#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006349.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_2006349 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 1039 _journal_page_last 1041 _publ_section_title ; Triphenyl[2-(triphenylsilyl)phenylthio]phosphonium Tetraoxorhenate(1--)-- Dichloromethane (1/1) ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Miller, John R.' 'Lu, Canzhong' 'Zheng, Yifan' _chemical_formula_moiety 'C42 H34 P1 S1 Si1 +, Re1 O4 -, C1 H2 Cl2' _chemical_formula_sum 'C43 H36 Cl2 P O4 Re S Si' _chemical_formula_structural '[((C6 H5)3 Si C6 H4 S2) P (C6 H5)3] + , [Re O4] - , C H2 Cl2' _chemical_formula_weight 964.94 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.055(3) _cell_length_b 22.575(4) _cell_length_c 18.227(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.359(12) _cell_angle_gamma 90.00 _cell_volume 4082.5(1.7) _cell_formula_units_Z 4 _cell_measurement_temperature 291.0(10) _exptl_crystal_density_diffrn 1.570 _diffrn_ambient_temperature 291(2) _refine_ls_R_factor_obs .0308 _refine_ls_wR_factor_obs .0760 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 Re .02264(2) .180564(9) .048058(12) .05540(9) Uani d . 1 . Re O1 .0928(4) .2497(2) .0553(2) .0795(12) Uani d . 1 . O O2 .0959(5) .1375(2) -.0104(3) .101(2) Uani d . 1 . O O3 .0513(6) .1500(3) .1344(3) .119(2) Uani d . 1 . O O4 -.1439(5) .1867(2) .0158(4) .147(3) Uani d . 1 . O S .39432(12) .10514(5) .20916(7) .0456(3) Uani d . 1 . S Si .34900(12) -.00213(5) .32485(7) .0377(3) Uani d . 1 . Si P .56027(11) .11848(5) .15682(7) .0397(3) Uani d . 1 . P C11 .3007(4) -.0082(2) .2207(2) .0362(9) Uani d . 1 . C C12 .3158(4) .0382(2) .1703(2) .0392(10) Uani d . 1 . C C13 .2633(5) .0344(3) .0950(3) .0489(12) Uani d . 1 . C C14 .2012(5) -.0165(3) .0663(3) .0537(13) Uani d . 1 . C C15 .1898(5) -.0637(3) .1129(3) .0539(13) Uani d . 1 . C C16 .2372(5) -.0590(2) .1887(3) .0476(12) Uani d . 1 . C C21 .2535(5) .0606(2) .3594(3) .0419(10) Uani d . 1 . C C22 .1591(5) .0946(2) .3133(3) .0486(12) Uani d . 1 . C C23 .0851(6) .1379(3) .3408(4) .065(2) Uani d . 1 . C C24 .1039(7) .1500(3) .4154(4) .073(2) Uani d . 1 . C C25 .1951(7) .1175(3) .4622(4) .076(2) Uani d . 1 . C C26 .2696(6) .0733(3) .4352(3) .0601(14) Uani d . 1 . C C31 .2923(5) -.0710(2) .3687(2) .0407(10) Uani d . 1 . C C32 .1552(5) -.0816(2) .3678(3) .0524(12) Uani d . 1 . C C33 .1091(7) -.1294(3) .4030(3) .064(2) Uani d . 1 . C C34 .1976(8) -.1682(3) .4403(3) .070(2) Uani d . 1 . C C35 .3325(9) -.1598(3) .4432(3) .066(2) Uani d . 1 . C C36 .3805(6) -.1115(2) .4067(3) .0509(12) Uani d . 1 . C C41 .5371(4) .0040(2) .3505(2) .0401(10) Uani d . 1 . C C42 .6189(5) -.0329(3) .3151(3) .0590(14) Uani d . 1 . C C43 .7570(6) -.0314(3) .3328(4) .069(2) Uani d . 1 . C C44 .8174(6) .0062(3) .3859(4) .069(2) Uani d . 1 . C C45 .7404(6) .0431(3) .4217(3) .064(2) Uani d . 1 . C C46 .6017(5) .0420(2) .4037(3) .0512(12) Uani d . 1 . C C51 .6497(4) .1735(2) .2171(3) .0428(10) Uani d . 1 . C C52 .7093(6) .2208(2) .1884(3) .0599(14) Uani d . 1 . C C53 .7781(7) .2630(3) .2353(4) .076(2) Uani d . 1 . C C54 .7881(7) .2563(3) .3106(4) .067(2) Uani d . 1 . C C55 .7327(7) .2091(3) .3392(4) .072(2) Uani d . 1 . C C56 .6642(6) .1669(3) .2939(3) .066(2) Uani d . 1 . C C61 .6652(4) .0554(2) .1503(3) .0432(11) Uani d . 1 . C C62 .6158(5) .0031(2) .1170(3) .0561(13) Uani d . 1 . C C63 .7021(6) -.0427(3) .1089(3) .0601(14) Uani d . 1 . C C64 .8381(6) -.0371(3) .1320(3) .0607(15) Uani d . 1 . C C65 .8880(6) .0147(3) .1629(4) .071(2) Uani d . 1 . C C66 .8039(5) .0613(3) .1732(3) .0619(15) Uani d . 1 . C C71 .5105(4) .1498(2) .0664(2) .0450(11) Uani d . 1 . C C72 .5803(6) .1363(3) .0087(3) .0616(14) Uani d . 1 . C C73 .5484(7) .1659(4) -.0586(4) .078(2) Uani d . 1 . C C74 .4493(6) .2090(3) -.0686(3) .072(2) Uani d . 1 . C C75 .3807(6) .2205(3) -.0127(4) .070(2) Uani d . 1 . C C76 .4094(5) .1924(2) .0553(3) .0568(13) Uani d . 1 . C C77 .2102(10) .2277(4) .7297(5) .138(4) Uani d . 1 . C H77A .2117 .2688 .7455 .166 Uiso calc R 1 . H H77B .1521 .2252 .6818 .166 Uiso calc R 1 . H Cl1 .3712(3) .20726(14) .7189(2) .1465(10) Uani d . 1 . Cl Cl2 .1428(3) .18622(13) .7917(2) .1501(11) Uani d . 1 . Cl H13 .271(4) .0625(19) .068(2) .029(12) Uiso d . 1 . H H14 .162(5) -.018(2) .022(3) .053(15) Uiso d . 1 . H H15 .154(5) -.098(2) .098(3) .051(14) Uiso d . 1 . H H16 .229(4) -.0876(19) .216(2) .031(12) Uiso d . 1 . H H22 .142(5) .089(2) .266(3) .050(15) Uiso d . 1 . H H23 .027(6) .159(3) .312(3) .060(17) Uiso d . 1 . H H24 .066(7) .179(3) .428(4) .08(2) Uiso d . 1 . H H25 .212(6) .128(3) .508(4) .09(2) Uiso d . 1 . H H26 .320(5) .052(2) .467(3) .064(18) Uiso d . 1 . H H32 .091(5) -.058(2) .343(3) .046(14) Uiso d . 1 . H H33 .025(7) -.135(3) .397(4) .09(2) Uiso d . 1 . H H34 .177(7) -.200(3) .463(4) .10(2) Uiso d . 1 . H H35 .396(8) -.180(3) .455(4) .09(3) Uiso d . 1 . H H36 .466(4) -.1059(19) .408(2) .035(12) Uiso d . 1 . H H42 .583(6) -.057(3) .284(3) .069(19) Uiso d . 1 . H H43 .797(6) -.058(3) .312(3) .08(2) Uiso d . 1 . H H44 .903(6) .007(3) .398(3) .072(18) Uiso d . 1 . H H45 .776(5) .065(2) .455(3) .055(16) Uiso d . 1 . H H46 .554(5) .069(3) .425(3) .065(17) Uiso d . 1 . H H52 .699(7) .226(3) .128(4) .11(2) Uiso d . 1 . H H53 .827(7) .297(3) .214(4) .10(2) Uiso d . 1 . H H54 .835(5) .280(2) .337(3) .043(14) Uiso d . 1 . H H55 .736(7) .207(3) .382(4) .09(2) Uiso d . 1 . H H56 .624(6) .132(3) .319(3) .09(2) Uiso d . 1 . H H62 .529(5) .002(2) .106(3) .047(13) Uiso d . 1 . H H63 .674(6) -.077(3) .092(4) .09(2) Uiso d . 1 . H H64 .895(5) -.065(2) .126(3) .059(15) Uiso d . 1 . H H65 .969(6) .020(3) .178(3) .075(19) Uiso d . 1 . H H66 .842(6) .096(3) .197(3) .078(18) Uiso d . 1 . H H72 .638(6) .104(3) .013(3) .069(17) Uiso d . 1 . H H73 .590(6) .157(3) -.090(3) .063(18) Uiso d . 1 . H H74 .429(6) .228(3) -.112(4) .09(2) Uiso d . 1 . H H75 .321(5) .250(2) -.019(3) .058(15) Uiso d . 1 . H H76 .363(5) .197(2) .099(3) .063(15) Uiso d . 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 Re .05273(13) .05018(13) .06062(14) .00222(11) .00117(9) -.00875(11) O1 .089(3) .063(3) .089(3) -.005(2) .020(2) -.004(2) O2 .113(4) .083(3) .105(4) .017(3) .013(3) -.030(3) O3 .165(5) .106(4) .093(4) -.003(4) .038(4) .022(3) O4 .067(3) .119(5) .234(8) .017(3) -.041(4) -.078(5) S .0492(6) .0407(6) .0508(7) -.0035(5) .0193(5) .0012(5) Si .0438(7) .0344(6) .0361(7) -.0006(5) .0104(5) -.0012(5) P .0397(6) .0376(6) .0434(6) -.0009(5) .0115(5) .0031(5) C11 .035(2) .036(2) .039(2) .004(2) .008(2) -.002(2) C12 .036(2) .042(2) .041(3) .004(2) .013(2) .001(2) C13 .049(3) .055(3) .043(3) .006(2) .009(2) .011(3) C14 .046(3) .074(4) .041(3) .003(3) .005(2) -.008(3) C15 .057(3) .055(3) .050(3) -.009(3) .009(2) -.016(3) C16 .060(3) .038(3) .045(3) -.002(2) .011(2) -.003(2) C21 .049(3) .034(2) .046(3) -.004(2) .019(2) -.001(2) C22 .045(3) .047(3) .056(3) .001(2) .015(2) -.006(3) C23 .055(3) .059(4) .083(5) .014(3) .018(3) -.003(3) C24 .080(4) .058(4) .087(5) .012(3) .033(4) -.021(4) C25 .097(5) .079(5) .057(4) .003(4) .032(4) -.018(4) C26 .078(4) .057(3) .048(3) .009(3) .020(3) .001(3) C31 .054(3) .034(2) .035(2) -.001(2) .009(2) -.002(2) C32 .054(3) .053(3) .052(3) .000(3) .011(2) -.001(2) C33 .071(4) .066(4) .058(3) -.024(3) .018(3) -.004(3) C34 .117(6) .045(4) .052(3) -.027(4) .029(4) -.006(3) C35 .105(5) .042(3) .052(3) .009(4) .010(3) .005(3) C36 .059(3) .047(3) .048(3) -.002(3) .012(2) -.002(2) C41 .045(2) .043(3) .033(2) -.002(2) .007(2) .006(2) C42 .052(3) .070(4) .056(3) -.001(3) .013(3) -.014(3) C43 .051(3) .087(5) .071(4) .010(3) .013(3) -.010(4) C44 .042(3) .092(5) .071(4) -.003(3) .003(3) .002(4) C45 .060(3) .069(4) .057(3) -.014(3) -.010(3) -.003(3) C46 .058(3) .051(3) .044(3) .001(3) .005(2) -.002(2) C51 .045(2) .040(3) .044(3) .003(2) .011(2) .004(2) C52 .080(4) .048(3) .052(3) -.018(3) .012(3) .007(3) C53 .102(5) .056(4) .068(4) -.032(3) .007(3) .002(3) C54 .077(4) .057(4) .063(4) -.008(3) -.002(3) -.012(3) C55 .081(4) .091(5) .044(4) -.014(4) .005(3) -.001(3) C56 .079(4) .069(4) .049(3) -.022(3) .007(3) .007(3) C61 .042(2) .043(3) .046(3) .002(2) .013(2) .003(2) C62 .040(3) .058(3) .071(4) .000(2) .012(2) -.012(3) C63 .064(4) .047(3) .073(4) -.004(3) .023(3) -.011(3) C64 .062(3) .050(3) .075(4) .015(3) .024(3) -.003(3) C65 .044(3) .066(4) .102(5) .008(3) .009(3) -.022(3) C66 .050(3) .055(3) .079(4) .002(3) .005(3) -.013(3) C71 .043(2) .046(3) .045(3) -.004(2) .001(2) .000(2) C72 .058(3) .076(4) .054(3) .006(3) .018(3) .010(3) C73 .070(4) .115(6) .051(4) -.007(4) .022(3) .011(4) C74 .066(4) .103(5) .043(3) -.023(4) .001(3) .020(3) C75 .057(3) .075(4) .074(4) .009(3) .001(3) .017(3) C76 .058(3) .063(4) .050(3) .005(3) .009(2) .006(3) C77 .172(10) .115(7) .119(7) .022(7) -.003(7) .051(6) Cl1 .177(3) .151(2) .118(2) .007(2) .044(2) .022(2) Cl2 .104(2) .159(2) .179(3) -.006(2) -.002(2) .071(2) 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 Re O4 . 1.688(5) yes Re O2 . 1.697(4) yes Re O3 . 1.699(5) yes Re O1 . 1.709(4) yes S P . 2.074(2) yes S C12 . 1.797(5) yes P C61 . 1.787(4) yes P C71 . 1.788(5) yes P C51 . 1.800(5) yes Si C21 . 1.877(4) yes Si C41 . 1.878(4) yes Si C31 . 1.879(4) yes Si C11 . 1.887(4) yes C11 C16 . 1.394(6) ? C11 C12 . 1.417(6) ? C12 C13 . 1.390(6) ? C13 C14 . 1.370(7) ? C13 H13 . .82(4) ? C14 C15 . 1.379(8) ? C14 H14 . .85(5) ? C15 C16 . 1.389(7) ? C15 H15 . .88(5) ? C16 H16 . .82(4) ? C21 C22 . 1.392(7) ? C21 C26 . 1.395(7) ? C22 C23 . 1.372(7) ? C22 H22 . .85(5) ? C23 C24 . 1.369(9) ? C23 H23 . .86(5) ? C24 C25 . 1.360(9) ? C24 H24 . .80(6) ? C25 C26 . 1.385(8) ? C25 H25 . .86(6) ? C26 H26 . .86(5) ? C31 C36 . 1.380(7) ? C31 C32 . 1.397(7) ? C32 C33 . 1.374(8) ? C32 H32 . .90(5) ? C33 C34 . 1.350(9) ? C33 H33 . .84(6) ? C34 C35 . 1.362(10) ? C34 H34 . .86(7) ? C35 C36 . 1.404(8) ? C35 H35 . .79(7) ? C36 H36 . .86(4) ? C41 C46 . 1.377(7) ? C41 C42 . 1.399(7) ? C42 C43 . 1.374(8) ? C42 H42 . .83(6) ? C43 C44 . 1.354(9) ? C43 H43 . .85(6) ? C44 C45 . 1.372(9) ? C44 H44 . .85(6) ? C45 C46 . 1.380(8) ? C45 H45 . .82(5) ? C46 H46 . .90(5) ? C51 C52 . 1.371(6) ? C51 C56 . 1.391(7) ? C52 C53 . 1.387(8) ? C52 H52 . 1.10(7) ? C53 C54 . 1.370(8) ? C53 H53 . 1.03(7) ? C54 C55 . 1.347(9) ? C54 H54 . .81(5) ? C55 C56 . 1.370(9) ? C55 H55 . .78(6) ? C56 H56 . 1.03(6) ? C61 C62 . 1.384(7) ? C61 C66 . 1.395(7) ? C62 C63 . 1.373(7) ? C62 H62 . .86(5) ? C63 C64 . 1.370(8) ? C63 H63 . .87(6) ? C64 C65 . 1.357(8) ? C64 H64 . .87(5) ? C65 C66 . 1.383(8) ? C65 H65 . .82(6) ? C66 H66 . .94(6) ? C71 C72 . 1.390(7) ? C71 C76 . 1.390(7) ? C72 C73 . 1.387(8) ? C72 H72 . .92(6) ? C73 C74 . 1.384(10) ? C73 H73 . .79(5) ? C74 C75 . 1.347(9) ? C74 H74 . .90(6) ? C75 C76 . 1.380(8) ? C75 H75 . .90(5) ? C76 H76 . .99(5) ? C77 Cl2 . 1.692(9) yes C77 Cl1 . 1.726(10) yes C77 H77A . .97 ? C77 H77B . .97 ?