data_2010537 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first 33 _journal_page_last 34 _publ_section_title ; The cyclic vanadylacetate (C~24~H~20~P)[V~4~O~8~(C~2~H~3~O~2~)~4~(NO~3~)] ; loop_ _publ_author_name 'Wulff-Molder, Dirk' 'Meisel, Manfred' _chemical_name_common Oxovanadiumacetate _chemical_formula_moiety '(PPh4) + , [V4 O8 (Me C O O)4 (N O3)] -' _chemical_formula_sum 'C32 H32 N O19 P V4' _chemical_formula_structural '(PPh4) [V4 O8 (Me C O O)4 (N O3)]' _chemical_formula_iupac '(C24 H20 P) [V4 O8 (C2 H3 O2)4 (N O3)]' _chemical_formula_weight 969.32 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 15.856(2) _cell_length_b 15.856(2) _cell_length_c 29.753(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7480.3(18) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _exptl_crystal_density_diffrn 1.721 _diffrn_ambient_temperature 200(2) _refine_ls_R_factor_obs .042 _refine_ls_wR_factor_obs .100 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol V1 .43804(3) .37781(3) .10358(2) .0271(2) Uani d . 1 . V O11 .39943(13) .45712(13) .07856(7) .0317(5) Uani d . 1 . O O21 .38597(13) .29100(13) .07629(7) .0297(5) Uani d . 1 . O O31 .53999(13) .36437(13) .07606(7) .0302(5) Uani d . 1 . O V2 .63420(3) .31484(3) .09685(2) .0314(2) Uani d . 1 . V O12 .70589(14) .34932(15) .06478(8) .0423(6) Uani d . 1 . O C23 .5777(2) .4455(2) .16236(10) .0290(7) Uani d . 1 . C O13 .63637(13) .40452(13) .14377(7) .0347(5) Uani d . 1 . O O23 .50058(13) .43955(13) .15293(7) .0325(5) Uani d . 1 . O C13 .6027(2) .5050(2) .19885(11) .0421(8) Uani d . 1 . C H13A .6648(15) .5034(2) .2028(2) .063 Uiso calc PR .19(3) . H H13B .5749(7) .4881(4) .2274(7) .063 Uiso calc PR .19(3) . H H13C .5849(5) .5630(14) .1907(2) .063 Uiso calc PR .19(3) . H H13D .5516(12) .5329(7) .2111(3) .063 Uiso calc PR .81(3) . H H13E .6415(10) .5483(11) .1865(3) .063 Uiso calc PR .81(3) . H H13F .6315(7) .4733(8) .2232(6) .063 Uiso calc PR .81(3) . H C24 .6978(2) .1888(2) .16351(10) .0295(7) Uani d . 1 . C O14 .70448(14) .25896(14) .14434(7) .0357(5) Uani d . 1 . O O24 .64552(13) .13147(13) .15352(6) .0309(5) Uani d . 1 . O C14 .7567(2) .1700(2) .20183(11) .0408(8) Uani d . 1 . C H14A .7453(3) .1156(14) .2132(3) .061 Uiso calc PR .19(3) . H H14B .7489(3) .2103(10) .2248(6) .061 Uiso calc PR .19(3) . H H14C .8130(14) .1723(2) .1915(3) .061 Uiso calc PR .19(3) . H H14D .7928(9) .2165(11) .2065(2) .061 Uiso calc PR .81(3) . H H14E .7892(8) .1218(12) .1949(2) .061 Uiso calc PR .81(3) . H H14F .7251(8) .1599(3) .2282(7) .061 Uiso calc PR .81(3) . H N5 .5000 .2500 .1852(2) .0517(12) Uani d S 1 . N O15 .5000 .2500 .14813(13) .0341(7) Uani d S 1 . O O25 .4388(2) .2209(2) .20781(8) .0580(7) Uani d . 1 . O P6 .5000 .7500 .1250 .0236(3) Uani d S 1 . P C16 .4480(2) .8253(2) .08975(9) .0254(6) Uani d . 1 . C C26 .3709(2) .8596(2) .10246(10) .0312(7) Uani d . 1 . C H26 .3434(11) .8404(8) .1286(10) .037 Uiso calc R 1 . H C36 .3350(2) .9222(2) .07653(11) .0391(8) Uani d . 1 . C H36 .289(2) .9433(10) .0840(4) .047 Uiso calc R 1 . H C46 .3753(2) .9496(2) .03808(11) .0385(8) Uani d . 1 . C H46 .3541(11) .9882(19) .0231(7) .046 Uiso calc R 1 . H C56 .4496(2) .9142(2) .02427(10) .0364(7) Uani d . 1 . C H56 .4760(10) .9326(7) -.0037(11) .044 Uiso calc R 1 . H C66 .4871(2) .8522(2) .05013(10) .0309(7) Uani d . 1 . C H66 .537(2) .8287(9) .0413(4) .037 Uiso calc R 1 . H P7 .0000 .2500 .1250 .0240(3) Uani d S 1 . P C17 .0764(2) .3030(2) .09078(9) .0251(6) Uani d . 1 . C C27 .1156(2) .3750(2) .10787(11) .0296(6) Uani d . 1 . C H27 .0997(7) .3959(9) .1332(11) .036 Uiso calc R 1 . H C37 .1800(2) .4126(2) .08392(11) .0362(7) Uani d . 1 . C H37 .2058(11) .4582(19) .0950(5) .043 Uiso calc R 1 . H C47 .2044(2) .3802(2) .04315(11) .0395(8) Uani d . 1 . C H47 .2498(19) .4061(11) .0270(7) .047 Uiso calc R 1 . H C57 .1646(2) .3114(2) .02531(11) .0413(8) Uani d . 1 . C H57 .1802(7) .2915(9) -.0028(12) .050 Uiso calc R 1 . H C67 .1012(2) .2712(2) .04904(10) .0352(7) Uani d . 1 . C H67 .0772(11) .2271(19) .0382(5) .042 Uiso calc R 1 . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V1 .0321(3) .0254(3) .0239(3) .0034(2) .0012(2) .0015(2) O11 .0370(12) .0279(11) .0301(11) .0043(9) .0019(9) .0015(9) O21 .0318(11) .0310(11) .0264(10) .0036(9) -.0015(8) .0007(8) O31 .0348(12) .0278(11) .0281(11) .0007(9) .0019(8) .0007(8) V2 .0286(3) .0298(3) .0357(3) -.0013(2) .0030(2) -.0003(2) O12 .0354(13) .0369(13) .0546(14) -.0007(10) .0129(11) .0041(11) C23 .033(2) .027(2) .0279(15) -.0059(13) -.0017(12) .0032(12) O13 .0287(12) .0302(12) .0452(12) -.0007(9) -.0004(10) -.0043(10) O23 .0320(12) .0364(12) .0291(11) -.0007(9) .0009(9) -.0013(9) C13 .044(2) .044(2) .039(2) -.009(2) -.0026(15) -.008(2) C24 .024(2) .037(2) .0273(15) .0008(13) .0025(12) -.0047(13) O14 .0305(12) .0324(12) .0442(12) -.0017(9) -.0019(10) -.0002(10) O24 .0328(12) .0319(12) .0279(10) -.0035(10) -.0014(9) .0006(9) C14 .038(2) .052(2) .033(2) -.004(2) -.0047(14) -.0017(15) N5 .024(2) .028(2) .103(4) -.002(2) .000 .000 O15 .032(2) .019(2) .051(2) .0069(12) .000 .000 O25 .059(2) .074(2) .0419(14) -.0034(15) -.0019(12) .0014(13) P6 .0251(5) .0251(5) .0207(7) .000 .000 .000 C16 .029(2) .0265(15) .0204(13) -.0017(12) -.0016(11) .0007(11) C26 .029(2) .036(2) .029(2) -.0009(13) -.0001(13) -.0009(13) C36 .032(2) .041(2) .044(2) .0076(15) -.0066(14) -.0007(15) C46 .048(2) .030(2) .037(2) .000(2) -.020(2) .0036(14) C56 .048(2) .035(2) .026(2) -.008(2) -.0068(14) .0054(13) C66 .031(2) .036(2) .0263(15) -.0004(13) -.0003(12) .0027(13) P7 .0247(5) .0247(5) .0228(7) .000 .000 .000 C17 .0249(15) .0263(15) .0239(14) .0005(12) -.0019(11) .0018(11) C27 .032(2) .028(2) .0293(14) .0037(13) -.0012(12) -.0011(12) C37 .033(2) .028(2) .048(2) -.0058(14) .0006(14) .0030(14) C47 .035(2) .038(2) .046(2) -.0014(15) .0102(15) .010(2) C57 .049(2) .044(2) .031(2) .002(2) .0139(15) .0008(14) C67 .042(2) .032(2) .031(2) -.0049(14) .0067(14) -.0046(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag V1 O11 . 1.584(2) yes V1 O21 . 1.799(2) yes V1 O31 . 1.825(2) yes V1 O24 7_554 1.996(2) yes V1 O23 . 2.024(2) yes V1 O15 . 2.613(2) yes O21 V2 7_554 1.815(2) no V2 O12 . 1.582(2) yes V2 O31 . 1.797(2) yes V2 O21 7_554 1.815(2) yes V2 O13 . 1.993(2) yes V2 O14 . 2.006(2) yes V2 O15 . 2.813(2) yes C23 O23 . 1.258(4) no C23 O13 . 1.262(4) no C23 C13 . 1.492(4) no C13 H13A . .99(2) no C13 H13B . .99(2) no C13 H13C . .99(2) no C13 H13D . .99(2) no C13 H13E . .99(2) no C13 H13F . .99(2) no C24 O14 . 1.255(4) no C24 O24 . 1.265(4) no C24 C14 . 1.503(4) no O24 V1 7_554 1.996(2) no C14 H14A . .94(2) no C14 H14B . .94(2) no C14 H14C . .94(2) no C14 H14D . .94(2) no C14 H14E . .94(2) no C14 H14F . .94(2) no N5 O15 . 1.102(6) yes N5 O25 7_554 1.268(4) yes N5 O25 . 1.268(4) yes O15 V1 7_554 2.613(2) no O15 V2 7_554 2.813(2) no P6 C16 14_565 1.791(3) no P6 C16 7_564 1.791(3) no P6 C16 . 1.791(3) no P6 C16 12_766 1.791(3) no C16 C26 . 1.390(4) no C16 C66 . 1.399(4) no C26 C36 . 1.379(5) no C26 H26 . .94(4) no C36 C46 . 1.381(5) no C36 H36 . .83(4) no C46 C56 . 1.367(5) no C46 H46 . .83(4) no C56 C66 . 1.383(4) no C56 H56 . .98(4) no C66 H66 . .92(3) no P7 C17 12_666 1.792(3) no P7 C17 7_454 1.792(3) no P7 C17 . 1.792(3) no P7 C17 14 1.792(3) no C17 C27 . 1.396(4) no C17 C67 . 1.397(4) no C27 C37 . 1.380(4) no C27 H27 . .86(4) no C37 C47 . 1.373(5) no C37 H37 . .89(4) no C47 C57 . 1.368(5) no C47 H47 . .96(4) no C57 C67 . 1.383(5) no C57 H57 . .93(4) no C67 H67 . .86(4) no