#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200070.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_2200070 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first o94 _journal_page_last o95 _publ_section_title ; [4-(Diphenylphosphino)-9,9-dimethylxanthen-5-yl]diphenylphosphine oxide toluene solvate ; loop_ _publ_author_name 'Ellis, Dianne D.' 'Spek, Anthony L.' _chemical_formula_moiety 'C39 H32 O2 P2, 0.5C7 H8' _chemical_formula_sum 'C42.5 H36 O2 P2' _[local]_cod_chemical_formula_sum_orig 'C42.50 H36 O2 P2' _chemical_formula_iupac 'C39 H32 O2 P2, 0.5C7 H8' _chemical_formula_weight 640.15 _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 10.7700(11) _cell_length_b 11.1547(11) _cell_length_c 15.941(3) _cell_angle_alpha 91.088(11) _cell_angle_beta 102.471(11) _cell_angle_gamma 116.993(7) _cell_volume 1651.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 1.288 _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 P1 .20793(9) .94189(8) .29904(5) .0212(2) Uani d . 1 . . P P2 .30943(9) .70846(9) .09805(5) .0236(2) Uani d . 1 . . P O1 .4584(2) .8873(2) .26752(14) .0228(5) Uani d . 1 . . O O2 .1413(2) 1.0221(2) .32667(15) .0280(5) Uani d . 1 . . O C1 .5061(3) .9973(3) .3310(2) .0200(7) Uani d . 1 . . C C2 .3998(3) 1.0270(3) .3475(2) .0202(7) Uani d . 1 . . C C3 .4443(4) 1.1379(3) .4095(2) .0267(7) Uani d . 1 . . C H3 .3745 1.1607 .4218 .032 Uiso calc R 1 . . H C4 .5864(4) 1.2151(3) .4531(2) .0315(8) Uani d . 1 . . C H4 .6149 1.2913 .4943 .038 Uiso calc R 1 . . H C5 .6874(4) 1.1800(3) .4361(2) .0258(7) Uani d . 1 . . C H5 .7852 1.2316 .4675 .031 Uiso calc R 1 . . H C6 .6498(3) 1.0712(3) .3742(2) .0222(7) Uani d . 1 . . C C7 .5597(3) .8773(3) .2304(2) .0209(7) Uani d . 1 . . C C8 .5045(3) .7940(3) .1504(2) .0213(7) Uani d . 1 . . C C9 .6025(3) .7806(3) .1116(2) .0249(7) Uani d . 1 . . C H9 .5685 .7245 .0577 .030 Uiso calc R 1 . . H C10 .7480(4) .8478(3) .1505(2) .0284(8) Uani d . 1 . . C H10 .8136 .8388 .1227 .034 Uiso calc R 1 . . H C11 .7993(3) .9284(3) .2298(2) .0246(7) Uani d . 1 . . C H11 .8998 .9730 .2563 .030 Uiso calc R 1 . . H C12 .7058(3) .9452(3) .2715(2) .0202(7) Uani d . 1 . . C C13 .1818(3) .9226(3) .1839(2) .0229(7) Uani d . 1 . . C C14 .2784(4) 1.0227(3) .1462(2) .0299(8) Uani d . 1 . . C H14 .3655 1.0931 .1818 .036 Uiso calc R 1 . . H C15 .2483(4) 1.0203(4) .0572(2) .0350(9) Uani d . 1 . . C H15 .3143 1.0894 .0318 .042 Uiso calc R 1 . . H C16 .1231(4) .9180(4) .0053(2) .0337(8) Uani d . 1 . . C H16 .1027 .9168 -.0558 .040 Uiso calc R 1 . . H C17 .0266(4) .8166(4) .0419(2) .0308(8) Uani d . 1 . . C H17 -.0601 .7462 .0060 .037 Uiso calc R 1 . . H C18 .0571(3) .8184(3) .1308(2) .0255(7) Uani d . 1 . . C H18 -.0078 .7477 .1558 .031 Uiso calc R 1 . . H C19 .1290(3) .7746(3) .3319(2) .0236(7) Uani d . 1 . . C C20 .1798(4) .6817(3) .3275(2) .0283(8) Uani d . 1 . . C H20 .2609 .7036 .3046 .034 Uiso calc R 1 . . H C21 .1139(4) .5572(3) .3560(2) .0353(9) Uani d . 1 . . C H21 .1507 .4946 .3539 .042 Uiso calc R 1 . . H C22 -.0056(4) .5239(4) .3876(2) .0384(9) Uani d . 1 . . C H22 -.0513 .4382 .4070 .046 Uiso calc R 1 . . H C23 -.0586(4) .6143(4) .3910(2) .0422(10) Uani d . 1 . . C H23 -.1409 .5907 .4129 .051 Uiso calc R 1 . . H C24 .0068(4) .7398(4) .3629(2) .0336(8) Uani d . 1 . . C H24 -.0312 .8016 .3647 .040 Uiso calc R 1 . . H C25 .3134(3) .6801(3) -.0154(2) .0235(7) Uani d . 1 . . C C26 .3458(4) .7916(4) -.0607(2) .0325(8) Uani d . 1 . . C H26 .3677 .8767 -.0318 .039 Uiso calc R 1 . . H C27 .3466(4) .7801(4) -.1466(3) .0420(10) Uani d . 1 . . C H27 .3711 .8579 -.1760 .050 Uiso calc R 1 . . H C28 .3123(4) .6576(4) -.1906(2) .0445(10) Uani d . 1 . . C H28 .3112 .6501 -.2502 .053 Uiso calc R 1 . . H C29 .2795(5) .5460(4) -.1471(3) .0498(11) Uani d . 1 . . C H29 .2571 .4611 -.1766 .060 Uiso calc R 1 . . H C30 .2789(4) .5569(4) -.0599(2) .0379(9) Uani d . 1 . . C H30 .2545 .4790 -.0307 .045 Uiso calc R 1 . . H C31 .2556(4) .5393(3) .1322(2) .0269(8) Uani d . 1 . . C C32 .3418(5) .4774(4) .1485(3) .0473(11) Uani d . 1 . . C H32 .4360 .5216 .1397 .057 Uiso calc R 1 . . H C33 .2937(5) .3521(4) .1773(3) .0566(12) Uani d . 1 . . C H33 .3560 .3122 .1894 .068 Uiso calc R 1 . . H C34 .1571(5) .2844(4) .1887(2) .0475(11) Uani d . 1 . . C H34 .1244 .1980 .2084 .057 Uiso calc R 1 . . H C35 .0690(5) .3426(4) .1713(2) .0449(11) Uani d . 1 . . C H35 -.0260 .2962 .1787 .054 Uiso calc R 1 . . H C36 .1165(4) .4691(4) .1428(2) .0368(9) Uani d . 1 . . C H36 .0534 .5081 .1305 .044 Uiso calc R 1 . . H C43 .9075(4) 1.1511(4) .3689(3) .0451(11) Uani d . 1 . . C H43A .9766 1.1201 .3612 .068 Uiso calc R 1 . . H H43B .9406 1.2033 .4266 .068 Uiso calc R 1 . . H H43C .8996 1.2087 .3246 .068 Uiso calc R 1 . . H C44 .7747(5) .9380(4) .4297(2) .0411(10) Uani d . 1 . . C H44A .8470 .9107 .4228 .062 Uiso calc R 1 . . H H44B .6817 .8569 .4229 .062 Uiso calc R 1 . . H H44C .8046 .9887 .4875 .062 Uiso calc R 1 . . H C45 .7605(3) 1.0285(3) .3603(2) .0235(7) Uani d . 1 . . C C46 .4044(5) .4421(4) .4208(3) .0476(11) Uani d . 1 . . C H46 .3367 .4020 .3663 .057 Uiso calc R 1 . . H C47 .3631(5) .3993(4) .4959(3) .0476(11) Uani d . 1 . . C H47 .2686 .3288 .4918 .057 Uiso calc R 1 . . H C48 .5430(5) .5428(4) .4235(3) .0461(10) Uani d . 1 . . C C49 .5890(10) .5856(8) .3400(6) .050(2) Uani d P .50 . . C H49A .6910 .6533 .3544 .075 Uiso calc PR .50 . . H H49B .5309 .6249 .3083 .075 Uiso calc PR .50 . . H H49C .5746 .5061 .3038 .075 Uiso calc PR .50 . . 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 .0211(4) .0230(4) .0223(4) .0118(4) .0073(3) .0009(3) P2 .0225(5) .0237(4) .0243(5) .0105(4) .0062(4) -.0010(3) O1 .0190(11) .0203(11) .0270(12) .0065(9) .0086(9) -.0054(9) O2 .0279(13) .0322(13) .0292(13) .0187(11) .0074(10) -.0024(10) C1 .0247(17) .0153(15) .0196(16) .0081(13) .0077(13) .0028(12) C2 .0214(16) .0188(15) .0201(16) .0087(13) .0063(13) .0011(13) C3 .0273(18) .0277(18) .0265(18) .0142(15) .0071(15) -.0020(14) C4 .034(2) .0241(18) .033(2) .0122(16) .0054(16) -.0096(15) C5 .0232(17) .0241(17) .0222(17) .0064(14) .0018(14) -.0019(14) C6 .0250(17) .0226(17) .0205(16) .0110(14) .0088(13) .0054(13) C7 .0233(17) .0186(15) .0255(17) .0110(14) .0124(14) .0063(13) C8 .0204(16) .0209(16) .0239(17) .0107(14) .0053(13) .0048(13) C9 .0275(18) .0288(18) .0215(17) .0155(15) .0074(14) -.0008(14) C10 .0284(18) .0355(19) .0307(19) .0194(16) .0152(15) .0067(15) C11 .0215(17) .0286(18) .0255(18) .0127(15) .0070(14) .0064(14) C12 .0228(17) .0175(15) .0219(16) .0096(13) .0084(13) .0047(13) C13 .0245(17) .0243(17) .0262(17) .0149(14) .0106(14) .0023(14) C14 .0314(19) .0242(18) .0306(19) .0097(15) .0087(15) .0016(15) C15 .040(2) .0292(19) .033(2) .0116(17) .0139(17) .0097(16) C16 .042(2) .035(2) .0240(18) .0185(18) .0092(16) .0028(15) C17 .0282(19) .036(2) .0266(19) .0149(16) .0060(15) -.0007(15) C18 .0216(17) .0294(18) .0272(18) .0122(15) .0086(14) .0019(14) C19 .0247(17) .0269(17) .0164(16) .0112(14) .0022(13) -.0001(13) C20 .0310(19) .0258(18) .0273(18) .0114(15) .0101(15) .0020(14) C21 .047(2) .0246(18) .032(2) .0140(17) .0107(17) .0043(15) C22 .048(2) .0232(18) .0280(19) .0030(17) .0105(17) .0010(15) C23 .034(2) .042(2) .040(2) .0051(18) .0197(18) .0017(18) C24 .031(2) .032(2) .035(2) .0109(16) .0132(16) -.0028(16) C25 .0185(16) .0279(18) .0217(17) .0104(14) .0018(13) -.0003(14) C26 .036(2) .0316(19) .036(2) .0198(17) .0100(17) .0068(16) C27 .038(2) .050(2) .041(2) .021(2) .0131(18) .020(2) C28 .037(2) .061(3) .024(2) .013(2) .0093(17) .0047(19) C29 .056(3) .042(2) .036(2) .008(2) .017(2) -.0120(19) C30 .046(2) .0247(19) .032(2) .0054(17) .0158(18) -.0021(15) C31 .0288(18) .0269(18) .0214(17) .0107(15) .0050(14) -.0002(14) C32 .042(2) .031(2) .073(3) .0167(19) .022(2) .023(2) C33 .053(3) .034(2) .078(3) .019(2) .010(2) .020(2) C34 .061(3) .030(2) .031(2) .006(2) .007(2) .0081(17) C35 .047(2) .034(2) .032(2) -.0021(19) .0176(19) -.0023(17) C36 .036(2) .031(2) .035(2) .0069(17) .0147(17) -.0052(16) C43 .0217(19) .043(2) .054(3) .0007(17) .0130(18) -.0219(19) C44 .058(3) .059(3) .0228(19) .043(2) .0051(18) .0027(18) C45 .0184(16) .0251(17) .0233(17) .0082(14) .0033(13) -.0023(13) C46 .066(3) .049(3) .036(2) .041(2) .000(2) -.0012(19) C47 .057(3) .041(2) .052(3) .030(2) .009(2) .003(2) C48 .063(3) .041(2) .049(3) .037(2) .013(2) .007(2) C49 .055(5) .036(5) .054(5) .019(4) .008(4) .002(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 P1 O2 . 1.488(2) y P1 C2 . 1.809(3) y P1 C13 . 1.790(3) y P1 C19 . 1.808(3) y P2 C8 . 1.848(3) y P2 C25 . 1.844(3) y P2 C31 . 1.837(3) y O1 C7 . 1.392(4) ? O1 C1 . 1.396(4) ? C1 C6 . 1.382(4) ? C1 C2 . 1.400(4) ? C2 C3 . 1.396(4) ? C3 C4 . 1.374(5) ? C3 H3 . .9500 ? C4 C5 . 1.386(5) ? C4 H4 . .9500 ? C5 C6 . 1.395(4) ? C5 H5 . .9500 ? C6 C45 . 1.524(4) ? C7 C12 . 1.390(4) ? C7 C8 . 1.403(4) ? C8 C9 . 1.393(4) ? C9 C10 . 1.378(5) ? C9 H9 . .9500 ? C10 C11 . 1.384(5) ? C10 H10 . .9500 ? C11 C12 . 1.395(4) ? C11 H11 . .9500 ? C12 C45 . 1.519(4) ? C13 C18 . 1.387(5) ? C13 C14 . 1.389(4) ? C14 C15 . 1.383(5) ? C14 H14 . .9500 ? C15 C16 . 1.374(5) ? C15 H15 . .9500 ? C16 C17 . 1.385(5) ? C16 H16 . .9500 ? C17 C18 . 1.382(5) ? C17 H17 . .9500 ? C18 H18 . .9500 ? C19 C20 . 1.382(5) ? C19 C24 . 1.397(5) ? C20 C21 . 1.381(5) ? C20 H20 . .9500 ? C21 C22 . 1.379(5) ? C21 H21 . .9500 ? C22 C23 . 1.371(6) ? C22 H22 . .9500 ? C23 C24 . 1.386(5) ? C23 H23 . .9500 ? C24 H24 . .9500 ? C25 C30 . 1.383(5) ? C25 C26 . 1.392(5) ? C26 C27 . 1.376(5) ? C26 H26 . .9500 ? C27 C28 . 1.373(6) ? C27 H27 . .9500 ? C28 C29 . 1.377(6) ? C28 H28 . .9500 ? C29 C30 . 1.395(5) ? C29 H29 . .9500 ? C30 H30 . .9500 ? C31 C32 . 1.375(5) ? C31 C36 . 1.392(5) ? C32 C33 . 1.380(5) ? C32 H32 . .9500 ? C33 C34 . 1.371(6) ? C33 H33 . .9500 ? C34 C35 . 1.360(6) ? C34 H34 . .9500 ? C35 C36 . 1.388(5) ? C35 H35 . .9500 ? C36 H36 . .9500 ? C43 C45 . 1.526(5) ? C43 H43A . .9800 ? C43 H43B . .9800 ? C43 H43C . .9800 ? C44 C45 . 1.542(5) ? C44 H44A . .9800 ? C44 H44B . .9800 ? C44 H44C . .9800 ? C46 C47 . 1.384(6) ? C46 C48 . 1.393(6) ? C46 H46 . .9500 ? C47 C48 2_666 1.380(6) ? C47 H47 . .9500 ? C48 C47 2_666 1.380(6) ? C48 C49 . 1.530(9) ? C49 H49A . .9800 ? C49 H49B . .9800 ? C49 H49C . .9800 ? _cod_database_code 2200070