#------------------------------------------------------------------------------ #$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2011807.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_2011807 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2001 _journal_volume 57 _journal_page_first 235 _journal_page_last 236 _publ_section_title ; [\h^2^-(E)-But-2-enedinitrile](N,N'-diphenyl-1,7,7,-trimethylbicyclo[2.2.1] heptane-2,3-diimine-N,N')palladium(0) ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Ellis, Dianne D.' 'Spek, Anthony L.' _chemical_formula_moiety 'C26 H26 N4 Pd' _chemical_formula_sum 'C26 H26 N4 Pd' _chemical_formula_iupac '[Pd(C22 H24 N2 )(C4 H2 N2 )]' _chemical_formula_weight 500.91 _symmetry_cell_setting monoclinic 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 11.8073(13) _cell_length_b 10.0751(12) _cell_length_c 21.453(3) _cell_angle_alpha 90 _cell_angle_beta 116.024(8) _cell_angle_gamma 90 _cell_volume 2293.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 1.451 _diffrn_ambient_temperature 150(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 .224795(18) .08720(2) .189247(9) .02215(8) Uani d . 1 A . Pd N1 .3558(2) .1375(3) .14774(12) .0276(5) Uani d . 1 . . N N2 .1028(2) .1608(2) .08716(11) .0263(5) Uani d . 1 . . N N3 .4469(3) .1934(3) .37370(14) .0420(7) Uani d . 1 . . N N4 .0082(3) -.1524(4) .23466(16) .0575(10) Uani d . 1 A . N C1 .3036(4) .1966(4) .08894(19) .0288(9) Uani d PD .872(4) A 1 C C2 .3455(4) .2694(4) .04120(19) .0364(8) Uani d PD .872(4) A 1 C C3 .3040(5) .1768(4) -.0232(2) .0451(11) Uani d PD .872(4) A 1 C H3A .3393 .2079 -.0549 .054 Uiso calc PR .872(4) A 1 H H3B .3323 .0845 -.0089 .054 Uiso calc PR .872(4) A 1 H C4 .1599(5) .1851(4) -.0584(2) .0449(11) Uani d PD .872(4) A 1 C H4A .1216 .0969 -.0603 .054 Uiso calc PR .872(4) A 1 H H4B .1286 .2206 -.1061 .054 Uiso calc PR .872(4) A 1 H C5 .1303(4) .2817(4) -.01120(17) .0369(9) Uani d PD .872(4) A 1 C H5 .0444 .3225 -.0327 .044 Uiso calc PR .872(4) A 1 H C6 .1631(4) .2064(3) .05521(16) .0279(8) Uani d PD .872(4) A 1 C C7 .2395(4) .3787(4) .0129(2) .0404(9) Uani d PD .872(4) A 1 C C8 .2408(12) .4581(10) -.0483(5) .0616(17) Uani d PD .872(4) A 1 C H8A .2516 .3970 -.0808 .092 Uiso calc PR .872(4) A 1 H H8B .3107 .5217 -.0307 .092 Uiso calc PR .872(4) A 1 H H8C .1610 .5061 -.0721 .092 Uiso calc PR .872(4) A 1 H C9 .2453(6) .4725(4) .0708(2) .0499(11) Uani d PD .872(4) A 1 C H9A .1724 .5322 .0525 .075 Uiso calc PR .872(4) A 1 H H9B .3231 .5248 .0878 .075 Uiso calc PR .872(4) A 1 H H9C .2442 .4201 .1090 .075 Uiso calc PR .872(4) A 1 H C10 .4758(3) .3160(4) .0671(2) .0371(8) Uani d PD .872(4) A 1 C H10A .4955 .3750 .1069 .056 Uiso calc PR .872(4) A 1 H H10B .4861 .3643 .0303 .056 Uiso calc PR .872(4) A 1 H H10C .5331 .2397 .0816 .056 Uiso calc PR .872(4) A 1 H C1B .160(2) .238(2) .0699(12) .028(2) Uiso d PD .128(4) A 2 C C2B .1287(15) .3485(17) .0188(8) .028(2) Uiso d PD .128(4) A 2 C C3B .1769(19) .4753(19) .0619(11) .028(2) Uiso d PD .128(4) A 2 C H3B1 .1458 .4817 .0978 .034 Uiso calc PR .128(4) A 2 H H3B2 .1495 .5551 .0320 .034 Uiso calc PR .128(4) A 2 H C4B .3246(19) .4610(19) .0961(10) .028(2) Uiso d PD .128(4) A 2 C H4B1 .3650 .5374 .0847 .034 Uiso calc PR .128(4) A 2 H H4B2 .3600 .4514 .1471 .034 Uiso calc PR .128(4) A 2 H C5B .3390(16) .3324(19) .0614(9) .028(2) Uiso d PD .128(4) A 2 C H5B .4240 .3199 .0627 .034 Uiso calc PR .128(4) A 2 H C6B .302(2) .225(3) .0987(15) .028(2) Uiso d PD .128(4) A 2 C C7B .2326(16) .3250(18) -.0087(8) .028(2) Uiso d PD .128(4) A 2 C C8B .232(5) .454(4) -.0492(19) .028(2) Uiso d PD .128(4) A 2 C H8B1 .2246 .4310 -.0951 .042 Uiso calc PR .128(4) A 2 H H8B2 .3100 .5037 -.0233 .042 Uiso calc PR .128(4) A 2 H H8B3 .1596 .5097 -.0545 .042 Uiso calc PR .128(4) A 2 H C9B .215(3) .197(2) -.0481(13) .028(2) Uiso d PD .128(4) A 2 C H9B1 .2871 .1824 -.0581 .042 Uiso calc PR .128(4) A 2 H H9B2 .1376 .2028 -.0918 .042 Uiso calc PR .128(4) A 2 H H9B3 .2075 .1237 -.0202 .042 Uiso calc PR .128(4) A 2 H C10B .0267(16) .3510(17) -.0479(8) .028(2) Uiso d PD .128(4) A 2 C H10D .0210 .4285 -.0768 .042 Uiso d PR .128(4) A 2 H H10E -.0354 .3592 -.0294 .042 Uiso d PRD .128(4) A 2 H H10F .0096 .2703 -.0761 .042 Uiso d PRD .128(4) A 2 H C11 .4901(3) .1218(3) .18427(15) .0304(6) Uani d . 1 A . C C12 .5497(3) .0231(4) .1663(2) .0440(8) Uani d . 1 . . C H12 .5021 -.0348 .1289 .053 Uiso calc R 1 A . H C13 .6788(4) .0071(4) .2021(2) .0516(9) Uani d . 1 A . C H13 .7199 -.0614 .1894 .062 Uiso calc R 1 . . H C14 .7474(3) .0906(4) .25625(19) .0473(9) Uani d . 1 . . C H14 .8363 .0805 .2807 .057 Uiso calc R 1 A . H C15 .6877(4) .1886(4) .27494(17) .0473(9) Uani d . 1 A . C H15 .7356 .2466 .3122 .057 Uiso calc R 1 . . H C16 .5574(3) .2039(4) .23984(15) .0385(7) Uani d . 1 . . C H16 .5156 .2696 .2539 .046 Uiso calc R 1 A . H C17 -.0322(3) .1677(3) .05820(14) .0277(6) Uani d . 1 A . C C18 -.0848(3) .1911(3) .10305(15) .0330(6) Uani d . 1 . . C H18 -.0320 .2022 .1512 .040 Uiso calc R 1 A . H C19 -.2150(3) .1984(3) .07812(17) .0386(7) Uani d . 1 A . C H19 -.2516 .2151 .1089 .046 Uiso calc R 1 . . H C20 -.2905(3) .1809(3) .00783(17) .0383(7) Uani d . 1 . . C H20 -.3795 .1870 -.0098 .046 Uiso calc R 1 A . H C21 -.2380(3) .1549(3) -.03645(16) .0378(8) Uani d . 1 A . C H21 -.2911 .1424 -.0844 .045 Uiso calc R 1 . . H C22 -.1080(3) .1467(3) -.01225(15) .0330(7) Uani d . 1 . . C H22 -.0718 .1271 -.0430 .040 Uiso calc RD 1 A . H C23 .3771(3) .1190(3) .33632(14) .0297(6) Uani d . 1 A . C C24 .2913(3) .0241(3) .28937(13) .0275(6) Uani d . 1 . . C H24 .3162 -.0663 .2956 .033 Uiso d R 1 A . H C25 .1575(3) .0477(3) .26053(13) .0280(6) Uani d . 1 A . C H25 .1238 .1236 .2719 .034 Uiso d R 1 . . H C26 .0750(3) -.0644(4) .24611(15) .0365(7) Uani d . 1 . . C 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 .02105(10) .02605(11) .01807(10) -.00027(8) .00739(8) .00115(8) N1 .0258(11) .0327(12) .0266(11) -.0045(10) .0136(9) -.0025(10) N2 .0258(11) .0261(12) .0217(10) -.0006(10) .0055(9) .0022(9) N3 .0375(14) .0483(17) .0341(14) -.0054(13) .0100(12) -.0060(12) N4 .0497(18) .070(2) .0420(17) -.0257(19) .0106(14) .0098(16) C1 .0341(17) .028(2) .0268(18) -.0054(15) .0157(14) -.0047(15) C2 .047(2) .0293(18) .044(2) -.0091(16) .0293(17) -.0048(16) C3 .081(3) .0292(19) .046(2) -.006(2) .047(2) -.0041(16) C4 .073(3) .036(2) .0299(19) -.012(2) .027(2) -.0034(15) C5 .050(2) .0315(19) .0282(17) -.0006(16) .0163(16) .0074(14) C6 .0352(17) .0241(17) .0217(16) -.0021(14) .0101(14) -.0002(12) C7 .055(2) .0271(18) .049(2) -.0018(17) .032(2) -.0011(16) C8 .072(4) .047(3) .081(3) .003(3) .046(3) .028(3) C9 .068(3) .030(2) .063(3) -.007(2) .039(3) -.0131(19) C10 .0309(17) .039(2) .049(2) -.0042(15) .0250(16) .0034(16) C11 .0247(13) .0365(16) .0297(14) -.0060(12) .0115(11) .0022(12) C12 .0344(16) .0413(19) .057(2) -.0046(15) .0206(16) -.0098(16) C13 .0370(18) .047(2) .070(2) .0057(16) .0229(18) -.0012(19) C14 .0287(15) .060(2) .0498(19) .0007(16) .0141(15) .0126(18) C15 .0380(17) .066(2) .0302(16) -.0093(18) .0079(14) -.0014(16) C16 .0347(16) .0497(19) .0292(14) -.0038(14) .0123(13) -.0069(13) C17 .0278(13) .0221(13) .0258(13) .0006(11) .0051(11) .0057(10) C18 .0305(15) .0334(15) .0296(14) .0062(13) .0079(12) .0029(12) C19 .0329(16) .0368(17) .0422(17) .0060(13) .0127(14) .0027(14) C20 .0245(14) .0331(16) .0436(17) .0015(12) .0022(13) .0074(14) C21 .0330(15) .0337(17) .0306(15) -.0095(13) -.0007(13) .0075(13) C22 .0376(16) .0309(15) .0249(13) -.0093(13) .0086(12) .0028(12) C23 .0267(13) .0387(17) .0208(12) .0016(12) .0079(11) .0033(11) C24 .0287(14) .0299(14) .0198(12) .0011(12) .0068(11) .0025(11) C25 .0286(13) .0346(15) .0201(12) .0016(12) .0102(11) .0041(11) C26 .0324(15) .050(2) .0234(13) -.0066(14) .0090(12) .0094(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 Pd1 C24 . 2.037(3) y Pd1 C25 . 2.047(3) y Pd1 N1 . 2.157(2) y Pd1 N2 . 2.157(2) y N1 C1 . 1.281(5) y N1 C6B . 1.31(2) ? N1 C11 . 1.436(4) ? N2 C1B . 1.19(2) ? N2 C6 . 1.271(5) y N2 C17 . 1.436(4) ? N3 C23 . 1.142(4) ? N4 C26 . 1.139(5) ? C1 C6 . 1.495(5) y C1 C2 . 1.509(5) ? C2 C10 . 1.465(5) ? C2 C3 . 1.558(5) ? C2 C7 . 1.575(6) ? C3 C4 . 1.531(7) ? C3 H3A . .9900 ? C3 H3B . .9900 ? C4 C5 . 1.552(6) ? C4 H4A . .9900 ? C4 H4B . .9900 ? C5 C6 . 1.507(5) ? C5 C7 . 1.517(6) ? C5 H5 . 1.0000 ? C5 H10F . 1.4967 ? C7 C9 . 1.538(6) ? C7 C8 . 1.542(7) ? C8 H8A . .9800 ? C8 H8B . .9800 ? C8 H8C . .9800 ? C9 H9A . .9800 ? C9 H9B . .9800 ? C9 H9C . .9800 ? C10 H10A . .9800 ? C10 H10B . .9800 ? C10 H10C . .9800 ? C1B C2B . 1.490(17) ? C1B C6B . 1.511(18) ? C2B C10B . 1.410(16) ? C2B C3B . 1.533(17) ? C2B C7B . 1.595(17) ? C3B C4B . 1.574(18) ? C3B H3B1 . .9900 ? C3B H3B2 . .9900 ? C4B C5B . 1.540(18) ? C4B H4B1 . .9900 ? C4B H4B2 . .9900 ? C5B C7B . 1.480(16) ? C5B C6B . 1.520(18) ? C5B H5B . 1.0000 ? C7B C9B . 1.502(17) ? C7B C8B . 1.563(18) ? C8B H8B1 . .9800 ? C8B H8B2 . .9800 ? C8B H8B3 . .9800 ? C9B H9B1 . .9800 ? C9B H9B2 . .9800 ? C9B H9B3 . .9800 ? C10B H10D . .9800 ? C10B H10E . .9800 ? C10B H10F . .9800 ? C11 C12 . 1.368(5) ? C11 C16 . 1.381(4) ? C12 C13 . 1.383(5) ? C12 H12 . .9500 ? C13 C14 . 1.374(6) ? C13 H13 . .9500 ? C14 C15 . 1.372(6) ? C14 H14 . .9500 ? C15 C16 . 1.393(5) ? C15 H15 . .9500 ? C16 H16 . .9500 ? C17 C18 . 1.375(5) ? C17 C22 . 1.394(4) ? C18 C19 . 1.390(5) ? C18 H18 . .9500 ? C19 C20 . 1.386(4) ? C19 H19 . .9500 ? C20 C21 . 1.368(5) ? C20 H20 . .9500 ? C21 C22 . 1.390(5) ? C21 H21 . .9500 ? C22 H22 . .9500 ? C23 C24 . 1.435(4) y C24 C25 . 1.441(4) y C24 H24 . .9490 ? C25 C26 . 1.433(4) y C25 H25 . .9426 ? _cod_database_code 2011807