# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author_name 'Prof M. Stanley Whittingham' _publ_contact_author_address ; Chemistry and Materials SUNY at Binghamton Vestal Parkway East Binghamton New York 13902 UNITED STATES OF AMERICA ; _publ_contact_author_email STANWHIT@BINGHAMTON.EDU loop_ _publ_author_name 'M. Stanley Whittingham' 'Natasha A. Chernova' 'Samuel T. Lutta' 'Peter Y. Zavalij' data_0332_prdV3O7 _database_code_depnum_ccdc_archive 'CCDC 235652' _chemical_name_systematic 'Pyrrolidinium trivanadium heptaoxide' _chemical_name_common 'Pyrrolidinium trivanadium heptaoxide' _chemical_formula_moiety '(C4 H10 N) 1+, V3 O7 1-' _chemical_formula_sum 'C4 H10 N O7 V3' _chemical_formula_weight 336.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.971(3) _cell_length_b 6.5997(17) _cell_length_c 15.375(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.351(5) _cell_angle_gamma 90.00 _cell_volume 1007.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 1629 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 28.2 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.005 _exptl_crystal_density_diffrn 2.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 2.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9858 _exptl_absorpt_correction_T_max 0.9864 _exptl_absorpt_process_details 'XPREP (Sheldrick, 1997)' _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SmartApex CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% -0.12 _diffrn_reflns_number 6021 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1729 _reflns_number_gt 1316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997), ATOMS (Dowty,1999)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.054P)^2^+5.5P], 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 1729 _refine_ls_number_parameters 136 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1359 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _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 V1 V 0.06446(14) 0.26033(16) 0.43988(7) 0.0159(3) Uani 1 1 d . . . V3 V 0.06375(14) 0.03391(16) 0.24111(7) 0.0144(3) Uani 1 1 d . . . V2 V -0.12907(13) 0.25591(17) 0.11360(7) 0.0157(3) Uani 1 1 d . . . O1 O 0.1933(6) 0.2852(8) 0.5083(3) 0.0298(14) Uani 1 1 d . . . O2 O 0.2061(6) 0.1045(8) 0.2126(3) 0.0289(14) Uani 1 1 d . . . O3 O -0.2876(6) 0.2265(8) 0.1012(4) 0.0331(14) Uani 1 1 d . . . O4 O 0.0851(5) 0.0451(7) 0.3707(3) 0.0189(12) Uani 1 1 d . . . O5 O 0.0451(5) 0.4830(6) 0.3738(3) 0.0181(12) Uani 1 1 d . . . O6 O -0.0740(6) 0.2283(7) 0.4957(3) 0.0224(13) Uani 1 1 d . . . O7 O -0.0637(5) 0.2501(7) 0.2363(3) 0.0191(12) Uani 1 1 d . . . N1 N 0.3239(9) 0.8041(13) 0.1117(6) 0.056(3) Uani 1 1 d . . . H1A H 0.2718 0.8021 0.0606 0.067 Uiso 1 1 calc R . . H1B H 0.2897 0.8959 0.1468 0.067 Uiso 1 1 calc R . . C1 C 0.3245(14) 0.6032(19) 0.1524(9) 0.077(4) Uani 1 1 d . . . H1C H 0.3058 0.6138 0.2130 0.093 Uiso 1 1 calc R . . H1D H 0.2571 0.5165 0.1219 0.093 Uiso 1 1 calc R . . C2 C 0.4576(18) 0.523(3) 0.1461(12) 0.115(6) Uani 1 1 d U . . H2A H 0.4920 0.4633 0.2015 0.138 Uiso 1 1 calc R . . H2B H 0.4547 0.4181 0.1017 0.138 Uiso 1 1 calc R . . C3 C 0.5431(14) 0.684(3) 0.1239(12) 0.106(6) Uani 1 1 d . . . H3A H 0.5949 0.6424 0.0766 0.127 Uiso 1 1 calc R . . H3B H 0.6053 0.7192 0.1739 0.127 Uiso 1 1 calc R . . C4 C 0.4586(15) 0.859(2) 0.0969(9) 0.083(4) Uani 1 1 d . . . H4A H 0.4871 0.9773 0.1312 0.100 Uiso 1 1 calc R . . H4B H 0.4646 0.8890 0.0357 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0337(8) 0.0020(5) 0.0115(6) 0.0007(4) -0.0006(5) 0.0011(6) V3 0.0285(8) 0.0040(5) 0.0104(5) 0.0003(5) 0.0010(5) -0.0014(5) V2 0.0266(8) 0.0057(6) 0.0148(6) 0.0009(5) 0.0024(5) 0.0004(6) O1 0.040(4) 0.022(3) 0.026(3) 0.001(2) -0.004(3) 0.000(3) O2 0.043(4) 0.021(3) 0.023(3) 0.001(2) 0.009(3) -0.007(3) O3 0.037(4) 0.021(3) 0.041(3) 0.000(2) 0.005(3) -0.005(3) O4 0.040(4) 0.005(2) 0.012(2) -0.0017(19) 0.004(2) 0.003(2) O5 0.035(3) 0.002(2) 0.016(2) 0.0009(18) -0.001(2) -0.001(2) O6 0.037(4) 0.013(3) 0.017(2) -0.003(2) 0.004(2) -0.003(2) O7 0.039(3) 0.004(2) 0.014(2) -0.0036(18) 0.004(2) 0.001(2) N1 0.044(6) 0.050(6) 0.069(6) -0.026(5) -0.024(5) 0.019(5) C1 0.063(10) 0.075(9) 0.098(10) -0.027(8) 0.026(8) -0.015(7) C2 0.091(11) 0.109(11) 0.151(12) 0.050(10) 0.036(10) 0.040(10) C3 0.035(8) 0.152(16) 0.134(14) -0.016(12) 0.018(9) 0.009(10) C4 0.073(11) 0.080(10) 0.095(10) 0.026(8) 0.002(9) -0.014(8) _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. SHELX plane for tetrahydropyrazonium molecule. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 0.9019 (0.0732) x + 2.2916 (0.0503) y + 14.1588 (0.0487) z = 3.7587 (0.0412) * -0.0427 (0.0082) N1 * 0.0742 (0.0094) C1 * -0.0792 (0.0115) C2 * 0.0522 (0.0114) C3 * -0.0044 (0.0096) C4 Rms deviation of fitted atoms = 0.0572 ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.591(6) . yes V1 O6 1.705(5) . yes V1 O5 1.787(4) . yes V1 O4 1.798(4) . yes V3 O2 1.594(6) . yes V3 O7 1.905(5) 2_545 yes V3 O7 1.907(5) . yes V3 O4 1.986(4) . yes V3 O5 2.014(5) 2_545 yes V3 V2 2.9171(16) 2_545 ? V3 V2 2.9973(18) . ? V2 O3 1.586(6) . yes V2 O7 1.938(5) . yes V2 O6 1.945(5) 4_565 yes V2 O4 1.968(5) 2 yes V2 O5 1.988(5) 2_545 yes V2 V3 2.9171(16) 2 ? N1 C4 1.430(15) . yes N1 C1 1.466(15) . yes C1 C2 1.441(18) . yes C2 C3 1.42(2) . yes C3 C4 1.466(19) . yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 O6 108.8(3) . . ? O1 V1 O5 109.2(3) . . ? O6 V1 O5 109.8(2) . . ? O1 V1 O4 110.0(3) . . ? O6 V1 O4 110.0(2) . . ? O5 V1 O4 109.0(2) . . ? O2 V3 O7 110.7(3) . 2_545 ? O2 V3 O7 112.2(2) . . ? O7 V3 O7 136.97(12) 2_545 . yes O2 V3 O4 104.5(3) . . ? O7 V3 O4 81.67(19) 2_545 . ? O7 V3 O4 91.15(19) . . ? O2 V3 O5 103.2(2) . 2_545 ? O7 V3 O5 89.24(19) 2_545 2_545 ? O7 V3 O5 77.75(19) . 2_545 ? O4 V3 O5 152.3(2) . 2_545 yes O2 V3 V2 104.7(2) . 2_545 ? O7 V3 V2 41.03(14) 2_545 2_545 ? O7 V3 V2 126.92(15) . 2_545 ? O4 V3 V2 42.22(13) . 2_545 ? O5 V3 V2 129.09(13) 2_545 2_545 ? O2 V3 V2 102.2(2) . . ? O7 V3 V2 126.07(16) 2_545 . ? O7 V3 V2 39.15(14) . . ? O4 V3 V2 129.83(15) . . ? O5 V3 V2 41.17(13) 2_545 . ? O3 V2 O7 110.8(3) . . ? O3 V2 O6 105.0(3) . 4_565 ? O7 V2 O6 144.0(2) . 4_565 yes O3 V2 O4 110.0(3) . 2 ? O7 V2 O4 81.31(19) . 2 ? O6 V2 O4 89.0(2) 4_565 2 ? O3 V2 O5 107.9(2) . 2_545 ? O7 V2 O5 77.69(19) . 2_545 ? O6 V2 O5 89.2(2) 4_565 2_545 yes O4 V2 O5 141.2(2) 2 2_545 ? O3 V2 V3 108.5(2) . 2 ? O7 V2 V3 40.20(13) . 2 ? O6 V2 V3 128.15(16) 4_565 2 ? O4 V2 V3 42.68(13) 2 2 ? O5 V2 V3 115.68(14) 2_545 2 ? O3 V2 V3 126.2(2) . . ? O7 V2 V3 38.42(14) . . ? O6 V2 V3 114.58(17) 4_565 . ? O4 V2 V3 105.77(15) 2 . ? O5 V2 V3 41.82(13) 2_545 . ? V1 O4 V2 136.9(2) . 2_545 ? V1 O4 V3 128.0(2) . . ? V2 O4 V3 95.10(19) 2_545 . ? V1 O5 V2 131.9(3) . 2 ? V1 O5 V3 131.1(3) . 2 ? V2 O5 V3 97.01(19) 2 2 ? V1 O6 V2 140.8(3) . 4_566 ? V3 O7 V3 137.7(3) 2 . ? V3 O7 V2 98.8(2) 2 . ? V3 O7 V2 102.4(2) . . ? C4 N1 C1 109.2(10) . . ? C2 C1 N1 105.8(11) . . ? C3 C2 C1 108.4(13) . . ? C2 C3 C4 108.4(12) . . ? N1 C4 C3 106.2(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 V1 O4 V2 52.8(5) . . . 2_545 ? O6 V1 O4 V2 -67.1(5) . . . 2_545 ? O5 V1 O4 V2 172.5(4) . . . 2_545 ? O1 V1 O4 V3 -128.5(4) . . . . ? O6 V1 O4 V3 111.7(4) . . . . ? O5 V1 O4 V3 -8.8(4) . . . . ? O2 V3 O4 V1 84.9(4) . . . . ? O7 V3 O4 V1 -165.8(4) 2_545 . . . ? O7 V3 O4 V1 -28.4(4) . . . . ? O5 V3 O4 V1 -93.7(5) 2_545 . . . ? O2 V3 O4 V2 -96.0(3) . . . 2_545 ? O7 V3 O4 V2 13.3(2) 2_545 . . 2_545 ? O7 V3 O4 V2 150.7(2) . . . 2_545 ? O5 V3 O4 V2 85.4(4) 2_545 . . 2_545 ? O1 V1 O5 V2 -13.4(4) . . . 2 ? O6 V1 O5 V2 105.8(4) . . . 2 ? O4 V1 O5 V2 -133.6(3) . . . 2 ? O1 V1 O5 V3 163.5(4) . . . 2 ? O6 V1 O5 V3 -77.3(4) . . . 2 ? O4 V1 O5 V3 43.3(4) . . . 2 ? O1 V1 O6 V2 9.9(5) . . . 4_566 ? O5 V1 O6 V2 -109.5(5) . . . 4_566 ? O4 V1 O6 V2 130.5(4) . . . 4_566 ? O2 V3 O7 V3 -36.4(4) . . . 2 ? O7 V3 O7 V3 148.7(4) 2_545 . . 2 ? O4 V3 O7 V3 69.8(4) . . . 2 ? O5 V3 O7 V3 -135.9(4) 2_545 . . 2 ? O2 V3 O7 V2 81.9(3) . . . . ? O7 V3 O7 V2 -92.92(19) 2_545 . . . ? O4 V3 O7 V2 -171.9(2) . . . . ? O5 V3 O7 V2 -17.5(2) 2_545 . . . ? O3 V2 O7 V3 -94.4(3) . . . 2 ? O6 V2 O7 V3 89.9(4) 4_565 . . 2 ? O4 V2 O7 V3 13.8(2) 2 . . 2 ? O5 V2 O7 V3 161.0(3) 2_545 . . 2 ? O3 V2 O7 V3 122.4(3) . . . . ? O6 V2 O7 V3 -53.3(4) 4_565 . . . ? O4 V2 O7 V3 -129.4(3) 2 . . . ? O5 V2 O7 V3 17.8(2) 2_545 . . . ? O2 V3 V2 O3 172.0(3) . . . . ? O7 V3 V2 O3 44.8(3) 2_545 . . . ? O7 V3 V2 O3 -77.7(3) . . . . ? O4 V3 V2 O3 -67.2(3) . . . . ? O5 V3 V2 O3 75.7(3) 2_545 . . . ? O2 V3 V2 O7 -110.3(3) . . . . ? O7 V3 V2 O7 122.52(17) 2_545 . . . ? O4 V3 V2 O7 10.5(3) . . . . ? O5 V3 V2 O7 153.4(3) 2_545 . . . ? O2 V3 V2 O6 38.5(3) . . . 4_565 ? O7 V3 V2 O6 -88.7(3) 2_545 . . 4_565 ? O7 V3 V2 O6 148.8(3) . . . 4_565 ? O4 V3 V2 O6 159.4(3) . . . 4_565 ? O5 V3 V2 O6 -57.7(3) 2_545 . . 4_565 ? O2 V3 V2 O4 -57.8(2) . . . 2 ? O7 V3 V2 O4 175.0(2) 2_545 . . 2 ? O7 V3 V2 O4 52.5(3) . . . 2 ? O4 V3 V2 O4 63.1(3) . . . 2 ? O5 V3 V2 O4 -154.1(3) 2_545 . . 2 ? O2 V3 V2 O5 96.3(3) . . . 2_545 ? O7 V3 V2 O5 -30.9(3) 2_545 . . 2_545 ? O7 V3 V2 O5 -153.4(3) . . . 2_545 ? O4 V3 V2 O5 -142.9(3) . . . 2_545 ? C4 N1 C1 C2 -10.9(15) . . . . yes N1 C1 C2 C3 14.2(18) . . . . yes C1 C2 C3 C4 -12(2) . . . . yes C1 N1 C4 C3 3.5(15) . . . . yes C2 C3 C4 N1 5.4(19) . . . . yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1A O6 0.90 2.14 2.901(10) 142.4 2 yes N1 H1B O2 0.90 1.94 2.839(10) 174.4 1_565 yes _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.556 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.137 # REFERENCES: # Data collection & reduction - SMART & SAINT (Bruker, 1999). # Absorption correction - SADABS (Sheldrick, 1996). # Structure solving - SHELXS-90 (Sheldrick, 1990). # Structure refinement - SHELXL-97 (Sheldrick, 1997) and # Structure drawing - ATOMS (Dowty, 1999). # Ellipsoids plot - ORTEP3 (Farrugia, 1997). _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Dowty, E. (1999). ATOMS for Windows and Macintosh. Version 5. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, USA. Farrugia, L. J. (1997). J. Appl. Cryst., 30, 565-565. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. ; data_dmaV3O7_0324 _database_code_depnum_ccdc_archive 'CCDC 235653' _chemical_name_systematic 'dimethylammonium trivanadium heptaoxide' _chemical_name_common 'dimethylammonium trivanadium heptaoxide' _chemical_formula_moiety '(C2 H8 N), V3 O7' _chemical_formula_sum 'C2 H8 N O7 V3' _chemical_formula_weight 310.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.6453(8) _cell_length_b 6.6842(7) _cell_length_c 8.5667(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.068(2) _cell_angle_gamma 90.00 _cell_volume 433.45(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1386 _cell_measurement_theta_min 3.85 _cell_measurement_theta_max 30.99 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 3.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5655 _exptl_absorpt_correction_T_max 0.8533 _exptl_absorpt_process_details 'XPREP (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SmartApex CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% -0.04 _diffrn_reflns_number 4272 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 30.50 _reflns_number_total 2392 _reflns_number_gt 2243 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997), ATOMS (Dowty,1999)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.06P)^2^], 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 constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 2392 _refine_ls_number_parameters 122 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _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 V1 V 0.38239(6) 0.67798(9) 0.56527(7) 0.01571(13) Uani 1 1 d . . . V2 V 0.27970(6) 1.18425(8) 0.65075(7) 0.01417(12) Uani 1 1 d . . . V3 V -0.01157(7) 0.91199(9) 0.57426(7) 0.01433(12) Uani 1 1 d . . . O7 O 0.0312(3) 1.1899(4) 0.5675(3) 0.0187(5) Uani 1 1 d . . . O2 O 0.2993(4) 1.1991(5) 0.8399(3) 0.0292(6) Uani 1 1 d . . . O6 O 0.2532(3) 0.9001(4) 0.5904(3) 0.0187(5) Uani 1 1 d . . . O5 O 0.2472(3) 0.4585(4) 0.5601(3) 0.0195(6) Uani 1 1 d . . . O4 O 0.4766(3) 0.6904(5) 0.3964(3) 0.0234(6) Uani 1 1 d . . . O1 O 0.5376(4) 0.6567(5) 0.7118(4) 0.0309(7) Uani 1 1 d . . . O3 O -0.0571(4) 0.8521(5) 0.7436(4) 0.0290(7) Uani 1 1 d . . . N1 N 0.2908(7) 0.8416(10) 0.0742(7) 0.0701(17) Uani 1 1 d . . . H1D H 0.3184 0.9366 0.0073 0.105 Uiso 1 1 calc R . . H1E H 0.3745 0.8437 0.1593 0.105 Uiso 1 1 calc R . . C1 C 0.1227(7) 0.8928(11) 0.1239(7) 0.0481(13) Uani 1 1 d . . . H1A H 0.0374 0.9190 0.0329 0.072 Uiso 1 1 calc R . . H1B H 0.1367 1.0098 0.1895 0.072 Uiso 1 1 calc R . . H1C H 0.0828 0.7834 0.1824 0.072 Uiso 1 1 calc R . . C2 C 0.2955(8) 0.6537(12) 0.0001(8) 0.0618(19) Uani 1 1 d . . . H2A H 0.2716 0.5503 0.0719 0.093 Uiso 1 1 calc R . . H2B H 0.4103 0.6329 -0.0303 0.093 Uiso 1 1 calc R . . H2C H 0.2079 0.6499 -0.0918 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0098(2) 0.0092(2) 0.0279(3) -0.0004(2) 0.0020(2) -0.0001(2) V2 0.0120(2) 0.0107(2) 0.0198(3) -0.0002(2) 0.00211(19) 0.0001(2) V3 0.0120(2) 0.0101(2) 0.0212(3) 0.0011(2) 0.00342(19) -0.0001(2) O7 0.0132(9) 0.0107(11) 0.0312(13) 0.0026(11) -0.0006(9) -0.0021(9) O2 0.0282(13) 0.0364(17) 0.0224(13) -0.0022(14) 0.0020(11) -0.0020(14) O6 0.0130(10) 0.0095(11) 0.0336(13) -0.0035(12) 0.0032(9) -0.0012(10) O5 0.0112(10) 0.0094(12) 0.0371(16) 0.0021(10) 0.0003(10) -0.0020(8) O4 0.0160(10) 0.0182(12) 0.0369(15) -0.0005(14) 0.0075(10) -0.0013(11) O1 0.0234(12) 0.0231(16) 0.0420(17) 0.0005(14) -0.0097(12) -0.0002(12) O3 0.0311(15) 0.0294(17) 0.0284(15) 0.0071(12) 0.0106(13) -0.0044(12) N1 0.054(3) 0.079(4) 0.073(4) -0.011(3) -0.007(3) -0.011(3) C1 0.047(3) 0.052(3) 0.045(3) -0.007(3) 0.007(2) 0.010(3) C2 0.044(3) 0.083(5) 0.055(4) -0.023(4) -0.001(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.609(3) . yes V1 O4 1.707(3) . yes V1 O5 1.791(3) . yes V1 O6 1.813(3) . yes V2 O2 1.610(3) . yes V2 O7 1.934(2) . yes V2 O4 1.961(2) 2_656 yes V2 O6 1.971(3) . yes V2 O5 1.993(3) 1_565 yes V2 V3 2.8793(8) . ? V2 V3 3.0209(8) 2_556 ? V3 O3 1.590(3) . yes V3 O7 1.889(3) . yes V3 O7 1.911(3) 2_546 yes V3 O6 2.011(2) . yes V3 O5 2.021(3) 2_556 yes V3 V2 3.0209(8) 2_546 ? N1 C2 1.411(9) . yes N1 C1 1.450(6) . yes N1 H1D 0.9000 . ? N1 H1E 0.9000 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 O4 108.24(16) . . ? O1 V1 O5 107.87(15) . . ? O4 V1 O5 109.23(14) . . ? O1 V1 O6 109.54(14) . . ? O4 V1 O6 111.27(14) . . ? O5 V1 O6 110.60(10) . . ? O2 V2 O7 108.53(13) . . ? O2 V2 O4 104.42(13) . 2_656 ? O7 V2 O4 146.75(12) . 2_656 yes O2 V2 O6 108.36(16) . . ? O7 V2 O6 82.12(11) . . ? O4 V2 O6 91.81(12) 2_656 . ? O2 V2 O5 108.96(16) . 1_565 ? O7 V2 O5 77.05(11) . 1_565 ? O4 V2 O5 88.32(12) 2_656 1_565 ? O6 V2 O5 141.38(11) . 1_565 yes O2 V2 V3 103.16(12) . . ? O7 V2 V3 40.54(9) . . ? O4 V2 V3 133.87(9) 2_656 . ? O6 V2 V3 44.25(7) . . ? O5 V2 V3 116.27(8) 1_565 . ? O2 V2 V3 124.78(12) . 2_556 ? O7 V2 V3 37.93(8) . 2_556 ? O4 V2 V3 115.93(9) 2_656 2_556 ? O6 V2 V3 106.42(8) . 2_556 ? O5 V2 V3 41.53(7) 1_565 2_556 ? O3 V3 O7 109.68(14) . . ? O3 V3 O7 112.13(15) . 2_546 ? O7 V3 O7 138.01(6) . 2_546 yes O3 V3 O6 105.93(14) . . ? O7 V3 O6 82.18(11) . . ? O7 V3 O6 90.09(11) 2_546 . ? O3 V3 O5 105.45(14) . 2_556 ? O7 V3 O5 88.61(10) . 2_556 ? O7 V3 O5 76.90(10) 2_546 2_556 ? O6 V3 O5 148.58(13) . 2_556 yes O7 V3 V2 41.71(7) . . ? O7 V3 V2 128.68(7) 2_546 . ? O6 V3 V2 43.15(8) . . ? O5 V3 V2 129.16(8) 2_556 . ? O3 V3 V2 103.85(12) . 2_546 ? O7 V3 V2 125.53(8) . 2_546 ? O7 V3 V2 38.47(7) 2_546 2_546 ? O6 V3 V2 127.61(8) . 2_546 ? O5 V3 V2 40.83(7) 2_556 2_546 ? V3 O7 V3 141.73(15) . 2_556 ? V3 O7 V2 97.75(12) . . ? V3 O7 V2 103.60(12) 2_556 . ? V1 O6 V2 141.52(13) . . ? V1 O6 V3 125.73(14) . . ? V2 O6 V3 92.59(11) . . ? V1 O5 V2 134.72(14) . 1_545 ? V1 O5 V3 127.25(14) . 2_546 ? V2 O5 V3 97.63(11) 1_545 2_546 ? V1 O4 V2 134.41(16) . 2_646 ? C2 N1 C1 115.0(6) . . yes C2 N1 H1D 108.5 . . ? C1 N1 H1D 108.5 . . ? C2 N1 H1E 108.5 . . ? C1 N1 H1E 108.5 . . ? H1D N1 H1E 107.5 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 V3 O7 V3 -149.8(2) . . . 2_556 ? O7 V3 O7 V3 24.7(2) 2_546 . . 2_556 ? O6 V3 O7 V3 106.1(2) . . . 2_556 ? O5 V3 O7 V3 -43.8(2) 2_556 . . 2_556 ? O3 V3 O7 V2 86.49(16) . . . . ? O7 V3 O7 V2 -99.06(11) 2_546 . . . ? O6 V3 O7 V2 -17.70(11) . . . . ? O5 V3 O7 V2 -167.59(13) 2_556 . . . ? O2 V2 O7 V3 -88.72(18) . . . . ? O4 V2 O7 V3 99.3(2) 2_656 . . . ? O6 V2 O7 V3 18.08(12) . . . . ? O5 V2 O7 V3 165.35(14) 1_565 . . . ? O2 V2 O7 V3 123.27(17) . . . 2_556 ? O4 V2 O7 V3 -48.7(3) 2_656 . . 2_556 ? O6 V2 O7 V3 -129.93(14) . . . 2_556 ? O5 V2 O7 V3 17.34(13) 1_565 . . 2_556 ? O1 V1 O6 V2 44.5(3) . . . . ? O4 V1 O6 V2 -75.2(3) . . . . ? O5 V1 O6 V2 163.2(2) . . . . ? O1 V1 O6 V3 -129.55(19) . . . . ? O4 V1 O6 V3 110.81(18) . . . . ? O5 V1 O6 V3 -10.8(2) . . . . ? O2 V2 O6 V1 -85.0(3) . . . . ? O7 V2 O6 V1 168.1(3) . . . . ? O4 V2 O6 V1 20.9(3) 2_656 . . . ? O5 V2 O6 V1 110.5(3) 1_565 . . . ? O2 V2 O6 V3 90.18(14) . . . . ? O7 V2 O6 V3 -16.80(11) . . . . ? O4 V2 O6 V3 -163.97(12) 2_656 . . . ? O5 V2 O6 V3 -74.40(16) 1_565 . . . ? O3 V3 O6 V1 85.2(2) . . . . ? O7 V3 O6 V1 -166.52(19) . . . . ? O7 V3 O6 V1 -27.92(19) 2_546 . . . ? O5 V3 O6 V1 -92.3(3) 2_556 . . . ? O3 V3 O6 V2 -91.11(15) . . . . ? O7 V3 O6 V2 17.21(11) . . . . ? O7 V3 O6 V2 155.81(12) 2_546 . . . ? O5 V3 O6 V2 91.4(2) 2_556 . . . ? O1 V1 O5 V2 -18.9(3) . . . 1_545 ? O4 V1 O5 V2 98.5(2) . . . 1_545 ? O6 V1 O5 V2 -138.7(2) . . . 1_545 ? O1 V1 O5 V3 170.05(19) . . . 2_546 ? O4 V1 O5 V3 -72.5(2) . . . 2_546 ? O6 V1 O5 V3 50.3(2) . . . 2_546 ? O1 V1 O4 V2 0.0(3) . . . 2_646 ? O5 V1 O4 V2 -117.2(2) . . . 2_646 ? O6 V1 O4 V2 120.4(2) . . . 2_646 ? O2 V2 V3 O3 -2.65(17) . . . . ? O7 V2 V3 O3 -105.86(17) . . . . ? O4 V2 V3 O3 122.78(17) 2_656 . . . ? O6 V2 V3 O3 100.27(17) . . . . ? O5 V2 V3 O3 -121.82(15) 1_565 . . . ? O2 V2 V3 O7 103.22(18) . . . . ? O4 V2 V3 O7 -131.36(18) 2_656 . . . ? O6 V2 V3 O7 -153.87(17) . . . . ? O5 V2 V3 O7 -15.96(15) 1_565 . . . ? O2 V2 V3 O7 -134.59(16) . . . 2_546 ? O7 V2 V3 O7 122.20(10) . . . 2_546 ? O4 V2 V3 O7 -9.16(17) 2_656 . . 2_546 ? O6 V2 V3 O7 -31.67(15) . . . 2_546 ? O5 V2 V3 O7 106.24(14) 1_565 . . 2_546 ? O2 V2 V3 O6 -102.92(17) . . . . ? O7 V2 V3 O6 153.87(17) . . . . ? O4 V2 V3 O6 22.50(17) 2_656 . . . ? O5 V2 V3 O6 137.91(14) 1_565 . . . ? O2 V2 V3 O5 119.31(17) . . . 2_556 ? O7 V2 V3 O5 16.09(16) . . . 2_556 ? O4 V2 V3 O5 -115.27(16) 2_656 . . 2_556 ? O6 V2 V3 O5 -137.78(17) . . . 2_556 ? O5 V2 V3 O5 0.1(2) 1_565 . . 2_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1D O2 0.90 2.26 3.127(7) 162.3 1_554 yes N1 H1E O4 0.90 2.31 3.091(7) 145.0 . yes N1 H1E O1 0.90 2.42 2.973(7) 120.3 2_656 yes _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 1.020 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.119 # REFERENCES: # Data collection & reduction - SMART & SAINT (Bruker, 1999). # Absorption correction - SADABS (Sheldrick, 1996). # Structure solving - SHELXS-90 (Sheldrick, 1990). # Structure refinement - SHELXL-97 (Sheldrick, 1997) and # Geometry - PLATON (Spek, 1990). # Structure drawing - ATOMS (Dowty, 1999). # Ellipsoids plot - ORTEP3 (Farrugia, 1997). _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Dowty, E. (1999). ATOMS for Windows and Macintosh. Version 5. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, USA. Farrugia, L. J. (1997). J. Appl. Cryst., 30, 565-565. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. ; data_0365_ppdV3O7 _database_code_depnum_ccdc_archive 'CCDC 235654' _chemical_name_systematic 'Piperidinium trivanadium heptaoxide' _chemical_name_common 'Piperidinium trivanadium heptaoxide' _chemical_formula_structural (C5H12N)V3O7 _chemical_formula_moiety '(C5 H12 N), (V3 O7)' _chemical_formula_sum 'C5 H12 N O7 V3' _chemical_formula_weight 350.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 10.678(3) _cell_length_b 6.6375(18) _cell_length_c 15.506(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.343(5) _cell_angle_gamma 90.00 _cell_volume 1084.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2388 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 31.8 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 2.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 2.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7558 _exptl_absorpt_correction_T_max 0.9264 _exptl_absorpt_process_details 'XPREP (Sheldrick, 1997)' _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SmartApex CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0.25 _diffrn_reflns_number 10096 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 30.03 _reflns_number_total 3121 _reflns_number_gt 2205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997), ATOMS (Dowty,1999)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)] _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3121 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 V1 V 0.44013(5) 0.73855(7) 0.05735(3) 0.00677(11) Uani 1 1 d . . . V3 V 0.56364(5) 0.46657(7) 0.24416(3) 0.00650(11) Uani 1 1 d . . . V2 V 0.38038(5) 0.24412(7) 0.10842(3) 0.00658(11) Uani 1 1 d . . . O1 O 0.31666(19) 0.7054(3) -0.01543(12) 0.0118(5) Uani 1 1 d . . . O2 O 0.69910(19) 0.3959(3) 0.22116(12) 0.0105(4) Uani 1 1 d . . . O3 O 0.23037(18) 0.2828(3) 0.08687(12) 0.0101(4) Uani 1 1 d . . . O4 O 0.56978(18) 0.7743(3) 0.00703(11) 0.0098(4) Uani 1 1 d . . . O5 O 0.46185(18) 0.5156(2) 0.12385(11) 0.0083(4) Uani 1 1 d . . . O6 O 0.58234(18) 0.4543(3) 0.37429(11) 0.0084(4) Uani 1 1 d . . . O7 O 0.44225(17) 0.2506(3) 0.23333(11) 0.0072(4) Uani 1 1 d . . . N11 N 0.1837(2) 0.3527(3) 0.88951(15) 0.0142(6) Uani 1 1 d . . . H11A H 0.2214 0.3209 0.9455 0.017 Uiso 1 1 calc R . . H11B H 0.2289 0.4569 0.8703 0.017 Uiso 1 1 calc R . . C12 C 0.0507(3) 0.4213(4) 0.8911(2) 0.0158(7) Uani 1 1 d . . . H12A H 0.0128 0.4712 0.8325 0.019 Uiso 1 1 calc R . . H12B H 0.0515 0.5337 0.9331 0.019 Uiso 1 1 calc R . . C13 C -0.0287(3) 0.2511(4) 0.91719(19) 0.0191(7) Uani 1 1 d . . . H13A H -0.1173 0.2975 0.9144 0.023 Uiso 1 1 calc R . . H13B H 0.0038 0.2115 0.9783 0.023 Uiso 1 1 calc R . . C14 C -0.0263(3) 0.0682(4) 0.8575(2) 0.0162(7) Uani 1 1 d . . . H14A H -0.0752 -0.0436 0.8782 0.019 Uiso 1 1 calc R . . H14B H -0.0665 0.1033 0.7973 0.019 Uiso 1 1 calc R . . C15 C 0.1103(3) 0.0016(4) 0.85757(19) 0.0160(7) Uani 1 1 d . . . H15A H 0.1472 -0.0462 0.9167 0.019 Uiso 1 1 calc R . . H15B H 0.1112 -0.1122 0.8164 0.019 Uiso 1 1 calc R . . C16 C 0.1904(3) 0.1720(4) 0.8313(2) 0.0165(7) Uani 1 1 d . . . H16A H 0.2797 0.1271 0.8359 0.020 Uiso 1 1 calc R . . H16B H 0.1596 0.2098 0.7698 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0110(3) 0.0050(2) 0.0044(2) 0.00024(19) 0.0016(2) 0.0002(2) V3 0.0097(3) 0.0054(2) 0.0047(2) -0.00002(19) 0.00223(19) 0.0004(2) V2 0.0095(3) 0.0055(2) 0.0050(2) 0.0000(2) 0.00204(19) -0.0004(2) O1 0.0163(12) 0.0105(11) 0.0083(10) 0.0002(8) 0.0016(9) -0.0001(9) O2 0.0117(12) 0.0112(10) 0.0087(11) -0.0008(8) 0.0021(9) 0.0010(8) O3 0.0110(12) 0.0119(11) 0.0070(10) 0.0024(8) 0.0005(8) 0.0009(9) O4 0.0171(12) 0.0061(10) 0.0069(10) -0.0001(8) 0.0045(9) -0.0005(8) O5 0.0149(11) 0.0047(10) 0.0054(10) 0.0010(8) 0.0019(8) -0.0010(8) O6 0.0159(12) 0.0061(9) 0.0034(9) 0.0012(8) 0.0025(8) -0.0002(9) O7 0.0112(11) 0.0075(9) 0.0031(9) 0.0003(8) 0.0013(8) 0.0008(9) N11 0.0167(16) 0.0148(14) 0.0106(13) 0.0013(10) 0.0005(11) -0.0071(11) C12 0.0191(19) 0.0157(17) 0.0129(16) -0.0021(13) 0.0029(14) 0.0034(14) C13 0.0190(18) 0.0241(18) 0.0160(17) 0.0005(15) 0.0078(14) 0.0004(16) C14 0.0155(18) 0.0153(16) 0.0172(17) 0.0039(13) 0.0006(14) -0.0058(13) C15 0.0224(19) 0.0099(16) 0.0151(16) -0.0003(13) 0.0016(14) -0.0010(13) C16 0.0145(18) 0.0175(16) 0.0174(17) -0.0039(13) 0.0027(14) 0.0003(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 V1 O1 1.605(2) . yes V1 O4 1.7124(19) . yes V1 O5 1.7968(17) . yes V1 O6 1.8205(18) 2_655 yes V3 O2 1.614(2) . yes V3 O7 1.9204(18) 2_655 yes V3 O7 1.9214(19) . yes V3 O6 1.9968(18) . yes V3 O5 2.0272(19) . yes V3 V2 2.9211(8) 2_655 yes V3 V2 3.0169(8) . yes V2 O3 1.603(2) . yes V2 O7 1.9428(18) . yes V2 O4 1.9525(18) 3_665 yes V2 O6 1.9740(18) 2_645 yes V2 O5 1.9986(18) . yes V2 V3 2.9211(8) 2_645 yes N11 C12 1.496(4) . yes N11 C16 1.509(3) . yes N11 H11A 0.9200 . ? N11 H11B 0.9200 . ? C12 C13 1.506(4) . yes C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.529(4) . yes C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.524(4) . yes C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.514(4) . yes C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 O4 109.33(10) . . ? O1 V1 O5 107.78(9) . . ? O4 V1 O5 109.70(9) . . ? O1 V1 O6 110.26(9) . 2_655 ? O4 V1 O6 110.42(9) . 2_655 ? O5 V1 O6 109.30(8) . 2_655 ? O2 V3 O7 112.47(9) . 2_655 ? O2 V3 O7 112.33(9) . . ? O7 V3 O7 134.97(4) 2_655 . ? O2 V3 O6 105.38(9) . . ? O7 V3 O6 81.80(7) 2_655 . ? O7 V3 O6 90.76(7) . . ? O2 V3 O5 102.07(9) . . ? O7 V3 O5 88.91(7) 2_655 . ? O7 V3 O5 77.65(7) . . ? O6 V3 O5 152.53(8) . . ? O3 V2 O7 111.76(9) . . ? O3 V2 O4 103.35(9) . 3_665 ? O7 V2 O4 144.71(8) . 3_665 ? O3 V2 O6 110.93(9) . 2_645 ? O7 V2 O6 81.83(7) . 2_645 ? O4 V2 O6 89.11(7) 3_665 2_645 ? O3 V2 O5 106.33(9) . . ? O7 V2 O5 77.86(7) . . ? O4 V2 O5 89.32(7) 3_665 . ? O6 V2 O5 142.03(8) 2_645 . ? O2 V3 V2 106.21(7) . 2_655 ? O7 V3 V2 41.16(5) 2_655 2_655 ? O7 V3 V2 126.04(5) . 2_655 ? O6 V3 V2 42.34(5) . 2_655 ? O5 V3 V2 129.04(5) . 2_655 ? O2 V3 V2 101.92(7) . . ? O7 V3 V2 124.79(6) 2_655 . ? O7 V3 V2 38.93(5) . . ? O6 V3 V2 129.21(6) . . ? O5 V3 V2 41.10(5) . . ? V2 V3 V2 151.86(2) 2_655 . ? O3 V2 O7 111.76(9) . . ? O3 V2 O4 103.35(9) . 3_665 ? O7 V2 O4 144.71(8) . 3_665 ? O3 V2 O6 110.93(9) . 2_645 ? O7 V2 O6 81.83(7) . 2_645 ? O4 V2 O6 89.11(7) 3_665 2_645 ? O3 V2 O5 106.33(9) . . ? O7 V2 O5 77.86(7) . . ? O4 V2 O5 89.32(7) 3_665 . ? O6 V2 O5 142.03(8) 2_645 . ? O3 V2 V3 109.56(7) . 2_645 ? O7 V2 V3 40.59(5) . 2_645 ? O4 V2 V3 128.78(6) 3_665 2_645 ? O6 V2 V3 42.94(5) 2_645 2_645 ? O5 V2 V3 116.44(6) . 2_645 ? O3 V2 V3 125.44(7) . . ? O7 V2 V3 38.42(5) . . ? O4 V2 V3 115.33(6) 3_665 . ? O6 V2 V3 106.77(6) 2_645 . ? O5 V2 V3 41.82(5) . . ? V1 O4 V2 140.35(11) . 3_665 ? V1 O5 V2 131.35(10) . . ? V1 O5 V3 131.33(10) . . ? V2 O5 V3 97.08(7) . . ? V1 O6 V2 136.90(10) 2_645 2_655 ? V1 O6 V3 128.28(9) 2_645 . ? V2 O6 V3 94.72(7) 2_655 . ? V3 O7 V3 139.29(10) 2_645 . ? V3 O7 V2 98.25(8) 2_645 . ? V3 O7 V2 102.66(8) . . ? C12 N11 C16 112.9(2) . . ? C12 N11 H11A 109.0 . . ? C16 N11 H11A 109.0 . . ? C12 N11 H11B 109.0 . . ? C16 N11 H11B 109.0 . . ? H11A N11 H11B 107.8 . . ? N11 C12 C13 110.7(2) . . ? N11 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C12 C13 C14 111.6(2) . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 109.8(2) . . ? C15 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C14 111.5(2) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? N11 C16 C15 110.4(2) . . ? N11 C16 H16A 109.6 . . ? C15 C16 H16A 109.6 . . ? N11 C16 H16B 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 V3 V2 O3 -168.62(10) . . . . ? O7 V3 V2 O3 -40.12(11) 2_655 . . . ? O7 V3 V2 O3 80.50(12) . . . . ? O6 V3 V2 O3 69.91(11) . . . . ? O5 V3 V2 O3 -73.86(11) . . . . ? O2 V3 V2 O7 110.88(11) . . . . ? O7 V3 V2 O7 -120.62(7) 2_655 . . . ? O6 V3 V2 O7 -10.58(11) . . . . ? O5 V3 V2 O7 -154.36(12) . . . . ? O2 V3 V2 O4 -38.04(9) . . . 3_665 ? O7 V3 V2 O4 90.45(9) 2_655 . . 3_665 ? O7 V3 V2 O4 -148.93(10) . . . 3_665 ? O6 V3 V2 O4 -159.51(9) . . . 3_665 ? O5 V3 V2 O4 56.71(10) . . . 3_665 ? O2 V3 V2 O6 59.12(9) . . . 2_645 ? O7 V3 V2 O6 -172.38(8) 2_655 . . 2_645 ? O7 V3 V2 O6 -51.76(10) . . . 2_645 ? O6 V3 V2 O6 -62.35(11) . . . 2_645 ? O5 V3 V2 O6 153.88(10) . . . 2_645 ? O2 V3 V2 O5 -94.76(10) . . . . ? O7 V3 V2 O5 33.73(10) 2_655 . . . ? O7 V3 V2 O5 154.36(12) . . . . ? O6 V3 V2 O5 143.77(10) . . . . ? O2 V3 V2 V3 88.03(7) . . . 2_645 ? O7 V3 V2 V3 -143.48(7) 2_655 . . 2_645 ? O7 V3 V2 V3 -22.86(8) . . . 2_645 ? O6 V3 V2 V3 -33.44(7) . . . 2_645 ? O5 V3 V2 V3 -177.22(8) . . . 2_645 ? O1 V1 O4 V2 -9.95(19) . . . 3_665 ? O5 V1 O4 V2 108.04(16) . . . 3_665 ? O6 V1 O4 V2 -131.44(15) 2_655 . . 3_665 ? O1 V1 O5 V2 11.14(15) . . . . ? O4 V1 O5 V2 -107.81(13) . . . . ? O6 V1 O5 V2 130.99(12) 2_655 . . . ? O1 V1 O5 V3 -161.91(12) . . . . ? O4 V1 O5 V3 79.13(14) . . . . ? O6 V1 O5 V3 -42.07(15) 2_655 . . . ? O3 V2 O5 V1 -49.38(15) . . . . ? O7 V2 O5 V1 -158.78(14) . . . . ? O4 V2 O5 V1 54.33(14) 3_665 . . . ? O6 V2 O5 V1 142.01(12) 2_645 . . . ? O3 V2 O5 V3 125.37(9) . . . . ? O7 V2 O5 V3 15.97(7) . . . . ? O4 V2 O5 V3 -130.92(8) 3_665 . . . ? O6 V2 O5 V3 -43.24(14) 2_645 . . . ? O2 V3 O5 V1 -90.87(14) . . . . ? O7 V3 O5 V1 21.89(13) 2_655 . . . ? O7 V3 O5 V1 158.59(14) . . . . ? O6 V3 O5 V1 91.65(19) . . . . ? O2 V3 O5 V2 94.38(9) . . . . ? O7 V3 O5 V2 -152.86(8) 2_655 . . . ? O7 V3 O5 V2 -16.16(7) . . . . ? O6 V3 O5 V2 -83.10(16) . . . . ? O2 V3 O6 V1 -85.71(14) . . . 2_645 ? O7 V3 O6 V1 163.14(14) 2_655 . . 2_645 ? O7 V3 O6 V1 27.72(13) . . . 2_645 ? O5 V3 O6 V1 91.73(18) . . . 2_645 ? O2 V3 O6 V2 97.36(9) . . . 2_655 ? O7 V3 O6 V2 -13.80(8) 2_655 . . 2_655 ? O7 V3 O6 V2 -149.21(8) . . . 2_655 ? O5 V3 O6 V2 -85.20(17) . . . 2_655 ? O2 V3 O7 V3 37.91(16) . . . 2_645 ? O7 V3 O7 V3 -148.21(16) 2_655 . . 2_645 ? O6 V3 O7 V3 -69.08(14) . . . 2_645 ? O5 V3 O7 V3 136.04(15) . . . 2_645 ? O2 V3 O7 V2 -81.20(10) . . . . ? O7 V3 O7 V2 92.68(7) 2_655 . . . ? O6 V3 O7 V2 171.82(8) . . . . ? O5 V3 O7 V2 16.93(8) . . . . ? O3 V2 O7 V3 95.06(10) . . . 2_645 ? O4 V2 O7 V3 -90.99(13) 3_665 . . 2_645 ? O6 V2 O7 V3 -14.29(8) 2_645 . . 2_645 ? O5 V2 O7 V3 -162.01(9) . . . 2_645 ? O3 V2 O7 V3 -120.10(9) . . . . ? O4 V2 O7 V3 53.86(15) 3_665 . . . ? O6 V2 O7 V3 130.56(9) 2_645 . . . ? O5 V2 O7 V3 -17.17(8) . . . . ? C16 N11 C12 C13 55.4(3) . . . . yes N11 C12 C13 C14 -55.7(3) . . . . yes C12 C13 C14 C15 56.2(3) . . . . yes C13 C14 C15 C16 -56.0(3) . . . . yes C12 N11 C16 C15 -55.2(3) . . . . yes C14 C15 C16 N11 55.3(3) . . . . yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N11 H11B O1 0.92 2.49 2.998(3) 115.1 1_556 yes N11 H11B O2 0.92 1.98 2.827(3) 152.7 3_666 yes N11 H11A O3 0.92 2.19 3.055(3) 155.6 1_556 yes N11 H11A O4 0.92 2.32 2.973(3) 127.8 3_666 yes _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.757 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.124 # REFERENCES: # Data collection & reduction - SMART & SAINT (Bruker, 1999). # Absorption correction - SADABS (Sheldrick, 1996). # Structure solving - SHELXS-90 (Sheldrick, 1990). # Structure refinement - SHELXL-97 (Sheldrick, 1997) and # Geometry - PLATON (Spek, 1990). # Structure drawing - ATOMS (Dowty, 1999). # Ellipsoids plot - ORTEP3 (Farrugia, 1997). _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Dowty, E. (1999). ATOMS for Windows and Macintosh. Version 5. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, USA. Farrugia, L. J. (1997). J. Appl. Cryst., 30, 565-565. Spek A. L. (1990) Acta Cryst., A46, C-34. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. ; data_0368_eaV3O7_RT _database_code_depnum_ccdc_archive 'CCDC 235655' _chemical_name_systematic 'Ethyleneammonium trivanadium heptaoxide' _chemical_name_common 'Ethyleneammonium trivanadium heptaoxide' _chemical_formula_moiety '(C2 H8 N), (V3 O7)' _chemical_formula_sum 'C2 H8 N O7 V3' _chemical_formula_weight 310.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 8.564(6) _cell_length_b 6.646(4) _cell_length_c 15.549(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.106(13) _cell_angle_gamma 90.00 _cell_volume 878.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 3022 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 31.2 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 3.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7995 _exptl_absorpt_correction_T_max 0.9393 _exptl_absorpt_process_details 'XPREP (Sheldrick, 1997)' _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SmartApex CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 5480 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1524 _reflns_number_gt 1111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997), ATOMS (Dowty,1999)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.055P)^2^+5.3P], 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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 1524 _refine_ls_number_parameters 141 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.000 _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 V1 V 0.42376(15) 0.75465(16) 0.06011(7) 0.0149(4) Uani 1 1 d . . . V2 V 0.35369(14) 0.25052(16) 0.11103(7) 0.0131(3) Uani 1 1 d . . . V3A V 0.57629(18) 0.02511(18) 0.24234(8) 0.0114(4) Uani 0.828(5) 1 d P . 1 O3A O 0.7454(8) 0.0851(9) 0.2168(4) 0.0238(15) Uani 0.828(5) 1 d P . 1 V3B V 0.4233(9) -0.0279(9) 0.2593(4) 0.0114(4) Uani 0.17 1 d P . 2 O3B O 0.253(4) -0.086(4) 0.2943(18) 0.0238(15) Uani 0.17 1 d P . 2 O1 O 0.4078(6) 0.5386(7) 0.1274(3) 0.0217(12) Uani 1 1 d . . . O2 O 0.1660(6) 0.2244(8) 0.0939(3) 0.0288(13) Uani 1 1 d . . . O3 O 0.2678(7) 0.7765(9) -0.0069(4) 0.0385(15) Uani 1 1 d . . . O4 O 0.4413(7) 0.9754(7) 0.1258(3) 0.0271(13) Uani 1 1 d . . . O6 O 0.5824(7) 0.7353(7) 0.0038(3) 0.0274(13) Uani 1 1 d . . . O7 O 0.4329(6) 0.2464(6) 0.2332(3) 0.0161(11) Uani 1 1 d . . . C1A C 0.0079(15) 0.2059(19) 0.3745(12) 0.049(4) Uani 0.828(5) 1 d PD . 1 H1A H -0.0330 0.1429 0.4234 0.059 Uiso 0.828(5) 1 calc PR . 1 H1B H -0.0801 0.2290 0.3301 0.059 Uiso 0.828(5) 1 calc PR . 1 C2A C 0.1181(16) 0.0660(16) 0.3404(8) 0.051(3) Uani 0.828(5) 1 d PD . 1 H2A1 H 0.1655 0.1303 0.2948 0.077 Uiso 0.828(5) 1 calc PR . 1 H2A2 H 0.0623 -0.0519 0.3181 0.077 Uiso 0.828(5) 1 calc PR . 1 H2A3 H 0.1986 0.0281 0.3861 0.077 Uiso 0.828(5) 1 calc PR . 1 N1A N 0.0770(12) 0.4016(13) 0.4026(5) 0.036(2) Uani 0.828(5) 1 d PD . 1 H1A1 H 0.1405 0.3861 0.4520 0.053 Uiso 0.828(5) 1 calc PR . 1 H1A2 H 0.0005 0.4876 0.4108 0.053 Uiso 0.828(5) 1 calc PR . 1 H1A3 H 0.1318 0.4495 0.3620 0.053 Uiso 0.828(5) 1 calc PR . 1 C1B C 0.994(5) -0.224(12) 0.133(7) 0.049(4) Uani 0.17 1 d PD . 2 H1B1 H 1.0681 -0.2590 0.1829 0.059 Uiso 0.172(5) 1 calc PR . 2 H1B2 H 1.0513 -0.1548 0.0920 0.059 Uiso 0.172(5) 1 calc PR . 2 N1B N 0.928(6) -0.412(5) 0.092(3) 0.036(2) Uani 0.17 1 d PD . 2 H2B1 H 0.9023 -0.4950 0.1332 0.053 Uiso 0.172(5) 1 calc PR . 2 H2B2 H 0.9996 -0.4704 0.0637 0.053 Uiso 0.172(5) 1 calc PR . 2 H2B3 H 0.8428 -0.3835 0.0556 0.053 Uiso 0.172(5) 1 calc PR . 2 C2B C 0.876(8) -0.086(6) 0.161(4) 0.051(3) Uani 0.17 1 d PD . 2 H1B3 H 0.7894 -0.0736 0.1155 0.077 Uiso 0.172(5) 1 calc PR . 2 H1B4 H 0.9228 0.0435 0.1730 0.077 Uiso 0.172(5) 1 calc PR . 2 H1B5 H 0.8382 -0.1380 0.2120 0.077 Uiso 0.172(5) 1 calc PR . 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 V1 0.0274(7) 0.0079(6) 0.0089(6) 0.0000(5) 0.0001(5) 0.0004(6) V2 0.0185(7) 0.0101(6) 0.0104(6) 0.0008(5) 0.0000(5) -0.0005(5) V3A 0.0203(8) 0.0068(6) 0.0065(6) 0.0002(5) -0.0002(5) -0.0007(6) O3A 0.028(4) 0.028(3) 0.017(3) 0.002(2) 0.009(3) -0.006(3) V3B 0.0203(8) 0.0068(6) 0.0065(6) 0.0002(5) -0.0002(5) -0.0007(6) O3B 0.028(4) 0.028(3) 0.017(3) 0.002(2) 0.009(3) -0.006(3) O1 0.043(3) 0.009(2) 0.012(2) 0.0044(19) -0.002(2) -0.013(2) O2 0.021(3) 0.038(3) 0.026(3) -0.003(3) -0.002(2) -0.004(3) O3 0.038(4) 0.050(4) 0.024(3) -0.003(3) -0.008(3) 0.003(3) O4 0.054(4) 0.011(2) 0.014(2) -0.003(2) -0.006(2) 0.006(3) O6 0.047(4) 0.019(3) 0.018(3) 0.006(2) 0.011(3) 0.002(3) O7 0.029(3) 0.007(2) 0.010(2) -0.0010(18) -0.002(2) 0.001(2) C1A 0.032(6) 0.059(12) 0.055(8) -0.007(8) 0.003(6) -0.018(7) C2A 0.065(9) 0.033(6) 0.054(7) 0.007(5) 0.000(7) 0.003(6) N1A 0.040(6) 0.042(5) 0.023(5) 0.003(4) -0.001(4) -0.001(4) C1B 0.032(6) 0.059(12) 0.055(8) -0.007(8) 0.003(6) -0.018(7) N1B 0.040(6) 0.042(5) 0.023(5) 0.003(4) -0.001(4) -0.001(4) C2B 0.065(9) 0.033(6) 0.054(7) 0.007(5) 0.000(7) 0.003(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 V1 O3 1.596(6) . ? V1 O6 1.710(5) . ? V1 O4 1.783(5) . ? V1 O1 1.792(4) . ? V2 O2 1.606(6) . ? V2 O6 1.933(5) 3_665 ? V2 O7 1.937(5) . ? V2 O1 1.979(5) . ? V2 O4 1.979(5) 1_545 ? V2 V3A 2.924(2) 2_655 ? V2 V3B 2.959(6) . ? V2 V3B 2.988(7) 2_655 ? V2 V3A 3.014(2) . ? V3A O3A 1.599(6) . ? V3A O7 1.894(5) 2_645 ? V3A O7 1.910(5) . ? V3A O1 2.015(5) 2_645 ? V3A O4 2.052(5) 1_545 ? V3A V2 2.924(2) 2_645 ? V3B O3B 1.66(3) . ? V3B O7 1.872(7) . ? V3B O7 1.935(8) 2_645 ? V3B O4 2.102(8) 1_545 ? V3B O1 2.182(8) 2_645 ? V3B V2 2.988(7) 2_645 ? O1 V3A 2.015(5) 2_655 ? O1 V3B 2.182(8) 2_655 ? O4 V2 1.979(5) 1_565 ? O4 V3A 2.052(5) 1_565 ? O4 V3B 2.102(8) 1_565 ? O6 V2 1.933(5) 3_665 ? O7 V3A 1.894(4) 2_655 ? O7 V3B 1.935(8) 2_655 ? C1A C2A 1.470(18) . ? C1A N1A 1.473(16) . ? C1A H1A 0.9700 . ? C1A H1B 0.9700 . ? C2A H2A1 0.9600 . ? C2A H2A2 0.9600 . ? C2A H2A3 0.9600 . ? N1A H1A1 0.8900 . ? N1A H1A2 0.8900 . ? N1A H1A3 0.8900 . ? C1B C2B 1.47(2) . ? C1B N1B 1.48(2) . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? N1B H2B1 0.8900 . ? N1B H2B2 0.8900 . ? N1B H2B3 0.8900 . ? C2B H1B3 0.9600 . ? C2B H1B4 0.9600 . ? C2B H1B5 0.9600 . ? 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 O3 V1 O6 109.0(3) . . ? O3 V1 O4 107.7(3) . . ? O6 V1 O4 109.8(3) . . ? O3 V1 O1 109.6(3) . . ? O6 V1 O1 111.2(2) . . ? O4 V1 O1 109.4(2) . . ? O2 V2 O6 104.1(3) . 3_665 ? O2 V2 O7 112.5(2) . . ? O6 V2 O7 143.3(2) 3_665 . ? O2 V2 O1 109.8(3) . . ? O6 V2 O1 89.0(2) 3_665 . ? O7 V2 O1 80.76(18) . . ? O2 V2 O4 106.1(3) . 1_545 ? O6 V2 O4 90.3(2) 3_665 1_545 ? O7 V2 O4 77.98(18) . 1_545 ? O1 V2 O4 143.1(2) . 1_545 ? O2 V2 V3A 107.6(2) . 2_655 ? O6 V2 V3A 129.45(17) 3_665 2_655 ? O7 V2 V3A 39.71(13) . 2_655 ? O1 V2 V3A 43.42(13) . 2_655 ? O4 V2 V3A 116.62(15) 1_545 2_655 ? O2 V2 V3B 99.4(2) . . ? O6 V2 V3B 134.2(2) 3_665 . ? O7 V2 V3B 38.23(17) . . ? O1 V2 V3B 118.91(18) . . ? O4 V2 V3B 45.19(18) 1_545 . ? V3A V2 V3B 77.32(13) 2_655 . ? O2 V2 V3B 135.1(2) . 2_655 ? O6 V2 V3B 111.6(2) 3_665 2_655 ? O7 V2 V3B 39.48(18) . 2_655 ? O1 V2 V3B 46.88(18) . 2_655 ? O4 V2 V3B 100.1(2) 1_545 2_655 ? V3A V2 V3B 27.63(13) 2_655 2_655 ? V3B V2 V3B 74.47(10) . 2_655 ? O2 V2 V3A 126.5(2) . . ? O6 V2 V3A 114.98(18) 3_665 . ? O7 V2 V3A 38.11(14) . . ? O1 V2 V3A 105.99(16) . . ? O4 V2 V3A 42.55(14) 1_545 . ? V3A V2 V3A 74.36(5) 2_655 . ? V3B V2 V3A 27.35(14) . . ? V3B V2 V3A 59.34(13) 2_655 . ? O3A V3A O7 110.8(3) . 2_645 ? O3A V3A O7 112.5(3) . . ? O7 V3A O7 136.52(12) 2_645 . ? O3A V3A O1 106.7(3) . 2_645 ? O7 V3A O1 80.87(19) 2_645 2_645 ? O7 V3A O1 90.19(19) . 2_645 ? O3A V3A O4 104.4(3) . 1_545 ? O7 V3A O4 89.3(2) 2_645 1_545 ? O7 V3A O4 76.8(2) . 1_545 ? O1 V3A O4 148.8(2) 2_645 1_545 ? O3A V3A V2 104.2(2) . 2_645 ? O7 V3A V2 40.80(14) 2_645 2_645 ? O7 V3A V2 127.33(15) . 2_645 ? O1 V3A V2 42.45(13) 2_645 2_645 ? O4 V3A V2 128.83(15) 1_545 2_645 ? O3A V3A V2 102.9(2) . . ? O7 V3A V2 125.69(16) 2_645 . ? O7 V3A V2 38.75(14) . . ? O1 V3A V2 128.12(15) 2_645 . ? O4 V3A V2 40.70(14) 1_545 . ? V2 V3A V2 152.87(6) 2_645 . ? O3B V3B O7 111.1(11) . . ? O3B V3B O7 112.2(11) . 2_645 ? O7 V3B O7 136.3(4) . 2_645 ? O3B V3B O4 120.0(11) . 1_545 ? O7 V3B O4 76.4(3) . 1_545 ? O7 V3B O4 86.7(3) 2_645 1_545 ? O3B V3B O1 107.7(11) . 2_645 ? O7 V3B O1 86.3(3) . 2_645 ? O7 V3B O1 75.8(3) 2_645 2_645 ? O4 V3B O1 132.3(4) 1_545 2_645 ? O3B V3B V2 107.4(11) . . ? O7 V3B V2 39.82(19) . . ? O7 V3B V2 126.6(3) 2_645 . ? O4 V3B V2 41.90(17) 1_545 . ? O1 V3B V2 123.5(3) 2_645 . ? O3B V3B V2 100.3(11) . 2_645 ? O7 V3B V2 125.8(3) . 2_645 ? O7 V3B V2 39.52(18) 2_645 2_645 ? O4 V3B V2 123.5(3) 1_545 2_645 ? O1 V3B V2 41.45(16) 2_645 2_645 ? V2 V3B V2 152.1(3) . 2_645 ? V1 O1 V2 137.2(3) . . ? V1 O1 V3A 128.5(2) . 2_655 ? V2 O1 V3A 94.12(18) . 2_655 ? V1 O1 V3B 122.9(3) . 2_655 ? V2 O1 V3B 91.7(2) . 2_655 ? V3A O1 V3B 39.1(2) 2_655 2_655 ? V1 O4 V2 133.6(3) . 1_565 ? V1 O4 V3A 129.5(3) . 1_565 ? V2 O4 V3A 96.8(2) 1_565 1_565 ? V1 O4 V3B 123.1(3) . 1_565 ? V2 O4 V3B 92.9(3) 1_565 1_565 ? V3A O4 V3B 39.8(2) 1_565 1_565 ? V1 O6 V2 143.4(3) . 3_665 ? V3B O7 V3A 154.8(3) . 2_655 ? V3B O7 V3A 43.9(2) . . ? V3A O7 V3A 141.3(3) 2_655 . ? V3B O7 V3B 141.9(3) . 2_655 ? V3A O7 V3B 43.3(2) 2_655 2_655 ? V3A O7 V3B 101.2(3) . 2_655 ? V3B O7 V2 101.9(3) . . ? V3A O7 V2 99.5(2) 2_655 . ? V3A O7 V2 103.1(2) . . ? V3B O7 V2 101.0(3) 2_655 . ? C2A C1A N1A 114.4(10) . . ? C2A C1A H1A 108.7 . . ? N1A C1A H1A 108.7 . . ? C2A C1A H1B 108.7 . . ? N1A C1A H1B 108.7 . . ? H1A C1A H1B 107.6 . . ? C2B C1B N1B 114.5(18) . . ? C2B C1B H1B1 108.6 . . ? N1B C1B H1B1 108.6 . . ? C2B C1B H1B2 108.6 . . ? N1B C1B H1B2 108.6 . . ? H1B1 C1B H1B2 107.6 . . ? C1B N1B H2B1 109.5 . . ? C1B N1B H2B2 109.5 . . ? H2B1 N1B H2B2 109.5 . . ? C1B N1B H2B3 109.5 . . ? H2B1 N1B H2B3 109.5 . . ? H2B2 N1B H2B3 109.5 . . ? C1B C2B H1B3 109.5 . . ? C1B C2B H1B4 109.5 . . ? H1B3 C2B H1B4 109.5 . . ? C1B C2B H1B5 109.5 . . ? H1B3 C2B H1B5 109.5 . . ? H1B4 C2B H1B5 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 V2 V3A O3A 169.9(3) . . . . ? O6 V2 V3A O3A 37.1(3) 3_665 . . . ? O7 V2 V3A O3A -110.0(3) . . . . ? O1 V2 V3A O3A -59.5(3) . . . . ? O4 V2 V3A O3A 97.2(3) 1_545 . . . ? O2 V2 V3A O7 42.0(3) . . . 2_645 ? O6 V2 V3A O7 -90.8(3) 3_665 . . 2_645 ? O7 V2 V3A O7 122.16(17) . . . 2_645 ? O1 V2 V3A O7 172.7(2) . . . 2_645 ? O4 V2 V3A O7 -30.7(3) 1_545 . . 2_645 ? O2 V2 V3A O7 -80.2(3) . . . . ? O6 V2 V3A O7 147.1(3) 3_665 . . . ? O1 V2 V3A O7 50.5(3) . . . . ? O4 V2 V3A O7 -152.9(3) 1_545 . . . ? O2 V2 V3A O1 -66.4(3) . . . 2_645 ? O6 V2 V3A O1 160.8(3) 3_665 . . 2_645 ? O7 V2 V3A O1 13.8(3) . . . 2_645 ? O1 V2 V3A O1 64.3(3) . . . 2_645 ? O4 V2 V3A O1 -139.1(3) 1_545 . . 2_645 ? O2 V2 V3A O4 72.7(3) . . . 1_545 ? O6 V2 V3A O4 -60.1(3) 3_665 . . 1_545 ? O7 V2 V3A O4 152.9(3) . . . 1_545 ? O1 V2 V3A O4 -156.6(3) . . . 1_545 ? O2 V2 V3B O3B -12.4(11) . . . . ? O6 V2 V3B O3B -132.8(11) 3_665 . . . ? O7 V2 V3B O3B 102.3(11) . . . . ? O1 V2 V3B O3B 106.5(11) . . . . ? O4 V2 V3B O3B -115.8(11) 1_545 . . . ? O2 V2 V3B O7 -114.7(4) . . . . ? O6 V2 V3B O7 124.9(4) 3_665 . . . ? O1 V2 V3B O7 4.2(4) . . . . ? O4 V2 V3B O7 141.9(5) 1_545 . . . ? O2 V2 V3B O7 124.2(4) . . . 2_645 ? O6 V2 V3B O7 3.9(6) 3_665 . . 2_645 ? O7 V2 V3B O7 -121.0(5) . . . 2_645 ? O1 V2 V3B O7 -116.8(4) . . . 2_645 ? O4 V2 V3B O7 20.9(4) 1_545 . . 2_645 ? O2 V2 V3B O4 103.4(3) . . . 1_545 ? O6 V2 V3B O4 -17.0(4) 3_665 . . 1_545 ? O7 V2 V3B O4 -141.9(5) . . . 1_545 ? O1 V2 V3B O4 -137.7(3) . . . 1_545 ? O2 V2 V3B O1 -138.5(4) . . . 2_645 ? O6 V2 V3B O1 101.1(4) 3_665 . . 2_645 ? O7 V2 V3B O1 -23.8(3) . . . 2_645 ? O1 V2 V3B O1 -19.6(5) . . . 2_645 ? O4 V2 V3B O1 118.1(5) 1_545 . . 2_645 ? O3 V1 O1 V2 50.6(5) . . . . ? O6 V1 O1 V2 -70.0(5) . . . . ? O4 V1 O1 V2 168.5(4) . . . . ? O3 V1 O1 V3A -122.7(4) . . . 2_655 ? O6 V1 O1 V3A 116.6(4) . . . 2_655 ? O4 V1 O1 V3A -4.9(5) . . . 2_655 ? O3 V1 O1 V3B -170.9(4) . . . 2_655 ? O6 V1 O1 V3B 68.4(4) . . . 2_655 ? O4 V1 O1 V3B -53.0(4) . . . 2_655 ? O2 V2 O1 V1 -79.9(5) . . . . ? O6 V2 O1 V1 24.8(5) 3_665 . . . ? O7 V2 O1 V1 169.4(5) . . . . ? O4 V2 O1 V1 114.0(5) 1_545 . . . ? O2 V2 O1 V3A 94.9(3) . . . 2_655 ? O6 V2 O1 V3A -160.5(3) 3_665 . . 2_655 ? O7 V2 O1 V3A -15.9(2) . . . 2_655 ? O4 V2 O1 V3A -71.2(4) 1_545 . . 2_655 ? O2 V2 O1 V3B 134.0(3) . . . 2_655 ? O6 V2 O1 V3B -121.4(3) 3_665 . . 2_655 ? O7 V2 O1 V3B 23.2(3) . . . 2_655 ? O4 V2 O1 V3B -32.2(4) 1_545 . . 2_655 ? O3 V1 O4 V2 -21.0(5) . . . 1_565 ? O6 V1 O4 V2 97.6(4) . . . 1_565 ? O1 V1 O4 V2 -140.1(4) . . . 1_565 ? O3 V1 O4 V3A 163.1(4) . . . 1_565 ? O6 V1 O4 V3A -78.3(4) . . . 1_565 ? O1 V1 O4 V3A 44.0(5) . . . 1_565 ? O3 V1 O4 V3B 113.8(4) . . . 1_565 ? O6 V1 O4 V3B -127.6(4) . . . 1_565 ? O1 V1 O4 V3B -5.3(5) . . . 1_565 ? O3 V1 O6 V2 6.6(6) . . . 3_665 ? O4 V1 O6 V2 -111.2(5) . . . 3_665 ? O1 V1 O6 V2 127.6(5) . . . 3_665 ? O3B V3B O7 V3A 55.5(15) . . . 2_655 ? O7 V3B O7 V3A -117.0(8) 2_645 . . 2_655 ? O4 V3B O7 V3A 172.8(8) 1_545 . . 2_655 ? O1 V3B O7 V3A -52.0(9) 2_645 . . 2_655 ? O3B V3B O7 V3A 171.2(12) . . . . ? O7 V3B O7 V3A -1.3(3) 2_645 . . . ? O4 V3B O7 V3A -71.5(3) 1_545 . . . ? O1 V3B O7 V3A 63.7(3) 2_645 . . . ? O3B V3B O7 V3B 142.0(12) . . . 2_655 ? O7 V3B O7 V3B -30.5(6) 2_645 . . 2_655 ? O4 V3B O7 V3B -100.7(5) 1_545 . . 2_655 ? O1 V3B O7 V3B 34.5(4) 2_645 . . 2_655 ? O3B V3B O7 V2 -92.2(11) . . . . ? O7 V3B O7 V2 95.3(5) 2_645 . . . ? O4 V3B O7 V2 25.1(3) 1_545 . . . ? O1 V3B O7 V2 160.3(3) 2_645 . . . ? O3A V3A O7 V3B 176.2(4) . . . . ? O7 V3A O7 V3B 1.3(3) 2_645 . . . ? O1 V3A O7 V3B -75.5(3) 2_645 . . . ? O4 V3A O7 V3B 75.9(3) 1_545 . . . ? O3A V3A O7 V3A -41.6(5) . . . 2_655 ? O7 V3A O7 V3A 143.5(5) 2_645 . . 2_655 ? O1 V3A O7 V3A 66.6(4) 2_645 . . 2_655 ? O4 V3A O7 V3A -142.0(4) 1_545 . . 2_655 ? O3A V3A O7 V3B -21.7(4) . . . 2_655 ? O7 V3A O7 V3B 163.4(3) 2_645 . . 2_655 ? O1 V3A O7 V3B 86.6(3) 2_645 . . 2_655 ? O4 V3A O7 V3B -122.0(3) 1_545 . . 2_655 ? O3A V3A O7 V2 82.6(3) . . . . ? O7 V3A O7 V2 -92.33(19) 2_645 . . . ? O1 V3A O7 V2 -169.2(2) 2_645 . . . ? O4 V3A O7 V2 -17.8(2) 1_545 . . . ? O2 V2 O7 V3B 76.0(4) . . . . ? O6 V2 O7 V3B -100.6(4) 3_665 . . . ? O1 V2 O7 V3B -176.3(3) . . . . ? O4 V2 O7 V3B -26.6(3) 1_545 . . . ? O2 V2 O7 V3A -90.7(3) . . . 2_655 ? O6 V2 O7 V3A 92.8(4) 3_665 . . 2_655 ? O1 V2 O7 V3A 17.1(2) . . . 2_655 ? O4 V2 O7 V3A 166.8(3) 1_545 . . 2_655 ? O2 V2 O7 V3A 121.0(3) . . . . ? O6 V2 O7 V3A -55.6(4) 3_665 . . . ? O1 V2 O7 V3A -131.3(3) . . . . ? O4 V2 O7 V3A 18.4(2) 1_545 . . . ? O2 V2 O7 V3B -134.7(3) . . . 2_655 ? O6 V2 O7 V3B 48.8(4) 3_665 . . 2_655 ? O1 V2 O7 V3B -26.9(3) . . . 2_655 ? O4 V2 O7 V3B 122.7(3) 1_545 . . 2_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1A1 O2 0.89 2.31 3.093(10) 146.7 4_566 N1A H1A1 O6 0.89 2.59 3.286(11) 135.7 2_645 N1A H1A2 O2 0.89 2.12 2.994(11) 167.4 2 N1A H1A3 O3A 0.89 1.93 2.818(11) 172.4 2_655 N1B H2B1 O3B 0.89 1.94 2.74(5) 148.8 2_645 N1B H2B2 O2 0.89 2.49 3.16(4) 132.5 1_645 N1B H2B3 O6 0.89 2.41 3.26(5) 159.5 1_545 N1B H2B3 O2 0.89 2.55 3.16(4) 127.1 3_655 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.577 _refine_diff_density_min -1.312 _refine_diff_density_rms 0.138 # REFERENCES: # Data collection & reduction - SMART & SAINT (Bruker, 1999). # Absorption correction - SADABS (Sheldrick, 1996). # Structure solving - SHELXS-90 (Sheldrick, 1990). # Structure refinement - SHELXL-97 (Sheldrick, 1997) and # Geometry - PLATON (Spek, 1990). # Structure drawing - ATOMS (Dowty, 1999). # Ellipsoids plot - ORTEP3 (Farrugia, 1997). _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Dowty, E. (1999). ATOMS for Windows and Macintosh. Version 5. Shape Software, 521 Hidden Valley Road, Kingsport, TN 37663, USA. Farrugia, L. J. (1997). J. Appl. Cryst., 30, 565-565. Spek A. L. (1990) Acta Cryst., A46, C-34. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. ;