? OE1 V1A V3A 136.38(8) . 3_666 ? OE2 V1A V3A 83.27(8) 3_666 3_666 ? OB2 V1A V3A 37.03(7) 3_666 3_666 ? OB1 V1A V3A 126.57(7) . 3_666 ? OA1 V1A V3A 89.67(6) . 3_666 ? OA1 V1A V3A 47.43(6) 3_666 3_666 ? V2A V1A V3A 120.66(2) . 3_666 ? OE1 V1A V2B 143.90(9) . 3_666 ? OE2 V1A V2B 36.52(8) 3_666 3_666 ? OB2 V1A V2B 93.02(7) 3_666 3_666 ? OB1 V1A V2B 85.08(7) . 3_666 ? OA1 V1A V2B 126.94(7) . 3_666 ? OA1 V1A V2B 49.72(6) 3_666 3_666 ? V2A V1A V2B 174.29(3) . 3_666 ? V3A V1A V2B 61.022(19) 3_666 3_666 ? OG1 V2A OD1 105.99(13) . . ? OG1 V2A OC3 103.42(13) . 3_666 ? OD1 V2A OC3 92.96(12) . 3_666 ? OG1 V2A OC1 99.59(14) . . ? OD1 V2A OC1 90.88(13) . . ? OC3 V2A OC1 154.61(12) 3_666 . ? OG1 V2A OE1 98.60(12) . . ? OD1 V2A OE1 155.27(10) . . ? OC3 V2A OE1 83.60(11) 3_666 . ? OC1 V2A OE1 82.49(12) . . ? OG1 V2A OA1 170.54(12) . . ? OD1 V2A OA1 82.53(10) . . ? OC3 V2A OA1 79.81(9) 3_666 . ? OC1 V2A OA1 75.83(11) . . ? OE1 V2A OA1 72.76(9) . . ? OG1 V2A V1A 129.42(11) . . ? OD1 V2A V1A 124.53(8) . . ? OC3 V2A V1A 78.04(8) 3_666 . ? OC1 V2A V1A 79.13(9) . . ? OE1 V2A V1A 30.82(6) . . ? OA1 V2A V1A 42.04(6) . . ? OG1 V2A V3B 134.58(10) . 3_666 ? OD1 V2A V3B 83.17(8) . 3_666 ? OC3 V2A V3B 31.17(7) 3_666 3_666 ? OC1 V2A V3B 125.08(10) . 3_666 ? OE1 V2A V3B 81.33(7) . 3_666 ? OA1 V2A V3B 49.25(5) . 3_666 ? V1A V2A V3B 61.217(19) . 3_666 ? OG1 V2A V2B 139.20(11) . . ? OD1 V2A V2B 33.22(8) . . ? OC3 V2A V2B 83.63(8) 3_666 . ? OC1 V2A V2B 85.97(10) . . ? OE1 V2A V2B 122.19(7) . . ? OA1 V2A V2B 49.51(6) . . ? V1A V2A V2B 91.37(2) . . ? V3B V2A V2B 60.60(2) 3_666 . ? OF1 V3A OC2 106.74(13) . . ? OF1 V3A OC1 98.79(13) . . ? OC2 V3A OC1 95.15(13) . . ? OF1 V3A OB2 102.89(12) . . ? OC2 V3A OB2 97.89(11) . . ? OC1 V3A OB2 150.19(11) . . ? OF1 V3A OB1 97.41(12) . . ? OC2 V3A OB1 155.75(11) . . ? OC1 V3A OB1 83.08(12) . . ? OB2 V3A OB1 74.10(9) . . ? OF1 V3A OA1 169.59(11) . . ? OC2 V3A OA1 83.40(10) . . ? OC1 V3A OA1 77.52(11) . . ? OB2 V3A OA1 77.51(9) . . ? OB1 V3A OA1 72.58(9) . . ? OF1 V3A V1A 138.39(10) . 3_666 ? OC2 V3A V1A 80.97(8) . 3_666 ? OC1 V3A V1A 121.61(9) . 3_666 ? OB2 V3A V1A 36.00(7) . 3_666 ? OB1 V3A V1A 79.49(7) . 3_666 ? OA1 V3A V1A 44.09(6) . 3_666 ? OF2 V3B OC3 105.88(13) . . ? OF2 V3B OC4 102.52(13) . . ? OC3 V3B OC4 95.63(12) . . ? OF2 V3B OB2 101.63(12) . . ? OC3 V3B OB2 92.60(11) . . ? OC4 V3B OB2 151.22(11) . . ? OF2 V3B OB1 98.81(12) . . ? OC3 V3B OB1 154.05(10) . . ? OC4 V3B OB1 86.59(11) . . ? OB2 V3B OB1 74.42(10) . . ? OF2 V3B OA1 172.29(12) . 3_666 ? OC3 V3B OA1 81.11(10) . 3_666 ? OC4 V3B OA1 79.68(10) . 3_666 ? OB2 V3B OA1 74.41(9) . 3_666 ? OB1 V3B OA1 73.84(8) . 3_666 ? OF2 V3B V2A 138.84(10) . 3_666 ? OC3 V3B V2A 33.28(8) . 3_666 ? OC4 V3B V2A 83.22(8) . 3_666 ? OB2 V3B V2A 88.81(7) . 3_666 ? OB1 V3B V2A 122.31(7) . 3_666 ? OA1 V3B V2A 48.47(6) 3_666 3_666 ? OF2 V3B V2B 133.79(11) . 3_666 ? OC3 V3B V2B 84.47(9) . 3_666 ? OC4 V3B V2B 31.31(8) . 3_666 ? OB2 V3B V2B 123.16(7) . 3_666 ? OB1 V3B V2B 84.20(7) . 3_666 ? OA1 V3B V2B 48.99(6) 3_666 3_666 ? V2A V3B V2B 59.75(2) 3_666 3_666 ? V1A OE2 V2B 113.47(12) 3_666 . ? V1A OE1 V2A 109.87(12) . . ? V2A OD1 V2B 115.17(13) . . ? V3A OC2 V2B 115.86(13) . . ? V1A OB2 V3A 106.97(11) 3_666 . ? V1A OB2 V3B 107.75(11) 3_666 . ? V3A OB2 V3B 107.61(11) . . ? V3B OC3 V2A 115.54(13) . 3_666 ? V2B OC4 V3B 117.00(13) 3_666 . ? V1A OB1 V3B 108.06(10) . . ? V1A OB1 V3A 105.60(10) . . ? V3B OB1 V3A 96.58(10) . . ? V3A OC1 V2A 113.34(16) . . ? V1A OA1 V1A 102.45(10) . 3_666 ? V1A OA1 V3A 101.29(9) . . ? V1A OA1 V3A 88.47(8) 3_666 . ? V1A OA1 V2A 88.90(8) . . ? V1A OA1 V2A 168.62(12) 3_666 . ? V3A OA1 V2A 90.17(8) . . ? V1A OA1 V3B 90.22(8) . 3_666 ? V1A OA1 V3B 96.64(8) 3_666 3_666 ? V3A OA1 V3B 166.14(11) . 3_666 ? V2A OA1 V3B 82.28(7) . 3_666 ? V1A OA1 V2B 169.03(12) . . ? V1A OA1 V2B 86.51(8) 3_666 . ? V3A OA1 V2B 85.10(8) . . ? V2A OA1 V2B 82.11(7) . . ? V3B OA1 V2B 82.37(7) 3_666 . ? C9 N1 C1 106.3(3) . . ? C9 N1 C5 111.1(3) . . ? C1 N1 C5 110.2(3) . . ? C9 N1 C13 111.3(3) . . ? C1 N1 C13 111.0(3) . . ? C5 N1 C13 107.0(3) . . ? N1 C1 C2 116.2(4) . . ? C3 C2 C1 109.7(4) . . ? C4 C3 C2 116.5(6) . . ? C6 C5 N1 117.0(4) . . ? C5 C6 C7 110.5(4) . . ? C8 C7 C6 113.0(5) . . ? C10 C9 N1 115.9(4) . . ? C11 C10 C9 110.7(5) . . ? C12 C11 C10 118.5(6) . . ? C14 C13 N1 115.3(4) . . ? C15 C14 C13 111.5(4) . . ? C16 C15 C14 112.8(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_publ_flag OB1 H2 OF1 0.74(4) 2.01(4) 2.725(3) 162(4) ? OC1 H1 OF2 0.48(5) 2.29(5) 2.742(4) 160(8) ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.644 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.133 #===END data_TBAh _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Tris(tetra-n-butylammonium) trihydrogendecavanadate ; _chemical_melting_point ? _chemical_formula_moiety '(C16 H36 N +)3, (H3 V10 O28 3-)' _chemical_formula_sum 'C48 H111 N3 O28 V10' _chemical_formula_weight 1687.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.968(2) _cell_length_b 18.677(2) _cell_length_c 12.785(2) _cell_angle_alpha 91.38(1) _cell_angle_beta 96.48(1) _cell_angle_gamma 107.26(1) _cell_volume 3611.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.92 _cell_measurement_theta_max 15.03 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_T_max 0.821 _exptl_absorpt_process_details 'de Meulenaar & Tompa (1965)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 17.9 _diffrn_reflns_number 17185 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.59 _reflns_number_total 16587 _reflns_number_gt 8020 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Control Software' _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_reduction 'teXsan PROCESS (Molecular Structure Corporation, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997a)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997a)' _refine_special_details ; H atoms attached to surface O atoms of decavanadate frameworks, H1, H2 and H3, were found from difference Fourier syntheses and their positional and isotropic displacement parameters were refined. H atoms in the [(C~4~H~9~)~4~N]^+^ cations were included in ideal positions and refined with the riding model. Distances between the following atom pairs were restrained to 1.54\%A with estimated standard deviation 0.02: C46 and C47A, C47A and C48, C11 and C12, C31 and C32. ; _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^)+(0.1828P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16587 _refine_ls_number_parameters 799 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1540 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.2678 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.006 _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 V2B' V 0.27385(7) 0.60329(6) 0.39635(8) 0.0447(3) Uani 1 1 d . . . V1A V 0.46964(6) 0.62195(4) 0.46805(6) 0.0290(2) Uani 1 1 d . . . V2A V 0.66402(6) 0.64832(5) 0.54582(8) 0.0402(2) Uani 1 1 d . . . V2B V 0.66677(7) 0.76743(6) 0.71531(9) 0.0497(3) Uani 1 1 d . . . V1A' V 0.46807(6) 0.74821(5) 0.64721(7) 0.0347(2) Uani 1 1 d . . . V2A' V 0.27174(7) 0.72354(6) 0.56440(9) 0.0458(3) Uani 1 1 d . . . V3A' V 0.40979(6) 0.76231(5) 0.40632(7) 0.0376(2) Uani 1 1 d . . . V3B' V 0.60445(6) 0.78486(5) 0.48091(8) 0.0402(2) Uani 1 1 d . . . V3B V 0.32905(6) 0.58997(5) 0.65131(8) 0.0406(2) Uani 1 1 d . . . V3A V 0.52939(7) 0.61155(5) 0.72585(7) 0.0391(2) Uani 1 1 d . . . OG2' O 0.2026(3) 0.5476(3) 0.3096(4) 0.0663(13) Uani 1 1 d . . . OG1 O 0.7313(3) 0.6051(2) 0.5112(4) 0.0526(11) Uani 1 1 d . . . OG2 O 0.7380(4) 0.8214(3) 0.8024(4) 0.0803(16) Uani 1 1 d . . . OG1' O 0.2010(3) 0.7628(3) 0.5975(4) 0.0634(13) Uani 1 1 d . . . OF1' O 0.4375(3) 0.8246(2) 0.3212(3) 0.0543(11) Uani 1 1 d . . . OF2' O 0.6314(3) 0.8465(2) 0.3962(4) 0.0572(12) Uani 1 1 d . . . OF2 O 0.3007(3) 0.5253(2) 0.7315(4) 0.0603(12) Uani 1 1 d . . . OF1 O 0.5025(3) 0.5458(2) 0.8060(3) 0.0548(11) Uani 1 1 d . . . OE2' O 0.3809(2) 0.56703(19) 0.3872(3) 0.0376(8) Uani 1 1 d . . . OE1 O 0.5529(2) 0.58574(19) 0.4518(3) 0.0361(8) Uani 1 1 d . . . OD1 O 0.7266(3) 0.7124(2) 0.6577(4) 0.0523(11) Uani 1 1 d . . . OE2 O 0.5561(3) 0.7963(2) 0.7339(3) 0.0445(9) Uani 1 1 d . . . OE1' O 0.3815(3) 0.7776(2) 0.6679(3) 0.0441(9) Uani 1 1 d . . . OD1' O 0.2098(3) 0.6545(2) 0.4619(4) 0.0520(10) Uani 1 1 d . . . OC2' O 0.3272(3) 0.6830(2) 0.3258(3) 0.0444(9) Uani 1 1 d . . . OB2' O 0.5008(2) 0.70709(18) 0.3952(3) 0.0317(7) Uani 1 1 d . . . OC3' O 0.6726(3) 0.7215(2) 0.4570(3) 0.0474(10) Uani 1 1 d . . . OC4' O 0.6733(3) 0.8280(2) 0.6002(3) 0.0477(10) Uani 1 1 d . . . OB1' O 0.5010(2) 0.80481(19) 0.5269(3) 0.0352(8) Uani 1 1 d . . . OC1' O 0.3277(3) 0.7892(2) 0.4689(3) 0.0427(9) Uani 1 1 d . . . OC4 O 0.2605(3) 0.5391(3) 0.5205(4) 0.0488(11) Uani 1 1 d . . . OB1 O 0.4345(3) 0.5581(2) 0.5970(3) 0.0351(9) Uani 1 1 d . . . OC1 O 0.6106(3) 0.5776(2) 0.6530(3) 0.0409(9) Uani 1 1 d . . . OC2 O 0.6104(3) 0.6846(2) 0.7970(3) 0.0518(11) Uani 1 1 d . . . OB2 O 0.4360(3) 0.6575(2) 0.7269(3) 0.0387(9) Uani 1 1 d . . . OC3 O 0.2618(3) 0.6461(2) 0.6651(3) 0.0508(10) Uani 1 1 d . . . OA1' O 0.3843(2) 0.67146(18) 0.5298(3) 0.0323(8) Uani 1 1 d . . . OA1 O 0.5535(2) 0.68866(18) 0.5929(3) 0.0335(8) Uani 1 1 d . . . N1 N 0.9732(4) 0.6786(4) 0.6969(6) 0.0763(19) Uani 1 1 d . . . C1 C 1.0553(5) 0.6683(5) 0.7571(7) 0.076(2) Uani 1 1 d . . . H1A H 1.0813 0.7107 0.8079 0.092 Uiso 1 1 calc R . . H1B H 1.0977 0.6693 0.7080 0.092 Uiso 1 1 calc R . . C2 C 1.0413(6) 0.5962(6) 0.8156(8) 0.101(3) Uani 1 1 d . . . H2A H 1.0016 0.5960 0.8677 0.121 Uiso 1 1 calc R . . H2B H 1.0134 0.5535 0.7659 0.121 Uiso 1 1 calc R . . C3 C 1.1257(6) 0.5875(6) 0.8697(9) 0.106(3) Uani 1 1 d . . . H3A H 1.1632 0.5840 0.8163 0.127 Uiso 1 1 calc R . . H3B H 1.1559 0.6327 0.9142 0.127 Uiso 1 1 calc R . . C4 C 1.1163(8) 0.5218(8) 0.9353(11) 0.146(5) Uani 1 1 d . . . H4A H 1.1737 0.5213 0.9665 0.220 Uiso 1 1 calc R . . H4B H 1.0884 0.4765 0.8920 0.220 Uiso 1 1 calc R . . H4C H 1.0808 0.5252 0.9900 0.220 Uiso 1 1 calc R . . C5 C 0.9038(6) 0.6748(7) 0.7667(10) 0.116(4) Uani 1 1 d . . . H5A H 0.8893 0.6265 0.7979 0.139 Uiso 1 1 calc R . . H5B H 0.8508 0.6782 0.7244 0.139 Uiso 1 1 calc R . . C6 C 0.9331(11) 0.7402(11) 0.8589(14) 0.180(8) Uani 1 1 d . . . H6A H 0.9908 0.7411 0.8934 0.216 Uiso 1 1 calc R . . H6B H 0.9402 0.7877 0.8266 0.216 Uiso 1 1 calc R . . C7 C 0.8785(16) 0.7362(14) 0.935(3) 0.246(13) Uani 1 1 d . . . H7A H 0.8700 0.6881 0.9661 0.296 Uiso 1 1 calc R . . H7B H 0.8214 0.7369 0.9010 0.296 Uiso 1 1 calc R . . C8 C 0.9062(16) 0.7928(13) 1.0176(17) 0.215(11) Uani 1 1 d . . . H8A H 0.8636 0.7833 1.0669 0.323 Uiso 1 1 calc R . . H8B H 0.9112 0.8408 0.9891 0.323 Uiso 1 1 calc R . . H8C H 0.9626 0.7929 1.0529 0.323 Uiso 1 1 calc R . . C9 C 0.9378(5) 0.6161(5) 0.6043(9) 0.101(4) Uani 1 1 d . . . H9A H 0.9222 0.5675 0.6345 0.122 Uiso 1 1 calc R . . H9B H 0.8841 0.6221 0.5671 0.122 Uiso 1 1 calc R . . C10 C 1.0006(8) 0.6159(6) 0.5259(10) 0.117(4) Uani 1 1 d . . . H10A H 1.0485 0.5994 0.5598 0.141 Uiso 1 1 calc R . . H10B H 1.0259 0.6671 0.5070 0.141 Uiso 1 1 calc R . . C11 C 0.9595(9) 0.5645(6) 0.4200(15) 0.177(8) Uani 1 1 d D . . H11A H 1.0066 0.5571 0.3835 0.212 Uiso 1 1 calc R . . H11B H 0.9228 0.5157 0.4369 0.212 Uiso 1 1 calc R . . C12 C 0.9085(11) 0.5992(10) 0.3549(14) 0.190(7) Uani 1 1 d D . . H12A H 0.8840 0.5682 0.2912 0.285 Uiso 1 1 calc R . . H12B H 0.9451 0.6472 0.3378 0.285 Uiso 1 1 calc R . . H12C H 0.8615 0.6058 0.3909 0.285 Uiso 1 1 calc R . . C13 C 1.0017(5) 0.7555(4) 0.6523(7) 0.074(2) Uani 1 1 d . . . H13A H 1.0239 0.7931 0.7107 0.089 Uiso 1 1 calc R . . H13B H 1.0503 0.7578 0.6121 0.089 Uiso 1 1 calc R . . C14 C 0.9304(5) 0.7758(5) 0.5826(9) 0.094(3) Uani 1 1 d . . . H14A H 0.9045 0.7363 0.5275 0.113 Uiso 1 1 calc R . . H14B H 0.8842 0.7785 0.6243 0.113 Uiso 1 1 calc R . . C15 C 0.9624(7) 0.8477(6) 0.5334(11) 0.118(4) Uani 1 1 d . . . H15A H 1.0094 0.8447 0.4930 0.142 Uiso 1 1 calc R . . H15B H 0.9883 0.8867 0.5891 0.142 Uiso 1 1 calc R . . C16 C 0.8960(8) 0.8714(6) 0.4625(10) 0.131(4) Uani 1 1 d . . . H16A H 0.9242 0.9188 0.4352 0.197 Uiso 1 1 calc R . . H16B H 0.8499 0.8764 0.5016 0.197 Uiso 1 1 calc R . . H16C H 0.8711 0.8344 0.4052 0.197 Uiso 1 1 calc R . . N2 N 0.4956(5) 0.7137(4) 0.0646(4) 0.081(2) Uani 1 1 d . . . C17 C 0.4190(9) 0.7481(6) 0.0726(9) 0.123(4) Uani 1 1 d . . . H17A H 0.3754 0.7147 0.1105 0.148 Uiso 1 1 calc R . . H17B H 0.4423 0.7954 0.1143 0.148 Uiso 1 1 calc R . . C18 C 0.3726(8) 0.7622(8) -0.0315(10) 0.125(4) Uani 1 1 d . . . H18A H 0.3393 0.7147 -0.0690 0.150 Uiso 1 1 calc R . . H18B H 0.4159 0.7896 -0.0751 0.150 Uiso 1 1 calc R . . C19 C 0.3085(11) 0.8088(9) -0.0097(13) 0.175(6) Uiso 1 1 d . . . H19A H 0.2663 0.7818 0.0353 0.210 Uiso 1 1 calc R . . H19B H 0.3421 0.8567 0.0265 0.210 Uiso 1 1 calc R . . C20 C 0.2637(14) 0.8210(12) -0.1044(17) 0.236(9) Uiso 1 1 d . . . H20A H 0.2246 0.8494 -0.0902 0.354 Uiso 1 1 calc R . . H20B H 0.2301 0.7736 -0.1399 0.354 Uiso 1 1 calc R . . H20C H 0.3057 0.8484 -0.1484 0.354 Uiso 1 1 calc R . . C21 C 0.5323(9) 0.7080(7) 0.1738(7) 0.119(4) Uani 1 1 d . . . H21A H 0.4842 0.6810 0.2114 0.143 Uiso 1 1 calc R . . H21B H 0.5562 0.7583 0.2070 0.143 Uiso 1 1 calc R . . C22 C 0.6021(11) 0.6704(8) 0.1874(9) 0.128(4) Uani 1 1 d . . . H22A H 0.5947 0.6426 0.2505 0.154 Uiso 1 1 calc R . . H22B H 0.5915 0.6339 0.1283 0.154 Uiso 1 1 calc R . . C23 C 0.6936(13) 0.7159(13) 0.1954(15) 0.220(10) Uani 1 1 d . . . H23A H 0.7065 0.7319 0.1258 0.264 Uiso 1 1 calc R . . H23B H 0.7011 0.7607 0.2400 0.264 Uiso 1 1 calc R . . C24 C 0.7569(11) 0.6800(10) 0.2367(10) 0.179(7) Uani 1 1 d . . . H24A H 0.8154 0.7142 0.2390 0.268 Uiso 1 1 calc R . . H24B H 0.7514 0.6363 0.1922 0.268 Uiso 1 1 calc R . . H24C H 0.7463 0.6653 0.3066 0.268 Uiso 1 1 calc R . . C25 C 0.4593(7) 0.6360(5) 0.0062(6) 0.093(3) Uani 1 1 d . . . H25A H 0.5082 0.6167 -0.0027 0.112 Uiso 1 1 calc R . . H25B H 0.4316 0.6414 -0.0635 0.112 Uiso 1 1 calc R . . C26 C 0.3904(9) 0.5776(6) 0.0638(9) 0.115(4) Uani 1 1 d . . . H26A H 0.4175 0.5722 0.1338 0.138 Uiso 1 1 calc R . . H26B H 0.3405 0.5960 0.0716 0.138 Uiso 1 1 calc R . . C27 C 0.3592(9) 0.5044(7) 0.0053(10) 0.129(4) Uani 1 1 d . . . H27A H 0.4097 0.4874 -0.0044 0.155 Uiso 1 1 calc R . . H27B H 0.3313 0.5103 -0.0640 0.155 Uiso 1 1 calc R . . C28 C 0.2948(8) 0.4452(7) 0.0579(11) 0.148(6) Uani 1 1 d . . . H28A H 0.2763 0.3991 0.0147 0.222 Uiso 1 1 calc R . . H28B H 0.2442 0.4612 0.0674 0.222 Uiso 1 1 calc R . . H28C H 0.3226 0.4372 0.1254 0.222 Uiso 1 1 calc R . . C29 C 0.5617(7) 0.7638(6) 0.0010(7) 0.103(3) Uani 1 1 d . . . H29A H 0.5336 0.7622 -0.0708 0.124 Uiso 1 1 calc R . . H29B H 0.6108 0.7436 -0.0014 0.124 Uiso 1 1 calc R . . C30 C 0.5978(10) 0.8456(7) 0.0433(9) 0.136(5) Uani 1 1 d . . . H30A H 0.5487 0.8662 0.0436 0.163 Uiso 1 1 calc R . . H30B H 0.6240 0.8470 0.1159 0.163 Uiso 1 1 calc R . . C31 C 0.6618(14) 0.8928(8) -0.0137(12) 0.211(10) Uani 1 1 d D . . H31A H 0.6355 0.8888 -0.0867 0.254 Uiso 1 1 calc R . . H31B H 0.7107 0.8719 -0.0123 0.254 Uiso 1 1 calc R . . C32 C 0.6985(15) 0.9711(10) 0.0166(14) 0.260(12) Uani 1 1 d D . . H32A H 0.7413 0.9941 -0.0291 0.390 Uiso 1 1 calc R . . H32B H 0.7267 0.9772 0.0881 0.390 Uiso 1 1 calc R . . H32C H 0.6523 0.9944 0.0113 0.390 Uiso 1 1 calc R . . N3 N 0.2408(3) 0.9473(3) 0.3584(4) 0.0532(13) Uani 1 1 d . . . C33 C 0.2072(4) 0.9894(4) 0.2710(6) 0.0609(18) Uani 1 1 d . . . H33A H 0.2404 1.0422 0.2821 0.073 Uiso 1 1 calc R . . H33B H 0.2195 0.9714 0.2044 0.073 Uiso 1 1 calc R . . C34 C 0.1110(5) 0.9825(5) 0.2619(7) 0.082(2) Uani 1 1 d . . . H34A H 0.0987 1.0041 0.3260 0.098 Uiso 1 1 calc R . . H34B H 0.0771 0.9297 0.2551 0.098 Uiso 1 1 calc R . . C35 C 0.0818(6) 1.0209(6) 0.1693(8) 0.100(3) Uani 1 1 d . . . H35A H 0.1163 1.0736 0.1765 0.120 Uiso 1 1 calc R . . H35B H 0.0948 0.9993 0.1057 0.120 Uiso 1 1 calc R . . C36 C -0.0138(7) 1.0156(7) 0.1566(10) 0.134(4) Uani 1 1 d . . . H36A H -0.0271 1.0414 0.0959 0.202 Uiso 1 1 calc R . . H36B H -0.0272 1.0383 0.2183 0.202 Uiso 1 1 calc R . . H36C H -0.0487 0.9638 0.1476 0.202 Uiso 1 1 calc R . . C37 C 0.1862(4) 0.8653(3) 0.3541(5) 0.0539(16) Uani 1 1 d . . . H37A H 0.2098 0.8422 0.4129 0.065 Uiso 1 1 calc R . . H37B H 0.1264 0.8631 0.3650 0.065 Uiso 1 1 calc R . . C38 C 0.1813(5) 0.8184(4) 0.2554(6) 0.069(2) Uani 1 1 d . . . H38A H 0.1648 0.8437 0.1946 0.082 Uiso 1 1 calc R . . H38B H 0.2391 0.8128 0.2492 0.082 Uiso 1 1 calc R . . C39 C 0.1153(6) 0.7426(4) 0.2565(7) 0.087(3) Uani 1 1 d . . . H39A H 0.0571 0.7488 0.2566 0.105 Uiso 1 1 calc R . . H39B H 0.1287 0.7202 0.3215 0.105 Uiso 1 1 calc R . . C40 C 0.1123(8) 0.6891(5) 0.1650(9) 0.125(4) Uani 1 1 d . . . H40A H 0.0690 0.6417 0.1719 0.187 Uiso 1 1 calc R . . H40B H 0.1693 0.6817 0.1647 0.187 Uiso 1 1 calc R . . H40C H 0.0967 0.7096 0.1002 0.187 Uiso 1 1 calc R . . C41 C 0.3358(4) 0.9504(4) 0.3470(6) 0.0601(17) Uani 1 1 d . . . H41A H 0.3542 0.9189 0.3981 0.072 Uiso 1 1 calc R . . H41B H 0.3370 0.9292 0.2774 0.072 Uiso 1 1 calc R . . C42 C 0.4029(5) 1.0285(4) 0.3616(8) 0.077(2) Uani 1 1 d . . . H42A H 0.4093 1.0482 0.4339 0.093 Uiso 1 1 calc R . . H42B H 0.3833 1.0625 0.3156 0.093 Uiso 1 1 calc R . . C43 C 0.4915(5) 1.0216(5) 0.3342(10) 0.093(3) Uani 1 1 d . . . H43A H 0.5382 1.0657 0.3649 0.112 Uiso 1 1 calc R . . H43B H 0.5018 0.9783 0.3672 0.112 Uiso 1 1 calc R . . C44 C 0.4982(8) 1.0141(8) 0.2210(13) 0.149(5) Uani 1 1 d . . . H44A H 0.5559 1.0110 0.2117 0.224 Uiso 1 1 calc R . . H44B H 0.4890 1.0571 0.1874 0.224 Uiso 1 1 calc R . . H44C H 0.4542 0.9694 0.1901 0.224 Uiso 1 1 calc R . . C45 C 0.2340(5) 0.9841(4) 0.4652(6) 0.0636(19) Uani 1 1 d . A . H45A H 0.2634 1.0376 0.4650 0.076 Uiso 1 1 calc R . . H45B H 0.1721 0.9776 0.4701 0.076 Uiso 1 1 calc R . . C46 C 0.2716(8) 0.9561(5) 0.5616(7) 0.098(3) Uani 1 1 d D . . H46A H 0.3343 0.9816 0.5783 0.117 Uiso 0.72(3) 1 calc PR A 1 H46B H 0.2623 0.9024 0.5535 0.117 Uiso 0.72(3) 1 calc PR A 1 H46C H 0.2411 0.9027 0.5608 0.117 Uiso 0.28(3) 1 calc PR A 2 H46D H 0.3327 0.9610 0.5539 0.117 Uiso 0.28(3) 1 calc PR A 2 C47A C 0.216(2) 0.9761(13) 0.6517(17) 0.160(9) Uiso 0.72(3) 1 d PD A 1 H47A H 0.2397 1.0291 0.6731 0.192 Uiso 0.72(3) 1 calc PR A 1 H47B H 0.1549 0.9661 0.6223 0.192 Uiso 0.72(3) 1 calc PR A 1 C47B C 0.2708(18) 0.9869(12) 0.6637(16) 0.042(8) Uiso 0.28(3) 1 d P A 2 H47C H 0.2452 1.0279 0.6558 0.051 Uiso 0.28(3) 1 calc PR A 2 H47D H 0.3316 1.0084 0.6955 0.051 Uiso 0.28(3) 1 calc PR A 2 C48 C 0.221(2) 0.9335(15) 0.741(2) 0.342(16) Uiso 1 1 d D . . H48A H 0.2814 0.9373 0.7640 0.513 Uiso 0.72(3) 1 calc PR A 1 H48B H 0.1879 0.8818 0.7229 0.513 Uiso 0.72(3) 1 calc PR A 1 H48C H 0.1963 0.9525 0.7969 0.513 Uiso 0.72(3) 1 calc PR A 1 H48D H 0.2623 0.9187 0.7893 0.513 Uiso 0.28(3) 1 calc PR A 2 H48E H 0.1805 0.8898 0.7025 0.513 Uiso 0.28(3) 1 calc PR A 2 H48F H 0.1885 0.9586 0.7797 0.513 Uiso 0.28(3) 1 calc PR A 2 H1 H 0.613(4) 0.538(3) 0.647(4) 0.033(16) Uiso 1 1 d . . . H2 H 0.444(4) 0.526(3) 0.583(4) 0.025(16) Uiso 1 1 d . . . H3 H 0.269(4) 0.510(3) 0.510(4) 0.016(15) Uiso 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 V2B' 0.0384(5) 0.0393(5) 0.0555(6) 0.0009(4) -0.0060(4) 0.0146(4) V1A 0.0341(5) 0.0256(4) 0.0291(4) 0.0015(3) 0.0056(3) 0.0112(3) V2A 0.0318(5) 0.0336(5) 0.0574(6) 0.0001(4) 0.0079(4) 0.0126(4) V2B 0.0476(6) 0.0417(6) 0.0546(6) -0.0130(5) -0.0093(5) 0.0125(5) V1A' 0.0448(5) 0.0292(5) 0.0336(5) -0.0012(4) 0.0086(4) 0.0155(4) V2A' 0.0419(6) 0.0434(6) 0.0627(7) 0.0109(5) 0.0178(5) 0.0243(5) V3A' 0.0467(6) 0.0339(5) 0.0384(5) 0.0094(4) 0.0086(4) 0.0201(4) V3B' 0.0400(5) 0.0281(5) 0.0530(6) 0.0049(4) 0.0152(4) 0.0075(4) V3B 0.0441(6) 0.0368(5) 0.0472(6) 0.0119(4) 0.0199(4) 0.0158(4) V3A 0.0525(6) 0.0386(5) 0.0304(5) 0.0030(4) 0.0024(4) 0.0211(4) OG2' 0.060(3) 0.060(3) 0.073(3) -0.005(2) -0.017(2) 0.018(2) OG1 0.042(2) 0.047(2) 0.075(3) -0.001(2) 0.013(2) 0.0193(19) OG2 0.080(4) 0.067(3) 0.080(4) -0.032(3) -0.027(3) 0.018(3) OG1' 0.053(3) 0.055(3) 0.098(4) 0.014(2) 0.031(3) 0.031(2) OF1' 0.074(3) 0.052(3) 0.049(2) 0.021(2) 0.016(2) 0.034(2) OF2' 0.061(3) 0.039(2) 0.076(3) 0.017(2) 0.033(2) 0.014(2) OF2 0.065(3) 0.055(3) 0.068(3) 0.027(2) 0.030(2) 0.020(2) OF1 0.076(3) 0.058(3) 0.040(2) 0.0159(19) 0.011(2) 0.032(2) OE2' 0.039(2) 0.0327(19) 0.041(2) -0.0004(15) 0.0003(16) 0.0127(16) OE1 0.040(2) 0.0329(19) 0.039(2) -0.0009(15) 0.0092(16) 0.0147(16) OD1 0.038(2) 0.046(2) 0.070(3) -0.007(2) -0.005(2) 0.0148(18) OE2 0.058(3) 0.034(2) 0.042(2) -0.0074(16) 0.0000(18) 0.0188(18) OE1' 0.056(2) 0.038(2) 0.046(2) 0.0016(17) 0.0174(19) 0.0214(18) OD1' 0.039(2) 0.048(2) 0.072(3) 0.002(2) 0.004(2) 0.0191(19) OC2' 0.051(2) 0.039(2) 0.047(2) 0.0053(17) -0.0014(18) 0.0217(18) OB2' 0.041(2) 0.0219(16) 0.0344(18) 0.0018(13) 0.0101(15) 0.0112(14) OC3' 0.042(2) 0.035(2) 0.068(3) 0.0022(19) 0.023(2) 0.0115(17) OC4' 0.039(2) 0.0295(19) 0.070(3) -0.0070(18) 0.0043(19) 0.0053(16) OB1' 0.040(2) 0.0269(17) 0.042(2) 0.0017(15) 0.0101(16) 0.0131(15) OC1' 0.047(2) 0.036(2) 0.053(2) 0.0094(17) 0.0113(18) 0.0214(17) OC4 0.040(2) 0.039(3) 0.071(3) 0.006(2) 0.012(2) 0.016(2) OB1 0.040(2) 0.032(2) 0.040(2) 0.0075(16) 0.0107(16) 0.0178(17) OC1 0.051(2) 0.033(2) 0.045(2) 0.0015(17) 0.0032(17) 0.0229(19) OC2 0.072(3) 0.049(2) 0.036(2) -0.0025(18) -0.007(2) 0.027(2) OB2 0.053(2) 0.036(2) 0.0347(19) 0.0077(15) 0.0135(17) 0.0225(17) OC3 0.058(3) 0.042(2) 0.064(3) 0.0125(19) 0.029(2) 0.024(2) OA1' 0.0327(19) 0.0297(18) 0.0370(19) 0.0052(15) 0.0087(15) 0.0116(15) OA1 0.0354(19) 0.0291(18) 0.0362(19) -0.0019(14) 0.0022(15) 0.0110(15) N1 0.039(3) 0.078(4) 0.108(5) 0.036(4) 0.004(3) 0.012(3) C1 0.043(4) 0.093(6) 0.090(6) 0.008(5) -0.003(4) 0.020(4) C2 0.065(6) 0.128(8) 0.117(8) 0.039(7) -0.006(5) 0.040(6) C3 0.071(6) 0.134(9) 0.119(8) 0.031(7) -0.002(5) 0.044(6) C4 0.122(10) 0.185(13) 0.166(12) 0.083(10) 0.019(8) 0.091(9) C5 0.060(6) 0.154(10) 0.155(11) 0.087(9) 0.041(6) 0.050(6) C6 0.146(13) 0.26(2) 0.189(16) 0.076(15) 0.118(13) 0.103(14) C7 0.18(2) 0.22(3) 0.38(4) 0.10(3) 0.09(3) 0.10(2) C8 0.26(3) 0.25(3) 0.20(2) 0.099(18) 0.13(2) 0.12(2) C9 0.045(5) 0.080(6) 0.153(9) 0.038(6) -0.031(5) -0.008(4) C10 0.095(8) 0.097(8) 0.150(11) -0.007(7) 0.018(7) 0.013(6) C11 0.127(11) 0.073(7) 0.31(2) -0.052(10) -0.083(12) 0.036(7) C12 0.148(14) 0.179(15) 0.238(19) 0.030(14) 0.054(14) 0.030(12) C13 0.048(4) 0.063(5) 0.112(7) 0.012(4) 0.013(4) 0.015(4) C14 0.059(5) 0.085(6) 0.147(9) 0.046(6) 0.018(5) 0.029(5) C15 0.085(7) 0.094(7) 0.182(12) 0.048(8) 0.025(7) 0.029(6) C16 0.122(9) 0.105(8) 0.178(12) 0.053(8) 0.022(9) 0.048(7) N2 0.125(6) 0.086(5) 0.038(3) 0.001(3) 0.028(3) 0.034(4) C17 0.180(12) 0.092(7) 0.114(9) -0.001(6) 0.087(9) 0.043(8) C18 0.125(10) 0.149(11) 0.124(10) 0.016(8) 0.031(8) 0.071(9) C21 0.169(12) 0.119(9) 0.058(6) 0.005(6) -0.005(6) 0.035(9) C22 0.151(12) 0.138(11) 0.085(8) 0.015(7) 0.011(8) 0.029(10) C23 0.203(19) 0.32(3) 0.213(18) 0.162(18) 0.124(16) 0.15(2) C24 0.206(16) 0.27(2) 0.106(10) 0.066(12) 0.035(10) 0.139(16) C25 0.146(9) 0.090(6) 0.054(5) -0.009(4) 0.019(5) 0.050(6) C26 0.162(11) 0.082(7) 0.105(8) 0.016(6) 0.042(8) 0.033(7) C27 0.133(10) 0.123(10) 0.129(10) 0.007(8) -0.021(8) 0.048(8) C28 0.116(10) 0.138(11) 0.169(12) 0.081(10) -0.022(9) 0.015(8) C29 0.120(8) 0.130(9) 0.065(5) 0.008(6) 0.038(5) 0.037(7) C30 0.185(13) 0.113(9) 0.090(8) -0.004(7) 0.046(8) 0.005(9) C31 0.34(3) 0.114(11) 0.134(12) -0.022(9) 0.103(15) -0.028(14) C32 0.32(3) 0.23(2) 0.152(15) -0.029(15) 0.093(16) -0.06(2) N3 0.051(3) 0.045(3) 0.067(3) 0.011(2) 0.003(3) 0.021(2) C33 0.059(4) 0.042(4) 0.079(5) 0.017(3) -0.002(4) 0.015(3) C34 0.067(5) 0.095(6) 0.092(6) 0.016(5) -0.004(4) 0.041(5) C35 0.065(6) 0.116(8) 0.118(8) 0.037(6) -0.015(5) 0.032(5) C36 0.098(8) 0.169(12) 0.148(11) 0.031(9) -0.013(7) 0.067(8) C37 0.052(4) 0.040(3) 0.071(4) 0.011(3) 0.009(3) 0.016(3) C38 0.071(5) 0.058(4) 0.072(5) 0.004(4) 0.002(4) 0.014(4) C39 0.093(6) 0.058(5) 0.096(6) -0.003(4) -0.005(5) 0.007(4) C40 0.168(11) 0.069(6) 0.112(8) -0.020(6) -0.001(8) 0.007(7) C41 0.050(4) 0.056(4) 0.078(5) 0.006(3) 0.005(3) 0.022(3) C42 0.065(5) 0.040(4) 0.125(7) -0.009(4) 0.004(5) 0.017(3) C43 0.055(5) 0.053(5) 0.171(11) -0.003(6) 0.015(6) 0.016(4) C44 0.091(9) 0.154(12) 0.200(15) 0.006(11) 0.044(9) 0.022(8) C45 0.080(5) 0.039(3) 0.080(5) 0.005(3) 0.011(4) 0.030(3) C46 0.149(9) 0.087(6) 0.070(6) 0.006(5) 0.010(6) 0.056(6) _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 V2B' OG2' 1.601(4) . ? V2B' OC2' 1.801(4) . ? V2B' OD1' 1.843(4) . ? V2B' OC4 2.004(5) . ? V2B' OE2' 2.031(4) . ? V2B' OA1' 2.351(4) . ? V2B' V1A 3.0705(12) . ? V2B' V2A' 3.0805(15) . ? V2B' V3A' 3.1053(14) . ? V1A OE1 1.691(3) . ? V1A OE2' 1.698(4) . ? V1A OB2' 1.830(3) . ? V1A OA1' 2.072(3) . ? V1A OA1 2.080(3) . ? V1A OB1 2.089(4) . ? V1A V2A 3.0393(12) . ? V2A OG1 1.614(4) . ? V2A OC3' 1.782(4) . ? V2A OD1 1.833(4) . ? V2A OC1 2.008(4) . ? V2A OE1 2.044(4) . ? V2A OA1 2.247(3) . ? V2A V2B 3.0552(14) . ? V2A V3B' 3.0756(13) . ? V2B OG2 1.590(5) . ? V2B OD1 1.794(4) . ? V2B OC4' 1.871(4) . ? V2B OC2 1.939(5) . ? V2B OE2 2.031(4) . ? V2B OA1 2.357(4) . ? V2B V3A 3.0987(14) . ? V2B V1A' 3.1048(14) . ? V2B V3B' 3.1054(15) . ? V1A' OE1' 1.676(4) . ? V1A' OE2 1.692(4) . ? V1A' OB1' 1.921(4) . ? V1A' OB2 1.964(4) . ? V1A' OA1' 2.098(3) . ? V1A' OA1 2.158(3) . ? V1A' V2A' 3.0873(13) . ? V2A' OG1' 1.605(4) . ? V2A' OD1' 1.797(4) . ? V2A' OC1' 1.860(4) . ? V2A' OC3 1.943(4) . ? V2A' OE1' 2.050(4) . ? V2A' OA1' 2.360(3) . ? V2A' V3B 3.0911(13) . ? V2A' V3A' 3.0978(13) . ? V3A' OF1' 1.612(4) . ? V3A' OC1' 1.795(4) . ? V3A' OC2' 1.858(4) . ? V3A' OB1' 1.970(4) . ? V3A' OB2' 2.030(3) . ? V3A' OA1' 2.324(3) . ? V3A' V3B' 3.0470(13) . ? V3B' OF2' 1.598(4) . ? V3B' OC4' 1.795(4) . ? V3B' OC3' 1.871(4) . ? V3B' OB1' 1.946(4) . ? V3B' OB2' 2.034(4) . ? V3B' OA1 2.337(4) . ? V3B OF2 1.598(4) . ? V3B OC3 1.727(4) . ? V3B OB2 1.932(4) . ? V3B OC4 1.947(5) . ? V3B OB1 2.124(4) . ? V3B OA1' 2.266(3) . ? V3A OF1 1.609(4) . ? V3A OC2 1.729(4) . ? V3A OC1 1.919(4) . ? V3A OB2 1.930(4) . ? V3A OB1 2.113(4) . ? V3A OA1 2.247(4) . ? N1 C5 1.486(12) . ? N1 C1 1.510(9) . ? N1 C13 1.518(9) . ? N1 C9 1.574(12) . ? C1 C2 1.527(11) . ? C2 C3 1.497(11) . ? C3 C4 1.484(13) . ? C5 C6 1.602(19) . ? C6 C7 1.37(3) . ? C7 C8 1.41(3) . ? C9 C10 1.495(14) . ? C10 C11 1.596(16) . ? C11 C12 1.399(14) . ? C13 C14 1.510(11) . ? C14 C15 1.470(12) . ? C15 C16 1.492(14) . ? N2 C21 1.470(11) . ? N2 C29 1.515(11) . ? N2 C25 1.533(10) . ? N2 C17 1.552(13) . ? C17 C18 1.517(15) . ? C18 C19 1.570(17) . ? C19 C20 1.39(2) . ? C21 C22 1.482(16) . ? C22 C23 1.45(2) . ? C23 C24 1.433(18) . ? C25 C26 1.566(13) . ? C26 C27 1.464(14) . ? C27 C28 1.500(15) . ? C29 C30 1.525(14) . ? C30 C31 1.421(17) . ? C31 C32 1.429(14) . ? N3 C37 1.518(8) . ? N3 C33 1.521(8) . ? N3 C41 1.524(8) . ? N3 C45 1.542(9) . ? C33 C34 1.493(10) . ? C34 C35 1.500(11) . ? C35 C36 1.490(12) . ? C37 C38 1.499(9) . ? C38 C39 1.496(10) . ? C39 C40 1.507(12) . ? C41 C42 1.524(9) . ? C42 C43 1.535(11) . ? C43 C44 1.470(16) . ? C45 C46 1.484(10) . ? C46 C47B 1.42(2) . ? C46 C47A 1.628(16) . ? C47A C48 1.415(17) . ? C47B C48 1.54(3) . ? 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 OG1 OC4 H3 12(5) 2_666 . ? OE1 OB1 H2 9(5) 2_666 . ? OE2' OC1 H1 5(4) 2_666 . ? V1A OB1 H2 101(5) . . ? V3B OB1 H2 139(5) . . ? V3A OB1 H2 107(5) . . ? V2B' OC4 H3 109(5) . . ? V3B OC4 H3 111(5) . . ? V2A OC1 H1 116(4) . . ? V3A OC1 H1 128(4) . . ? OG2' V2B' OC2' 104.9(2) . . ? OG2' V2B' OD1' 104.3(2) . . ? OC2' V2B' OD1' 93.21(19) . . ? OG2' V2B' OC4 100.0(2) . . ? OC2' V2B' OC4 154.52(19) . . ? OD1' V2B' OC4 85.5(2) . . ? OG2' V2B' OE2' 101.3(2) . . ? OC2' V2B' OE2' 87.74(17) . . ? OD1' V2B' OE2' 153.27(18) . . ? OC4 V2B' OE2' 82.38(17) . . ? OG2' V2B' OA1' 172.60(19) . . ? OC2' V2B' OA1' 79.93(15) . . ? OD1' V2B' OA1' 80.77(16) . . ? OC4 V2B' OA1' 74.73(16) . . ? OE2' V2B' OA1' 73.09(13) . . ? OG2' V2B' V1A 132.37(19) . . ? OC2' V2B' V1A 78.62(13) . . ? OD1' V2B' V1A 123.15(14) . . ? OC4 V2B' V1A 80.85(13) . . ? OE2' V2B' V1A 31.18(10) . . ? OA1' V2B' V1A 42.39(8) . . ? OG2' V2B' V2A' 135.98(19) . . ? OC2' V2B' V2A' 83.93(13) . . ? OD1' V2B' V2A' 31.73(13) . . ? OC4 V2B' V2A' 81.70(15) . . ? OE2' V2B' V2A' 122.36(11) . . ? OA1' V2B' V2A' 49.28(8) . . ? V1A V2B' V2A' 91.54(4) . . ? OG2' V2B' V3A' 137.33(19) . . ? OC2' V2B' V3A' 32.50(13) . . ? OD1' V2B' V3A' 82.36(14) . . ? OC4 V2B' V3A' 122.62(15) . . ? OE2' V2B' V3A' 84.27(11) . . ? OA1' V2B' V3A' 48.02(8) . . ? V1A V2B' V3A' 61.00(3) . . ? V2A' V2B' V3A' 60.10(3) . . ? OE1 V1A OE2' 105.26(17) . . ? OE1 V1A OB2' 101.28(17) . . ? OE2' V1A OB2' 101.66(17) . . ? OE1 V1A OA1' 164.37(16) . . ? OE2' V1A OA1' 87.56(16) . . ? OB2' V1A OA1' 84.44(14) . . ? OE1 V1A OA1 86.60(16) . . ? OE2' V1A OA1 165.04(16) . . ? OB2' V1A OA1 84.53(15) . . ? OA1' V1A OA1 79.43(14) . . ? OE1 V1A OB1 92.62(17) . . ? OE2' V1A OB1 92.41(17) . . ? OB2' V1A OB1 156.74(16) . . ? OA1' V1A OB1 77.68(14) . . ? OA1 V1A OB1 77.71(15) . . ? OE1 V1A V2A 39.60(12) . . ? OE2' V1A V2A 144.85(12) . . ? OB2' V1A V2A 88.91(12) . . ? OA1' V1A V2A 127.09(10) . . ? OA1 V1A V2A 47.68(10) . . ? OB1 V1A V2A 90.11(11) . . ? OE1 V1A V2B' 143.52(13) . . ? OE2' V1A V2B' 38.27(12) . . ? OB2' V1A V2B' 89.77(12) . . ? OA1' V1A V2B' 49.91(10) . . ? OA1 V1A V2B' 129.34(10) . . ? OB1 V1A V2B' 89.97(11) . . ? V2A V1A V2B' 176.86(4) . . ? OG1 V2A OC3' 104.5(2) . . ? OG1 V2A OD1 104.7(2) . . ? OC3' V2A OD1 93.8(2) . . ? OG1 V2A OC1 97.7(2) . . ? OC3' V2A OC1 156.84(17) . . ? OD1 V2A OC1 86.72(19) . . ? OG1 V2A OE1 98.06(19) . . ? OC3' V2A OE1 88.60(17) . . ? OD1 V2A OE1 155.75(17) . . ? OC1 V2A OE1 81.89(16) . . ? OG1 V2A OA1 170.14(18) . . ? OC3' V2A OA1 82.04(15) . . ? OD1 V2A OA1 81.96(16) . . ? OC1 V2A OA1 75.09(15) . . ? OE1 V2A OA1 74.46(13) . . ? OG1 V2A V1A 129.84(16) . . ? OC3' V2A V1A 79.94(13) . . ? OD1 V2A V1A 125.12(13) . . ? OC1 V2A V1A 80.90(12) . . ? OE1 V2A V1A 31.82(9) . . ? OA1 V2A V1A 43.17(9) . . ? OG1 V2A V2B 136.87(16) . . ? OC3' V2A V2B 85.37(13) . . ? OD1 V2A V2B 32.21(13) . . ? OC1 V2A V2B 82.77(12) . . ? OE1 V2A V2B 124.43(10) . . ? OA1 V2A V2B 49.99(9) . . ? V1A V2A V2B 93.01(3) . . ? OG1 V2A V3B' 138.00(17) . . ? OC3' V2A V3B' 33.54(12) . . ? OD1 V2A V3B' 83.09(13) . . ? OC1 V2A V3B' 124.11(12) . . ? OE1 V2A V3B' 85.70(10) . . ? OA1 V2A V3B' 49.11(9) . . ? V1A V2A V3B' 62.02(3) . . ? V2B V2A V3B' 60.86(3) . . ? OG2 V2B OD1 104.0(3) . . ? OG2 V2B OC4' 101.8(3) . . ? OD1 V2B OC4' 92.0(2) . . ? OG2 V2B OC2 101.8(3) . . ? OD1 V2B OC2 91.0(2) . . ? OC4' V2B OC2 154.61(18) . . ? OG2 V2B OE2 102.2(2) . . ? OD1 V2B OE2 153.73(18) . . ? OC4' V2B OE2 84.42(17) . . ? OC2 V2B OE2 81.79(18) . . ? OG2 V2B OA1 176.0(2) . . ? OD1 V2B OA1 79.68(15) . . ? OC4' V2B OA1 79.42(15) . . ? OC2 V2B OA1 76.35(15) . . ? OE2 V2B OA1 74.08(14) . . ? OG2 V2B V2A 136.8(2) . . ? OD1 V2B V2A 33.00(13) . . ? OC4' V2B V2A 82.47(12) . . ? OC2 V2B V2A 86.48(12) . . ? OE2 V2B V2A 120.91(11) . . ? OA1 V2B V2A 46.91(8) . . ? OG2 V2B V3A 132.2(2) . . ? OD1 V2B V3A 82.66(14) . . ? OC4' V2B V3A 125.52(12) . . ? OC2 V2B V3A 30.34(12) . . ? OE2 V2B V3A 78.44(12) . . ? OA1 V2B V3A 46.20(9) . . ? V2A V2B V3A 64.24(3) . . ? OG2 V2B V1A' 132.4(2) . . ? OD1 V2B V1A' 123.61(14) . . ? OC4' V2B V1A' 78.95(12) . . ? OC2 V2B V1A' 78.41(13) . . ? OE2 V2B V1A' 30.19(11) . . ? OA1 V2B V1A' 43.95(8) . . ? V2A V2B V1A' 90.72(3) . . ? V3A V2B V1A' 60.85(3) . . ? OG2 V2B V3B' 133.2(2) . . ? OD1 V2B V3B' 82.79(15) . . ? OC4' V2B V3B' 31.38(12) . . ? OC2 V2B V3B' 124.57(12) . . ? OE2 V2B V3B' 80.70(11) . . ? OA1 V2B V3B' 48.30(9) . . ? V2A V2B V3B' 59.89(3) . . ? V3A V2B V3B' 94.49(3) . . ? V1A' V2B V3B' 61.09(3) . . ? OE1' V1A' OE2 108.66(19) . . ? OE1' V1A' OB1' 98.03(17) . . ? OE2 V1A' OB1' 97.28(18) . . ? OE1' V1A' OB2 96.82(17) . . ? OE2 V1A' OB2 95.95(18) . . ? OB1' V1A' OB2 155.78(15) . . ? OE1' V1A' OA1' 87.87(17) . . ? OE2 V1A' OA1' 163.36(16) . . ? OB1' V1A' OA1' 81.82(14) . . ? OB2 V1A' OA1' 79.73(15) . . ? OE1' V1A' OA1 164.88(17) . . ? OE2 V1A' OA1 86.33(16) . . ? OB1' V1A' OA1 81.54(14) . . ? OB2 V1A' OA1 79.16(14) . . ? OA1' V1A' OA1 77.09(13) . . ? OE1' V1A' V2A' 38.16(14) . . ? OE2 V1A' V2A' 146.81(13) . . ? OB1' V1A' V2A' 89.28(11) . . ? OB2 V1A' V2A' 90.68(12) . . ? OA1' V1A' V2A' 49.77(9) . . ? OA1 V1A' V2A' 126.86(10) . . ? OE1' V1A' V2B 145.76(14) . . ? OE2 V1A' V2B 37.12(13) . . ? OB1' V1A' V2B 88.56(11) . . ? OB2 V1A' V2B 89.85(12) . . ? OA1' V1A' V2B 126.36(10) . . ? OA1 V1A' V2B 49.28(9) . . ? V2A' V1A' V2B 175.87(4) . . ? OG1' V2A' OD1' 103.7(2) . . ? OG1' V2A' OC1' 101.6(2) . . ? OD1' V2A' OC1' 92.8(2) . . ? OG1' V2A' OC3 101.5(2) . . ? OD1' V2A' OC3 90.6(2) . . ? OC1' V2A' OC3 155.10(17) . . ? OG1' V2A' OE1' 101.8(2) . . ? OD1' V2A' OE1' 154.43(17) . . ? OC1' V2A' OE1' 84.28(17) . . ? OC3 V2A' OE1' 82.06(18) . . ? OG1' V2A' OA1' 174.7(2) . . ? OD1' V2A' OA1' 81.44(15) . . ? OC1' V2A' OA1' 79.08(14) . . ? OC3 V2A' OA1' 77.07(14) . . ? OE1' V2A' OA1' 73.05(14) . . ? OG1' V2A' V2B' 136.2(2) . . ? OD1' V2A' V2B' 32.64(13) . . ? OC1' V2A' V2B' 82.99(12) . . ? OC3 V2A' V2B' 86.76(12) . . ? OE1' V2A' V2B' 122.04(11) . . ? OA1' V2A' V2B' 49.04(9) . . ? OG1' V2A' V1A' 132.1(2) . . ? OD1' V2A' V1A' 124.20(13) . . ? OC1' V2A' V1A' 78.79(12) . . ? OC3 V2A' V1A' 78.90(13) . . ? OE1' V2A' V1A' 30.34(10) . . ? OA1' V2A' V1A' 42.76(9) . . ? V2B' V2A' V1A' 91.70(3) . . ? OG1' V2A' V3B 132.04(18) . . ? OD1' V2A' V3B 82.89(14) . . ? OC1' V2A' V3B 125.80(12) . . ? OC3 V2A' V3B 30.52(11) . . ? OE1' V2A' V3B 78.39(11) . . ? OA1' V2A' V3B 46.78(8) . . ? V2B' V2A' V3B 64.96(3) . . ? V1A' V2A' V3B 60.91(3) . . ? OG1' V2A' V3A' 132.93(17) . . ? OD1' V2A' V3A' 83.26(14) . . ? OC1' V2A' V3A' 31.41(11) . . ? OC3 V2A' V3A' 125.17(12) . . ? OE1' V2A' V3A' 81.15(11) . . ? OA1' V2A' V3A' 48.11(8) . . ? V2B' V2A' V3A' 60.35(3) . . ? V1A' V2A' V3A' 61.35(3) . . ? V3B V2A' V3A' 94.84(3) . . ? OF1' V3A' OC1' 103.79(19) . . ? OF1' V3A' OC2' 102.7(2) . . ? OC1' V3A' OC2' 93.62(18) . . ? OF1' V3A' OB1' 101.6(2) . . ? OC1' V3A' OB1' 92.01(17) . . ? OC2' V3A' OB1' 152.98(16) . . ? OF1' V3A' OB2' 100.69(18) . . ? OC1' V3A' OB2' 154.36(16) . . ? OC2' V3A' OB2' 88.34(15) . . ? OB1' V3A' OB2' 75.59(14) . . ? OF1' V3A' OA1' 174.17(18) . . ? OC1' V3A' OA1' 81.33(15) . . ? OC2' V3A' OA1' 79.56(15) . . ? OB1' V3A' OA1' 75.21(13) . . ? OB2' V3A' OA1' 73.89(13) . . ? OF1' V3A' V3B' 89.79(17) . . ? OC1' V3A' V3B' 130.63(14) . . ? OC2' V3A' V3B' 129.83(12) . . ? OB1' V3A' V3B' 38.62(10) . . ? OB2' V3A' V3B' 41.48(10) . . ? OA1' V3A' V3B' 84.69(9) . . ? OF1' V3A' V2A' 136.27(15) . . ? OC1' V3A' V2A' 32.70(12) . . ? OC2' V3A' V2A' 82.57(13) . . ? OB1' V3A' V2A' 88.10(11) . . ? OB2' V3A' V2A' 122.97(10) . . ? OA1' V3A' V2A' 49.08(8) . . ? V3B' V3A' V2A' 120.30(4) . . ? OF1' V3A' V2B' 133.95(17) . . ? OC1' V3A' V2B' 83.24(13) . . ? OC2' V3A' V2B' 31.39(12) . . ? OB1' V3A' V2B' 123.88(11) . . ? OB2' V3A' V2B' 85.30(10) . . ? OA1' V3A' V2B' 48.75(9) . . ? V3B' V3A' V2B' 120.21(4) . . ? V2A' V3A' V2B' 59.55(3) . . ? OF2' V3B' OC4' 103.9(2) . . ? OF2' V3B' OC3' 102.7(2) . . ? OC4' V3B' OC3' 93.35(19) . . ? OF2' V3B' OB1' 101.85(19) . . ? OC4' V3B' OB1' 92.61(17) . . ? OC3' V3B' OB1' 152.46(16) . . ? OF2' V3B' OB2' 100.7(2) . . ? OC4' V3B' OB2' 154.54(17) . . ? OC3' V3B' OB2' 87.37(16) . . ? OB1' V3B' OB2' 76.02(15) . . ? OF2' V3B' OA1 174.5(2) . . ? OC4' V3B' OA1 81.45(16) . . ? OC3' V3B' OA1 77.83(15) . . ? OB1' V3B' OA1 76.52(13) . . ? OB2' V3B' OA1 73.82(13) . . ? OF2' V3B' V3A' 89.91(17) . . ? OC4' V3B' V3A' 131.79(13) . . ? OC3' V3B' V3A' 128.77(13) . . ? OB1' V3B' V3A' 39.18(11) . . ? OB2' V3B' V3A' 41.40(10) . . ? OA1 V3B' V3A' 85.58(9) . . ? OF2' V3B' V2A 134.40(16) . . ? OC4' V3B' V2A 83.00(13) . . ? OC3' V3B' V2A 31.75(13) . . ? OB1' V3B' V2A 123.09(11) . . ? OB2' V3B' V2A 84.39(10) . . ? OA1 V3B' V2A 46.64(8) . . ? V3A' V3B' V2A 119.15(4) . . ? OF2' V3B' V2B 136.57(18) . . ? OC4' V3B' V2B 32.85(13) . . ? OC3' V3B' V2B 82.51(14) . . ? OB1' V3B' V2B 88.11(11) . . ? OB2' V3B' V2B 122.67(10) . . ? OA1 V3B' V2B 48.86(9) . . ? V3A' V3B' V2B 120.55(4) . . ? V2A V3B' V2B 59.24(3) . . ? OF2 V3B OC3 105.4(2) . . ? OF2 V3B OB2 102.6(2) . . ? OC3 V3B OB2 97.17(19) . . ? OF2 V3B OC4 100.7(2) . . ? OC3 V3B OC4 93.6(2) . . ? OB2 V3B OC4 150.66(18) . . ? OF2 V3B OB1 97.86(19) . . ? OC3 V3B OB1 156.54(18) . . ? OB2 V3B OB1 74.30(16) . . ? OC4 V3B OB1 85.09(18) . . ? OF2 V3B OA1' 170.65(19) . . ? OC3 V3B OA1' 83.95(16) . . ? OB2 V3B OA1' 76.27(14) . . ? OC4 V3B OA1' 77.83(17) . . ? OB1 V3B OA1' 72.85(13) . . ? OF2 V3B V2A' 139.87(17) . . ? OC3 V3B V2A' 34.85(13) . . ? OB2 V3B V2A' 91.17(11) . . ? OC4 V3B V2A' 82.26(15) . . ? OB1 V3B V2A' 122.21(11) . . ? OA1' V3B V2A' 49.37(9) . . ? OF1 V3A OC2 106.0(2) . . ? OF1 V3A OC1 100.2(2) . . ? OC2 V3A OC1 94.6(2) . . ? OF1 V3A OB2 102.7(2) . . ? OC2 V3A OB2 95.85(18) . . ? OC1 V3A OB2 151.03(16) . . ? OF1 V3A OB1 97.1(2) . . ? OC2 V3A OB1 156.58(18) . . ? OC1 V3A OB1 85.23(17) . . ? OB2 V3A OB1 74.61(16) . . ? OF1 V3A OA1 170.36(19) . . ? OC2 V3A OA1 83.49(17) . . ? OC1 V3A OA1 76.81(15) . . ? OB2 V3A OA1 77.67(14) . . ? OB1 V3A OA1 73.66(14) . . ? OF1 V3A V2B 140.02(17) . . ? OC2 V3A V2B 34.49(14) . . ? OC1 V3A V2B 82.94(13) . . ? OB2 V3A V2B 90.65(12) . . ? OB1 V3A V2B 122.87(11) . . ? OA1 V3A V2B 49.22(9) . . ? V1A OE2' V2B' 110.55(18) . . ? V1A OE1 V2A 108.58(17) . . ? V2B OD1 V2A 114.8(2) . . ? V1A' OE2 V2B 112.70(19) . . ? V1A' OE1' V2A' 111.50(19) . . ? V2A' OD1' V2B' 115.6(2) . . ? V2B' OC2' V3A' 116.1(2) . . ? V1A OB2' V3A' 108.46(17) . . ? V1A OB2' V3B' 109.14(17) . . ? V3A' OB2' V3B' 97.12(14) . . ? V2A OC3' V3B' 114.7(2) . . ? V3B' OC4' V2B 115.8(2) . . ? V1A' OB1' V3B' 109.43(17) . . ? V1A' OB1' V3A' 108.41(17) . . ? V3B' OB1' V3A' 102.19(16) . . ? V3A' OC1' V2A' 115.89(19) . . ? V3B OC4 V2B' 114.0(2) . . ? V1A OB1 V3A 105.88(17) . . ? V1A OB1 V3B 106.14(17) . . ? V3A OB1 V3B 95.47(17) . . ? V3A OC1 V2A 112.87(19) . . ? V3A OC2 V2B 115.2(2) . . ? V3A OB2 V3B 108.57(17) . . ? V3A OB2 V1A' 107.57(18) . . ? V3B OB2 V1A' 106.99(17) . . ? V3B OC3 V2A' 114.6(2) . . ? V1A OA1' V1A' 102.63(15) . . ? V1A OA1' V3B 101.80(14) . . ? V1A' OA1' V3B 91.63(13) . . ? V1A OA1' V3A' 90.78(13) . . ? V1A' OA1' V3A' 90.90(12) . . ? V3B OA1' V3A' 166.29(17) . . ? V1A OA1' V2B' 87.70(12) . . ? V1A' OA1' V2B' 168.22(17) . . ? V3B OA1' V2B' 91.75(12) . . ? V3A' OA1' V2B' 83.24(11) . . ? V1A OA1' V2A' 168.16(18) . . ? V1A' OA1' V2A' 87.47(12) . . ? V3B OA1' V2A' 83.85(11) . . ? V3A' OA1' V2A' 82.80(11) . . ? V2B' OA1' V2A' 81.68(11) . . ? V1A OA1 V1A' 100.35(15) . . ? V1A OA1 V3A 101.54(14) . . ? V1A' OA1 V3A 90.98(13) . . ? V1A OA1 V2A 89.15(12) . . ? V1A' OA1 V2A 168.51(18) . . ? V3A OA1 V2A 93.46(13) . . ? V1A OA1 V3B' 90.83(13) . . ? V1A' OA1 V3B' 89.11(12) . . ? V3A OA1 V3B' 167.40(17) . . ? V2A OA1 V3B' 84.25(12) . . ? V1A OA1 V2B 170.44(18) . . ? V1A' OA1 V2B 86.77(12) . . ? V3A OA1 V2B 84.58(12) . . ? V2A OA1 V2B 83.10(12) . . ? V3B' OA1 V2B 82.84(12) . . ? C5 N1 C1 111.4(7) . . ? C5 N1 C13 110.3(7) . . ? C1 N1 C13 106.1(6) . . ? C5 N1 C9 110.3(8) . . ? C1 N1 C9 108.8(6) . . ? C13 N1 C9 109.9(6) . . ? N1 C1 C2 115.5(6) . . ? C3 C2 C1 112.9(8) . . ? C4 C3 C2 115.8(9) . . ? N1 C5 C6 113.1(9) . . ? C7 C6 C5 117.6(19) . . ? C6 C7 C8 117(2) . . ? C10 C9 N1 115.5(7) . . ? C9 C10 C11 115.9(10) . . ? C12 C11 C10 109.6(12) . . ? C14 C13 N1 115.2(6) . . ? C15 C14 C13 113.6(7) . . ? C14 C15 C16 116.8(9) . . ? C21 N2 C29 113.6(8) . . ? C21 N2 C25 110.9(7) . . ? C29 N2 C25 108.1(6) . . ? C21 N2 C17 106.0(8) . . ? C29 N2 C17 108.5(7) . . ? C25 N2 C17 109.5(8) . . ? C18 C17 N2 115.7(7) . . ? C17 C18 C19 109.2(11) . . ? C20 C19 C18 110.1(15) . . ? N2 C21 C22 116.3(10) . . ? C23 C22 C21 118.7(14) . . ? C24 C23 C22 115.3(18) . . ? N2 C25 C26 113.8(7) . . ? C27 C26 C25 111.4(9) . . ? C26 C27 C28 114.1(12) . . ? N2 C29 C30 114.7(8) . . ? C31 C30 C29 115.4(10) . . ? C30 C31 C32 120.4(14) . . ? C37 N3 C33 112.1(5) . . ? C37 N3 C41 107.8(5) . . ? C33 N3 C41 109.2(5) . . ? C37 N3 C45 107.9(5) . . ? C33 N3 C45 108.2(5) . . ? C41 N3 C45 111.6(5) . . ? C34 C33 N3 115.8(6) . . ? C33 C34 C35 112.5(7) . . ? C36 C35 C34 114.6(9) . . ? C38 C37 N3 117.3(6) . . ? C39 C38 C37 111.0(7) . . ? C38 C39 C40 114.6(8) . . ? C42 C41 N3 115.5(5) . . ? C41 C42 C43 107.8(6) . . ? C44 C43 C42 115.4(9) . . ? C46 C45 N3 117.0(6) . . ? C47B C46 C45 121.8(11) . . ? C47B C46 C47A 30.6(11) . . ? C45 C46 C47A 102.9(11) . . ? C48 C47A C46 112(2) . . ? C46 C47B C48 117.2(18) . . ? C47A C48 C47B 32.2(14) . . ? 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_publ_flag OC4 H3 OG1 0.62(5) 2.16(5) 2.759(6) 165(7) ? OB1 H2 OE1 0.68(5) 2.14(5) 2.812(5) 168(6) ? OC1 H1 OE2' 0.76(6) 2.03(6) 2.783(5) 174(6) ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.740 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.127 #==END