#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200462.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_2200462 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first o624 _journal_page_last o626 _publ_section_title ; Polymorphic form of 1,3,5-tris[(diphenylphosphine oxide)methyl]benzene acetonitrile solvate monohydrate ; loop_ _publ_author_name 'Kruszynski, Rafal' 'Wieczorek, Wanda' _chemical_formula_moiety 'C45 H39 O3 P3, C2 H3 N, H2 O' _chemical_formula_sum 'C47 H44 N O4 P3' _chemical_formula_iupac 'C45 H39 O3 P3, C2 H3 N, H2 O' _chemical_formula_weight 779.74 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 15.3382(14) _cell_length_b 8.6418(9) _cell_length_c 15.9748(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.034(10) _cell_angle_gamma 90.00 _cell_volume 2045.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _exptl_crystal_density_diffrn 1.266 _diffrn_ambient_temperature 291.0(10) 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 P1 -.89339(10) -.96860(17) -.31681(10) .0421(3) Uani d . 1 . . P P2 -.74371(11) -.77740(19) -.71926(11) .0489(4) Uani d . 1 . . P P3 -.62228(12) -.43955(18) -.34069(13) .0543(4) Uani d . 1 . . P O1 -.8595(3) -.8535(5) -.2459(3) .0549(11) Uani d . 1 . . O O2 -.6797(4) -.6471(7) -.6904(4) .0841(18) Uani d . 1 . . O O3 -.6191(3) -.5182(5) -.2568(3) .0649(13) Uani d . 1 . . O C1 -.8119(4) -.8575(7) -.4433(4) .0409(12) Uani d . 1 . . C C2 -.8334(4) -.8705(7) -.5331(4) .0451(14) Uani d . 1 . . C H2 -.8548 -.9642 -.5591 .054 Uiso calc R 1 . . H C3 -.8236(4) -.7484(7) -.5838(4) .0460(14) Uani d . 1 . . C C4 -.7914(4) -.6084(7) -.5443(4) .0486(14) Uani d . 1 . . C H4 -.7857 -.5240 -.5786 .058 Uiso calc R 1 . . H C5 -.7679(4) -.5925(7) -.4557(4) .0447(13) Uani d . 1 . . C C6 -.7793(4) -.7163(6) -.4047(4) .0460(14) Uani d . 1 . . C H6 -.7653 -.7057 -.3448 .055 Uiso calc R 1 . . H C7 -.8193(4) -.9931(7) -.3874(4) .0462(14) Uani d . 1 . . C H7A -.7594 -1.0177 -.3519 .055 Uiso calc R 1 . . H H7B -.8402 -1.0814 -.4247 .055 Uiso calc R 1 . . H C8 -.8437(4) -.7613(8) -.6824(4) .0539(16) Uani d . 1 . . C H8A -.8773 -.6706 -.7085 .065 Uiso calc R 1 . . H H8B -.8814 -.8513 -.7015 .065 Uiso calc R 1 . . H C9 -.7334(4) -.4362(7) -.4158(4) .0514(15) Uani d . 1 . . C H9A -.7760 -.3961 -.3857 .062 Uiso calc R 1 . . H H9B -.7322 -.3647 -.4623 .062 Uiso calc R 1 . . H C10 -.8994(4) -1.1607(7) -.2757(3) .0399(12) Uani d . 1 . . C C11 -.9778(6) -1.2482(9) -.2949(7) .088(3) Uani d . 1 . . C H11 -1.0321 -1.2063 -.3268 .105 Uiso calc R 1 . . H C12 -.9733(7) -1.3976(10) -.2658(8) .119(4) Uani d . 1 . . C H12 -1.0256 -1.4571 -.2803 .143 Uiso calc R 1 . . H C13 -.8980(6) -1.4623(9) -.2179(6) .073(2) Uani d . 1 . . C H13 -.8982 -1.5640 -.1989 .087 Uiso calc R 1 . . H C14 -.8217(6) -1.3783(9) -.1977(5) .073(2) Uani d . 1 . . C H14 -.7681 -1.4226 -.1658 .088 Uiso calc R 1 . . H C15 -.8232(5) -1.2258(9) -.2243(5) .073(2) Uani d . 1 . . C H15 -.7711 -1.1664 -.2068 .088 Uiso calc R 1 . . H C16 -1.0023(4) -.9187(7) -.3845(4) .0441(13) Uani d . 1 . . C C17 -1.0510(5) -.8008(8) -.3574(6) .068(2) Uani d . 1 . . C H17 -1.0262 -.7486 -.3058 .082 Uiso calc R 1 . . H C18 -1.1356(6) -.7621(11) -.4071(7) .094(3) Uani d . 1 . . C H18 -1.1683 -.6842 -.3889 .113 Uiso calc R 1 . . H C19 -1.1724(6) -.8396(12) -.4849(6) .086(3) Uani d . 1 . . C H19 -1.2290 -.8114 -.5190 .103 Uiso calc R 1 . . H C20 -1.1273(6) -.9531(13) -.5103(6) .094(3) Uani d . 1 . . C H20 -1.1541 -1.0068 -.5609 .113 Uiso calc R 1 . . H C21 -1.0414(5) -.9937(9) -.4634(5) .0639(19) Uani d . 1 . . C H21 -1.0096 -1.0702 -.4839 .077 Uiso calc R 1 . . H C22 -.6971(5) -.9642(9) -.6866(4) .0587(18) Uani d . 1 . . C C23 -.6045(6) -.9815(15) -.6644(6) .106(4) Uani d . 1 . . C H23 -.5683 -.8940 -.6605 .128 Uiso calc R 1 . . H C24 -.5641(11) -1.124(2) -.6480(10) .167(9) Uani d . 1 . . C H24 -.5016 -1.1346 -.6331 .201 Uiso calc R 1 . . H C25 -.6174(17) -1.248(2) -.6541(9) .182(12) Uani d . 1 . . C H25 -.5903 -1.3447 -.6449 .218 Uiso calc R 1 . . H C26 -.7071(13) -1.2407(13) -.6725(7) .134(6) Uani d . 1 . . C H26 -.7415 -1.3298 -.6740 .161 Uiso calc R 1 . . H C27 -.7477(7) -1.0970(8) -.6894(5) .075(2) Uani d . 1 . . C H27 -.8103 -1.0899 -.7029 .090 Uiso calc R 1 . . H C28 -.7794(4) -.7865(7) -.8352(4) .0504(15) Uani d . 1 . . C C29 -.7380(6) -.6925(10) -.8824(5) .073(2) Uani d . 1 . . C H29 -.6934 -.6234 -.8546 .087 Uiso calc R 1 . . H C30 -.7632(6) -.7014(12) -.9715(6) .087(3) Uani d . 1 . . C H30 -.7353 -.6357 -1.0028 .104 Uiso calc R 1 . . H C31 -.8264(6) -.8006(12) -1.0156(5) .089(3) Uani d . 1 . . C H31 -.8402 -.8056 -1.0757 .107 Uiso calc R 1 . . H C32 -.8700(7) -.8946(15) -.9698(6) .113(4) Uani d . 1 . . C H32 -.9148 -.9626 -.9985 .136 Uiso calc R 1 . . H C33 -.8454(6) -.8858(13) -.8778(5) .094(3) Uani d . 1 . . C H33 -.8746 -.9484 -.8462 .113 Uiso calc R 1 . . H C34 -.5964(4) -.2366(7) -.3248(5) .0589(18) Uani d . 1 . . C C35 -.5912(5) -.1390(8) -.3930(6) .072(2) Uani d . 1 . . C H35 -.5990 -.1800 -.4483 .086 Uiso calc R 1 . . H C36 -.5748(7) .0162(10) -.3798(7) .086(3) Uani d . 1 . . C H36 -.5717 .0803 -.4257 .103 Uiso calc R 1 . . H C37 -.5630(5) .0758(9) -.2976(7) .083(3) Uani d . 1 . . C H37 -.5529 .1813 -.2887 .100 Uiso calc R 1 . . H C38 -.5659(5) -.0181(9) -.2273(6) .075(2) Uani d . 1 . . C H38 -.5561 .0224 -.1717 .089 Uiso calc R 1 . . H C39 -.5840(5) -.1739(8) -.2436(5) .0610(19) Uani d . 1 . . C H39 -.5879 -.2381 -.1980 .073 Uiso calc R 1 . . H C40 -.5428(4) -.5204(7) -.3927(5) .0570(18) Uani d . 1 . . C C41 -.5594(5) -.5348(9) -.4825(5) .071(2) Uani d . 1 . . C H41 -.6140 -.4995 -.5176 .085 Uiso calc R 1 . . H C42 -.4960(6) -.6009(11) -.5211(7) .089(3) Uani d . 1 . . C H42 -.5083 -.6127 -.5809 .107 Uiso calc R 1 . . H C43 -.4160(6) -.6473(11) -.4679(8) .091(3) Uani d . 1 . . C H43 -.3727 -.6904 -.4923 .109 Uiso calc R 1 . . H C44 -.3968(6) -.6327(12) -.3801(8) .095(3) Uani d . 1 . . C H44 -.3408 -.6632 -.3457 .114 Uiso calc R 1 . . H C45 -.4618(5) -.5716(9) -.3418(6) .075(2) Uani d . 1 . . C H45 -.4500 -.5658 -.2817 .090 Uiso calc R 1 . . H C98 -1.0181(7) -.4915(14) -.5388(7) .103(3) Uani d . 1 . . C C99 -.9645(6) -.3658(13) -.5603(6) .084(3) Uani d . 1 . . C N99 -.9239(7) -.2692(11) -.5813(8) .122(4) Uani d . 1 . . N O99 -.6897(4) -.7247(7) -.1543(3) .0827(16) Uani d . 1 . . O H99O -.6751 -.6597 -.1804 .124 Uiso d R 1 . . H H99P -.7357 -.7767 -.1833 .124 Uiso d R 1 . . H 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 P1 .0525(8) .0398(7) .0331(8) -.0046(7) .0093(7) -.0009(6) P2 .0561(9) .0514(9) .0383(9) -.0073(8) .0108(7) -.0018(7) P3 .0556(9) .0382(8) .0675(12) -.0049(7) .0133(8) -.0012(8) O1 .071(3) .050(2) .037(2) -.009(2) .001(2) -.0115(19) O2 .095(4) .087(4) .081(4) -.050(3) .043(3) -.036(3) O3 .081(3) .048(3) .061(3) -.010(2) .010(3) .011(2) C1 .046(3) .045(3) .034(3) .004(2) .015(3) .010(2) C2 .056(4) .049(3) .031(3) .001(3) .014(3) .001(3) C3 .051(3) .052(3) .035(3) .006(3) .012(3) .010(3) C4 .052(3) .045(3) .047(4) .005(3) .010(3) .012(3) C5 .041(3) .040(3) .049(4) -.006(2) .005(3) -.001(3) C6 .052(3) .039(3) .048(4) -.009(3) .015(3) -.005(3) C7 .048(3) .041(3) .051(4) .000(2) .014(3) .016(3) C8 .054(4) .074(4) .031(3) .007(3) .006(3) .015(3) C9 .052(3) .043(3) .058(4) -.003(3) .012(3) -.002(3) C10 .048(3) .046(3) .025(3) .000(3) .009(2) .008(2) C11 .064(5) .053(4) .139(9) -.005(4) .015(5) .032(5) C12 .087(6) .052(5) .191(13) -.014(5) -.012(7) .045(6) C13 .089(6) .049(4) .082(6) .003(4) .027(5) .019(4) C14 .088(6) .068(5) .057(5) .010(4) .005(4) .019(4) C15 .068(5) .079(5) .058(5) -.016(4) -.009(4) .033(4) C16 .051(3) .045(3) .038(3) .000(3) .017(3) .004(3) C17 .073(5) .058(4) .078(6) .007(4) .024(4) -.011(4) C18 .068(5) .107(7) .105(8) .035(5) .017(5) -.010(6) C19 .066(5) .104(7) .075(6) .010(5) -.006(5) -.005(5) C20 .076(6) .116(8) .077(6) .014(5) -.006(5) -.014(6) C21 .062(4) .073(5) .046(4) .005(3) -.004(3) -.021(3) C22 .061(4) .082(5) .026(3) .015(4) -.002(3) -.006(3) C23 .073(6) .164(11) .067(6) .046(6) -.010(5) -.037(6) C24 .136(12) .26(2) .076(8) .136(15) -.034(8) -.045(13) C25 .31(3) .174(17) .048(7) .16(2) .015(13) .012(9) C26 .281(19) .081(7) .059(6) .058(10) .075(10) .039(5) C27 .114(7) .049(4) .061(5) .000(4) .022(5) .010(3) C28 .061(4) .050(3) .042(3) .002(3) .015(3) .010(3) C29 .078(5) .080(5) .061(5) -.013(4) .019(4) .016(4) C30 .080(6) .117(7) .064(6) -.003(5) .018(5) .037(5) C31 .080(6) .141(8) .045(4) .007(6) .013(4) .034(5) C32 .094(7) .165(11) .064(6) -.039(7) -.010(5) .010(7) C33 .089(6) .145(9) .035(4) -.047(6) -.010(4) .028(5) C34 .048(4) .036(3) .088(5) -.007(3) .010(4) -.009(3) C35 .082(5) .048(4) .095(6) -.013(4) .040(5) -.001(4) C36 .101(7) .061(5) .105(7) -.008(5) .046(6) .007(5) C37 .072(5) .042(4) .135(9) -.007(4) .028(6) -.003(5) C38 .074(5) .051(4) .093(6) -.001(4) .011(5) -.018(4) C39 .065(4) .042(3) .059(4) -.006(3) -.013(4) .002(3) C40 .051(4) .031(3) .088(6) -.003(3) .018(4) -.001(3) C41 .057(4) .082(5) .077(5) .013(4) .024(4) .001(4) C42 .085(6) .092(6) .105(7) -.003(5) .050(6) -.022(5) C43 .070(6) .091(7) .119(9) .022(5) .037(6) .007(6) C44 .056(5) .102(7) .119(9) .017(5) .009(5) .013(6) C45 .053(4) .066(5) .094(6) -.001(4) -.001(4) .009(4) C98 .097(7) .123(9) .085(7) -.010(6) .020(6) .017(6) C99 .076(6) .095(7) .064(5) .029(5) -.011(4) -.028(5) N99 .114(8) .072(5) .160(10) .008(5) .000(7) .004(6) O99 .096(4) .090(4) .060(3) -.019(3) .015(3) .020(3) 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 P1 O1 . 1.496(4) no P1 C16 . 1.791(6) no P1 C10 . 1.796(6) no P1 C7 . 1.809(6) no P2 O2 . 1.486(5) no P2 C8 . 1.785(6) no P2 C22 . 1.787(7) no P2 C28 . 1.792(7) no P3 O3 . 1.492(5) no P3 C40 . 1.786(7) no P3 C34 . 1.801(6) no P3 C9 . 1.812(6) no C1 C2 . 1.392(8) no C1 C6 . 1.400(8) no C1 C7 . 1.496(7) no C2 C3 . 1.361(8) no C2 H2 . .9300 no C3 C4 . 1.395(9) no C3 C8 . 1.529(8) no C4 C5 . 1.374(9) no C4 H4 . .9300 no C5 C6 . 1.382(8) no C5 C9 . 1.529(8) no C6 H6 . .9300 no C7 H7A . .9700 no C7 H7B . .9700 no C8 H8A . .9700 no C8 H8B . .9700 no C9 H9A . .9700 no C9 H9B . .9700 no C10 C15 . 1.363(9) no C10 C11 . 1.385(9) no C11 C12 . 1.368(10) no C11 H11 . .9300 no C12 C13 . 1.333(12) no C12 H12 . .9300 no C13 C14 . 1.343(11) no C13 H13 . .9300 no C14 C15 . 1.384(10) no C14 H14 . .9300 no C15 H15 . .9300 no C16 C17 . 1.396(9) no C16 C21 . 1.405(9) no C17 C18 . 1.376(11) no C17 H17 . .9300 no C18 C19 . 1.395(12) no C18 H18 . .9300 no C19 C20 . 1.323(13) no C19 H19 . .9300 no C20 C21 . 1.382(11) no C20 H20 . .9300 no C21 H21 . .9300 no C22 C27 . 1.380(11) no C22 C23 . 1.381(11) no C23 C24 . 1.376(18) no C23 H23 . .9300 no C24 C25 . 1.33(3) no C24 H24 . .9300 no C25 C26 . 1.33(2) no C25 H25 . .9300 no C26 C27 . 1.384(13) no C26 H26 . .9300 no C27 H27 . .9300 no C28 C33 . 1.366(10) no C28 C29 . 1.371(9) no C29 C30 . 1.377(11) no C29 H29 . .9300 no C30 C31 . 1.347(12) no C30 H30 . .9300 no C31 C32 . 1.377(12) no C31 H31 . .9300 no C32 C33 . 1.421(11) no C32 H32 . .9300 no C33 H33 . .9300 no C34 C39 . 1.373(10) no C34 C35 . 1.397(10) no C35 C36 . 1.370(11) no C35 H35 . .9300 no C36 C37 . 1.379(13) no C36 H36 . .9300 no C37 C38 . 1.395(12) no C37 H37 . .9300 no C38 C39 . 1.386(10) no C38 H38 . .9300 no C39 H39 . .9300 no C40 C45 . 1.370(10) no C40 C41 . 1.396(10) no C41 C42 . 1.400(10) no C41 H41 . .9300 no C42 C43 . 1.360(13) no C42 H42 . .9300 no C43 C44 . 1.362(13) no C43 H43 . .9300 no C44 C45 . 1.402(12) no C44 H44 . .9300 no C45 H45 . .9300 no C98 C99 . 1.457(15) no C99 N99 . 1.142(13) no O99 H99O . .7674 no O99 H99P . .8627 no