#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007036.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_2007036 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1998 _journal_volume 54 _journal_page_first 227 _journal_page_last 228 _publ_section_title ; Ligands with Cycloalkane Backbones, IV. Dichloro{(S,S)-trans-diphenyl[(2- diphenylphosphinyl)cyclohexyl]phosphinic acid ester}palladium(II) ; _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _publ_author_name 'Thurner, C. L.' 'Barz, M.' 'Spiegler, M.' 'Thiel, W. R.' _chemical_formula_sum ' C30 H30 Cl2 O P2 Pd' _chemical_formula_iupac '[Pd Cl2 (C30 H30 O P2)]' _chemical_formula_weight 645.84 _symmetry_cell_setting Monoclinic loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 14.4070(10) _cell_length_b 8.4250(10) _cell_length_c 11.7770(10) _cell_angle_alpha 90 _cell_angle_beta 100.930(10) _cell_angle_gamma 90 _cell_volume 1403.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _exptl_crystal_density_diffrn 1.528 _diffrn_ambient_temperature 293 _refine_ls_R_factor_obs .0237 _refine_ls_wR_factor_obs .0634 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_occupancy Pd1 .23480(2) .32028(3) .76253(2) .03040(10) Uani 1.000 Cl1 .16231(7) .53728(11) .83403(9) .0489(3) Uani 1.000 Cl2 .27157(8) .47087(11) .60676(9) .0536(3) Uani 1.000 P1 .29030(6) .10178(9) .68575(6) .0298(2) Uani 1.000 P2 .19170(6) .18483(10) .90452(7) .0312(2) Uani 1.000 O1 .2197(2) -.0003(3) .9098(2) .0369(7) Uani 1.000 C1 .3167(2) -.0397(4) .9050(3) .0336(11) Uani 1.000 C2 .3197(2) -.0793(4) .7791(3) .0338(12) Uani 1.000 C3 .4132(3) -.1583(5) .7682(3) .0457(12) Uani 1.000 C4 .4362(3) -.2986(5) .8507(4) .0510(12) Uani 1.000 C5 .4381(3) -.2489(5) .9749(4) .0516(12) Uani 1.000 C6 .3439(3) -.1783(7) .9864(3) .0456(12) Uani 1.000 C11 .0652(2) .1655(4) .8876(3) .0369(12) Uani 1.000 C12 .0146(3) .2634(6) .9491(4) .0505(12) Uani 1.000 C13 -.0826(3) .2484(7) .9322(5) .0637(16) Uani 1.000 C14 -.1288(3) .1440(6) .8540(5) .0677(16) Uani 1.000 C15 -.0787(3) .0471(6) .7922(5) .0633(16) Uani 1.000 C16 .0189(3) .0584(5) .8082(3) .0489(12) Uani 1.000 C21 .2379(2) .2484(4) 1.0514(3) .0394(12) Uani 1.000 C22 .3010(3) .3715(5) 1.0766(4) .0462(12) Uani 1.000 C23 .3378(3) .4050(7) 1.1921(5) .0615(16) Uani 1.000 C24 .3143(3) .3196(9) 1.2792(3) .0681(14) Uani 1.000 C25 .2526(4) .1950(8) 1.2548(4) .072(2) Uani 1.000 C26 .2131(3) .1592(6) 1.1405(3) .0576(16) Uani 1.000 C31 .2013(2) .0331(4) .5649(3) .0358(11) Uani 1.000 C32 .1316(3) .1346(5) .5109(3) .0530(12) Uani 1.000 C33 .0614(4) .0786(7) .4234(4) .0686(17) Uani 1.000 C34 .0597(4) -.0760(7) .3884(5) .0717(19) Uani 1.000 C35 .1281(3) -.1784(8) .4426(4) .0699(14) Uani 1.000 C36 .1985(3) -.1260(5) .5307(4) .0515(12) Uani 1.000 C41 .3996(2) .1457(4) .6360(3) .0345(11) Uani 1.000 C42 .4222(3) .0751(5) .5383(3) .0437(12) Uani 1.000 C43 .5110(4) .0984(5) .5105(4) .0546(16) Uani 1.000 C44 .5760(3) .1921(5) .5796(4) .0549(14) Uani 1.000 C45 .5532(3) .2671(5) .6746(4) .0522(12) Uani 1.000 C46 .4654(3) .2445(5) .7027(3) .0424(12) Uani 1.000 H1 .355(3) .050(5) .932(3) .037(9) Uiso 1.000 H2 .271(3) -.170(8) .752(3) .054(10) Uiso 1.000 H3A .413(3) -.188(7) .685(4) .060(11) Uiso 1.000 H3B .458(3) -.093(6) .786(4) .050(13) Uiso 1.000 H4A .385(3) -.376(5) .826(3) .045(11) Uiso 1.000 H4B .494(3) -.333(5) .842(3) .043(10) Uiso 1.000 H5A .453(3) -.334(6) 1.020(4) .054(11) Uiso 1.000 H5B .488(3) -.170(7) .995(4) .052(10) Uiso 1.000 H6A .340(3) -.143(6) 1.070(4) .063(13) Uiso 1.000 H6B .303(3) -.250(6) .972(4) .049(12) Uiso 1.000 H12 .049(4) .293(10) .997(6) .11(3) Uiso 1.000 H13 -.112(4) .310(9) .976(4) .079(15) Uiso 1.000 H14 -.198(4) .114(6) .847(4) .071(14) Uiso 1.000 H15 -.101(3) -.014(6) .748(4) .054(14) Uiso 1.000 H16 .054(3) -.003(4) .771(3) .031(9) Uiso 1.000 H22 .318(3) .424(5) 1.015(4) .042(10) Uiso 1.000 H23 .374(4) .449(7) 1.205(5) .063(18) Uiso 1.000 H24 .337(5) .307(12) 1.349(6) .13(2) Uiso 1.000 H25 .232(4) .130(7) 1.307(5) .072(15) Uiso 1.000 H26 .158(4) .092(8) 1.123(5) .091(18) Uiso 1.000 H32 .133(4) .245(6) .542(4) .073(15) Uiso 1.000 H33 .019(4) .135(7) .390(5) .080(17) Uiso 1.000 H34 .015(4) -.111(7) .338(5) .092(19) Uiso 1.000 H35 .134(5) -.287(8) .414(6) .11(2) Uiso 1.000 H36 .244(3) -.173(7) .561(3) .045(10) Uiso 1.000 H42 .372(3) .019(6) .492(4) .056(12) Uiso 1.000 H43 .527(3) .058(6) .454(4) .056(14) Uiso 1.000 H44 .636(4) .211(6) .560(5) .071(15) Uiso 1.000 H45 .596(3) .328(6) .715(3) .049(10) Uiso 1.000 H46 .453(3) .301(6) .770(3) .049(10) Uiso 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 Pd1 .03710(10) .02380(10) .03190(10) -.00070(10) .01080(10) -.00210(10) Cl1 .0539(5) .0364(4) .0577(5) .0064(4) .0136(4) -.0142(4) Cl2 .0741(6) .0371(5) .0556(5) .0053(4) .0279(5) .0142(4) P1 .0359(4) .0277(4) .0268(4) .0015(3) .0086(3) -.0018(3) P2 .0338(4) .0319(4) .0291(4) -.0039(3) .0087(3) -.0043(3) O1 .0423(12) .0325(12) .0388(12) -.0028(9) .0152(9) .0024(9) C1 .038(2) .031(2) .0312(15) -.0011(13) .0053(12) -.0008(12) C2 .038(2) .030(2) .034(2) .0032(12) .0083(13) .0026(12) C3 .046(2) .040(2) .054(2) .010(2) .017(2) .007(2) C4 .053(2) .040(2) .059(2) .012(2) .008(2) .008(2) C5 .050(2) .044(2) .056(2) .000(2) -.002(2) .015(2) C6 .055(2) .042(2) .038(2) -.005(2) .0043(14) .009(2) C11 .034(2) .043(2) .034(2) -.0048(14) .0072(13) .0043(13) C12 .043(2) .057(2) .056(2) .001(2) .021(2) .001(2) C13 .046(2) .072(3) .079(3) .005(2) .027(2) .014(3) C14 .037(2) .076(3) .090(3) -.007(2) .012(2) .030(3) C15 .054(2) .063(3) .066(3) -.024(2) -.006(2) .008(2) C16 .050(2) .051(2) .046(2) -.009(2) .010(2) -.001(2) C21 .040(2) .045(2) .033(2) .0022(15) .0064(13) -.0046(14) C22 .037(2) .050(2) .051(2) .0014(14) .007(2) -.009(2) C23 .042(2) .070(3) .065(3) .001(2) -.009(2) -.026(2) C24 .067(2) .086(3) .043(2) .015(4) -.011(2) -.016(3) C25 .089(4) .091(4) .035(2) .001(3) .013(2) .002(2) C26 .069(3) .066(3) .038(2) -.008(2) .011(2) .001(2) C31 .038(2) .038(2) .0305(15) .0023(13) .0041(12) -.0032(13) C32 .058(2) .050(2) .046(2) .010(2) -.003(2) -.001(2) C33 .058(3) .078(3) .060(3) .016(2) -.014(2) -.001(2) C34 .064(3) .081(4) .058(3) -.007(2) -.019(2) -.011(2) C35 .085(3) .056(2) .061(2) -.013(3) -.006(2) -.019(3) C36 .058(2) .043(2) .049(2) .004(2) -.001(2) -.007(2) C41 .040(2) .033(2) .0319(15) .0047(13) .0100(12) .0040(13) C42 .052(2) .042(2) .041(2) .003(2) .019(2) -.003(2) C43 .069(3) .050(3) .054(2) .004(2) .035(2) .004(2) C44 .049(2) .054(2) .068(3) .002(2) .027(2) .018(2) C45 .046(2) .054(2) .054(2) -.010(2) .003(2) .008(2) C46 .048(2) .041(2) .038(2) -.003(2) .0077(15) .004(2) 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 Pd1 Cl1 . . 2.3400(10) yes Pd1 Cl2 . . 2.3715(11) yes Pd1 P1 . . 2.2627(9) yes Pd1 P2 . . 2.2086(9) yes P1 C2 . . 1.881(3) yes P1 C31 . . 1.820(3) yes P1 C41 . . 1.819(3) yes P2 O1 . . 1.609(3) yes P2 C11 . . 1.803(3) yes P2 C21 . . 1.813(4) yes O1 C1 . . 1.448(4) yes C1 C2 . . 1.528(5) no C1 C6 . . 1.514(6) no C2 C3 . . 1.530(5) no C3 C4 . . 1.526(6) no C4 C5 . . 1.517(7) no C5 C6 . . 1.511(6) no C11 C12 . . 1.392(6) no C11 C16 . . 1.377(5) no C12 C13 . . 1.382(6) no C13 C14 . . 1.354(8) no C14 C15 . . 1.384(7) no C15 C16 . . 1.386(6) no C21 C22 . . 1.374(5) no C21 C26 . . 1.391(5) no C22 C23 . . 1.392(7) no C23 C24 . . 1.348(8) no C24 C25 . . 1.370(9) no C25 C26 . . 1.392(6) no C31 C32 . . 1.379(5) no C31 C36 . . 1.398(5) no C32 C33 . . 1.383(7) no C33 C34 . . 1.365(8) no C34 C35 . . 1.373(8) no C35 C36 . . 1.379(7) no C41 C42 . . 1.388(5) no C41 C46 . . 1.388(5) no C42 C43 . . 1.393(7) no C43 C44 . . 1.369(7) no C44 C45 . . 1.378(6) no C45 C46 . . 1.380(6) no C1 H1 . . .95(4) no C2 H2 . . 1.05(6) no C3 H3A . . 1.01(5) no C3 H3B . . .84(5) no C4 H4A . . .99(4) no C4 H4B . . .91(4) no C5 H5A . . .89(5) no C5 H5B . . .97(5) no C6 H6A . . 1.04(5) no C6 H6B . . .84(5) no C12 H12 . . .72(7) no C13 H13 . . .89(6) no C14 H14 . . 1.02(6) no C15 H15 . . .76(5) no C16 H16 . . .89(4) no C22 H22 . . .92(5) no C23 H23 . . .63(6) no C24 H24 . . .83(7) no C25 H25 . . .91(6) no C26 H26 . . .96(6) no C32 H32 . . 1.00(5) no C33 H33 . . .81(6) no C34 H34 . . .84(6) no C35 H35 . . .98(7) no C36 H36 . . .79(5) no C42 H42 . . .95(5) no C43 H43 . . .82(5) no C44 H44 . . .95(6) no C45 H45 . . .87(4) no C46 H46 . . .97(4) no