#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011366.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_2011366 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first e378 _journal_page_last e379 _publ_section_title ; Hemipentane and ditetrahydrofuran solvates of trans-dichlorobis[1,2-ethandiylbis(diphenylphosphine)-P,P']molybdenum(II) ; _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _publ_author_name 'Filippou, Alexander, C.' 'Portius, Peter' 'Philippopoulos, Athanassios, I.' 'Kociok-K\"ohn, Gabriele' 'Ziemer, Burkhard' _chemical_formula_moiety 'C52 H48 Cl2 Mo P4, 0.5C5 H12' _chemical_formula_sum 'C54.50 H54 Cl2 Mo P4' _chemical_formula_iupac '[Mo Cl2 (C26 H24 P2)2], 0.5C5 H12' _chemical_formula_weight 999.70 _symmetry_cell_setting Monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 49.542(11) _cell_length_b 10.958(3) _cell_length_c 18.123(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.03(3) _cell_angle_gamma 90.00 _cell_volume 9688(4) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _exptl_crystal_density_diffrn 1.371 _diffrn_ambient_temperature 180(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 C1 .14558(18) -.2861(8) .2353(5) .035(2) Uani d . 1 . . C H1A .1422 -.2491 .2828 .041 Uiso calc R 1 . . H H1B .1438 -.3757 .2395 .041 Uiso calc R 1 . . H C2 .1746(2) -.2545(9) .2235(5) .040(3) Uani d . 1 . . C H2A .1879 -.3007 .2601 .048 Uiso calc R 1 . . H H2B .1779 -.1665 .2337 .048 Uiso calc R 1 . . H C3 .1135(2) -.4313(9) -.1444(5) .040(3) Uani d . 1 . . C H3A .1180 -.4284 -.1955 .048 Uiso calc R 1 . . H H3B .1040 -.5093 -.1389 .048 Uiso calc R 1 . . H C4 .0945(2) -.3242(10) -.1340(5) .044(3) Uani d . 1 . . C H4A .0769 -.3333 -.1689 .053 Uiso calc R 1 . . H H4B .1030 -.2465 -.1458 .053 Uiso calc R 1 . . H C11 .0882(2) -.2785(10) .1907(5) .041(3) Uani d . 1 . . C C12 .0804(2) -.4009(10) .1848(6) .048(3) Uani d . 1 . . C H12 .0909 -.4588 .1628 .057 Uiso calc R 1 . . H C13 .0569(2) -.4365(12) .2122(7) .065(4) Uani d . 1 . . C H13 .0516 -.5199 .2086 .078 Uiso calc R 1 . . H C14 .0414(3) -.3568(14) .2434(6) .071(4) Uani d . 1 . . C H14 .0261 -.3852 .2636 .085 Uiso calc R 1 . . H C15 .0479(3) -.2331(13) .2462(8) .083(5) Uani d . 1 . . C H15 .0362 -.1763 .2648 .099 Uiso calc R 1 . . H C16 .0713(2) -.1928(12) .2218(7) .069(4) Uani d . 1 . . C H16 .0762 -.1089 .2256 .083 Uiso calc R 1 . . H C17 .1201(2) -.0667(9) .1715(5) .039(3) Uani d . 1 . . C C18 .1088(2) .0126(9) .1110(6) .047(3) Uani d . 1 . . C H18 .1010 -.0214 .0638 .056 Uiso calc R 1 . . H C19 .1091(2) .1372(10) .1204(6) .054(3) Uani d . 1 . . C H19 .1014 .1885 .0800 .065 Uiso calc R 1 . . H C20 .1206(2) .1875(11) .1876(6) .053(3) Uani d . 1 . . C H20 .1206 .2737 .1932 .064 Uiso calc R 1 . . H C21 .1325(2) .1141(10) .2490(6) .057(3) Uani d . 1 . . C H21 .1406 .1509 .2950 .068 Uiso calc R 1 . . H C22 .1320(2) -.0118(9) .2415(5) .043(3) Uani d . 1 . . C H22 .1396 -.0618 .2828 .051 Uiso calc R 1 . . H C31 .20196(19) -.1591(8) .1085(4) .028(2) Uani d . 1 . . C C32 .1918(2) -.0387(9) .1154(5) .040(3) Uani d . 1 . . C H32 .1746 -.0269 .1311 .048 Uiso calc R 1 . . H C33 .2069(2) .0611(10) .0991(5) .045(3) Uani d . 1 . . C H33 .1997 .1407 .1034 .054 Uiso calc R 1 . . H C34 .2320(2) .0481(10) .0768(5) .048(3) Uani d . 1 . . C H34 .2422 .1184 .0673 .057 Uiso calc R 1 . . H C35 .2424(2) -.0667(11) .0683(5) .054(3) Uani d . 1 . . C H35 .2593 -.0765 .0511 .065 Uiso calc R 1 . . H C36 .22741(19) -.1707(9) .0859(5) .036(2) Uani d . 1 . . C H36 .2349 -.2498 .0821 .043 Uiso calc R 1 . . H C37 .2066(2) -.4117(9) .1435(5) .034(2) Uani d . 1 . . C C38 .2269(2) -.4185(10) .2071(5) .044(3) Uani d . 1 . . C H38 .2278 -.3580 .2450 .053 Uiso calc R 1 . . H C39 .2458(2) -.5139(10) .2155(5) .046(3) Uani d . 1 . . C H39 .2591 -.5197 .2599 .056 Uiso calc R 1 . . H C40 .2453(2) -.6005(10) .1592(6) .048(3) Uani d . 1 . . C H40 .2584 -.6644 .1647 .057 Uiso calc R 1 . . H C41 .2254(2) -.5933(11) .0949(6) .055(3) Uani d . 1 . . C H41 .2249 -.6524 .0563 .066 Uiso calc R 1 . . H C42 .2065(2) -.5005(9) .0873(5) .043(3) Uani d . 1 . . C H42 .1931 -.4960 .0431 .052 Uiso calc R 1 . . H C51 .1697(2) -.3522(8) -.1262(4) .033(2) Uani d . 1 . . C C52 .1872(2) -.2589(9) -.0941(5) .037(3) Uani d . 1 . . C H52 .1870 -.2365 -.0436 .045 Uiso calc R 1 . . H C53 .2050(2) -.1972(9) -.1334(5) .041(3) Uani d . 1 . . C H53 .2168 -.1346 -.1101 .049 Uiso calc R 1 . . H C54 .2050(2) -.2301(10) -.2080(5) .047(3) Uani d . 1 . . C H54 .2166 -.1881 -.2360 .056 Uiso calc R 1 . . H C55 .1883(2) -.3232(10) -.2416(5) .044(3) Uani d . 1 . . C H55 .1888 -.3462 -.2919 .053 Uiso calc R 1 . . H C56 .1710(2) -.3822(9) -.2016(5) .043(3) Uani d . 1 . . C H56 .1595 -.4452 -.2254 .052 Uiso calc R 1 . . H C57 .1554(2) -.5840(8) -.0727(5) .034(2) Uani d . 1 . . C C58 .1376(2) -.6764(10) -.0551(5) .046(3) Uani d . 1 . . C H58 .1201 -.6532 -.0447 .055 Uiso calc R 1 . . H C59 .1446(3) -.8018(10) -.0522(5) .051(3) Uani d . 1 . . C H59 .1320 -.8615 -.0408 .061 Uiso calc R 1 . . H C60 .1700(2) -.8351(11) -.0663(5) .053(3) Uani d . 1 . . C H60 .1746 -.9193 -.0663 .064 Uiso calc R 1 . . H C61 .1893(2) -.7496(10) -.0807(5) .049(3) Uani d . 1 . . C H61 .2071 -.7747 -.0876 .058 Uiso calc R 1 . . H C62 .1819(2) -.6251(10) -.0847(5) .046(3) Uani d . 1 . . C H62 .1948 -.5667 -.0957 .055 Uiso calc R 1 . . H C71 .0627(2) -.4424(10) -.0402(5) .038(3) Uani d . 1 . . C C72 .0684(2) -.5485(11) .0022(6) .050(3) Uani d . 1 . . C H725 .0859 -.5589 .0329 .060 Uiso calc R 1 . . H C73 .0492(3) -.6365(11) -.0004(7) .064(4) Uani d . 1 . . C H73 .0535 -.7091 .0279 .076 Uiso calc R 1 . . H C74 .0230(3) -.6234(11) -.0439(8) .062(3) Uani d . 1 . . C H74 .0097 -.6861 -.0451 .074 Uiso calc R 1 . . H C75 .0170(2) -.5192(13) -.0843(7) .062(4) Uani d . 1 . . C H75 -.0008 -.5080 -.1129 .074 Uiso calc R 1 . . H C76 .0366(2) -.4298(11) -.0840(6) .052(3) Uani d . 1 . . C H76 .0324 -.3589 -.1139 .063 Uiso calc R 1 . . H C77 .0670(2) -.1852(10) -.0333(5) .045(3) Uani d . 1 . . C C78 .0690(2) -.0818(10) -.0771(6) .055(3) Uani d . 1 . . C H78 .0802 -.0830 -.1148 .066 Uiso calc R 1 . . H C79 .0541(3) .0255(11) -.0647(7) .064(3) Uani d . 1 . . C H79 .0557 .0978 -.0925 .076 Uiso calc R 1 . . H C80 .0370(3) .0222(13) -.0108(8) .073(4) Uani d . 1 . . C H80 .0266 .0925 -.0035 .087 Uiso calc R 1 . . H C81 .0349(2) -.0807(12) .0322(7) .060(3) Uani d . 1 . . C H81 .0234 -.0805 .0689 .072 Uiso calc R 1 . . H C82 .0495(2) -.1817(12) .0212(6) .056(3) Uani d . 1 . . C H82 .0481 -.2522 .0508 .067 Uiso calc R 1 . . H C83 .0000 -.210(3) -.2500 .21(2) Uani d SD 1 . . C H83A -.0126 -.2620 -.2848 .252 Uiso calc PR .50 . . H H83B .0126 -.2620 -.2152 .252 Uiso calc PR .50 . . H C84 -.0152(6) -.123(2) -.209(2) .288(19) Uani d D 1 . . C H84A -.0027 -.0930 -.1640 .345 Uiso calc R 1 . . H H84B -.0213 -.0525 -.2414 .345 Uiso calc R 1 . . H C85 -.0395(5) -.181(2) -.1853(13) .249(19) Uani d D 1 . . C H85A -.0452 -.1317 -.1454 .374 Uiso calc R 1 . . H H85B -.0348 -.2632 -.1668 .374 Uiso calc R 1 . . H H85C -.0546 -.1844 -.2282 .374 Uiso calc R 1 . . H Cl1 .13622(5) -.5178(2) .10646(12) .0399(6) Uani d . 1 . . Cl Cl2 .13788(5) -.1276(2) -.02028(13) .0422(6) Uani d . 1 . . Cl P1 .11998(6) -.2306(2) .15804(13) .0344(7) Uani d . 1 . . P P2 .18085(6) -.2888(2) .12733(13) .0341(7) Uani d . 1 . . P P3 .14594(5) -.4242(2) -.07361(12) .0335(6) Uani d . 1 . . P P4 .08827(5) -.3205(3) -.03786(13) .0357(7) Uani d . 1 . . P Mo .13465(2) -.32020(8) .04336(4) .0322(2) Uani d . 1 . . Mo 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 C1 .037(6) .038(6) .029(5) -.007(5) .008(4) -.017(4) C2 .058(8) .032(6) .033(5) .005(5) .015(5) .000(4) C3 .051(7) .047(6) .027(5) .003(5) .020(5) -.004(4) C4 .045(7) .067(7) .022(4) -.005(6) .010(4) -.001(5) C11 .043(7) .052(7) .031(5) -.010(5) .015(5) -.015(5) C12 .048(7) .038(7) .060(7) -.012(5) .018(6) .001(5) C13 .053(9) .068(9) .076(8) -.016(7) .016(7) .013(7) C14 .055(9) .105(12) .058(7) -.017(8) .026(7) -.005(7) C15 .074(11) .078(10) .111(12) -.011(8) .058(9) -.027(9) C16 .051(8) .070(9) .098(9) -.014(7) .042(7) -.036(8) C17 .041(7) .043(6) .036(5) -.002(5) .014(5) .000(5) C18 .069(9) .033(6) .041(6) .002(6) .020(6) -.005(5) C19 .071(9) .043(7) .050(7) .005(6) .012(6) .008(5) C20 .074(9) .036(6) .052(6) -.001(6) .019(6) -.006(6) C21 .074(9) .056(8) .042(6) -.009(7) .012(6) -.011(6) C22 .068(8) .034(6) .027(5) -.001(5) .009(5) -.003(4) C31 .039(6) .026(6) .022(4) -.009(5) .009(4) .003(4) C32 .052(7) .035(6) .031(5) -.012(5) .004(5) -.004(4) C33 .056(8) .042(7) .034(5) .005(6) .003(5) .004(5) C34 .067(9) .035(6) .043(6) -.004(6) .015(6) .004(5) C35 .073(9) .059(8) .032(5) -.009(7) .015(6) .006(5) C36 .043(6) .029(5) .036(5) -.005(5) .010(5) .002(5) C37 .038(7) .044(6) .024(5) .001(5) .012(4) .002(4) C38 .036(7) .060(7) .034(5) .008(6) -.004(5) -.012(5) C39 .046(8) .054(7) .036(5) .001(6) -.003(5) -.001(5) C40 .048(8) .052(7) .046(6) .018(6) .012(6) .019(5) C41 .072(9) .064(8) .030(5) .025(7) .012(6) -.004(5) C42 .055(8) .048(7) .027(5) .004(6) .011(5) .003(5) C51 .044(7) .040(6) .015(4) -.003(5) .002(4) .004(4) C52 .029(6) .062(7) .023(5) .000(5) .013(4) -.001(5) C53 .051(7) .031(6) .043(5) -.012(5) .012(5) -.008(5) C54 .052(8) .059(7) .034(5) -.004(6) .021(5) .006(5) C55 .061(7) .043(6) .030(5) -.002(6) .016(5) .000(5) C56 .066(8) .036(6) .030(5) .002(5) .015(5) .003(4) C57 .042(7) .030(6) .030(5) .005(5) .009(5) .006(4) C58 .064(8) .039(6) .039(5) -.008(6) .020(5) -.005(5) C59 .082(10) .031(7) .042(6) .005(6) .017(6) .010(5) C60 .082(9) .049(7) .029(5) -.006(7) .011(6) -.013(5) C61 .072(9) .043(7) .030(5) .006(6) .009(5) -.007(5) C62 .049(8) .059(8) .030(5) .009(6) .007(5) .007(5) C71 .035(7) .047(7) .033(5) .001(5) .012(5) -.009(5) C72 .046(8) .067(8) .039(6) -.022(6) .009(5) -.011(6) C73 .054(9) .058(9) .078(8) -.018(7) .009(7) -.002(7) C74 .050(9) .038(7) .100(10) -.017(6) .021(8) -.005(7) C75 .035(8) .085(10) .064(8) -.002(7) .007(6) -.025(7) C76 .034(7) .066(8) .057(7) -.012(6) .008(6) -.014(6) C77 .047(7) .045(7) .042(6) .006(6) .008(5) -.009(6) C78 .064(9) .041(7) .054(7) .015(6) -.005(6) .001(6) C79 .075(10) .040(7) .072(8) .013(7) .003(7) -.001(6) C80 .046(9) .082(11) .084(9) .018(7) -.004(7) -.024(8) C81 .052(8) .068(9) .062(7) -.003(7) .013(6) .000(7) C82 .035(7) .078(9) .057(7) .026(7) .010(6) -.015(7) C83 .38(6) .11(3) .10(2) .000 -.09(3) .000 C84 .36(6) .17(3) .31(6) -.02(3) .00(4) -.08(3) C85 .42(5) .22(3) .15(2) -.20(3) .15(3) -.09(2) Cl1 .0513(18) .0397(15) .0302(12) -.0025(13) .0116(12) .0038(11) Cl2 .0479(17) .0458(15) .0339(13) -.0031(12) .0102(12) -.0006(11) P1 .0429(18) .0381(16) .0236(12) .0011(13) .0097(12) -.0024(11) P2 .0406(18) .0405(17) .0228(12) .0009(13) .0102(12) .0001(11) P3 .0411(17) .0390(16) .0225(12) -.0015(13) .0115(12) .0016(11) P4 .0367(18) .0430(16) .0276(13) -.0011(15) .0066(12) -.0012(13) Mo .0393(6) .0372(5) .0216(4) -.0002(5) .0095(4) -.0004(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 C1 C2 . 1.529(12) ? C1 P1 . 1.822(10) ? C2 P2 . 1.861(8) ? C3 C4 . 1.537(13) ? C3 P3 . 1.876(10) ? C4 P4 . 1.823(8) ? C11 C12 . 1.394(13) ? C11 C16 . 1.435(13) ? C11 P1 . 1.852(10) ? C12 C13 . 1.399(13) ? C13 C14 . 1.350(16) ? C14 C15 . 1.392(16) ? C15 C16 . 1.384(14) ? C17 C18 . 1.434(13) ? C17 C22 . 1.435(13) ? C17 P1 . 1.813(10) ? C18 C19 . 1.376(13) ? C19 C20 . 1.368(15) ? C20 C21 . 1.415(15) ? C21 C22 . 1.387(13) ? C31 C36 . 1.398(11) ? C31 C32 . 1.426(12) ? C31 P2 . 1.831(9) ? C32 C33 . 1.385(13) ? C33 C34 . 1.384(13) ? C34 C35 . 1.378(14) ? C35 C36 . 1.427(13) ? C37 C38 . 1.392(13) ? C37 C42 . 1.408(12) ? C37 P2 . 1.844(10) ? C38 C39 . 1.395(13) ? C39 C40 . 1.390(13) ? C40 C41 . 1.391(14) ? C41 C42 . 1.372(14) ? C51 C52 . 1.399(13) ? C51 C56 . 1.417(11) ? C51 P3 . 1.820(9) ? C52 C53 . 1.402(12) ? C53 C54 . 1.399(12) ? C54 C55 . 1.386(14) ? C55 C56 . 1.375(12) ? C57 C58 . 1.415(13) ? C57 C62 . 1.441(13) ? C57 P3 . 1.813(9) ? C58 C59 . 1.416(14) ? C59 C60 . 1.380(14) ? C60 C61 . 1.394(14) ? C61 C62 . 1.411(13) ? C71 C72 . 1.395(14) ? C71 C76 . 1.401(14) ? C71 P4 . 1.836(11) ? C72 C73 . 1.352(14) ? C73 C74 . 1.402(16) ? C74 C75 . 1.360(16) ? C75 C76 . 1.379(15) ? C77 C78 . 1.398(14) ? C77 C82 . 1.421(12) ? C77 P4 . 1.830(11) ? C78 C79 . 1.428(14) ? C79 C80 . 1.398(16) ? C80 C81 . 1.384(16) ? C81 C82 . 1.356(15) ? C83 C84 . 1.489(17) ? C83 C84 2_554 1.489(17) ? C84 C85 . 1.483(18) ? Cl1 Mo . 2.444(3) ? Cl2 Mo . 2.424(3) ? P1 Mo . 2.518(2) ? P2 Mo . 2.542(3) ? P3 Mo . 2.553(2) ? P4 Mo . 2.504(3) ?