#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006939.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2006939 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1998 _journal_volume 54 _journal_page_first 99 _journal_page_last 101 _publ_section_title ; 2,2,6,6-Tetramethyl-4-oxopiperidinium Bis(pentafluorophenyl)phosphinate ; loop_ _publ_author_name 'Charles F. Campana' 'Katherine W. Oliver' 'Steven J. Rettig' 'Robert C. Thompson' 'James Trotter' 'Shihua Xia' _chemical_formula_moiety 'C9 H18 N O +,C12 F10 O2 P -' _chemical_formula_sum 'C21 H18 F10 N O3 P ' _chemical_formula_weight 553.34 _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 11.8450(10) _cell_length_b 14.1490(10) _cell_length_c 14.7660(10) _cell_angle_alpha 90.206(7) _cell_angle_beta 108.131(5) _cell_angle_gamma 91.112(5) _cell_volume 2351.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193.2 _exptl_crystal_density_diffrn 1.563 _diffrn_ambient_temperature 193.2 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_calc_attached_atom _atom_site_refinement_flags _atom_site_occupancy P(1) .04055(4) .15459(3) .36359(3) .03030(10) Uani d ? . 1.000 P(2) .33678(4) .34957(3) .04639(3) .03230(10) Uani d ? . 1.000 F(1) .31884(9) .17741(8) .41518(8) .0502(3) Uani d ? . 1.000 F(2) .44824(9) .33657(9) .44852(8) .0564(4) Uani d ? . 1.000 F(3) .34350(10) .50618(8) .43946(8) .0534(3) Uani d ? . 1.000 F(4) .10340(10) .51488(8) .39038(10) .0627(4) Uani d ? . 1.000 F(5) -.03059(9) .35695(7) .35168(8) .0492(3) Uani d ? . 1.000 F(6) .14924(10) .11959(9) .20781(8) .0566(4) Uani d ? . 1.000 F(7) .05020(10) .11410(10) .01863(9) .0860(5) Uani d ? . 1.000 F(8) -.18310(10) .15380(10) -.06062(9) .0944(6) Uani d ? . 1.000 F(9) -.31700(10) .19897(10) .05299(9) .0713(4) Uani d ? . 1.000 F(10) -.22343(9) .19810(8) .24026(8) .0526(3) Uani d ? . 1.000 F(11) .21958(9) .42510(10) .19429(7) .0603(4) Uani d ? . 1.000 F(12) -.00800(10) .45120(10) .17231(8) .0610(4) Uani d ? . 1.000 F(13) -.17694(9) .40235(10) .00644(8) .0590(4) Uani d ? . 1.000 F(14) -.11300(10) .32980(10) -.13960(9) .0738(4) Uani d ? . 1.000 F(15) .11450(10) .29640(10) -.11817(9) .0673(4) Uani d ? . 1.000 F(16) .37730(10) .24725(8) .23467(8) .0553(4) Uani d ? . 1.000 F(17) .41420(10) .06497(9) .27541(9) .0670(4) Uani d ? . 1.000 F(18) .41690(10) -.06087(9) .13680(10) .0767(5) Uani d ? . 1.000 F(19) .3706(2) -.00212(9) -.04600(10) .0848(5) Uani d ? . 1.000 F(20) .3327(2) .17790(9) -.08883(9) .0790(5) Uani d ? . 1.000 O(1) .11400(10) .06900(8) .38377(9) .0423(3) Uani d ? . 1.000 O(2) -.05030(10) .16987(9) .41149(8) .0410(4) Uani d ? . 1.000 O(3) .40910(10) .40365(9) .13122(9) .0427(4) Uani d ? . 1.000 O(4) .34760(10) .36875(9) -.04901(9) .0401(4) Uani d ? . 1.000 O(5) .3785(2) -.17790(10) .3236(2) .0982(8) Uani d ? . 1.000 O(6) .80910(10) .67860(10) .40486(10) .0736(5) Uani d ? . 1.000 N(1) .15040(10) -.10630(10) .45810(10) .0312(4) Uani d ? . 1.000 N(2) .57260(10) .54482(10) .18597(9) .0245(3) Uani d ? . 1.000 C(1) .13710(10) .25970(10) .38220(10) .0269(4) Uani d ? . 1.000 C(2) .26050(10) .25870(10) .40670(10) .0323(4) Uani d ? . 1.000 C(3) .32950(10) .34070(10) .42500(10) .0359(5) Uani d ? . 1.000 C(4) .2769(2) .42660(10) .42000(10) .0368(5) Uani d ? . 1.000 C(5) .1554(2) .43070(10) .39550(10) .0370(5) Uani d ? . 1.000 C(6) .08890(10) .34880(10) .37690(10) .0318(4) Uani d ? . 1.000 C(7) -.0320(2) .15760(10) .23330(10) .0337(4) Uani d ? . 1.000 C(8) .0324(2) .13680(10) .17220(10) .0426(5) Uani d ? . 1.000 C(9) -.0169(2) .1350(2) .07460(10) .0565(7) Uani d ? . 1.000 C(10) -.1352(2) .1552(2) .03430(10) .0596(7) Uani d ? . 1.000 C(11) -.2015(2) .17740(10) .09180(10) .0514(6) Uani d ? . 1.000 C(12) -.1511(2) .17750(10) .18950(10) .0394(5) Uani d ? . 1.000 C(13) .17910(10) .36160(10) .03800(10) .0320(4) Uani d ? . 1.000 C(14) .1422(2) .39880(10) .11050(10) .0364(5) Uani d ? . 1.000 C(15) .0239(2) .41230(10) .10130(10) .0391(5) Uani d ? . 1.000 C(16) -.0620(2) .38810(10) .01690(10) .0408(5) Uani d ? . 1.000 C(17) -.0297(2) .35130(10) -.05680(10) .0457(6) Uani d ? . 1.000 C(18) .0890(2) .33700(10) -.04460(10) .0416(5) Uani d ? . 1.000 C(19) .35830(10) .22320(10) .07180(10) .0327(4) Uani d ? . 1.000 C(20) .37890(10) .18870(10) .16380(10) .0367(5) Uani d ? . 1.000 C(21) .3971(2) .09510(10) .18620(10) .0447(5) Uani d ? . 1.000 C(22) .3963(2) .03090(10) .1161(2) .0515(6) Uani d ? . 1.000 C(23) .3740(2) .06080(10) .0240(2) .0544(7) Uani d ? . 1.000 C(24) .3550(2) .15490(10) .00340(10) .0485(6) Uani d ? . 1.000 C(25) .1047(2) -.16530(10) .36750(10) .0455(5) Uani d ? . 1.000 C(26) .1780(3) -.1354(2) .3027(2) .0617(8) Uani d ? . 1.000 C(27) .3089(2) -.13460(10) .3526(2) .0628(8) Uani d ? . 1.000 C(28) .3477(2) -.0743(2) .4407(2) .0514(7) Uani d ? . 1.000 C(29) .2825(2) -.09970(10) .51230(10) .0381(5) Uani d ? . 1.000 C(30) .1131(3) -.27100(10) .3875(2) .0595(8) Uani d ? . 1.000 C(31) -.0265(2) -.1405(2) .3241(2) .0590(7) Uani d ? . 1.000 C(32) .3269(2) -.1924(2) .5631(2) .0553(7) Uani d ? . 1.000 C(33) .2957(2) -.0203(2) .5850(2) .0462(6) Uani d ? . 1.000 C(34) .52870(10) .62770(10) .23010(10) .0313(4) Uani d ? . 1.000 C(35) .6349(2) .69570(10) .27200(10) .0426(5) Uani d ? . 1.000 C(36) .7475(2) .6488(2) .32810(10) .0452(5) Uani d ? . 1.000 C(37) .7832(2) .5665(2) .27980(10) .0448(5) Uani d ? . 1.000 C(38) .68300(10) .49260(10) .24250(10) .0347(4) Uani d ? . 1.000 C(39) .4743(2) .5939(2) .3059(2) .0443(6) Uani d ? . 1.000 C(40) .4342(2) .6729(2) .1492(2) .0454(6) Uani d ? . 1.000 C(41) .6628(2) .4349(2) .3230(2) .0492(6) Uani d ? . 1.000 C(42) .7095(2) .4259(2) .1708(2) .0469(6) Uani d ? . 1.000 H(1) .125(2) -.0450(10) .4390(10) .040(5) Uiso d ? . 1.000 H(2) .113(2) -.1280(10) .5010(10) .045(5) Uiso d ? . 1.000 H(3) .514(2) .5030(10) .1670(10) .033(5) Uiso d ? . 1.000 H(4) .5910(10) .5670(10) .1360(10) .026(4) Uiso d ? . 1.000 H(5) .159(2) -.073(2) .281(2) .064(7) Uiso d ? . 1.000 H(6) .158(2) -.173(2) .250(2) .075(8) Uiso d ? . 1.000 H(7) .334(2) -.006(2) .4230(10) .050(5) Uiso d ? . 1.000 H(8) .434(2) -.079(2) .4730(10) .060(6) Uiso d ? . 1.000 H(9) .062(2) -.302(2) .332(2) .084(9) Uiso d ? . 1.000 H(10) .080(2) -.288(2) .445(2) .059(6) Uiso d ? . 1.000 H(11) .197(2) -.290(2) .4030(10) .054(6) Uiso d ? . 1.000 H(12) -.063(2) -.176(2) .262(2) .070(7) Uiso d ? . 1.000 H(13) -.075(2) -.164(2) .366(2) .062(6) Uiso d ? . 1.000 H(14) -.040(2) -.072(2) .317(2) .084(8) Uiso d ? . 1.000 H(15) .402(2) -.180(2) .617(2) .076(8) Uiso d ? . 1.000 H(16) .272(2) -.217(2) .5980(10) .059(6) Uiso d ? . 1.000 H(17) .334(2) -.237(2) .519(2) .059(7) Uiso d ? . 1.000 H(18) .375(2) -.007(2) .6140(10) .054(6) Uiso d ? . 1.000 H(19) .254(2) -.035(2) .633(2) .059(6) Uiso d ? . 1.000 H(20) .264(2) .035(2) .5540(10) .048(6) Uiso d ? . 1.000 H(21) .646(2) .727(2) .218(2) .062(6) Uiso d ? . 1.000 H(22) .613(2) .737(2) .306(2) .054(6) Uiso d ? . 1.000 H(23) .811(2) .5920(10) .2280(10) .043(5) Uiso d ? . 1.000 H(24) .850(2) .5360(10) .3240(10) .046(5) Uiso d ? . 1.000 H(25) .432(2) .641(2) .3160(10) .053(6) Uiso d ? . 1.000 H(26) .416(2) .543(2) .2770(10) .045(5) Uiso d ? . 1.000 H(27) .533(2) .5770(10) .3660(10) .050(6) Uiso d ? . 1.000 H(28) .410(2) .732(2) .1710(10) .055(6) Uiso d ? . 1.000 H(29) .361(2) .626(2) .1230(10) .057(6) Uiso d ? . 1.000 H(30) .464(2) .6900(10) .0980(10) .050(6) Uiso d ? . 1.000 H(31) .731(2) .389(2) .348(2) .073(7) Uiso d ? . 1.000 H(32) .590(2) .398(2) .302(2) .064(7) Uiso d ? . 1.000 H(33) .655(2) .472(2) .372(2) .057(7) Uiso d ? . 1.000 H(34) .783(2) .394(2) .2030(10) .058(6) Uiso d ? . 1.000 H(35) .647(2) .373(2) .1520(10) .056(6) Uiso d ? . 1.000 H(36) .721(2) .466(2) .116(2) .062(6) Uiso d ? . 1.000 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 P(1) .0358(2) .0233(2) .0308(2) -.0010(2) .0088(2) .0061(2) P(2) .0375(2) .0294(2) .0354(2) -.0064(2) .0198(2) -.0008(2) F(1) .0386(6) .0404(6) .0709(8) .0123(5) .0154(5) -.0045(5) F(2) .0330(6) .0717(8) .0659(8) -.0109(5) .0186(5) -.0139(6) F(3) .0667(7) .0450(7) .0509(7) -.0274(6) .0234(6) -.0066(5) F(4) .0722(8) .0226(6) .0880(9) .0058(5) .0172(7) .0026(6) F(5) .0340(6) .0344(6) .0732(8) .0084(5) .0075(5) .0066(5) F(6) .0458(7) .0742(9) .0552(7) -.0052(6) .0238(5) -.0044(6) F(7) .1040(10) .1140(10) .0531(8) -.0220(10) .0446(8) -.0162(8) F(8) .1160(10) .1190(10) .0306(7) -.0200(10) -.0018(7) .0015(8) F(9) .0638(8) .0588(8) .0639(8) .0050(6) -.0203(6) .0081(7) F(10) .0440(6) .0525(7) .0572(7) .0130(5) .0091(5) .0028(6) F(11) .0421(6) .1100(10) .0273(5) .0085(6) .0092(5) -.0139(6) F(12) .0480(6) .0980(10) .0430(6) .0120(6) .0220(5) -.0169(6) F(13) .0359(6) .0817(9) .0594(7) .0018(6) .0151(5) -.0110(7) F(14) .0494(7) .1160(10) .0515(7) -.0246(7) .0110(6) -.0348(8) F(15) .0593(7) .0950(10) .0563(7) -.0265(7) .0326(6) -.0449(7) F(16) .0829(8) .0505(7) .0345(6) .0075(6) .0210(6) .0033(5) F(17) .0809(9) .0624(8) .0535(8) .0159(7) .0137(6) .0265(6) F(18) .0960(10) .0364(7) .1000(10) .0124(7) .0328(9) .0170(7) F(19) .1430(10) .0396(7) .0845(10) -.0008(8) .0537(10) -.0136(7) F(20) .1600(10) .0418(7) .0463(7) -.0052(8) .0477(8) -.0038(6) O(1) .0510(7) .0238(6) .0478(7) .0037(5) .0088(6) .0092(5) O(2) .0425(7) .0441(7) .0403(7) -.0068(6) .0193(6) .0065(6) O(3) .0439(7) .0405(7) .0470(7) -.0152(6) .0197(6) -.0072(6) O(4) .0497(7) .0378(7) .0428(7) -.0008(6) .0287(6) .0058(6) O(5) .145(2) .0610(10) .138(2) .0290(10) .114(2) .0050(10) O(6) .0710(10) .1070(10) .0332(8) -.0374(10) .0052(7) -.0116(8) N(1) .0414(8) .0202(7) .0367(8) .0038(6) .0188(6) .0036(6) N(2) .0249(7) .0271(7) .0234(6) .0001(5) .0103(5) .0014(5) C(1) .0329(8) .0245(8) .0242(7) .0021(6) .0101(6) .0035(6) C(2) .0357(9) .0316(9) .0317(8) .0037(7) .0135(7) .0001(7) C(3) .0319(9) .0460(10) .0327(9) -.0053(8) .0138(7) -.0041(8) C(4) .0500(10) .0328(9) .0301(8) -.0152(8) .0173(8) -.0027(7) C(5) .0510(10) .0218(8) .0376(9) .0021(7) .0126(8) .0029(7) C(6) .0324(9) .0291(9) .0333(8) .0029(7) .0092(7) .0039(7) C(7) .0408(9) .0250(8) .0329(9) -.0054(7) .0082(7) .0015(7) C(8) .0460(10) .0420(10) .0400(10) -.0109(8) .0139(8) .0006(8) C(9) .077(2) .0590(10) .0370(10) -.0180(10) .0240(10) -.0059(10) C(10) .080(2) .0570(10) .0300(10) -.0170(10) .0030(10) .0021(9) C(11) .0560(10) .0380(10) .0450(10) -.0061(9) -.0065(10) .0060(9) C(12) .0460(10) .0260(9) .0409(10) -.0018(8) .0065(8) .0046(7) C(13) .0396(9) .0279(8) .0325(8) -.0050(7) .0174(7) -.0008(7) C(14) .0406(10) .0430(10) .0269(8) .0004(8) .0122(7) -.0001(7) C(15) .0440(10) .0460(10) .0324(9) .0055(8) .0188(8) -.0009(8) C(16) .0346(9) .0460(10) .0430(10) -.0024(8) .0141(8) -.0033(8) C(17) .0440(10) .0560(10) .0360(10) -.0140(9) .0120(8) -.0119(9) C(18) .0490(10) .0450(10) .0366(9) -.0139(9) .0234(8) -.0155(8) C(19) .0334(9) .0334(9) .0354(9) -.0024(7) .0170(7) .0005(7) C(20) .0343(9) .0384(10) .0392(10) .0028(8) .0139(8) .0031(8) C(21) .0410(10) .0480(10) .0460(10) .0062(9) .0143(9) .0144(9) C(22) .0540(10) .0330(10) .0710(10) .0049(9) .0250(10) .0110(10) C(23) .0750(10) .0340(10) .0620(10) -.0020(10) .0340(10) -.0073(10) C(24) .0740(10) .0390(10) .0400(10) -.0051(10) .0291(10) .0021(8) C(25) .0750(10) .0227(8) .0430(10) -.0042(9) .0249(10) -.0056(7) C(26) .118(2) .0320(10) .0500(10) -.0040(10) .0490(10) -.0065(10) C(27) .102(2) .0310(10) .086(2) .0110(10) .072(2) .0080(10) C(28) .0530(10) .0380(10) .077(2) .0092(10) .0410(10) .0100(10) C(29) .0372(9) .0310(9) .0490(10) .0087(7) .0172(8) .0085(8) C(30) .094(2) .0236(10) .068(2) -.0040(10) .036(2) -.0051(10) C(31) .075(2) .0410(10) .0490(10) -.0140(10) .0030(10) -.0070(10) C(32) .0520(10) .0430(10) .074(2) .0190(10) .0230(10) .0210(10) C(33) .0410(10) .0440(10) .0480(10) .0046(9) .0049(9) .0023(9) C(34) .0365(9) .0318(9) .0303(8) .0021(7) .0170(7) -.0042(7) C(35) .0580(10) .0360(10) .0380(10) -.0102(9) .0209(9) -.0085(8) C(36) .0450(10) .0600(10) .0288(9) -.0233(9) .0095(8) .0023(8) C(37) .0278(9) .0590(10) .0410(10) -.0050(9) .0016(8) .0094(10) C(38) .0296(8) .0373(9) .0347(9) .0040(7) .0061(7) .0083(7) C(39) .0540(10) .0460(10) .0430(10) .0010(10) .0300(10) -.0036(9) C(40) .0460(10) .0460(10) .0470(10) .0179(10) .0170(9) .0032(10) C(41) .0530(10) .0510(10) .0420(10) .0040(10) .0122(10) .0170(10) C(42) .0420(10) .0430(10) .0610(10) .0154(9) .0212(10) .0080(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag P(1) O(1) . . 1.4810(10) yes P(1) O(2) . . 1.4790(10) yes P(1) C(1) . . 1.825(2) yes P(1) C(7) . . 1.847(2) yes P(2) O(3) . . 1.4790(10) yes P(2) O(4) . . 1.4790(10) yes P(2) C(13) . . 1.845(2) yes P(2) C(19) . . 1.834(2) yes F(1) C(2) . . 1.340(2) no F(2) C(3) . . 1.342(2) no F(3) C(4) . . 1.340(2) no F(4) C(5) . . 1.344(2) no F(5) C(6) . . 1.354(2) no F(6) C(8) . . 1.347(2) no F(7) C(9) . . 1.348(3) no F(8) C(10) . . 1.338(2) no F(9) C(11) . . 1.350(2) no F(10) C(12) . . 1.337(2) no F(11) C(14) . . 1.336(2) no F(12) C(15) . . 1.340(2) no F(13) C(16) . . 1.340(2) no F(14) C(17) . . 1.340(2) no F(15) C(18) . . 1.345(2) no F(16) C(20) . . 1.337(2) no F(17) C(21) . . 1.341(2) no F(18) C(22) . . 1.344(2) no F(19) C(23) . . 1.353(2) no F(20) C(24) . . 1.346(2) no O(5) C(27) . . 1.214(3) yes O(6) C(36) . . 1.211(2) no N(1) C(25) . . 1.518(2) yes N(1) C(29) . . 1.521(2) yes N(1) H(1) . . .94(2) no N(1) H(2) . . .92(2) no N(2) C(34) . . 1.517(2) no N(2) C(38) . . 1.522(2) no N(2) H(3) . . .88(2) no N(2) H(4) . . .89(2) no C(1) C(2) . . 1.392(2) no C(1) C(6) . . 1.387(2) no C(2) C(3) . . 1.383(2) no C(3) C(4) . . 1.368(3) no C(4) C(5) . . 1.372(3) no C(5) C(6) . . 1.366(2) no C(7) C(8) . . 1.385(3) no C(7) C(12) . . 1.392(2) no C(8) C(9) . . 1.376(3) no C(9) C(10) . . 1.378(3) no C(10) C(11) . . 1.363(3) no C(11) C(12) . . 1.380(3) no C(13) C(14) . . 1.382(2) no C(13) C(18) . . 1.386(2) no C(14) C(15) . . 1.382(2) no C(15) C(16) . . 1.378(3) no C(16) C(17) . . 1.367(3) no C(17) C(18) . . 1.380(3) no C(19) C(20) . . 1.395(2) no C(19) C(24) . . 1.387(3) no C(20) C(21) . . 1.372(3) no C(21) C(22) . . 1.371(3) no C(22) C(23) . . 1.372(3) no C(23) C(24) . . 1.374(3) no C(25) C(26) . . 1.535(3) yes C(25) C(30) . . 1.525(3) yes C(25) C(31) . . 1.533(3) yes C(26) C(27) . . 1.495(4) yes C(26) H(5) . . .95(2) no C(26) H(6) . . .91(3) no C(27) C(28) . . 1.496(3) yes C(28) C(29) . . 1.532(3) yes C(28) H(7) . . 1.00(2) no C(28) H(8) . . .99(2) no C(29) C(32) . . 1.532(3) yes C(29) C(33) . . 1.522(3) yes C(30) H(9) . . .95(3) no C(30) H(10) . . 1.06(2) no C(30) H(11) . . 1.00(2) no C(31) H(12) . . 1.01(2) no C(31) H(13) . . 1.02(2) no C(31) H(14) . . .98(3) no C(32) H(15) . . 1.00(3) no C(32) H(16) . . 1.00(2) no C(32) H(17) . . .93(2) no C(33) H(18) . . .92(2) no C(33) H(19) . . 1.00(2) no C(33) H(20) . . .93(2) no C(34) C(35) . . 1.535(3) no C(34) C(39) . . 1.527(2) no C(34) C(40) . . 1.513(3) no C(35) C(36) . . 1.502(3) no C(35) H(21) . . .96(2) no C(35) H(22) . . .86(2) no C(36) C(37) . . 1.498(3) no C(37) C(38) . . 1.532(3) no C(37) H(23) . . .98(2) no C(37) H(24) . . .96(2) no C(38) C(41) . . 1.521(3) no C(38) C(42) . . 1.523(3) no C(39) H(25) . . .89(2) no C(39) H(26) . . .99(2) no C(39) H(27) . . .97(2) no C(40) H(28) . . .97(2) no C(40) H(29) . . 1.05(2) no C(40) H(30) . . .96(2) no C(41) H(31) . . 1.02(2) no C(41) H(32) . . .97(2) no C(41) H(33) . . .92(2) no C(42) H(34) . . .97(2) no C(42) H(35) . . 1.02(2) no C(42) H(36) . . 1.03(2) no