data_Feng #============================================================= # 1. SUBMISSION DETAILS _publ_contact_author ; Feng,Shouhua College of Chemistry Jilin University Changchun, 130023 P. R. China ; _publ_contact_author_phone '86-431-5670650' _publ_contact_author_fax '86-431-5671974' _publ_contact_author_email 'shfeng@mail.jlu.edu.cn' _publ_requested_journal 'Inorganic Chemistry' _publ_requested_coeditor_name ? #============================================================ # 2. TITLE AND AUTHOR LIST _publ_section_title ; Hydrothermal Syntheses, Crystal Structures and Magnetic Properties of Inorganic-Organic Hybrid Vanadium Selenites with Zero- to Three- Dimensional Structures: (1,10-phen)2V2SeO7, (2,2¡¯-bipy)VSeO4, (4,4¡¯ -bipy)V2Se2O8 and (4,4¡¯-bipy)2V4Se3O15¡_H2O loop_ _publ_author_name _publ_author_address 'Dai, Zhimin' ; College of Chemistry Jilin University Changchun, 130023 P. R. China ; 'Shi, Zhan' ; College of Chemistry Jilin University Changchun, 130023 P. R. China ; 'Li, Guanghua' ; College of Chemistry Jilin University Changchun, 130023 P. R. China ; 'Zhang, Dong' ; College of Chemistry Jilin University Changchun, 130023 P. R. China ; 'Fu, Wensheng' ; College of Chemistry Jilin University Changchun, 130023 P. R. China ; 'Jin, Haiying' ; College of Chemistry Jilin University Changchun, 130023 P. R. China ; 'Xu, Wei' ; College of Chemistry Jilin University Changchun, 130023 P. R. China ; 'Feng, Shouhua' ; College of Chemistry Jilin University Changchun, 130023 P. R. China #============================================================ data_Compound 1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C24 H16 N4 O7 Se V2' _chemical_formula_sum 'C24 H16 N4 O7 Se V2' _chemical_formula_weight 653.25 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' 'Se' 'Se' -0.0929 2.2259 '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)/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 8.6509(3) _cell_length_b 7.8379(2) _cell_length_c 34.0998(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.503(2) _cell_angle_gamma 90.00 _cell_volume 2311.34(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 2.440 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.2342 _exptl_absorpt_correction_T_max 0.2676 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10750 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 23.24 _reflns_number_total 3306 _reflns_number_gt 2397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^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_number_reflns 3306 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 0.89031(8) 0.51505(8) 0.15238(2) 0.03046(19) Uani 1 1 d . . . V2 V 0.76063(8) 0.81369(9) 0.09998(2) 0.0346(2) Uani 1 1 d . . . Se1 Se 0.59171(5) 0.44542(6) 0.102473(13) 0.03740(15) Uani 1 1 d . . . O1 O 0.7974(3) 0.7963(3) 0.14763(8) 0.0374(7) Uani 1 1 d . . . O2 O 0.9177(3) 0.5562(3) 0.10532(8) 0.0371(7) Uani 1 1 d . . . O3 O 0.6767(3) 0.4518(3) 0.14920(8) 0.0339(7) Uani 1 1 d . . . O4 O 0.9713(3) 0.3337(3) 0.16214(8) 0.0420(8) Uani 1 1 d . . . O5 O 0.5905(3) 0.6614(4) 0.09140(9) 0.0468(8) Uani 1 1 d . . . O6 O 0.6783(3) 0.9950(3) 0.09289(9) 0.0504(8) Uani 1 1 d . . . O7 O 0.4124(3) 0.4061(3) 0.11089(9) 0.0472(8) Uani 1 1 d . . . N1 N 0.8372(4) 0.5769(4) 0.21431(9) 0.0296(8) Uani 1 1 d . . . N2 N 1.0935(4) 0.6439(4) 0.17615(10) 0.0322(8) Uani 1 1 d . . . N3 N 0.9884(4) 0.9097(4) 0.08988(10) 0.0345(9) Uani 1 1 d . . . N4 N 0.8168(4) 0.7443(4) 0.03782(10) 0.0376(9) Uani 1 1 d . . . C1 C 0.7083(5) 0.5443(5) 0.23260(13) 0.0384(11) Uani 1 1 d . . . H1 H 0.6232 0.5064 0.2178 0.080 Uiso 1 1 calc . . . C2 C 0.6927(5) 0.5635(6) 0.27297(14) 0.0473(12) Uani 1 1 d . . . H2 H 0.5996 0.5374 0.2846 0.080 Uiso 1 1 calc . . . C3 C 0.8155(6) 0.6209(5) 0.29522(13) 0.0449(12) Uani 1 1 d . . . H3 H 0.8078 0.6318 0.3223 0.080 Uiso 1 1 calc . . . C4 C 0.9530(5) 0.6632(5) 0.27684(13) 0.0370(11) Uani 1 1 d . . . C5 C 0.9590(5) 0.6384(5) 0.23628(12) 0.0319(10) Uani 1 1 d . . . C6 C 1.0956(4) 0.6743(5) 0.21533(12) 0.0304(10) Uani 1 1 d . . . C7 C 1.2284(5) 0.7382(5) 0.23593(14) 0.0386(11) Uani 1 1 d . . . C8 C 1.3599(5) 0.7659(5) 0.21336(16) 0.0494(13) Uani 1 1 d . . . H8 H 1.4495 0.8087 0.2254 0.080 Uiso 1 1 calc . . . C9 C 1.3582(5) 0.7313(5) 0.17450(16) 0.0494(13) Uani 1 1 d . . . H9 H 1.4463 0.7488 0.1600 0.080 Uiso 1 1 calc . . . C10 C 1.2219(5) 0.6684(5) 0.15618(13) 0.0413(12) Uani 1 1 d . . . H10 H 1.2215 0.6435 0.1295 0.080 Uiso 1 1 calc . . . C11 C 1.0883(6) 0.7318(5) 0.29658(13) 0.0463(13) Uani 1 1 d . . . H11 H 1.0857 0.7536 0.3234 0.080 Uiso 1 1 calc . . . C12 C 1.2174(6) 0.7648(5) 0.27737(15) 0.0502(14) Uani 1 1 d . . . H12 H 1.3032 0.8064 0.2913 0.080 Uiso 1 1 calc . . . C13 C 1.0682(6) 1.0028(5) 0.11638(14) 0.0504(13) Uani 1 1 d . . . H13 H 1.0209 1.0350 0.1394 0.080 Uiso 1 1 calc . . . C14 C 1.2179(7) 1.0520(7) 0.1104(2) 0.0739(18) Uani 1 1 d . . . H14 H 1.2697 1.1181 0.1291 0.080 Uiso 1 1 calc . . . C15 C 1.2916(6) 1.0052(7) 0.0773(2) 0.076(2) Uani 1 1 d . . . H15 H 1.3944 1.0353 0.0739 0.080 Uiso 1 1 calc . . . C16 C 1.2106(6) 0.9105(6) 0.04808(17) 0.0530(14) Uani 1 1 d . . . C17 C 1.0571(5) 0.8683(5) 0.05603(13) 0.0351(11) Uani 1 1 d . . . C18 C 0.9633(5) 0.7810(5) 0.02722(13) 0.0383(11) Uani 1 1 d . . . C19 C 1.0232(7) 0.7402(6) -0.00926(15) 0.0580(15) Uani 1 1 d . . . C20 C 0.9220(10) 0.6582(7) -0.03639(16) 0.080(2) Uani 1 1 d . . . H20 H 0.9556 0.6276 -0.0611 0.080 Uiso 1 1 calc . . . C21 C 0.7749(9) 0.6247(7) -0.02587(18) 0.076(2) Uani 1 1 d . . . H21 H 0.7065 0.5727 -0.0437 0.080 Uiso 1 1 calc . . . C22 C 0.7261(6) 0.6674(6) 0.01115(15) 0.0539(14) Uani 1 1 d . . . H22 H 0.6252 0.6411 0.0177 0.080 Uiso 1 1 calc . . . C23 C 1.2682(7) 0.8649(8) 0.0105(2) 0.084(2) Uani 1 1 d . . . H23 H 1.3701 0.8909 0.0048 0.080 Uiso 1 1 calc . . . C24 C 1.1804(10) 0.7865(8) -0.0164(2) 0.086(2) Uani 1 1 d . . . H24 H 1.2220 0.7608 -0.0406 0.080 Uiso 1 1 calc . . . 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 0.0294(4) 0.0347(4) 0.0271(4) -0.0032(3) -0.0014(3) -0.0012(3) V2 0.0305(4) 0.0412(5) 0.0324(5) 0.0036(3) 0.0042(3) 0.0007(3) Se1 0.0333(3) 0.0501(3) 0.0287(3) -0.0019(2) -0.00153(19) -0.0054(2) O1 0.0412(18) 0.0399(17) 0.0313(19) 0.0015(13) 0.0077(14) 0.0000(14) O2 0.0402(17) 0.0423(17) 0.0286(17) -0.0034(13) 0.0001(13) -0.0050(14) O3 0.0309(16) 0.0401(16) 0.0305(17) 0.0018(13) -0.0030(13) -0.0063(13) O4 0.0408(19) 0.0374(17) 0.047(2) -0.0015(14) -0.0091(15) 0.0003(14) O5 0.0285(17) 0.061(2) 0.051(2) 0.0201(15) -0.0058(15) -0.0076(15) O6 0.0412(19) 0.0498(19) 0.061(2) 0.0146(15) 0.0098(16) 0.0087(15) O7 0.0360(18) 0.060(2) 0.045(2) 0.0051(15) -0.0058(15) -0.0148(15) N1 0.033(2) 0.0287(19) 0.027(2) -0.0002(15) 0.0011(17) -0.0009(16) N2 0.027(2) 0.033(2) 0.037(2) 0.0023(16) -0.0005(17) 0.0005(16) N3 0.040(2) 0.029(2) 0.034(2) 0.0014(16) -0.0014(18) -0.0042(17) N4 0.048(2) 0.036(2) 0.028(2) 0.0010(16) -0.0074(19) -0.0034(18) C1 0.041(3) 0.035(3) 0.040(3) 0.001(2) 0.006(2) -0.004(2) C2 0.056(3) 0.042(3) 0.044(3) -0.003(2) 0.015(3) -0.005(2) C3 0.066(4) 0.039(3) 0.030(3) -0.004(2) 0.008(3) 0.007(3) C4 0.057(3) 0.027(2) 0.027(3) -0.0023(19) -0.008(2) 0.007(2) C5 0.033(3) 0.028(2) 0.034(3) 0.0000(19) -0.006(2) 0.002(2) C6 0.029(3) 0.028(2) 0.033(3) -0.0032(19) -0.006(2) 0.0021(19) C7 0.035(3) 0.031(2) 0.050(3) -0.005(2) -0.011(2) 0.001(2) C8 0.038(3) 0.036(3) 0.073(4) -0.004(3) -0.016(3) -0.002(2) C9 0.031(3) 0.047(3) 0.071(4) -0.001(3) 0.005(3) -0.003(2) C10 0.034(3) 0.040(3) 0.051(3) 0.001(2) 0.004(2) 0.002(2) C11 0.058(3) 0.046(3) 0.034(3) -0.006(2) -0.013(3) 0.009(3) C12 0.054(3) 0.043(3) 0.052(4) -0.018(2) -0.030(3) 0.007(3) C13 0.063(4) 0.043(3) 0.045(3) 0.005(2) -0.013(3) -0.012(3) C14 0.063(4) 0.071(4) 0.086(5) 0.025(4) -0.030(4) -0.036(3) C15 0.033(3) 0.069(4) 0.125(6) 0.051(4) -0.010(4) -0.019(3) C16 0.037(3) 0.038(3) 0.085(4) 0.029(3) 0.018(3) 0.005(2) C17 0.036(3) 0.032(2) 0.038(3) 0.012(2) 0.007(2) 0.004(2) C18 0.055(3) 0.028(2) 0.032(3) 0.006(2) 0.009(2) 0.012(2) C19 0.102(5) 0.039(3) 0.035(4) 0.015(2) 0.024(3) 0.027(3) C20 0.166(7) 0.046(4) 0.029(4) 0.001(3) 0.013(4) 0.042(4) C21 0.136(6) 0.052(4) 0.040(4) 0.000(3) -0.035(4) 0.014(4) C22 0.076(4) 0.050(3) 0.035(3) 0.010(2) -0.021(3) -0.004(3) C23 0.062(4) 0.070(4) 0.123(7) 0.042(4) 0.054(4) 0.020(3) C24 0.127(7) 0.060(4) 0.075(5) 0.032(3) 0.071(5) 0.040(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 V1 O4 1.616(3) . ? V1 O2 1.660(3) . ? V1 O3 1.914(3) . ? V1 N2 2.166(3) . ? V1 N1 2.227(3) . ? V1 O1 2.351(3) . ? V2 O6 1.605(3) . ? V2 O1 1.653(3) . ? V2 O5 1.911(3) . ? V2 N3 2.145(3) . ? V2 N4 2.254(4) . ? V2 O2 2.437(3) . ? Se1 O7 1.614(3) . ? Se1 O5 1.735(3) . ? Se1 O3 1.738(2) . ? N1 C1 1.316(5) . ? N1 C5 1.365(4) . ? N2 C10 1.332(5) . ? N2 C6 1.357(5) . ? N3 C13 1.339(5) . ? N3 C17 1.352(5) . ? N4 C22 1.330(5) . ? N4 C18 1.358(5) . ? C1 C2 1.395(6) . ? C1 H1 0.9300 . ? C2 C3 1.366(6) . ? C2 H2 0.9300 . ? C3 C4 1.399(6) . ? C3 H3 0.9300 . ? C4 C5 1.399(6) . ? C4 C11 1.439(6) . ? C5 C6 1.424(6) . ? C6 C7 1.422(5) . ? C7 C8 1.407(6) . ? C7 C12 1.434(6) . ? C8 C9 1.352(7) . ? C8 H8 0.9300 . ? C9 C10 1.408(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.335(7) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.372(7) . ? C13 H13 0.9300 . ? C14 C15 1.361(8) . ? C14 H14 0.9300 . ? C15 C16 1.412(8) . ? C15 H15 0.9300 . ? C16 C17 1.402(6) . ? C16 C23 1.432(8) . ? C17 C18 1.432(6) . ? C18 C19 1.397(6) . ? C19 C20 1.412(8) . ? C19 C24 1.435(8) . ? C20 C21 1.357(8) . ? C20 H20 0.9300 . ? C21 C22 1.383(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.327(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? 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 O4 V1 O2 107.34(14) . . ? O4 V1 O3 101.34(12) . . ? O2 V1 O3 99.09(12) . . ? O4 V1 N2 89.41(12) . . ? O2 V1 N2 97.81(13) . . ? O3 V1 N2 156.21(13) . . ? O4 V1 N1 95.48(13) . . ? O2 V1 N1 155.91(12) . . ? O3 V1 N1 83.51(12) . . ? N2 V1 N1 74.30(13) . . ? O4 V1 O1 170.07(12) . . ? O2 V1 O1 78.95(11) . . ? O3 V1 O1 84.91(10) . . ? N2 V1 O1 82.01(10) . . ? N1 V1 O1 77.43(10) . . ? O6 V2 O1 107.10(15) . . ? O6 V2 O5 101.12(14) . . ? O1 V2 O5 103.09(13) . . ? O6 V2 N3 94.08(14) . . ? O1 V2 N3 91.87(13) . . ? O5 V2 N3 154.31(14) . . ? O6 V2 N4 100.25(14) . . ? O1 V2 N4 149.76(13) . . ? O5 V2 N4 83.66(13) . . ? N3 V2 N4 73.27(13) . . ? O6 V2 O2 171.41(14) . . ? O1 V2 O2 76.45(11) . . ? O5 V2 O2 85.41(11) . . ? N3 V2 O2 77.86(10) . . ? N4 V2 O2 74.75(10) . . ? O7 Se1 O5 103.00(13) . . ? O7 Se1 O3 103.15(14) . . ? O5 Se1 O3 99.88(12) . . ? V2 O1 V1 101.62(12) . . ? V1 O2 V2 98.03(12) . . ? Se1 O3 V1 116.35(15) . . ? Se1 O5 V2 125.18(14) . . ? C1 N1 C5 117.4(4) . . ? C1 N1 V1 127.3(3) . . ? C5 N1 V1 114.9(3) . . ? C10 N2 C6 119.3(3) . . ? C10 N2 V1 123.7(3) . . ? C6 N2 V1 116.1(3) . . ? C13 N3 C17 118.5(4) . . ? C13 N3 V2 122.8(3) . . ? C17 N3 V2 118.6(3) . . ? C22 N4 C18 116.9(4) . . ? C22 N4 V2 127.9(3) . . ? C18 N4 V2 115.1(3) . . ? N1 C1 C2 123.5(4) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 119.3(4) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.2(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 117.7(4) . . ? C5 C4 C11 117.6(4) . . ? C3 C4 C11 124.7(4) . . ? N1 C5 C4 122.9(4) . . ? N1 C5 C6 115.7(4) . . ? C4 C5 C6 121.4(4) . . ? N2 C6 C7 122.5(4) . . ? N2 C6 C5 118.0(3) . . ? C7 C6 C5 119.4(4) . . ? C8 C7 C6 116.0(4) . . ? C8 C7 C12 126.3(4) . . ? C6 C7 C12 117.7(4) . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.5(5) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 121.5(4) . . ? N2 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C12 C11 C4 121.6(4) . . ? C12 C11 H11 119.2 . . ? C4 C11 H11 119.2 . . ? C11 C12 C7 122.2(4) . . ? C11 C12 H12 118.9 . . ? C7 C12 H12 118.9 . . ? N3 C13 C14 121.6(5) . . ? N3 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C15 C14 C13 120.9(5) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.4(5) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 116.3(5) . . ? C17 C16 C23 117.9(5) . . ? C15 C16 C23 125.7(6) . . ? N3 C17 C16 123.3(4) . . ? N3 C17 C18 116.5(4) . . ? C16 C17 C18 120.2(5) . . ? N4 C18 C19 124.0(5) . . ? N4 C18 C17 115.8(4) . . ? C19 C18 C17 120.2(5) . . ? C18 C19 C20 116.7(6) . . ? C18 C19 C24 117.9(5) . . ? C20 C19 C24 125.3(6) . . ? C21 C20 C19 119.0(5) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 120.4(5) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? N4 C22 C21 123.0(5) . . ? N4 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C24 C23 C16 121.9(6) . . ? C24 C23 H23 119.1 . . ? C16 C23 H23 119.1 . . ? C23 C24 C19 121.9(6) . . ? C23 C24 H24 119.1 . . ? C19 C24 H24 119.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.345 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.066 #================================================END data_Compound 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C10 H8 N2 O4 Se V' _chemical_formula_sum 'C10 H8 N2 O4 Se V' _chemical_formula_weight 350.08 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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.0895(12) _cell_length_b 14.7707(10) _cell_length_c 11.7657(8) _cell_angle_alpha 90.00 _cell_angle_beta 131.354(3) _cell_angle_gamma 90.00 _cell_volume 2229.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description pillar _exptl_crystal_colour blue-black _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 4.162 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6593 _exptl_absorpt_correction_T_max 0.8251 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5114 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 23.21 _reflns_number_total 1590 _reflns_number_gt 1300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^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_number_reflns 1590 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 0.38102(4) 0.21895(4) 0.29285(6) 0.01904(17) Uani 1 1 d . . . Se1 Se 0.36275(3) 0.22795(2) 0.00522(4) 0.01980(13) Uani 1 1 d . . . O1 O 0.36447(18) 0.28659(16) 0.1323(2) 0.0241(6) Uani 1 1 d . . . O2 O 0.4079(2) 0.11794(17) 0.2789(3) 0.0338(7) Uani 1 1 d . . . O3 O 0.27491(18) 0.28659(16) -0.1577(2) 0.0262(6) Uani 1 1 d . . . O4 O 0.47114(18) 0.26495(17) 0.0427(3) 0.0281(6) Uani 1 1 d . . . N1 N 0.3621(2) 0.3499(2) 0.3767(3) 0.0233(8) Uani 1 1 d . . . N2 N 0.3788(2) 0.1833(2) 0.4684(3) 0.0230(7) Uani 1 1 d . . . C1 C 0.3541(3) 0.4324(3) 0.3242(4) 0.0340(10) Uani 1 1 d . . . H1 H 0.3437 0.4372 0.2361 0.080 Uiso 1 1 calc . . . C2 C 0.3605(3) 0.5109(3) 0.3925(5) 0.0431(12) Uani 1 1 d . . . H2 H 0.3541 0.5672 0.3518 0.080 Uiso 1 1 calc . . . C3 C 0.3764(4) 0.5035(3) 0.5225(5) 0.0466(12) Uani 1 1 d . . . H3 H 0.3831 0.5554 0.5731 0.080 Uiso 1 1 calc . . . C4 C 0.3827(3) 0.4189(3) 0.5787(5) 0.0388(11) Uani 1 1 d . . . H4 H 0.3921 0.4132 0.6658 0.080 Uiso 1 1 calc . . . C5 C 0.3745(3) 0.3422(3) 0.5022(4) 0.0256(9) Uani 1 1 d . . . C6 C 0.3773(3) 0.2483(3) 0.5479(4) 0.0244(9) Uani 1 1 d . . . C7 C 0.3747(3) 0.2266(3) 0.6607(4) 0.0352(10) Uani 1 1 d . . . H7 H 0.3734 0.2719 0.7144 0.080 Uiso 1 1 calc . . . C8 C 0.3740(3) 0.1362(4) 0.6912(5) 0.0432(12) Uani 1 1 d . . . H8 H 0.3730 0.1202 0.7667 0.080 Uiso 1 1 calc . . . C9 C 0.3748(3) 0.0702(3) 0.6098(5) 0.0419(12) Uani 1 1 d . . . H9 H 0.3731 0.0093 0.6282 0.080 Uiso 1 1 calc . . . C10 C 0.3782(3) 0.0957(3) 0.5000(4) 0.0318(10) Uani 1 1 d . . . H10 H 0.3802 0.0510 0.4463 0.080 Uiso 1 1 calc . . . 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 0.0165(3) 0.0236(4) 0.0153(3) -0.0007(3) 0.0098(3) -0.0002(3) Se1 0.0183(2) 0.0232(2) 0.0168(2) -0.00009(16) 0.01117(17) -0.00074(17) O1 0.0263(14) 0.0273(15) 0.0211(13) -0.0007(11) 0.0167(12) -0.0008(11) O2 0.0425(17) 0.0272(16) 0.0320(16) -0.0003(12) 0.0248(14) 0.0048(13) O3 0.0174(13) 0.0397(17) 0.0167(13) 0.0016(11) 0.0092(11) -0.0024(11) O4 0.0189(14) 0.0427(16) 0.0221(13) 0.0068(12) 0.0133(11) 0.0023(12) N1 0.0210(17) 0.026(2) 0.0221(17) -0.0019(13) 0.0139(14) -0.0002(13) N2 0.0175(16) 0.0289(19) 0.0160(16) 0.0028(14) 0.0083(13) -0.0006(14) C1 0.038(3) 0.032(3) 0.038(2) -0.002(2) 0.027(2) -0.001(2) C2 0.056(3) 0.030(3) 0.058(3) -0.001(2) 0.043(3) 0.003(2) C3 0.058(3) 0.035(3) 0.056(3) -0.014(2) 0.042(3) -0.002(2) C4 0.041(3) 0.047(3) 0.036(3) -0.006(2) 0.029(2) 0.001(2) C5 0.019(2) 0.037(2) 0.021(2) -0.0047(17) 0.0127(17) -0.0003(17) C6 0.017(2) 0.039(3) 0.0161(19) 0.0014(17) 0.0105(17) 0.0006(17) C7 0.026(2) 0.055(3) 0.024(2) 0.003(2) 0.0159(19) 0.003(2) C8 0.025(2) 0.075(4) 0.028(2) 0.016(2) 0.017(2) 0.001(2) C9 0.038(3) 0.042(3) 0.038(3) 0.015(2) 0.022(2) -0.002(2) C10 0.028(2) 0.031(2) 0.028(2) 0.0058(18) 0.0151(19) -0.0023(18) _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 O2 1.601(3) . ? V1 O1 1.985(2) . ? V1 O3 2.009(2) 7 ? V1 O4 2.032(2) 2_655 ? V1 N2 2.156(3) . ? V1 N1 2.289(3) . ? Se1 O4 1.686(2) . ? Se1 O3 1.696(2) . ? Se1 O1 1.712(2) . ? O3 V1 2.009(2) 7 ? O4 V1 2.032(2) 2_655 ? N1 C1 1.332(5) . ? N1 C5 1.350(5) . ? N2 C10 1.348(5) . ? N2 C6 1.352(5) . ? C1 C2 1.374(5) . ? C1 H1 0.9300 . ? C2 C3 1.369(6) . ? C2 H2 0.9300 . ? C3 C4 1.385(6) . ? C3 H3 0.9300 . ? C4 C5 1.395(5) . ? C4 H4 0.9300 . ? C5 C6 1.477(5) . ? C6 C7 1.395(5) . ? C7 C8 1.385(6) . ? C7 H7 0.9300 . ? C8 C9 1.372(6) . ? C8 H8 0.9300 . ? C9 C10 1.384(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? 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 O2 V1 O1 103.98(12) . . ? O2 V1 O3 101.59(12) . 7 ? O1 V1 O3 89.24(9) . 7 ? O2 V1 O4 98.57(12) . 2_655 ? O1 V1 O4 92.49(10) . 2_655 ? O3 V1 O4 158.71(10) 7 2_655 ? O2 V1 N2 93.36(12) . . ? O1 V1 N2 162.34(11) . . ? O3 V1 N2 83.95(10) 7 . ? O4 V1 N2 88.14(10) 2_655 . ? O2 V1 N1 164.44(12) . . ? O1 V1 N1 90.73(10) . . ? O3 V1 N1 83.36(10) 7 . ? O4 V1 N1 75.41(10) 2_655 . ? N2 V1 N1 72.34(11) . . ? O4 Se1 O3 97.43(12) . . ? O4 Se1 O1 103.03(12) . . ? O3 Se1 O1 102.73(11) . . ? Se1 O1 V1 119.08(13) . . ? Se1 O3 V1 126.48(13) . 7 ? Se1 O4 V1 126.91(14) . 2_655 ? C1 N1 C5 118.6(3) . . ? C1 N1 V1 125.0(3) . . ? C5 N1 V1 115.8(2) . . ? C10 N2 C6 118.9(3) . . ? C10 N2 V1 120.4(3) . . ? C6 N2 V1 120.6(2) . . ? N1 C1 C2 123.8(4) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 117.9(4) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 118.8(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 120.9(4) . . ? N1 C5 C6 114.9(3) . . ? C4 C5 C6 124.1(4) . . ? N2 C6 C7 121.5(4) . . ? N2 C6 C5 115.2(3) . . ? C7 C6 C5 123.3(4) . . ? C8 C7 C6 118.6(4) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C9 C8 C7 119.9(4) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 118.9(4) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 122.1(4) . . ? N2 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.21 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.383 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.067 #================================================END data_Compound 3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C10 H8 N2 O8 Se2 V2' _chemical_formula_sum 'C10 H8 N2 O8 Se2 V2' _chemical_formula_weight 543.98 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' 'Se' 'Se' -0.0929 2.2259 '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 7.1810(10) _cell_length_b 10.8937(13) _cell_length_c 11.1811(15) _cell_angle_alpha 115.455(3) _cell_angle_beta 107.582(3) _cell_angle_gamma 91.957(4) _cell_volume 739.08(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 6.235 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.3106 _exptl_absorpt_correction_T_max 0.7040 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3597 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2064 _reflns_number_gt 1793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.9236P] 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 SHELXL _refine_ls_extinction_coef 0.0187(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2064 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _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 0.24070(10) 0.32680(7) -0.03484(7) 0.0168(2) Uani 1 1 d . . . V2 V 1.76708(10) 0.17772(7) 0.51163(7) 0.0179(2) Uani 1 1 d . . . Se1 Se 0.21322(6) 0.65079(4) 0.15433(4) 0.01802(18) Uani 1 1 d . . . Se2 Se 0.21302(6) 0.15045(4) -0.36626(4) 0.01946(18) Uani 1 1 d . . . O1 O 0.3039(4) 0.5032(3) 0.1316(3) 0.0256(7) Uani 1 1 d . . . O2 O 0.3323(4) 0.2663(3) -0.1943(3) 0.0218(7) Uani 1 1 d . . . O3 O 0.1186(4) 0.2058(3) -0.0295(3) 0.0292(7) Uani 1 1 d . . . O4 O 1.8973(4) 0.2862(3) 0.4944(3) 0.0343(8) Uani 1 1 d . . . O5 O 0.3299(4) 0.7403(3) 0.3325(3) 0.0286(8) Uani 1 1 d . . . O6 O -0.0249(4) 0.6036(3) 0.1356(3) 0.0211(6) Uani 1 1 d . . . O7 O -0.0231(4) 0.1160(3) -0.3737(3) 0.0203(6) Uani 1 1 d . . . O8 O 0.3030(4) 0.0099(3) -0.3596(3) 0.0319(8) Uani 1 1 d . . . N1 N 0.5327(5) 0.3032(4) 0.0706(3) 0.0211(8) Uani 1 1 d . . . N2 N 1.4822(5) 0.1936(4) 0.3898(3) 0.0209(8) Uani 1 1 d . . . C1 C 0.5803(7) 0.1773(5) 0.0190(5) 0.0276(11) Uani 1 1 d . . . H1 H 0.488(7) 0.112(5) -0.061(5) 0.032(13) Uiso 1 1 d . . . C2 C 0.7620(6) 0.1499(5) 0.0779(5) 0.0258(10) Uani 1 1 d . . . H2 H 0.779(6) 0.059(5) 0.034(4) 0.026(12) Uiso 1 1 d . . . C3 C 0.9066(6) 0.2571(4) 0.1960(4) 0.0213(9) Uani 1 1 d . . . C4 C 0.8577(7) 0.3870(5) 0.2474(5) 0.0263(10) Uani 1 1 d . . . H4 H 0.936(7) 0.452(5) 0.322(5) 0.033(14) Uiso 1 1 d . . . C5 C 0.6714(7) 0.4057(5) 0.1834(5) 0.0256(10) Uani 1 1 d . . . H5 H 0.637(8) 0.499(6) 0.214(5) 0.047(15) Uiso 1 1 d . . . C6 C 1.3222(7) 0.0939(5) 0.3257(5) 0.0255(10) Uani 1 1 d . . . H6 H 1.323(7) 0.018(5) 0.331(5) 0.037(15) Uiso 1 1 d . . . C7 C 1.1349(7) 0.1098(5) 0.2619(5) 0.0272(11) Uani 1 1 d . . . H7 H 1.040(7) 0.049(5) 0.236(5) 0.024(13) Uiso 1 1 d . . . C8 C 1.1047(6) 0.2336(4) 0.2614(4) 0.0212(10) Uani 1 1 d . . . C9 C 1.2741(7) 0.3379(5) 0.3246(5) 0.0307(11) Uani 1 1 d . . . H9 H 1.276(7) 0.431(5) 0.324(5) 0.039(13) Uiso 1 1 d . . . C10 C 1.4554(7) 0.3144(5) 0.3865(5) 0.0308(11) Uani 1 1 d . . . H10 H 1.561(7) 0.377(5) 0.427(5) 0.027(13) 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 V1 0.0119(4) 0.0160(4) 0.0190(4) 0.0060(3) 0.0035(3) 0.0054(3) V2 0.0128(4) 0.0172(4) 0.0189(4) 0.0057(3) 0.0027(3) 0.0065(3) Se1 0.0137(3) 0.0191(3) 0.0189(3) 0.00734(19) 0.00448(17) 0.00704(18) Se2 0.0148(3) 0.0227(3) 0.0172(3) 0.0065(2) 0.00416(18) 0.00887(19) O1 0.0210(17) 0.0204(17) 0.0244(15) 0.0043(13) 0.0016(13) 0.0121(13) O2 0.0157(15) 0.0201(16) 0.0201(15) 0.0024(13) 0.0044(12) 0.0022(12) O3 0.0244(17) 0.0275(18) 0.0351(17) 0.0157(15) 0.0076(14) 0.0048(14) O4 0.0233(18) 0.041(2) 0.0415(18) 0.0251(17) 0.0068(15) 0.0045(15) O5 0.0139(16) 0.0335(19) 0.0214(15) -0.0009(14) 0.0036(12) 0.0092(14) O6 0.0108(15) 0.0255(17) 0.0252(15) 0.0107(13) 0.0051(12) 0.0065(13) O7 0.0145(15) 0.0205(16) 0.0238(14) 0.0095(13) 0.0047(12) 0.0068(13) O8 0.0265(18) 0.0209(17) 0.0279(16) 0.0013(14) -0.0032(13) 0.0150(14) N1 0.018(2) 0.020(2) 0.0227(18) 0.0091(16) 0.0047(15) 0.0078(16) N2 0.015(2) 0.020(2) 0.0244(18) 0.0097(16) 0.0036(15) 0.0072(17) C1 0.023(3) 0.021(3) 0.027(2) 0.006(2) 0.001(2) 0.004(2) C2 0.020(3) 0.020(3) 0.031(2) 0.010(2) 0.0024(19) 0.009(2) C3 0.015(2) 0.026(2) 0.026(2) 0.015(2) 0.0062(18) 0.0060(19) C4 0.017(3) 0.023(3) 0.027(2) 0.008(2) -0.002(2) 0.004(2) C5 0.023(3) 0.017(3) 0.032(2) 0.009(2) 0.007(2) 0.009(2) C6 0.020(3) 0.021(3) 0.034(2) 0.016(2) 0.003(2) 0.008(2) C7 0.017(3) 0.021(3) 0.039(3) 0.014(2) 0.005(2) 0.001(2) C8 0.019(2) 0.023(3) 0.021(2) 0.0117(19) 0.0040(18) 0.008(2) C9 0.022(3) 0.022(3) 0.043(3) 0.016(2) 0.003(2) 0.005(2) C10 0.018(3) 0.023(3) 0.039(3) 0.013(2) -0.004(2) -0.002(2) _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 1.591(3) . ? V1 O1 1.928(3) . ? V1 O2 1.942(3) . ? V1 O6 2.002(3) 2_565 ? V1 N1 2.158(3) . ? V2 O4 1.593(3) . ? V2 O8 1.935(3) 2_755 ? V2 O5 1.938(3) 2_766 ? V2 O7 2.002(3) 1_756 ? V2 N2 2.148(3) . ? Se1 O6 1.692(3) . ? Se1 O5 1.699(3) . ? Se1 O1 1.701(3) . ? Se2 O7 1.693(3) . ? Se2 O2 1.694(3) . ? Se2 O8 1.704(3) . ? O5 V2 1.938(3) 2_766 ? O6 V1 2.002(3) 2_565 ? O7 V2 2.002(3) 1_354 ? O8 V2 1.935(3) 2_755 ? N1 C5 1.336(6) . ? N1 C1 1.342(5) . ? N2 C6 1.328(6) . ? N2 C10 1.351(6) . ? C1 C2 1.379(6) . ? C1 H1 0.90(5) . ? C2 C3 1.396(6) . ? C2 H2 0.92(4) . ? C3 C4 1.383(6) . ? C3 C8 1.477(6) . ? C4 C5 1.382(6) . ? C4 H4 0.84(5) . ? C5 H5 0.99(5) . ? C6 C7 1.376(6) . ? C6 H6 0.85(5) . ? C7 C8 1.375(6) . ? C7 H7 0.82(5) . ? C8 C9 1.402(6) . ? C9 C10 1.367(6) . ? C9 H9 1.01(5) . ? C10 H10 0.86(5) . ? 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 O1 114.12(14) . . ? O3 V1 O2 114.48(14) . . ? O1 V1 O2 130.74(13) . . ? O3 V1 O6 102.42(14) . 2_565 ? O1 V1 O6 88.55(11) . 2_565 ? O2 V1 O6 88.69(11) . 2_565 ? O3 V1 N1 96.57(14) . . ? O1 V1 N1 84.35(12) . . ? O2 V1 N1 82.71(12) . . ? O6 V1 N1 161.00(13) 2_565 . ? O4 V2 O8 115.51(16) . 2_755 ? O4 V2 O5 114.42(15) . 2_766 ? O8 V2 O5 129.35(14) 2_755 2_766 ? O4 V2 O7 101.82(14) . 1_756 ? O8 V2 O7 88.03(11) 2_755 1_756 ? O5 V2 O7 89.82(11) 2_766 1_756 ? O4 V2 N2 96.65(15) . . ? O8 V2 N2 82.77(12) 2_755 . ? O5 V2 N2 83.74(12) 2_766 . ? O7 V2 N2 161.48(13) 1_756 . ? O6 Se1 O5 103.46(13) . . ? O6 Se1 O1 102.17(14) . . ? O5 Se1 O1 96.95(13) . . ? O7 Se2 O2 102.87(13) . . ? O7 Se2 O8 101.93(14) . . ? O2 Se2 O8 97.73(13) . . ? Se1 O1 V1 130.28(15) . . ? Se2 O2 V1 130.02(16) . . ? Se1 O5 V2 132.84(16) . 2_766 ? Se1 O6 V1 119.17(15) . 2_565 ? Se2 O7 V2 117.23(14) . 1_354 ? Se2 O8 V2 127.04(16) . 2_755 ? C5 N1 C1 117.3(4) . . ? C5 N1 V1 124.6(3) . . ? C1 N1 V1 118.1(3) . . ? C6 N2 C10 116.6(4) . . ? C6 N2 V2 123.4(3) . . ? C10 N2 V2 119.7(3) . . ? N1 C1 C2 123.2(4) . . ? N1 C1 H1 115(3) . . ? C2 C1 H1 121(3) . . ? C1 C2 C3 119.4(4) . . ? C1 C2 H2 116(3) . . ? C3 C2 H2 125(3) . . ? C4 C3 C2 117.1(4) . . ? C4 C3 C8 121.4(4) . . ? C2 C3 C8 121.5(4) . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120(3) . . ? C3 C4 H4 120(3) . . ? N1 C5 C4 123.0(4) . . ? N1 C5 H5 116(3) . . ? C4 C5 H5 121(3) . . ? N2 C6 C7 123.4(4) . . ? N2 C6 H6 123(3) . . ? C7 C6 H6 113(3) . . ? C8 C7 C6 120.4(5) . . ? C8 C7 H7 121(3) . . ? C6 C7 H7 118(3) . . ? C7 C8 C9 116.5(4) . . ? C7 C8 C3 122.8(4) . . ? C9 C8 C3 120.8(4) . . ? C10 C9 C8 119.7(4) . . ? C10 C9 H9 115(3) . . ? C8 C9 H9 125(3) . . ? N2 C10 C9 123.3(5) . . ? N2 C10 H10 115(3) . . ? C9 C10 H10 122(3) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.424 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.100 #================================================END data_Compound 4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'not measured' _chemical_formula_moiety 'C20 H18 N4 O16 Se3 V4' _chemical_formula_sum 'C20 H18 N4 O16 Se3 V4' _chemical_formula_weight 1011.02 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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 7.9889(9) _cell_length_b 7.8448(9) _cell_length_c 23.048(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.389(4) _cell_angle_gamma 90.00 _cell_volume 1425.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 5.188 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.2451 _exptl_absorpt_correction_T_max 0.3092 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6497 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3848 _reflns_number_gt 3730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material 'SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^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 H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 3848 _refine_ls_number_parameters 424 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0233 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0561 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.003 _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 0.87821(11) -0.21741(11) 0.24917(4) 0.0177(2) Uani 1 1 d . . . V2 V 0.48590(11) -0.25613(11) 0.28290(4) 0.0186(2) Uani 1 1 d . . . V3 V 0.97243(11) -1.32909(12) 0.59829(4) 0.0179(2) Uani 1 1 d . . . V4 V 1.38953(10) -1.25147(11) 0.57743(4) 0.0155(2) Uani 1 1 d . . . Se1 Se 0.57095(6) 0.03556(7) 0.19489(2) 0.01782(13) Uani 1 1 d . . . Se2 Se 1.18898(6) -0.38291(7) 0.17596(2) 0.01716(13) Uani 1 1 d . . . Se3 Se 0.66134(6) -1.49824(7) 0.64522(2) 0.01801(13) Uani 1 1 d . . . O1 O 0.6964(5) -0.1933(5) 0.29560(15) 0.0196(8) Uani 1 1 d . . . O2 O 0.7384(5) -0.0857(5) 0.18436(17) 0.0253(9) Uani 1 1 d . . . O3 O 1.0158(5) -0.2705(5) 0.18694(16) 0.0250(9) Uani 1 1 d . . . O4 O 0.9965(5) -0.0720(5) 0.28169(18) 0.0288(9) Uani 1 1 d . . . O5 O 0.4300(5) -0.1116(5) 0.21417(17) 0.0289(10) Uani 1 1 d . . . O6 O 0.4053(5) -0.1589(5) 0.33235(17) 0.0287(10) Uani 1 1 d . . . O7 O 1.1862(4) -1.3110(5) 0.56425(15) 0.0229(9) Uani 1 1 d . . . O8 O 0.7816(4) -1.3187(5) 0.64427(17) 0.0225(8) Uani 1 1 d . . . O9 O 0.9068(5) -1.4929(5) 0.56013(17) 0.0263(9) Uani 1 1 d . . . O10 O 1.0688(5) -1.0849(5) 0.64942(19) 0.0337(11) Uani 1 1 d . . . O11 O 1.1106(5) -1.4177(5) 0.67082(16) 0.0218(9) Uani 1 1 d . . . O12 O 1.4887(5) -1.3346(5) 0.52908(17) 0.0252(9) Uani 1 1 d . . . O13 O 1.4666(4) -1.3978(5) 0.64346(16) 0.0203(8) Uani 1 1 d . . . O14 O 0.4775(5) 0.0577(5) 0.12433(17) 0.0218(9) Uani 1 1 d . . . O15 O 1.3085(5) -0.4036(5) 0.24396(16) 0.0221(9) Uani 1 1 d . . . O16 O 0.6992(5) -1.5633(5) 0.71509(17) 0.0236(9) Uani 1 1 d . . . N1 N 0.9919(5) -0.4074(6) 0.3097(2) 0.0201(11) Uani 1 1 d . . . N2 N 1.3178(6) -1.0326(6) 0.51858(19) 0.0194(10) Uani 1 1 d . . . N3 N 0.5518(6) -0.4784(6) 0.3366(2) 0.0215(11) Uani 1 1 d . . . N4 N 0.8605(5) -1.1389(6) 0.5360(2) 0.0218(11) Uani 1 1 d . . . C1 C 0.9853(8) -0.5745(8) 0.2979(3) 0.0281(14) Uani 1 1 d . . . H1 H 0.9346 -0.6105 0.2607 0.080 Uiso 1 1 calc . . . C2 C 1.0517(8) -0.6969(8) 0.3392(3) 0.0296(14) Uani 1 1 d . . . H2 H 1.0444 -0.8119 0.3294 0.080 Uiso 1 1 calc . . . C3 C 1.1284(7) -0.6473(7) 0.3949(2) 0.0213(13) Uani 1 1 d . . . C4 C 1.1371(8) -0.4734(7) 0.4065(3) 0.0279(14) Uani 1 1 d . . . H4 H 1.1880 -0.4339 0.4432 0.080 Uiso 1 1 calc . . . C5 C 1.0701(7) -0.3596(7) 0.3634(2) 0.0236(13) Uani 1 1 d . . . H5 H 1.0794 -0.2437 0.3718 0.080 Uiso 1 1 calc . . . C6 C 1.3226(7) -1.0488(7) 0.4614(2) 0.0235(13) Uani 1 1 d . . . H6 H 1.3687 -1.1479 0.4485 0.080 Uiso 1 1 calc . . . C7 C 1.2633(7) -0.9277(7) 0.4207(2) 0.0242(13) Uani 1 1 d . . . H7 H 1.2678 -0.9466 0.3811 0.080 Uiso 1 1 calc . . . C8 C 1.1966(7) -0.7769(8) 0.4380(3) 0.0250(14) Uani 1 1 d . . . C9 C 1.1951(8) -0.7585(8) 0.4982(3) 0.0290(14) Uani 1 1 d . . . H9 H 1.1545 -0.6585 0.5126 0.080 Uiso 1 1 calc . . . C10 C 1.2536(8) -0.8878(8) 0.5359(3) 0.0273(15) Uani 1 1 d . . . H10 H 1.2483 -0.8742 0.5757 0.080 Uiso 1 1 calc . . . C11 C 0.5518(8) -0.6390(8) 0.3174(2) 0.0283(14) Uani 1 1 d . . . H11 H 0.5116 -0.6602 0.2778 0.080 Uiso 1 1 calc . . . C12 C 0.6084(8) -0.7750(7) 0.3532(3) 0.0299(14) Uani 1 1 d . . . H12 H 0.6075 -0.8846 0.3378 0.080 Uiso 1 1 calc . . . C13 C 0.6669(7) -0.7464(7) 0.4128(2) 0.0215(13) Uani 1 1 d . . . C14 C 0.6610(9) -0.5808(8) 0.4329(2) 0.0322(15) Uani 1 1 d . . . H14 H 0.6947 -0.5568 0.4726 0.080 Uiso 1 1 calc . . . C15 C 0.6053(8) -0.4512(8) 0.3942(3) 0.0329(15) Uani 1 1 d . . . H15 H 0.6046 -0.3404 0.4085 0.080 Uiso 1 1 calc . . . C16 C 0.8724(7) -1.1546(8) 0.4775(2) 0.0280(14) Uani 1 1 d . . . H16 H 0.9252 -1.2503 0.4650 0.080 Uiso 1 1 calc . . . C17 C 0.8080(8) -1.0322(7) 0.4368(3) 0.0287(14) Uani 1 1 d . . . H17 H 0.8161 -1.0477 0.3974 0.080 Uiso 1 1 calc . . . C18 C 0.7311(7) -0.8859(7) 0.4542(2) 0.0223(13) Uani 1 1 d . . . C19 C 0.7200(8) -0.8739(8) 0.5139(3) 0.0278(14) Uani 1 1 d . . . H19 H 0.6689 -0.7792 0.5279 0.080 Uiso 1 1 calc . . . C20 C 0.7842(8) -1.0010(8) 0.5521(3) 0.0284(14) Uani 1 1 d . . . H20 H 0.7734 -0.9897 0.5915 0.080 Uiso 1 1 calc . . . 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 0.0181(5) 0.0164(5) 0.0184(5) 0.0023(4) 0.0021(4) 0.0018(4) V2 0.0210(5) 0.0167(5) 0.0172(5) 0.0015(4) 0.0004(4) -0.0015(4) V3 0.0170(5) 0.0174(5) 0.0188(5) 0.0029(4) 0.0011(4) -0.0012(4) V4 0.0166(5) 0.0143(5) 0.0150(5) 0.0003(4) 0.0007(4) -0.0003(4) Se1 0.0198(3) 0.0170(3) 0.0158(3) 0.0005(2) 0.0006(2) 0.0016(2) Se2 0.0165(3) 0.0179(3) 0.0168(3) -0.0004(2) 0.0022(2) 0.0002(2) Se3 0.0185(3) 0.0169(3) 0.0179(3) 0.0000(2) 0.0009(2) 0.0003(2) O1 0.024(2) 0.017(2) 0.018(2) -0.0007(16) 0.0025(16) 0.0004(17) O2 0.029(2) 0.024(2) 0.023(2) 0.0054(18) 0.0074(19) 0.0086(18) O3 0.021(2) 0.032(2) 0.023(2) -0.0010(18) 0.0034(17) 0.0046(17) O4 0.032(2) 0.019(2) 0.034(2) -0.0005(19) -0.0002(19) -0.0037(18) O5 0.022(2) 0.035(3) 0.027(2) 0.011(2) -0.0009(18) -0.0054(19) O6 0.030(2) 0.025(2) 0.032(2) -0.0033(19) 0.0080(19) 0.0009(18) O7 0.020(2) 0.027(2) 0.021(2) 0.0060(18) -0.0011(17) -0.0005(17) O8 0.0146(18) 0.022(2) 0.032(2) 0.0000(17) 0.0069(16) -0.0035(16) O9 0.026(2) 0.025(2) 0.028(2) -0.0018(17) 0.0048(19) -0.0051(17) O10 0.036(3) 0.024(2) 0.041(3) -0.005(2) 0.008(2) -0.0020(19) O11 0.024(2) 0.021(2) 0.019(2) 0.0011(17) -0.0004(17) 0.0016(17) O12 0.029(2) 0.024(2) 0.024(2) 0.0001(18) 0.0100(18) 0.0036(18) O13 0.0172(18) 0.022(2) 0.022(2) 0.0081(17) 0.0020(16) 0.0024(16) O14 0.027(2) 0.0154(19) 0.021(2) 0.0012(17) -0.0024(17) 0.0000(17) O15 0.021(2) 0.022(2) 0.021(2) 0.0021(17) -0.0021(17) -0.0008(17) O16 0.025(2) 0.019(2) 0.025(2) 0.0012(17) -0.0012(18) 0.0063(17) N1 0.017(2) 0.016(2) 0.027(3) 0.001(2) 0.001(2) 0.0012(19) N2 0.022(2) 0.020(2) 0.015(2) -0.004(2) -0.0003(19) 0.000(2) N3 0.028(3) 0.019(3) 0.017(3) 0.000(2) 0.001(2) -0.002(2) N4 0.018(2) 0.019(3) 0.029(3) 0.004(2) 0.002(2) -0.002(2) C1 0.031(3) 0.024(3) 0.026(3) 0.001(3) -0.003(3) 0.002(3) C2 0.040(4) 0.020(3) 0.027(3) -0.001(3) 0.000(3) 0.004(3) C3 0.023(3) 0.024(3) 0.016(3) 0.006(3) 0.001(3) 0.004(3) C4 0.030(3) 0.025(3) 0.026(3) -0.002(3) -0.004(3) 0.003(3) C5 0.030(3) 0.017(3) 0.022(3) -0.001(2) 0.000(3) 0.002(3) C6 0.026(3) 0.022(3) 0.021(3) 0.002(3) 0.000(3) 0.004(3) C7 0.031(3) 0.021(3) 0.022(3) -0.001(3) 0.009(3) 0.006(3) C8 0.022(3) 0.024(3) 0.028(3) 0.001(3) -0.003(3) -0.001(3) C9 0.045(4) 0.023(3) 0.017(3) -0.002(3) 0.001(3) 0.013(3) C10 0.038(4) 0.026(4) 0.019(3) -0.005(3) 0.007(3) 0.005(3) C11 0.046(4) 0.026(3) 0.012(3) 0.000(3) 0.004(3) -0.002(3) C12 0.043(4) 0.022(3) 0.023(3) -0.002(3) 0.002(3) 0.000(3) C13 0.022(3) 0.020(3) 0.024(3) 0.000(3) 0.007(3) 0.001(2) C14 0.049(4) 0.029(4) 0.014(3) 0.002(3) -0.008(3) 0.005(3) C15 0.049(4) 0.020(3) 0.025(4) 0.000(3) -0.008(3) 0.004(3) C16 0.030(3) 0.030(4) 0.023(3) 0.000(3) 0.002(3) 0.006(3) C17 0.037(4) 0.028(3) 0.019(3) 0.003(3) -0.003(3) 0.006(3) C18 0.025(3) 0.021(3) 0.019(3) 0.000(3) -0.003(2) 0.001(3) C19 0.026(3) 0.027(3) 0.032(4) 0.002(3) 0.009(3) 0.010(3) C20 0.030(3) 0.032(4) 0.024(3) 0.006(3) 0.006(3) 0.006(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 O4 1.589(4) . ? V1 O1 1.949(4) . ? V1 O3 1.988(4) . ? V1 O2 2.000(4) . ? V1 N1 2.140(5) . ? V1 O16 2.293(4) 2_534 ? V2 O6 1.592(4) . ? V2 O1 1.731(4) . ? V2 O15 1.933(4) 1_455 ? V2 O5 1.940(4) . ? V2 N3 2.154(5) . ? V3 O9 1.597(4) . ? V3 O11 1.973(4) . ? V3 O8 1.995(4) . ? V3 O7 1.998(4) . ? V3 N4 2.161(5) . ? V3 O10 2.314(4) . ? V4 O12 1.607(4) . ? V4 O7 1.669(4) . ? V4 O13 1.925(4) . ? V4 O14 1.930(4) 2_645 ? V4 N2 2.205(5) . ? Se1 O14 1.684(4) . ? Se1 O2 1.691(4) . ? Se1 O5 1.721(4) . ? Se2 O11 1.682(4) 2_534 ? Se2 O3 1.694(4) . ? Se2 O15 1.705(4) . ? Se3 O16 1.669(4) . ? Se3 O8 1.707(4) . ? Se3 O13 1.738(4) 1_455 ? O11 Se2 1.682(4) 2_535 ? O13 Se3 1.738(4) 1_655 ? O14 V4 1.930(4) 2_444 ? O15 V2 1.933(4) 1_655 ? O16 V1 2.293(4) 2_535 ? N1 C1 1.338(7) . ? N1 C5 1.346(7) . ? N2 C6 1.331(7) . ? N2 C10 1.334(7) . ? N3 C11 1.336(7) . ? N3 C15 1.343(7) . ? N4 C20 1.324(7) . ? N4 C16 1.371(7) . ? C1 C2 1.395(9) . ? C1 H1 0.9300 . ? C2 C3 1.385(8) . ? C2 H2 0.9300 . ? C3 C4 1.390(8) . ? C3 C8 1.462(8) . ? C4 C5 1.377(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.364(8) . ? C6 H6 0.9300 . ? C7 C8 1.383(8) . ? C7 H7 0.9300 . ? C8 C9 1.397(8) . ? C9 C10 1.368(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.379(8) . ? C11 H11 0.9300 . ? C12 C13 1.395(8) . ? C12 H12 0.9300 . ? C13 C14 1.383(8) . ? C13 C18 1.488(8) . ? C14 C15 1.377(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.382(8) . ? C16 H16 0.9300 . ? C17 C18 1.391(8) . ? C17 H17 0.9300 . ? C18 C19 1.396(8) . ? C19 C20 1.374(8) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? 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 O4 V1 O1 96.34(18) . . ? O4 V1 O3 97.72(19) . . ? O1 V1 O3 164.96(16) . . ? O4 V1 O2 101.44(19) . . ? O1 V1 O2 89.11(15) . . ? O3 V1 O2 82.91(15) . . ? O4 V1 N1 92.06(19) . . ? O1 V1 N1 89.14(16) . . ? O3 V1 N1 95.65(16) . . ? O2 V1 N1 166.50(17) . . ? O4 V1 O16 171.93(18) . 2_534 ? O1 V1 O16 77.39(14) . 2_534 ? O3 V1 O16 89.04(15) . 2_534 ? O2 V1 O16 83.71(16) . 2_534 ? N1 V1 O16 82.85(16) . 2_534 ? O6 V2 O1 103.77(19) . . ? O6 V2 O15 105.50(19) . 1_455 ? O1 V2 O15 150.16(17) . 1_455 ? O6 V2 O5 103.8(2) . . ? O1 V2 O5 93.41(16) . . ? O15 V2 O5 85.23(16) 1_455 . ? O6 V2 N3 93.76(19) . . ? O1 V2 N3 89.63(17) . . ? O15 V2 N3 82.80(17) 1_455 . ? O5 V2 N3 160.88(18) . . ? O9 V3 O11 105.74(19) . . ? O9 V3 O8 96.59(17) . . ? O11 V3 O8 86.27(15) . . ? O9 V3 O7 93.77(18) . . ? O11 V3 O7 87.80(15) . . ? O8 V3 O7 169.14(16) . . ? O9 V3 N4 97.27(19) . . ? O11 V3 N4 156.90(17) . . ? O8 V3 N4 93.17(16) . . ? O7 V3 N4 88.72(16) . . ? O9 V3 O10 177.23(18) . . ? O11 V3 O10 76.50(15) . . ? O8 V3 O10 85.14(16) . . ? O7 V3 O10 84.63(15) . . ? N4 V3 O10 80.45(17) . . ? O12 V4 O7 109.6(2) . . ? O12 V4 O13 100.14(18) . . ? O7 V4 O13 98.82(17) . . ? O12 V4 O14 122.16(19) . 2_645 ? O7 V4 O14 125.22(18) . 2_645 ? O13 V4 O14 89.23(16) . 2_645 ? O12 V4 N2 89.84(18) . . ? O7 V4 N2 87.61(18) . . ? O13 V4 N2 165.44(16) . . ? O14 V4 N2 76.44(16) 2_645 . ? O14 Se1 O2 98.97(19) . . ? O14 Se1 O5 96.48(18) . . ? O2 Se1 O5 103.05(18) . . ? O11 Se2 O3 101.02(18) 2_534 . ? O11 Se2 O15 97.04(18) 2_534 . ? O3 Se2 O15 105.11(17) . . ? O16 Se3 O8 104.54(19) . . ? O16 Se3 O13 100.47(17) . 1_455 ? O8 Se3 O13 97.39(18) . 1_455 ? V2 O1 V1 132.1(2) . . ? Se1 O2 V1 122.8(2) . . ? Se2 O3 V1 141.1(2) . . ? Se1 O5 V2 122.0(2) . . ? V4 O7 V3 144.8(2) . . ? Se3 O8 V3 117.0(2) . . ? Se2 O11 V3 122.5(2) 2_535 . ? Se3 O13 V4 117.29(19) 1_655 . ? Se1 O14 V4 133.3(2) . 2_444 ? Se2 O15 V2 128.9(2) . 1_655 ? Se3 O16 V1 124.4(2) . 2_535 ? C1 N1 C5 117.2(5) . . ? C1 N1 V1 123.5(4) . . ? C5 N1 V1 119.3(4) . . ? C6 N2 C10 116.9(5) . . ? C6 N2 V4 119.2(4) . . ? C10 N2 V4 123.5(4) . . ? C11 N3 C15 117.5(5) . . ? C11 N3 V2 125.8(4) . . ? C15 N3 V2 116.6(4) . . ? C20 N4 C16 117.3(5) . . ? C20 N4 V3 122.4(4) . . ? C16 N4 V3 120.2(4) . . ? N1 C1 C2 122.5(5) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 120.1(6) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 117.0(5) . . ? C2 C3 C8 119.6(5) . . ? C4 C3 C8 123.4(5) . . ? C5 C4 C3 119.8(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 123.4(5) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? N2 C6 C7 123.5(5) . . ? N2 C6 H6 118.3 . . ? C7 C6 H6 118.3 . . ? C6 C7 C8 120.3(5) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 116.2(5) . . ? C7 C8 C3 121.1(5) . . ? C9 C8 C3 122.7(5) . . ? C10 C9 C8 119.8(5) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C9 123.3(5) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N3 C11 C12 123.2(5) . . ? N3 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C13 119.3(6) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 117.2(5) . . ? C14 C13 C18 120.2(5) . . ? C12 C13 C18 122.6(5) . . ? C15 C14 C13 120.1(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? N3 C15 C14 122.6(6) . . ? N3 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? N4 C16 C17 121.8(5) . . ? N4 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C18 120.7(5) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 116.2(5) . . ? C17 C18 C13 122.9(5) . . ? C19 C18 C13 120.8(5) . . ? C20 C19 C18 120.4(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? N4 C20 C19 123.6(5) . . ? N4 C20 H20 118.2 . . ? C19 C20 H20 118.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.784 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.068 #===END