#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006450.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_2006450 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 1251 _journal_page_last 1254 _publ_section_title ; [Mo(CO)(C~25~H~22~P~2~)(C~34~H~33~P~3~)] ; loop_ _publ_author_name 'George, T. Adrian' 'DeBord, Jeffrey R. D.' 'Heier, Kevin' 'Tisdale, Robert C.' 'Davies, Marcia C.' 'Haas, Eric J.' 'Ross II, Charles R.' 'Stezowski, John J.' _chemical_name_common ; [Mo(CO)(dpepp)(dppm)] (dppm = Ph~2~PCH~2~PPh~2~, dpepp = Ph~2~PCH~2~CH~2~P(Ph)CH~2~CH~2~PPh~2~) ; _chemical_formula_sum 'C60 H55 Mo O P5' _chemical_formula_analytical 'C60 H55 Mo O P5' _chemical_formula_iupac '[Mo (C O) (C25 H22 P2) (C34 H33 P3)]' _chemical_formula_weight 1042.83 _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 12.108(2) _cell_length_b 12.155(2) _cell_length_c 18.884(4) _cell_angle_alpha 104.37(3) _cell_angle_beta 100.67(3) _cell_angle_gamma 100.80(3) _cell_volume 2565.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.350 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .051 _refine_ls_wR_factor_obs .116 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_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Mo1 .82354(2) .60815(2) .251000(10) .02480(7) Uani d . 1 . Mo P1 .73779(6) .61539(6) .36208(4) .02737(14) Uani d . 1 . P P2 .93907(6) .53989(6) .34655(4) .02805(15) Uani d . 1 . P P3 .93351(7) .57956(7) .15581(4) .0328(2) Uani d . 1 . P P4A .6920(2) .6952(2) .18062(15) .0324(4) Uani d P .901(10) 1 P P4B .680(2) .697(2) .2010(10) .038(4) Uani d P .099(10) 2 P P5 .68881(7) .42950(6) .15462(4) .0334(2) Uani d . 1 . P C11 .7436(3) .7525(2) .4342(2) .0322(6) Uani d . 1 . C C12 .8487(3) .8340(3) .4638(2) .0496(9) Uani d . 1 . C H12 .9131 .8198 .4462 .060 Uiso calc R 1 . H C13 .8593(4) .9376(3) .5197(2) .0602(11) Uani d . 1 . C H13 .9307 .9917 .5390 .072 Uiso calc R 1 . H C14 .7663(4) .9604(3) .5465(2) .0625(11) Uani d . 1 . C H14 .7736 1.0298 .5836 .075 Uiso calc R 1 . H C15 .6620(4) .8795(4) .5179(3) .0721(13) Uani d . 1 . C H15 .5982 .8940 .5361 .087 Uiso calc R 1 . H C16 .6497(3) .7758(3) .4620(2) .0559(10) Uani d . 1 . C H16 .5781 .7219 .4432 .067 Uiso calc R 1 . H C21 .5986(3) .5263(3) .3638(2) .0358(6) Uani d . 1 . C C22 .4975(3) .5359(3) .3202(2) .0499(8) Uani d . 1 . C H22 .5019 .5867 .2906 .060 Uiso calc R 1 . H C23 .3901(3) .4712(4) .3196(3) .0681(13) Uani d . 1 . C H23 .3233 .4809 .2910 .082 Uiso calc R 1 . H C24 .3820(5) .3949(5) .3599(4) .097(2) Uani d . 1 . C H24 .3099 .3489 .3574 .117 Uiso calc R 1 . H C25 .4796(5) .3850(6) .4045(4) .110(2) Uani d . 1 . C H25 .4737 .3333 .4334 .132 Uiso calc R 1 . H C26 .5869(4) .4509(4) .4072(3) .0736(14) Uani d . 1 . C H26 .6526 .4443 .4388 .088 Uiso calc R 1 . H C31 1.0850(3) .6288(3) .3997(2) .0322(6) Uani d . 1 . C C32 1.1186(3) .6725(3) .4774(2) .0468(8) Uani d . 1 . C H32 1.0652 .6589 .5058 .056 Uiso calc R 1 . H C33 1.2313(4) .7366(4) .5134(2) .0619(11) Uani d . 1 . C H33 1.2531 .7648 .5657 .074 Uiso calc R 1 . H C34 1.3097(3) .7584(4) .4729(3) .0621(11) Uani d . 1 . C H34 1.3846 .8025 .4975 .075 Uiso calc R 1 . H C35 1.2791(3) .7158(4) .3962(2) .0578(10) Uani d . 1 . C H35 1.3336 .7295 .3686 .069 Uiso calc R 1 . H C36 1.1663(3) .6520(3) .3592(2) .0447(8) Uani d . 1 . C H36 1.1454 .6248 .3068 .054 Uiso calc R 1 . H C41 .9594(3) .3916(3) .3427(2) .0335(6) Uani d . 1 . C C42 1.0633(3) .3674(3) .3711(2) .0389(7) Uani d . 1 . C H42 1.1292 .4285 .3935 .047 Uiso calc R 1 . H C43 1.0702(4) .2531(3) .3665(2) .0533(9) Uani d . 1 . C H43 1.1403 .2382 .3861 .064 Uiso calc R 1 . H C44 .9735(4) .1621(3) .3331(3) .0626(11) Uani d . 1 . C H44 .9779 .0857 .3305 .075 Uiso calc R 1 . H C45 .8701(4) .1843(3) .3035(3) .0666(12) Uani d . 1 . C H45 .8050 .1225 .2799 .080 Uiso calc R 1 . H C46 .8626(3) .2981(3) .3087(2) .0497(8) Uani d . 1 . C H46 .7921 .3123 .2892 .060 Uiso calc R 1 . H C51 1.0184(3) .7032(3) .1338(2) .0408(7) Uani d . 1 . C C52 1.0990(3) .7904(3) .1925(2) .0509(9) Uani d . 1 . C H52 1.1078 .7853 .2415 .061 Uiso calc R 1 . H C53 1.1668(4) .8850(4) .1789(3) .0676(12) Uani d . 1 . C H53 1.2193 .9434 .2188 .081 Uiso calc R 1 . H C54 1.1563(5) .8925(5) .1071(3) .083(2) Uani d . 1 . C H54 1.2024 .9553 .0979 .100 Uiso calc R 1 . H C55 1.0772(5) .8065(4) .0482(3) .0770(15) Uani d . 1 . C H55 1.0700 .8115 -.0007 .092 Uiso calc R 1 . H C56 1.0086(4) .7133(4) .0613(2) .0561(10) Uani d . 1 . C H56 .9551 .6563 .0211 .067 Uiso calc R 1 . H C61 1.0386(3) .4854(3) .1544(2) .0401(7) Uani d . 1 . C C62 1.1423(3) .5091(4) .1323(2) .0514(9) Uani d . 1 . C H62 1.1650 .5787 .1208 .062 Uiso calc R 1 . H C63 1.2114(4) .4305(5) .1273(2) .0685(12) Uani d . 1 . C H63 1.2796 .4475 .1118 .082 Uiso calc R 1 . H C64 1.1809(5) .3276(5) .1449(3) .0743(14) Uani d . 1 . C H64 1.2275 .2747 .1409 .089 Uiso calc R 1 . H C65 1.0809(5) .3041(4) .1685(2) .0698(13) Uani d . 1 . C H65 1.0607 .2356 .1818 .084 Uiso calc R 1 . H C66 1.0095(4) .3811(3) .1729(2) .0537(9) Uani d . 1 . C H66 .9414 .3631 .1883 .064 Uiso calc R 1 . H C71 .6075(3) .7835(3) .2338(2) .0475(8) Uani d . 1 . C C72 .6691(4) .8784(3) .2948(2) .0584(10) Uani d . 1 . C H72 .7497 .8966 .3067 .070 Uiso calc R 1 . H C73 .6125(6) .9468(5) .3385(3) .086(2) Uani d . 1 . C H73 .6539 1.0111 .3792 .104 Uiso calc R 1 . H C74 .4904(6) .9160(6) .3195(4) .092(2) Uani d . 1 . C H74 .4507 .9609 .3478 .110 Uiso calc R 1 . H C75 .4302(5) .8220(6) .2608(4) .096(2) Uani d . 1 . C H75 .3496 .8017 .2497 .115 Uiso calc R 1 . H C76 .4874(4) .7572(5) .2180(3) .0725(13) Uani d . 1 . C H76 .4449 .6938 .1771 .087 Uiso calc R 1 . H C81 .7406(4) .7974(3) .1295(2) .0452(8) Uani d . 1 . C C82 .6804(5) .7936(4) .0583(2) .0737(14) Uani d . 1 . C H82 .6102 .7388 .0349 .088 Uiso calc R 1 . H C83 .7254(7) .8719(6) .0218(3) .099(2) Uani d . 1 . C H83 .6855 .8668 -.0264 .118 Uiso calc R 1 . H C84 .8256(7) .9550(5) .0548(4) .099(2) Uani d . 1 . C H84 .8541 1.0067 .0297 .119 Uiso calc R 1 . H C85 .8837(5) .9617(4) .1246(3) .082(2) Uani d . 1 . C H85 .9521 1.0193 .1481 .099 Uiso calc R 1 . H C86 .8424(3) .8837(2) .1618(2) .0598(10) Uani d . 1 . C H86 .8844 .8896 .2097 .072 Uiso calc R 1 . H C91A .6207(3) .2822(2) .1619(2) .043(4) Uiso d PRD .542(9) 1 C C92A .5279(3) .2757(2) .1963(2) .052(2) Uiso d PRD .542(9) 1 C H92A .5043 .3429 .2162 .063 Uiso calc PR .542(9) 1 H C93A .4713(5) .1679(4) .2007(4) .063(2) Uiso d PD .542(9) 1 C H93A .4107 .1633 .2246 .076 Uiso calc PR .542(9) 1 H C94A .5047(8) .0675(4) .1696(6) .068(5) Uiso d PD .542(9) 1 C H94A .4628 -.0052 .1692 .081 Uiso calc PR .542(9) 1 H C95A .6013(6) .0750(4) .1388(5) .067(2) Uiso d PD .542(9) 1 C H95A .6283 .0088 .1224 .080 Uiso calc PR .542(9) 1 H C96A .6567(6) .1825(4) .1330(4) .053(2) Uiso d PD .542(9) 1 C H96A .7179 .1872 .1097 .064 Uiso calc PR .542(9) 1 H C91B .6205(6) .2806(5) .1556(4) .035(4) Uiso d PD .458(9) 2 C C92B .5700(6) .2728(5) .2153(4) .047(2) Uiso d PD .458(9) 2 C H92B .5719 .3408 .2519 .057 Uiso calc PR .458(9) 2 H C93B .5167(8) .1645(6) .2208(4) .057(2) Uiso d PD .458(9) 2 C H93B .4801 .1603 .2596 .068 Uiso calc PR .458(9) 2 H C94B .5190(10) .0626(5) .1680(7) .089(7) Uiso d PD .458(9) 2 C H94B .493 -.0101 .1749 .107 Uiso calc PR .458(9) 2 H C95B .5600(10) .0701(5) .1049(5) .074(3) Uiso d PD .458(9) 2 C H95B .548 .0031 .0649 .089 Uiso calc PR .458(9) 2 H C96B .6187(9) .1780(6) .1016(5) .062(3) Uiso d PD .458(9) 2 C H96B .6567 .1816 .0634 .074 Uiso calc PR .458(9) 2 H C2 .8470(3) .5570(3) .4144(2) .0407(7) Uani d . 1 . C H2A .8889 .6122 .4628 .061 Uiso calc R 1 . H H2B .8128 .4827 .4213 .061 Uiso calc R 1 . H C3 .8329(3) .4959(3) .0627(2) .0449(8) Uani d . 1 . C H3A .7907 .5471 .0435 .067 Uiso calc R 1 . H H3B .8771 .4678 .0272 .067 Uiso calc R 1 . H C4 .7470(3) .3917(3) .0698(2) .0504(9) Uani d . 1 . C H4A .7853 .3289 .0719 .076 Uiso calc R 1 . H H4B .6830 .3632 .0252 .076 Uiso calc R 1 . H C5A .5805(4) .5830(3) .1014(2) .0479(13) Uani d P .901(10) 1 C H5A1 .5101 .6100 .0930 .072 Uiso calc PR .901(10) 1 H H5A2 .6082 .5729 .0557 .072 Uiso calc PR .901(10) 1 H C5B .542(2) .589(2) .144(2) .027(7) Uiso d P .099(10) 2 C H5B1 .485 .590 .175 .041 Uiso calc PR .099(10) 2 H H5B2 .512 .614 .101 .041 Uiso calc PR .099(10) 2 H C6 .5540(3) .4680(3) .1176(2) .0528(9) Uani d . 1 . C H6A .5098 .4076 .0718 .079 Uiso calc R 1 1 H H6B .5071 .4724 .1542 .079 Uiso calc R 1 1 H C1 .9233(3) .7635(3) .3020(2) .0347(6) Uani d . 1 . C O1 .9836(2) .8579(2) .33080(10) .0546(7) Uani d . 1 . 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 Mo1 .02553(12) .02355(11) .02307(11) .00320(8) .00431(8) .00609(8) P1 .0251(3) .0290(3) .0275(3) .0056(3) .0072(3) .0076(3) P2 .0260(3) .0312(4) .0283(3) .0072(3) .0072(3) .0105(3) P3 .0352(4) .0358(4) .0263(3) .0044(3) .0099(3) .0086(3) P4A .0366(7) .0264(5) .0294(10) .0049(5) -.0017(7) .0085(6) P4B .039(7) .041(6) .026(8) -.011(5) -.007(6) .020(7) P5 .0339(4) .0261(3) .0327(4) .0014(3) .0033(3) .0036(3) C11 .037(2) .0283(13) .0294(13) .0055(12) .0096(11) .0050(10) C12 .046(2) .046(2) .043(2) -.006(2) .017(2) -.0028(14) C13 .064(3) .046(2) .047(2) -.013(2) .014(2) -.007(2) C14 .079(3) .041(2) .054(2) .007(2) .019(2) -.008(2) C15 .057(3) .060(2) .084(3) .013(2) .032(2) -.016(2) C16 .039(2) .045(2) .069(2) .003(2) .018(2) -.009(2) C21 .0309(15) .0323(14) .041(2) .0026(12) .0125(12) .0061(12) C22 .034(2) .053(2) .055(2) .006(2) .008(2) .008(2) C23 .031(2) .076(3) .077(3) .003(2) .011(2) -.005(2) C24 .048(3) .082(4) .156(6) -.006(3) .046(3) .027(4) C25 .077(4) .109(5) .178(7) .006(3) .055(4) .096(5) C26 .047(2) .089(3) .102(4) .006(2) .022(2) .064(3) C31 .0300(14) .0311(14) .0369(14) .0093(12) .0061(11) .0128(11) C32 .039(2) .055(2) .038(2) .001(2) .0054(14) .0100(15) C33 .048(2) .067(3) .049(2) -.003(2) -.006(2) .004(2) C34 .036(2) .060(2) .071(3) -.006(2) -.006(2) .012(2) C35 .034(2) .067(3) .072(3) .001(2) .016(2) .024(2) C36 .035(2) .055(2) .043(2) .0063(15) .0095(14) .0151(15) C41 .038(2) .0324(14) .0335(14) .0094(12) .0094(12) .0140(11) C42 .038(2) .036(2) .046(2) .0116(13) .0117(14) .0159(13) C43 .054(2) .053(2) .065(2) .025(2) .017(2) .029(2) C44 .083(3) .034(2) .073(3) .018(2) .017(2) .020(2) C45 .070(3) .035(2) .081(3) -.004(2) .002(2) .016(2) C46 .041(2) .042(2) .060(2) .0022(15) .001(2) .017(2) C51 .040(2) .046(2) .041(2) .0070(14) .0155(14) .0197(14) C52 .046(2) .056(2) .047(2) -.003(2) .005(2) .023(2) C53 .055(2) .066(3) .071(3) -.012(2) .002(2) .030(2) C54 .076(3) .086(3) .088(3) -.016(3) .017(3) .055(3) C55 .092(4) .081(3) .060(3) -.004(3) .021(3) .041(2) C56 .066(3) .061(2) .042(2) .004(2) .015(2) .022(2) C61 .046(2) .048(2) .0289(14) .0152(15) .0128(13) .0085(12) C62 .047(2) .071(2) .038(2) .018(2) .013(2) .015(2) C63 .053(2) .102(4) .054(2) .035(3) .018(2) .013(2) C64 .078(3) .084(3) .062(3) .048(3) .010(2) .007(2) C65 .100(4) .058(2) .058(2) .038(3) .017(2) .016(2) C66 .068(3) .049(2) .049(2) .020(2) .021(2) .012(2) C71 .044(2) .044(2) .069(2) .019(2) .017(2) .033(2) C72 .068(3) .051(2) .069(3) .025(2) .033(2) .020(2) C73 .130(5) .070(3) .086(4) .052(3) .058(4) .027(3) C74 .113(5) .107(4) .119(5) .081(4) .082(4) .066(4) C75 .072(4) .128(5) .132(5) .057(4) .051(4) .075(5) C76 .048(2) .087(3) .098(4) .024(2) .021(2) .048(3) C81 .068(2) .037(2) .035(2) .022(2) .011(2) .0135(13) C82 .108(4) .065(3) .042(2) .025(3) -.003(2) .016(2) C83 .170(7) .099(4) .049(3) .054(5) .029(3) .044(3) C84 .155(6) .086(4) .091(4) .040(4) .053(4) .061(3) C85 .103(4) .066(3) .096(4) .016(3) .032(3) .051(3) C86 .077(3) .046(2) .061(2) .009(2) .015(2) .028(2) C2 .038(2) .058(2) .038(2) .021(2) .0155(13) .0225(14) C3 .048(2) .052(2) .0262(14) .001(2) .0082(13) .0061(13) C4 .058(2) .046(2) .032(2) -.002(2) .010(2) -.0031(13) C5A .049(2) .036(2) .043(2) .002(2) -.014(2) .008(2) C6 .040(2) .038(2) .058(2) .0016(15) -.017(2) .002(2) C1 .039(2) .0332(14) .0277(13) .0031(13) .0041(12) .0084(11) O1 .066(2) .0341(12) .0429(13) -.0142(12) .0035(12) .0016(10) 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 Mo1 C1 . 1.940(3) Y Mo1 P4B . 2.37(3) Y Mo1 P3 . 2.4237(10) Y Mo1 P4A . 2.442(3) Y Mo1 P2 . 2.4788(10) Y Mo1 P1 . 2.4970(9) Y Mo1 P5 . 2.5100(15) Y P1 C21 . 1.835(3) ? P1 C11 . 1.853(3) ? P1 C2 . 1.856(3) Y P2 C31 . 1.840(3) ? P2 C2 . 1.847(3) Y P2 C41 . 1.850(3) ? P3 C51 . 1.838(3) ? P3 C3 . 1.861(3) Y P3 C61 . 1.863(3) ? P4A C81 . 1.831(4) ? P4A C71 . 1.862(4) ? P4A C5A . 1.863(4) Y P4B C71 . 1.58(3) ? P4B C5B . 1.87(4) Y P4B C81 . 2.18(2) ? P5 C6 . 1.844(4) Y P5 C91B . 1.849(5) ? P5 C4 . 1.857(4) Y P5 C91A . 1.875(3) ? C11 C12 . 1.379(4) ? C11 C16 . 1.384(5) ? C12 C13 . 1.395(5) ? C13 C14 . 1.364(6) ? C14 C15 . 1.368(6) ? C15 C16 . 1.392(5) ? C21 C26 . 1.379(5) ? C21 C22 . 1.384(5) ? C22 C23 . 1.384(5) ? C23 C24 . 1.340(8) ? C24 C25 . 1.363(8) ? C25 C26 . 1.378(6) ? C31 C32 . 1.383(4) ? C31 C36 . 1.384(4) ? C32 C33 . 1.388(5) ? C33 C34 . 1.352(6) ? C34 C35 . 1.364(6) ? C35 C36 . 1.391(5) ? C41 C42 . 1.387(4) ? C41 C46 . 1.392(5) ? C42 C43 . 1.389(5) ? C43 C44 . 1.374(6) ? C44 C45 . 1.376(6) ? C45 C46 . 1.384(5) ? C51 C52 . 1.390(5) ? C51 C56 . 1.390(5) ? C52 C53 . 1.391(5) ? C53 C54 . 1.366(6) ? C54 C55 . 1.378(7) ? C55 C56 . 1.377(6) ? C61 C66 . 1.397(5) ? C61 C62 . 1.397(5) ? C62 C63 . 1.381(6) ? C63 C64 . 1.375(7) ? C64 C65 . 1.372(7) ? C65 C66 . 1.386(6) ? C71 C72 . 1.384(6) ? C71 C76 . 1.387(6) ? C72 C73 . 1.388(6) ? C73 C74 . 1.408(9) ? C74 C75 . 1.351(9) ? C75 C76 . 1.360(8) ? C81 C86 . 1.383(5) ? C81 C82 . 1.392(5) ? C82 C83 . 1.395(7) ? C83 C84 . 1.352(9) ? C84 C85 . 1.349(8) ? C85 C86 . 1.388(5) ? C91A C96A . 1.384(3) ? C91A C92A . 1.40 ? C92A C93A . 1.390(4) ? C93A C94A . 1.385(4) ? C94A C95A . 1.397(4) ? C95A C96A . 1.392(4) ? C91B C92B . 1.393(4) ? C91B C96B . 1.394(4) ? C92B C93B . 1.391(4) ? C93B C94B . 1.392(4) ? C94B C95B . 1.390(4) ? C95B C96B . 1.393(4) ? C3 C4 . 1.531(5) Y C5A C6 . 1.493(5) Y C5B C6 . 1.48(3) Y C1 O1 . 1.172(4) Y