#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011600.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_2011600 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first 1440 _journal_page_last 1441 _publ_section_title ; Cyclometallated compounds. XV. A tetranuclear acetate-bridged cyclopalladated molecular box ; loop_ _publ_author_name "O'Keefe, Brendan J." 'Steel, Peter J.' _chemical_formula_moiety 'C40 H32 N4 O12 Pd4 , 2C1 H1 Cl3 , 2H2 O' _chemical_formula_sum 'C42 H38 Cl6 N4 O14 Pd4' _chemical_formula_iupac '[Pd4 (C16 H10 N2 O2)2 (C2 H3 O2)4] , 2C H Cl3 , 2H2 O' _chemical_formula_weight 1461.06 _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 12.225(5) _cell_length_b 15.052(5) _cell_length_c 14.135(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.797(5) _cell_angle_gamma 90.00 _cell_volume 2599.7(16) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _exptl_crystal_density_diffrn 1.861 _diffrn_ambient_temperature 168(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 .31144(4) .54255(3) .19048(4) .02685(17) Uani d . 1 . . Pd Pd2 .80465(4) .49483(3) -.01135(4) .02634(17) Uani d . 1 . . Pd C1 .5411(6) .5935(4) .1517(5) .0289(15) Uani d . 1 . . C C2 .4638(5) .5269(4) .1499(5) .0262(15) Uani d . 1 . . C C3 .4986(6) .4466(4) .1102(4) .0285(15) Uani d . 1 . . C H3 .4501 .3973 .1079 .034 Uiso calc R 1 . . H C4 .6020(6) .4377(4) .0746(4) .0248(15) Uani d . 1 . . C C5 .6764(6) .5074(4) .0677(5) .0282(15) Uani d . 1 . . C C6 .6432(5) .5865(5) .1103(4) .0285(15) Uani d . 1 . . C H6 .6909 .6363 .1111 .034 Uiso calc R 1 . . H O1 .5244(4) .6767(3) .1959(4) .0400(13) Uani d . 1 . . O N11 .3325(5) .6772(4) .1852(4) .0317(14) Uani d . 1 . . N C12 .4276(6) .7198(4) .1953(5) .0335(17) Uani d . 1 . . C C13 .4343(7) .8120(5) .2058(6) .043(2) Uani d . 1 . . C H13 .5033 .8402 .2153 .052 Uiso calc R 1 . . H C14 .3410(7) .8603(5) .2024(6) .050(2) Uani d . 1 . . C H14 .3436 .9229 .2105 .060 Uiso calc R 1 . . H C15 .2414(8) .8177(5) .1868(6) .051(2) Uani d . 1 . . C H15 .1753 .8507 .1808 .061 Uiso calc R 1 . . H C16 .2405(6) .7285(5) .1805(5) .0401(19) Uani d . 1 . . C H16 .1718 .6995 .1722 .048 Uiso calc R 1 . . H O4 .6256(4) .3517(3) .0401(3) .0317(11) Uani d . 1 . . O N41 .8167(4) .3706(4) .0396(4) .0281(13) Uani d . 1 . . N C42 .7275(6) .3184(4) .0505(4) .0273(15) Uani d . 1 . . C C43 .7377(7) .2288(5) .0704(5) .0369(17) Uani d . 1 . . C H43 .6741 .1933 .0761 .044 Uiso calc R 1 . . H C44 .8405(7) .1908(5) .0821(5) .0422(19) Uani d . 1 . . C H44 .8483 .1293 .0960 .051 Uiso calc R 1 . . H C45 .9317(7) .2445(5) .0731(6) .045(2) Uani d . 1 . . C H45 1.0030 .2201 .0818 .054 Uiso calc R 1 . . H C46 .9191(6) .3336(5) .0513(5) .0383(18) Uani d . 1 . . C H46 .9820 .3697 .0444 .046 Uiso calc R 1 . . H O1A .2912(4) .4079(3) .2043(3) .0308(11) Uani d . 1 . . O C1A .2491(5) .3557(5) .1423(5) .0299(16) Uani d . 1 . . C C2A .2488(8) .2582(5) .1683(7) .059(3) Uani d . 1 . . C H2A1 .2193 .2509 .2315 .089 Uiso calc R 1 . . H H2A2 .3238 .2351 .1681 .089 Uiso calc R 1 . . H H2A3 .2031 .2254 .1220 .089 Uiso calc R 1 . . H O2A .2103(4) .3768(3) .0619(3) .0319(11) Uani d . 1 . . O O1B .1448(4) .5543(3) .2377(3) .0375(12) Uani d . 1 . . O C1B .0596(6) .5397(5) .1865(5) .0319(16) Uani d . 1 . . C C2B -.0502(7) .5541(7) .2334(6) .063(3) Uani d . 1 . . C H2B1 -.0727 .6162 .2256 .094 Uiso calc R 1 . . H H2B2 -.0425 .5401 .3009 .094 Uiso calc R 1 . . H H2B3 -.1056 .5152 .2036 .094 Uiso calc R 1 . . H O2B .0568(4) .5231(3) .1003(3) .0368(12) Uani d . 1 . . O C70 .8801(19) .8743(11) .1312(12) .056(8) Uani d PDU .365(3) A 1 C H70 .8167 .9071 .1576 .067 Uiso calc PR .365(3) A 1 H Cl71 .9690(4) .8403(4) .2261(4) .0492(16) Uani d PDU .365(3) A 1 Cl Cl72 .8314(6) .7779(5) .0740(5) .062(2) Uani d PDU .365(3) A 1 Cl Cl73 .9463(7) .9439(4) .0506(5) .069(2) Uani d PDU .365(3) A 1 Cl C80 .7814(14) .5897(10) .5848(12) .115(6) Uani d PDU .416(7) B 2 C H80 .7607 .5495 .6377 .138 Uiso calc PR .416(7) B 2 H Cl81 .6787(9) .6717(5) .5660(6) .105(4) Uani d PDU .416(7) B 2 Cl Cl82 .7915(16) .5281(7) .4797(7) .246(10) Uani d PDU .416(7) B 2 Cl Cl83 .9089(11) .6404(11) .6123(13) .233(8) Uani d PDU .416(7) B 2 Cl C90 .665(2) .6198(14) .560(3) .134(11) Uani d PDU .219(7) C 3 C H90 .6386 .6087 .6251 .160 Uiso calc PR .219(7) C 3 H Cl91 .5664(17) .6846(10) .5001(12) .131(7) Uani d PDU .219(7) C 3 Cl Cl92 .684(3) .5162(10) .5068(15) .181(13) Uani d PDU .219(7) C 3 Cl Cl93 .789(2) .6790(17) .573(2) .204(13) Uani d PDU .219(7) C 3 Cl O70A .5919(19) .5102(14) .5751(14) .032(7) Uani d PU .26(2) D 4 O O70B .5147(11) .4590(7) .5992(5) .080(6) Uani d P .74(2) D 5 O 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 .0298(3) .0248(3) .0261(3) -.0027(2) .0015(2) -.0019(2) Pd2 .0293(3) .0236(3) .0261(3) -.0025(2) .0013(2) .0020(2) C1 .039(4) .020(3) .027(4) -.003(3) -.004(3) -.006(3) C2 .028(4) .026(4) .024(3) -.003(3) -.002(3) .002(3) C3 .037(4) .022(3) .026(3) -.006(3) -.005(3) .003(3) C4 .033(4) .015(3) .026(3) -.002(3) -.003(3) .003(3) C5 .036(4) .024(3) .024(3) -.006(3) -.007(3) .000(3) C6 .029(4) .030(4) .027(3) -.008(3) .002(3) -.006(3) O1 .033(3) .030(3) .056(3) -.005(2) .002(2) -.019(2) N11 .036(4) .030(3) .030(3) -.002(3) .003(3) -.001(3) C12 .044(5) .028(4) .028(4) -.005(3) .002(3) -.007(3) C13 .054(5) .027(4) .049(5) -.007(4) -.004(4) -.010(4) C14 .075(7) .029(4) .045(5) .005(4) -.003(4) -.005(4) C15 .068(6) .037(5) .047(5) .012(4) -.012(4) -.003(4) C16 .041(5) .038(4) .041(4) .003(4) -.006(4) -.004(4) O4 .041(3) .018(2) .037(3) -.001(2) .001(2) -.001(2) N41 .032(3) .027(3) .026(3) .002(3) .002(2) -.001(2) C42 .034(4) .026(4) .022(3) -.002(3) .000(3) .004(3) C43 .047(5) .025(4) .039(4) -.002(3) .004(4) .000(3) C44 .062(6) .027(4) .038(4) .007(4) .007(4) .004(3) C45 .050(5) .040(5) .045(5) .016(4) -.005(4) .004(4) C46 .035(4) .040(4) .039(4) .006(3) -.004(3) .000(3) O1A .034(3) .028(3) .031(3) -.005(2) .001(2) .001(2) C1A .023(4) .029(4) .037(4) -.004(3) -.001(3) .003(3) C2A .078(7) .030(4) .069(6) -.012(4) -.025(5) .014(4) O2A .038(3) .024(2) .033(3) -.004(2) -.002(2) .001(2) O1B .035(3) .041(3) .037(3) -.001(2) .004(2) -.009(2) C1B .031(4) .043(4) .021(3) .002(3) .007(3) .001(3) C2B .034(5) .094(8) .061(6) .000(5) .015(4) -.022(5) O2B .031(3) .041(3) .038(3) -.002(2) .004(2) .003(2) C70 .052(18) .015(10) .102(18) -.017(11) -.005(12) .016(10) Cl71 .031(3) .051(3) .065(4) .003(2) .001(3) -.011(3) Cl72 .087(5) .059(4) .039(3) -.031(4) .009(3) .002(3) Cl73 .114(6) .035(3) .061(4) -.027(3) .052(4) -.021(3) C80 .218(15) .041(13) .092(14) .054(10) .101(16) .052(8) Cl81 .183(9) .055(4) .081(5) .047(5) .053(6) .016(4) Cl82 .54(3) .097(7) .109(7) .178(11) .180(12) .045(5) Cl83 .137(9) .234(16) .334(19) .038(10) .116(11) .161(12) C90 .22(3) .08(2) .11(3) .002(19) .09(3) .024(19) Cl91 .216(19) .078(10) .103(13) -.014(10) .069(12) .011(9) Cl92 .36(4) .083(11) .091(14) .029(14) -.11(2) -.009(10) Cl93 .28(2) .18(2) .15(2) -.07(2) .01(2) -.01(2) O70A .039(10) .035(9) .021(9) .021(6) -.008(6) .010(6) O70B .144(12) .069(8) .028(4) .076(8) .004(5) -.004(4) 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 C2 . 1.980(7) yes Pd1 N11 . 2.044(6) yes Pd1 O1A . 2.052(5) yes Pd1 O1B . 2.171(5) yes Pd1 Pd2 3_665 2.9182(11) ? Pd2 C5 . 1.962(7) yes Pd2 N41 . 2.007(5) yes Pd2 O2A 3_665 2.067(4) yes Pd2 O2B 3_665 2.158(5) yes Pd2 Pd1 3_665 2.9182(11) ? C1 C2 . 1.378(9) yes C1 C6 . 1.399(9) yes C1 O1 . 1.417(8) yes C2 C3 . 1.403(9) yes C3 C4 . 1.381(10) yes C4 C5 . 1.395(9) yes C4 O4 . 1.417(7) yes C5 C6 . 1.400(9) yes O1 C12 . 1.350(9) ? N11 C12 . 1.332(9) ? N11 C16 . 1.364(9) ? C12 C13 . 1.398(9) ? C13 C14 . 1.352(11) ? C14 C15 . 1.388(11) ? C15 C16 . 1.346(10) ? O4 C42 . 1.346(8) ? N41 C42 . 1.356(8) ? N41 C46 . 1.375(9) ? C42 C43 . 1.383(9) ? C43 C44 . 1.386(10) ? C44 C45 . 1.387(11) ? C45 C46 . 1.383(10) ? O1A C1A . 1.273(8) yes C1A O2A . 1.258(8) yes C1A C2A . 1.514(9) yes O2A Pd2 3_665 2.067(4) ? O1B C1B . 1.269(8) yes C1B O2B . 1.243(8) yes C1B C2B . 1.531(10) yes O2B Pd2 3_665 2.158(5) ? C70 Cl72 . 1.756(14) ? C70 Cl73 . 1.763(15) ? C70 Cl71 . 1.775(14) ? C80 Cl82 . 1.759(13) ? C80 Cl83 . 1.767(14) ? C80 Cl81 . 1.774(13) ? C90 Cl92 . 1.749(16) ? C90 Cl91 . 1.752(16) ? C90 Cl93 . 1.763(16) ?