#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200790.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_2200790 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first m451 _journal_page_last m453 _publ_section_title ; Square [Pd~4~(\m-CN)~4~(C~6~F~5~)~4~(PEt~3~)~4~].2C~6~H~5~CH~3~ ; loop_ _publ_author_name 'Jonathan P. H. Charmant' 'Pablo Espinet' 'Katerina Soulantica' _chemical_formula_moiety 'C52 H60 F20 N4 P4 Pd4, 2C7 H8' _chemical_formula_sum 'C66 H76 F20 N4 P4 Pd4' _chemical_formula_iupac '[Pd4 (C N)4 (C6 F5)4 (C6 H15 P)4], 2C7 H8' _chemical_formula_weight 1854.79 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8845(10) _cell_length_b 14.8554(18) _cell_length_c 21.652(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.372(9) _cell_angle_gamma 90.00 _cell_volume 3791.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _exptl_crystal_density_diffrn 1.625 _diffrn_ambient_temperature 173(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_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Pd1 .549498(14) -.223794(11) .065058(8) .02383(5) Uani d . 1 . . Pd Pd2 .246938(14) .025756(11) .083650(8) .02292(5) Uani d . 1 . . Pd C1A .42579(17) -.12888(14) .06457(10) .0278(5) Uani d P .50 A 1 C C2A .30701(18) .09898(14) .01589(10) .0301(5) Uani d P .50 . 1 C N1A .35909(18) -.07465(14) .07015(10) .0285(5) Uani d P .50 A 1 N N2A .64715(16) -.14097(13) .01756(10) .0237(4) Uani d P .50 . 1 N N1B .42579(17) -.12888(14) .06457(10) .0278(5) Uani d P .50 A 2 N N2B .30701(18) .09898(14) .01589(10) .0301(5) Uani d P .50 . 2 N C1B .35909(18) -.07465(14) .07015(10) .0285(5) Uani d P .50 A 2 C C2B .64715(16) -.14097(13) .01756(10) .0237(4) Uani d P .50 . 2 C P1 .43375(6) -.31907(4) .10737(3) .03429(15) Uani d . 1 A . P P2 .11997(5) .13484(4) .10126(3) .02513(13) Uani d . 1 . . P C10 .67556(19) -.31656(15) .07088(11) .0270(5) Uani d . 1 A . C C11 .7011(2) -.36491(16) .02030(12) .0339(6) Uani d . 1 . . C F11 .63377(14) -.35788(11) -.03497(7) .0503(4) Uani d . 1 A . F C12 .7944(2) -.42179(17) .02241(15) .0437(7) Uani d . 1 A . C F12 .81750(15) -.46538(11) -.02906(9) .0643(5) Uani d . 1 . . F C13 .8634(2) -.43295(17) .07789(17) .0479(8) Uani d . 1 . . C F13 .95275(15) -.48974(12) .08120(11) .0752(6) Uani d . 1 A . F C14 .8396(2) -.38786(17) .12962(14) .0416(7) Uani d . 1 A . C F14 .90451(13) -.40133(11) .18475(9) .0600(5) Uani d . 1 . . F C15 .7478(2) -.33019(16) .12516(12) .0327(5) Uani d . 1 . . C F15 .72855(13) -.28742(10) .17839(7) .0439(4) Uani d . 1 A . F C20 .19911(19) -.04493(15) .15670(11) .0265(5) Uani d . 1 . . C C21 .2478(2) -.03018(15) .21721(12) .0325(5) Uani d . 1 . . C F21 .32964(14) .03387(10) .22920(7) .0500(4) Uani d . 1 . . F C22 .2184(2) -.07704(18) .26800(12) .0410(6) Uani d . 1 . . C F22 .27015(18) -.05946(12) .32598(7) .0659(5) Uani d . 1 . . F C23 .1357(2) -.14152(18) .25910(14) .0438(7) Uani d . 1 . . C F23 .10380(17) -.18584(12) .30849(9) .0682(6) Uani d . 1 . . F C24 .0861(2) -.16043(17) .19995(14) .0413(7) Uani d . 1 . . C F24 .00538(15) -.22464(11) .19080(10) .0670(5) Uani d . 1 . . F C25 .1193(2) -.11361(16) .15038(12) .0335(5) Uani d . 1 . . C F25 .06995(14) -.13713(11) .09261(8) .0559(5) Uani d . 1 . . F C30 .3051(2) -.33575(19) .04913(15) .0483(7) Uani d . 1 . . C H30A .2551 -.3809 .0654 .058 Uiso calc R 1 A . H H30B .2626 -.2784 .0437 .058 Uiso calc R 1 . . H C31 .3336(3) -.3668(3) -.01369(16) .0711(10) Uani d . 1 A . C H31A .3788 -.3205 -.0313 .107 Uiso calc R 1 . . H H31B .2633 -.3770 -.0418 .107 Uiso calc R 1 . . H H31C .3771 -.4230 -.0086 .107 Uiso calc R 1 . . H C40 .4880(2) -.43085(17) .12880(13) .0400(6) Uani d . 1 . . C H40A .5069 -.4610 .0906 .048 Uiso calc R 1 A . H H40B .5597 -.4238 .1572 .048 Uiso calc R 1 . . H C41 .4104(3) -.49317(19) .16005(14) .0493(7) Uani d . 1 A . C H41A .3971 -.4676 .2002 .074 Uiso calc R 1 . . H H41B .4464 -.5523 .1668 .074 Uiso calc R 1 . . H H41C .3379 -.4996 .1333 .074 Uiso calc R 1 . . H C50 .3752(2) -.27189(19) .17340(13) .0439(7) Uani d . 1 . . C H50A .3308 -.2174 .1598 .053 Uiso calc R 1 A . H H50B .3228 -.3161 .1885 .053 Uiso calc R 1 . . H C51 .4655(3) -.2471(3) .22655(15) .0681(10) Uani d . 1 A . C H51A .5133 -.2996 .2383 .102 Uiso calc R 1 . . H H51B .4291 -.2273 .2624 .102 Uiso calc R 1 . . H H51C .5124 -.1982 .2134 .102 Uiso calc R 1 . . H C60 .1715(2) .20602(17) .16768(12) .0367(6) Uani d . 1 . . C H60A .1131 .2519 .1732 .044 Uiso calc R 1 . . H H60B .1821 .1685 .2057 .044 Uiso calc R 1 . . H C61 .2820(2) .2532(2) .16072(14) .0523(8) Uani d . 1 . . C H61A .3391 .2086 .1528 .078 Uiso calc R 1 . . H H61B .3082 .2862 .1991 .078 Uiso calc R 1 . . H H61C .2701 .2955 .1257 .078 Uiso calc R 1 . . H C70 -.01827(19) .09583(17) .11888(12) .0334(6) Uani d . 1 . . C H70A -.0064 .0541 .1548 .040 Uiso calc R 1 . . H H70B -.0616 .1482 .1314 .040 Uiso calc R 1 . . H C71 -.0887(2) .0482(2) .06484(14) .0458(7) Uani d . 1 . . C H71A -.1108 .0914 .0313 .069 Uiso calc R 1 . . H H71B -.1569 .0226 .0791 .069 Uiso calc R 1 . . H H71C -.0437 -.0002 .0494 .069 Uiso calc R 1 . . H C80 .0884(2) .21135(16) .03553(11) .0304(5) Uani d . 1 . . C H80A .1598 .2414 .0280 .036 Uiso calc R 1 . . H H80B .0617 .1753 -.0020 .036 Uiso calc R 1 . . H C81 .0001(2) .28380(19) .04288(15) .0484(7) Uani d . 1 . . C H81A -.0718 .2552 .0494 .073 Uiso calc R 1 . . H H81B -.0114 .3209 .0052 .073 Uiso calc R 1 . . H H81C .0266 .3218 .0788 .073 Uiso calc R 1 . . H C90 .4079(3) -.4081(3) .38117(18) .0876(13) Uani d . 1 . . C H90A .4827 -.4230 .3695 .131 Uiso calc R 1 . . H H90B .3997 -.4356 .4215 .131 Uiso calc R 1 . . H H90C .4005 -.3426 .3842 .131 Uiso calc R 1 . . H C91 .3177(3) -.4434(2) .33287(14) .0549(8) Uani d . 1 . . C C92 .2981(3) -.5363(2) .32470(16) .0613(9) Uani d . 1 . . C H92 .3435 -.5781 .3501 .074 Uiso calc R 1 . . H C93 .2134(3) -.5675(2) .27999(17) .0627(9) Uani d . 1 . . C H93 .2006 -.6304 .2754 .075 Uiso calc R 1 . . H C94 .1490(3) -.5096(3) .24281(17) .0616(9) Uani d . 1 . . C H94 .0912 -.5316 .2121 .074 Uiso calc R 1 . . H C95 .1669(2) -.4188(2) .24934(16) .0564(9) Uani d . 1 . . C H95 .1221 -.3782 .2227 .068 Uiso calc R 1 . . H C96 .2488(2) -.3858(2) .29394(14) .0458(7) Uani d . 1 . . C H96 .2587 -.3226 .2983 .055 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 Pd1 .02402(9) .02250(9) .02620(10) .00150(7) .00799(7) .00186(7) Pd2 .02295(9) .02252(9) .02429(9) .00100(7) .00689(7) .00197(7) C1A .0278(11) .0279(11) .0294(12) .0017(9) .0100(9) .0047(9) C2A .0283(11) .0280(11) .0346(13) .0062(9) .0066(10) -.0009(9) N1A .0290(11) .0279(11) .0300(12) .0000(9) .0087(9) .0046(9) N2A .0238(10) .0212(10) .0278(11) .0031(8) .0095(9) .0033(8) N1B .0278(11) .0279(11) .0294(12) .0017(9) .0100(9) .0047(9) N2B .0283(11) .0280(11) .0346(13) .0062(9) .0066(10) -.0009(9) C1B .0290(11) .0279(11) .0300(12) .0000(9) .0087(9) .0046(9) C2B .0238(10) .0212(10) .0278(11) .0031(8) .0095(9) .0033(8) P1 .0366(4) .0275(3) .0418(4) -.0042(3) .0166(3) .0006(3) P2 .0246(3) .0265(3) .0250(3) .0023(2) .0061(2) -.0008(2) C10 .0253(11) .0222(11) .0351(14) .0018(9) .0103(10) .0034(10) C11 .0341(13) .0290(12) .0404(15) -.0015(11) .0120(11) .0008(11) F11 .0627(11) .0529(10) .0370(9) .0052(8) .0127(8) -.0090(8) C12 .0445(16) .0264(13) .066(2) -.0002(12) .0304(15) -.0070(13) F12 .0674(12) .0477(10) .0863(14) .0028(9) .0421(11) -.0236(9) C13 .0290(14) .0266(13) .090(3) .0077(11) .0159(15) .0056(15) F13 .0442(10) .0461(10) .137(2) .0238(8) .0192(11) .0014(11) C14 .0303(13) .0305(13) .062(2) .0022(11) -.0009(13) .0094(13) F14 .0413(9) .0504(10) .0821(14) .0071(8) -.0166(9) .0142(9) C15 .0308(13) .0259(12) .0423(15) .0007(10) .0084(11) .0021(11) F15 .0476(9) .0447(9) .0375(9) .0047(7) -.0012(7) .0000(7) C20 .0255(11) .0261(11) .0289(13) .0026(9) .0081(10) .0032(9) C21 .0397(14) .0268(12) .0309(13) .0006(11) .0046(11) .0019(10) F21 .0630(10) .0422(9) .0400(9) -.0174(8) -.0122(8) .0039(7) C22 .0627(18) .0351(14) .0265(14) .0111(14) .0103(12) .0041(11) F22 .1157(16) .0535(11) .0264(9) .0065(11) .0016(9) .0049(8) C23 .0562(17) .0358(14) .0450(17) .0119(13) .0282(14) .0183(12) F23 .0927(14) .0564(11) .0648(12) .0111(10) .0455(11) .0326(9) C24 .0339(14) .0294(13) .063(2) -.0027(11) .0155(13) .0124(13) F24 .0523(10) .0486(10) .1005(16) -.0206(9) .0109(10) .0240(10) C25 .0316(13) .0307(13) .0378(15) -.0011(11) .0032(11) .0020(11) F25 .0646(11) .0455(9) .0519(11) -.0229(8) -.0149(8) .0033(8) C30 .0361(15) .0385(15) .070(2) -.0060(12) .0064(14) .0045(14) C31 .074(2) .083(3) .052(2) -.025(2) -.0048(18) -.0018(19) C40 .0383(14) .0344(14) .0486(17) -.0001(12) .0102(12) .0152(12) C41 .0579(19) .0395(15) .0518(19) -.0122(14) .0124(15) .0121(13) C50 .0460(16) .0426(15) .0463(17) .0001(13) .0183(13) .0061(13) C51 .054(2) .115(3) .0368(18) -.021(2) .0110(15) -.0038(18) C60 .0423(15) .0371(14) .0304(14) .0065(12) .0037(11) -.0075(11) C61 .0505(18) .0564(18) .0478(18) -.0141(15) -.0014(14) -.0162(14) C70 .0282(12) .0355(13) .0397(15) .0041(10) .0167(11) .0028(11) C71 .0324(14) .0542(17) .0530(18) -.0110(13) .0141(13) -.0049(14) C80 .0288(12) .0313(13) .0317(13) .0041(10) .0060(10) .0069(10) C81 .0459(16) .0442(16) .0571(19) .0184(13) .0137(14) .0152(14) C90 .070(2) .134(4) .057(2) .002(3) .002(2) .004(2) C91 .0488(18) .082(2) .0376(17) .0106(17) .0179(14) .0087(16) C92 .072(2) .065(2) .050(2) .0305(18) .0223(18) .0268(17) C93 .077(2) .0516(19) .065(2) .0111(18) .030(2) .0057(17) C94 .0497(19) .077(2) .062(2) .0007(18) .0185(17) .0057(18) C95 .0393(16) .066(2) .068(2) .0114(15) .0213(16) .0264(17) C96 .0369(15) .0482(16) .0570(19) .0057(13) .0234(14) .0107(14) 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 Pd1 C1A . 2.036(2) yes Pd1 N2A . 2.0554(19) yes Pd1 P1 . 2.2490(7) yes Pd1 C10 . 2.028(2) yes Pd2 C2A . 2.028(2) yes Pd2 N1A . 2.046(2) yes Pd2 P2 . 2.2795(6) yes Pd2 C20 . 2.039(2) yes C1A N1A . 1.147(3) yes C2A N2A 3_655 1.145(3) yes N2A C2A 3_655 1.145(3) no P1 C50 . 1.809(3) no P1 C40 . 1.820(3) no P1 C30 . 1.870(3) no P2 C80 . 1.822(2) no P2 C60 . 1.826(3) no P2 C70 . 1.828(2) no C10 C11 . 1.376(3) no C10 C15 . 1.379(3) no C11 F11 . 1.356(3) no C11 C12 . 1.390(3) no C12 F12 . 1.347(3) no C12 C13 . 1.375(4) no C13 F13 . 1.351(3) no C13 C14 . 1.366(4) no C14 F14 . 1.350(3) no C14 C15 . 1.381(3) no C15 F15 . 1.361(3) no C20 C21 . 1.380(3) no C20 C25 . 1.388(3) no C21 F21 . 1.361(3) no C21 C22 . 1.384(3) no C22 F22 . 1.351(3) no C22 C23 . 1.368(4) no C23 F23 . 1.351(3) no C23 C24 . 1.368(4) no C24 F24 . 1.350(3) no C24 C25 . 1.378(4) no C25 F25 . 1.357(3) no C30 C31 . 1.515(4) no C40 C41 . 1.525(3) no C50 C51 . 1.514(4) no C60 C61 . 1.513(4) no C70 C71 . 1.523(4) no C80 C81 . 1.526(3) no C90 C91 . 1.493(5) no C91 C96 . 1.391(4) no C91 C92 . 1.407(5) no C92 C93 . 1.384(5) no C93 C94 . 1.348(5) no C94 C95 . 1.369(5) no C95 C96 . 1.371(4) no