#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008475.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_2008475 _journal_name_full 'Acta Crystallographica' _journal_year 1999 _journal_volume C55 _journal_page_first 733 _journal_page_last 739 _publ_section_title ; Salts of the bis(catecholato)borate anion with rhodium and iridium phosphine complex cations ; loop_ _publ_author_name 'Clegg, William' 'Elsegood, Mark R.J.' 'Scott, Andrew J.' 'Marder, Todd B.' 'Dai, Chaoyang' 'Norman, Nicholas C.' 'Pickett, Nigel L.' 'Robins, Edward G.' _chemical_formula_moiety '[RhClH(C26 H24 P2 )2] +, C12 H8 B O4 -, C H2 Cl2' _chemical_formula_sum 'C65 H59 B Cl3 O4 P4 Rh' _chemical_formula_weight 1248.07 _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 12.5401(8) _cell_length_b 13.5374(9) _cell_length_c 16.9310(11) _cell_angle_alpha 91.937(2) _cell_angle_beta 97.051(2) _cell_angle_gamma 90.121(2) _cell_volume 2850.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _exptl_crystal_density_diffrn 1.454 _diffrn_ambient_temperature 160(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 Rh .68697(2) .694003(19) .690983(15) .01995(7) Uani d . 1 . . Rh H1 .730(4) .757(4) .769(3) .076(17) Uiso d . 1 . . H Cl1 .62973(8) .59474(7) .56663(5) .0325(2) Uani d . 1 . . Cl P1 .53283(7) .78850(6) .70387(5) .02212(18) Uani d . 1 . . P C1 .4549(3) .7797(2) .7873(2) .0245(7) Uani d . 1 . . C C2 .3431(3) .7746(3) .7759(2) .0337(8) Uani d . 1 . . C H2 .3059 .7729 .7235 .040 Uiso calc R 1 . . H C3 .2855(3) .7719(3) .8413(3) .0416(10) Uani d . 1 . . C H3 .2092 .7690 .8333 .050 Uiso calc R 1 . . H C4 .3391(4) .7736(3) .9176(2) .0409(10) Uani d . 1 . . C H4 .2996 .7711 .9618 .049 Uiso calc R 1 . . H C5 .4502(3) .7789(3) .9299(2) .0352(9) Uani d . 1 . . C H5 .4869 .7804 .9824 .042 Uiso calc R 1 . . H C6 .5075(3) .7820(3) .8646(2) .0281(8) Uani d . 1 . . C H6 .5837 .7857 .8729 .034 Uiso calc R 1 . . H C7 .4350(3) .7864(3) .6152(2) .0275(8) Uani d . 1 . . C C8 .3925(3) .8716(3) .5804(3) .0410(10) Uani d . 1 . . C H8 .4043 .9340 .6075 .049 Uiso calc R 1 . . H C9 .3325(4) .8649(4) .5056(3) .0564(14) Uani d . 1 . . C H9 .3038 .9233 .4819 .068 Uiso calc R 1 . . H C10 .3140(4) .7758(4) .4655(3) .0547(13) Uani d . 1 . . C H10 .2758 .7727 .4134 .066 Uiso calc R 1 . . H C11 .3512(3) .6908(4) .5014(2) .0462(11) Uani d . 1 . . C H11 .3364 .6284 .4749 .055 Uiso calc R 1 . . H C12 .4101(3) .6961(3) .5760(2) .0326(8) Uani d . 1 . . C H12 .4338 .6369 .6009 .039 Uiso calc R 1 . . H P2 .74306(8) .83816(6) .63184(5) .02432(19) Uani d . 1 . . P C13 .7370(3) .8442(3) .5235(2) .0326(9) Uani d . 1 . . C C14 .8148(4) .8902(3) .4854(3) .0446(11) Uani d . 1 . . C H14 .8794 .9141 .5152 .054 Uiso calc R 1 . . H C15 .7975(5) .9010(3) .4033(3) .0583(14) Uani d . 1 . . C H15 .8516 .9312 .3774 .070 Uiso calc R 1 . . H C16 .7040(5) .8691(3) .3591(3) .0563(14) Uani d . 1 . . C H16 .6933 .8778 .3033 .068 Uiso calc R 1 . . H C17 .6252(4) .8242(3) .3965(2) .0470(11) Uani d . 1 . . C H17 .5599 .8023 .3665 .056 Uiso calc R 1 . . H C18 .6424(4) .8114(3) .4782(2) .0384(9) Uani d . 1 . . C H18 .5888 .7799 .5036 .046 Uiso calc R 1 . . H C19 .8749(3) .8868(3) .6726(2) .0278(8) Uani d . 1 . . C C20 .8832(3) .9575(3) .7350(2) .0313(8) Uani d . 1 . . C H20 .8201 .9821 .7544 .038 Uiso calc R 1 . . H C21 .9831(3) .9920(3) .7689(2) .0375(9) Uani d . 1 . . C H21 .9879 1.0410 .8107 .045 Uiso calc R 1 . . H C22 1.0769(3) .9556(3) .7421(3) .0375(9) Uani d . 1 . . C H22 1.1453 .9787 .7658 .045 Uiso calc R 1 . . H C23 1.0683(3) .8852(3) .6803(3) .0382(9) Uani d . 1 . . C H23 1.1314 .8598 .6613 .046 Uiso calc R 1 . . H C24 .9690(3) .8519(3) .6462(2) .0331(8) Uani d . 1 . . C H24 .9646 .8040 .6036 .040 Uiso calc R 1 . . H C25 .5813(3) .9161(2) .7165(2) .0279(8) Uani d . 1 . . C H25A .5196 .9617 .7150 .033 Uiso calc R 1 . . H H25B .6256 .9255 .7688 .033 Uiso calc R 1 . . H C26 .6483(3) .9394(3) .6500(2) .0278(8) Uani d . 1 . . C H26A .6895 1.0012 .6644 .033 Uiso calc R 1 . . H H26B .5998 .9502 .6005 .033 Uiso calc R 1 . . H P3 .63654(7) .55579(6) .75816(5) .02017(18) Uani d . 1 . . P C27 .6590(3) .5608(3) .86679(19) .0232(7) Uani d . 1 . . C C28 .6211(3) .4849(3) .9096(2) .0311(8) Uani d . 1 . . C H28 .5815 .4315 .8824 .037 Uiso calc R 1 . . H C29 .6412(3) .4874(3) .9919(2) .0399(10) Uani d . 1 . . C H29 .6150 .4358 1.0210 .048 Uiso calc R 1 . . H C30 .6993(3) .5649(3) 1.0320(2) .0406(10) Uani d . 1 . . C H30 .7110 .5674 1.0885 .049 Uiso calc R 1 . . H C31 .7404(3) .6386(3) .9897(2) .0358(9) Uani d . 1 . . C H31 .7822 .6908 1.0170 .043 Uiso calc R 1 . . H C32 .7204(3) .6361(3) .9074(2) .0289(8) Uani d . 1 . . C H32 .7491 .6865 .8783 .035 Uiso calc R 1 . . H C33 .4978(3) .5132(2) .73518(19) .0230(7) Uani d . 1 . . C C34 .4201(3) .5424(3) .7833(2) .0257(7) Uani d . 1 . . C H34 .4405 .5817 .8303 .031 Uiso calc R 1 . . H C35 .3134(3) .5145(3) .7634(2) .0309(8) Uani d . 1 . . C H35 .2611 .5352 .7965 .037 Uiso calc R 1 . . H C36 .2830(3) .4567(3) .6957(2) .0360(9) Uani d . 1 . . C H36 .2100 .4372 .6824 .043 Uiso calc R 1 . . H C37 .3587(3) .4272(3) .6471(2) .0351(9) Uani d . 1 . . C H37 .3375 .3876 .6004 .042 Uiso calc R 1 . . H C38 .4655(3) .4552(3) .6662(2) .0291(8) Uani d . 1 . . C H38 .5170 .4349 .6323 .035 Uiso calc R 1 . . H P4 .84691(7) .60425(6) .69546(5) .02145(18) Uani d . 1 . . P C39 .9327(3) .6132(3) .7901(2) .0251(7) Uani d . 1 . . C C40 .9759(3) .5293(3) .8274(2) .0358(9) Uani d . 1 . . C H40 .9601 .4657 .8033 .043 Uiso calc R 1 . . H C41 1.0415(3) .5381(3) .8993(3) .0433(10) Uani d . 1 . . C H41 1.0704 .4806 .9242 .052 Uiso calc R 1 . . H C42 1.0652(3) .6298(3) .9349(2) .0409(10) Uani d . 1 . . C H42 1.1109 .6355 .9840 .049 Uiso calc R 1 . . H C43 1.0225(3) .7132(3) .8992(2) .0378(9) Uani d . 1 . . C H43 1.0381 .7764 .9240 .045 Uiso calc R 1 . . H C44 .9566(3) .7052(3) .8270(2) .0315(8) Uani d . 1 . . C H44 .9276 .7632 .8027 .038 Uiso calc R 1 . . H C45 .9388(3) .6158(2) .6204(2) .0248(7) Uani d . 1 . . C C46 1.0497(3) .6176(3) .6409(2) .0318(8) Uani d . 1 . . C H46 1.0793 .6109 .6949 .038 Uiso calc R 1 . . H C47 1.1171(3) .6291(3) .5827(2) .0383(9) Uani d . 1 . . C H47 1.1928 .6307 .5970 .046 Uiso calc R 1 . . H C48 1.0746(3) .6381(3) .5044(2) .0372(9) Uani d . 1 . . C H48 1.1211 .6466 .4648 .045 Uiso calc R 1 . . H C49 .9642(3) .6349(3) .4831(2) .0368(9) Uani d . 1 . . C H49 .9353 .6403 .4289 .044 Uiso calc R 1 . . H C50 .8958(3) .6239(3) .5410(2) .0306(8) Uani d . 1 . . C H50 .8202 .6218 .5265 .037 Uiso calc R 1 . . H C51 .7202(3) .4484(2) .7340(2) .0270(7) Uani d . 1 . . C H51A .7555 .4215 .7841 .032 Uiso calc R 1 . . H H51B .6729 .3960 .7064 .032 Uiso calc R 1 . . H C52 .8061(3) .4747(2) .6813(2) .0247(7) Uani d . 1 . . C H52A .7778 .4614 .6248 .030 Uiso calc R 1 . . H H52B .8697 .4322 .6942 .030 Uiso calc R 1 . . H B .7080(4) 1.1984(3) .8069(3) .0303(9) Uani d . 1 . . B O1 .6689(2) 1.10200(18) .83114(16) .0344(6) Uani d . 1 . . O O2 .6115(2) 1.26228(18) .79989(16) .0347(6) Uani d . 1 . . O C53 .5659(3) 1.1159(3) .8471(2) .0304(8) Uani d . 1 . . C C54 .5316(3) 1.2105(3) .8272(2) .0301(8) Uani d . 1 . . C C55 .4291(3) 1.2410(3) .8360(2) .0392(9) Uani d . 1 . . C H55 .4055 1.3055 .8222 .047 Uiso calc R 1 . . H C56 .3610(4) 1.1733(3) .8660(3) .0455(11) Uani d . 1 . . C H56 .2891 1.1916 .8715 .055 Uiso calc R 1 . . H C57 .3963(4) 1.0811(3) .8875(3) .0459(11) Uani d . 1 . . C H57 .3490 1.0374 .9091 .055 Uiso calc R 1 . . H C58 .5004(4) 1.0500(3) .8782(2) .0401(10) Uani d . 1 . . C H58 .5248 .9860 .8929 .048 Uiso calc R 1 . . H O3 .7958(2) 1.2371(2) .86601(15) .0352(6) Uani d . 1 . . O O4 .7558(2) 1.18967(19) .73095(15) .0326(6) Uani d . 1 . . O C59 .8850(3) 1.2447(3) .8279(2) .0310(8) Uani d . 1 . . C C60 .8608(3) 1.2175(3) .7476(2) .0286(8) Uani d . 1 . . C C61 .9381(3) 1.2204(3) .6963(2) .0363(9) Uani d . 1 . . C H61 .9214 1.2025 .6414 .044 Uiso calc R 1 . . H C62 1.0419(3) 1.2507(3) .7280(3) .0397(10) Uani d . 1 . . C H62 1.0967 1.2542 .6940 .048 Uiso calc R 1 . . H C63 1.0655(3) 1.2753(3) .8077(3) .0421(10) Uani d . 1 . . C H63 1.1368 1.2947 .8280 .051 Uiso calc R 1 . . H C64 .9871(3) 1.2723(3) .8598(3) .0390(9) Uani d . 1 . . C H64 1.0039 1.2888 .9149 .047 Uiso calc R 1 . . H C65 .8213(6) 1.0102(4) .9575(3) .0765(19) Uani d . 1 . . C H65A .7542 1.0489 .9492 .092 Uiso calc R 1 . . H H65B .8727 1.0386 .9244 .092 Uiso calc R 1 . . H Cl3 .79368(13) .89027(9) .92553(8) .0663(4) Uani d . 1 . . Cl Cl4 .87420(11) 1.02319(11) 1.05622(8) .0665(4) Uani d . 1 . . Cl 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 Rh .02483(14) .01736(13) .01884(13) .00243(10) .00661(10) .00354(9) Cl1 .0373(5) .0331(5) .0277(5) .0041(4) .0062(4) .0009(4) P1 .0255(4) .0196(4) .0226(4) .0035(3) .0074(3) .0030(3) C1 .0306(18) .0193(16) .0255(18) .0043(14) .0106(14) .0027(13) C2 .0296(19) .039(2) .034(2) .0049(16) .0092(16) .0037(17) C3 .034(2) .049(3) .046(3) .0059(18) .0176(19) .008(2) C4 .053(3) .038(2) .037(2) .0084(19) .026(2) .0057(18) C5 .053(2) .028(2) .0264(19) .0029(17) .0124(17) .0011(15) C6 .035(2) .0234(18) .0273(19) .0024(15) .0073(15) .0025(14) C7 .0265(18) .0325(19) .0250(18) .0069(15) .0083(14) .0064(15) C8 .041(2) .035(2) .048(3) .0073(18) .0036(19) .0150(19) C9 .040(3) .071(4) .059(3) .006(2) -.002(2) .039(3) C10 .036(2) .098(4) .029(2) -.004(3) -.0020(18) .023(3) C11 .037(2) .072(3) .029(2) -.004(2) .0044(18) -.006(2) C12 .032(2) .038(2) .0282(19) .0043(16) .0039(16) .0028(16) P2 .0324(5) .0185(4) .0243(4) .0023(4) .0112(4) .0048(3) C13 .054(2) .0200(17) .0271(19) .0079(16) .0168(17) .0068(14) C14 .066(3) .035(2) .037(2) -.003(2) .023(2) .0059(18) C15 .100(4) .043(3) .041(3) -.004(3) .042(3) .011(2) C16 .111(5) .034(2) .027(2) .002(3) .020(3) .0028(18) C17 .078(3) .035(2) .027(2) .004(2) .006(2) .0014(17) C18 .060(3) .028(2) .029(2) .0051(18) .0102(19) .0055(16) C19 .0333(19) .0214(17) .0307(19) -.0008(14) .0104(15) .0078(14) C20 .037(2) .0282(19) .030(2) .0049(16) .0084(16) .0075(15) C21 .051(2) .029(2) .033(2) .0015(18) .0034(18) .0024(16) C22 .036(2) .031(2) .045(2) -.0038(17) .0038(18) .0088(17) C23 .034(2) .029(2) .056(3) -.0021(16) .0193(19) .0080(18) C24 .040(2) .0212(18) .041(2) -.0006(16) .0181(18) .0038(15) C25 .037(2) .0195(17) .0290(19) .0010(15) .0113(15) -.0011(14) C26 .0326(19) .0208(17) .0317(19) .0057(14) .0097(15) .0054(14) P3 .0259(4) .0171(4) .0186(4) .0015(3) .0065(3) .0026(3) C27 .0249(17) .0263(17) .0192(16) .0042(14) .0045(13) .0041(13) C28 .035(2) .0299(19) .0287(19) -.0012(16) .0043(16) .0071(15) C29 .047(2) .042(2) .033(2) .0045(19) .0092(18) .0167(18) C30 .048(2) .055(3) .0187(18) .008(2) .0032(17) .0054(17) C31 .039(2) .042(2) .0255(19) -.0013(18) .0018(16) -.0029(16) C32 .0323(19) .0293(19) .0265(19) .0006(15) .0098(15) .0003(15) C33 .0296(18) .0211(16) .0185(16) .0018(14) .0025(13) .0065(13) C34 .0311(19) .0239(17) .0231(17) .0023(14) .0064(14) .0026(14) C35 .0255(18) .033(2) .036(2) .0037(15) .0066(15) .0082(16) C36 .031(2) .032(2) .043(2) -.0082(16) -.0059(17) .0098(17) C37 .045(2) .029(2) .029(2) -.0065(17) -.0042(17) .0016(15) C38 .038(2) .0245(18) .0259(18) -.0008(15) .0090(15) .0012(14) P4 .0266(4) .0191(4) .0201(4) .0025(3) .0087(3) .0017(3) C39 .0275(18) .0275(18) .0218(17) .0035(14) .0094(14) .0014(14) C40 .040(2) .031(2) .036(2) .0083(17) .0020(17) .0030(16) C41 .044(2) .046(3) .039(2) .007(2) -.0035(19) .0116(19) C42 .034(2) .062(3) .026(2) -.003(2) .0007(16) .0024(19) C43 .037(2) .045(2) .032(2) -.0056(18) .0064(17) -.0032(18) C44 .036(2) .031(2) .0288(19) -.0024(16) .0092(16) .0008(15) C45 .0337(19) .0176(16) .0251(18) .0024(14) .0111(15) .0012(13) C46 .035(2) .033(2) .029(2) .0041(16) .0110(16) .0058(15) C47 .037(2) .041(2) .040(2) .0032(18) .0187(18) .0059(18) C48 .044(2) .035(2) .038(2) -.0001(18) .0242(18) -.0006(17) C49 .051(3) .036(2) .0258(19) -.0026(18) .0152(18) -.0002(16) C50 .038(2) .0274(19) .0285(19) -.0016(15) .0116(16) .0006(15) C51 .0331(19) .0175(16) .0325(19) .0030(14) .0117(15) .0055(14) C52 .0325(19) .0173(16) .0260(18) .0043(14) .0107(14) .0007(13) B .034(2) .027(2) .031(2) .0016(17) .0068(18) .0040(17) O1 .0378(15) .0231(13) .0448(16) .0051(11) .0138(12) .0065(11) O2 .0386(15) .0229(13) .0445(16) .0035(11) .0108(12) .0085(11) C53 .038(2) .0236(18) .031(2) .0001(15) .0097(16) -.0023(15) C54 .037(2) .0255(18) .0283(19) .0002(15) .0053(16) -.0005(15) C55 .042(2) .039(2) .038(2) .0110(18) .0084(18) .0007(18) C56 .040(2) .055(3) .043(3) .004(2) .0147(19) -.009(2) C57 .051(3) .044(3) .047(3) -.011(2) .023(2) -.007(2) C58 .058(3) .0249(19) .041(2) -.0032(18) .020(2) -.0007(17) O3 .0387(15) .0385(15) .0289(14) -.0002(12) .0072(11) -.0026(11) O4 .0338(14) .0383(15) .0256(13) .0011(11) .0037(11) .0028(11) C59 .034(2) .0242(18) .035(2) .0045(15) .0053(16) .0039(15) C60 .0315(19) .0238(18) .0304(19) .0046(15) .0014(15) .0072(14) C61 .045(2) .035(2) .031(2) .0072(18) .0104(17) .0125(16) C62 .035(2) .036(2) .051(3) .0089(17) .0135(19) .0113(19) C63 .029(2) .042(2) .055(3) .0032(17) .0026(19) .001(2) C64 .038(2) .035(2) .043(2) .0017(17) .0016(18) -.0052(18) C65 .126(5) .048(3) .046(3) -.017(3) -.030(3) .005(2) Cl3 .0900(10) .0432(7) .0632(8) -.0076(6) .0035(7) -.0111(6) Cl4 .0667(8) .0862(10) .0436(7) -.0148(7) -.0015(6) -.0129(6) 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 Rh H1 . 1.59(5) yes Rh P4 . 2.3418(9) yes Rh P3 . 2.3473(9) yes Rh P1 . 2.3484(9) yes Rh P2 . 2.3675(9) yes Rh Cl1 . 2.4875(9) yes P1 C7 . 1.817(4) no P1 C1 . 1.820(3) no P1 C25 . 1.827(3) no C1 C6 . 1.390(5) no C1 C2 . 1.394(5) no C2 C3 . 1.395(5) no C3 C4 . 1.381(6) no C4 C5 . 1.384(6) no C5 C6 . 1.393(5) no C7 C12 . 1.388(5) no C7 C8 . 1.391(5) no C8 C9 . 1.391(6) no C9 C10 . 1.369(7) no C10 C11 . 1.376(7) no C11 C12 . 1.382(5) no P2 C19 . 1.824(4) no P2 C13 . 1.831(4) no P2 C26 . 1.858(3) no C13 C14 . 1.390(6) no C13 C18 . 1.394(6) no C14 C15 . 1.393(6) no C15 C16 . 1.372(8) no C16 C17 . 1.387(7) no C17 C18 . 1.391(5) no C19 C24 . 1.390(5) no C19 C20 . 1.397(5) no C20 C21 . 1.385(6) no C21 C22 . 1.396(6) no C22 C23 . 1.385(6) no C23 C24 . 1.375(6) no C25 C26 . 1.524(5) no P3 C33 . 1.823(4) no P3 C27 . 1.825(3) no P3 C51 . 1.858(3) no C27 C32 . 1.387(5) no C27 C28 . 1.393(5) no C28 C29 . 1.384(5) no C29 C30 . 1.386(6) no C30 C31 . 1.382(6) no C31 C32 . 1.385(5) no C33 C34 . 1.394(5) no C33 C38 . 1.403(5) no C34 C35 . 1.388(5) no C35 C36 . 1.380(5) no C36 C37 . 1.380(6) no C37 C38 . 1.388(5) no P4 C39 . 1.817(4) no P4 C52 . 1.826(3) no P4 C45 . 1.827(3) no C39 C44 . 1.390(5) no C39 C40 . 1.396(5) no C40 C41 . 1.385(6) no C41 C42 . 1.377(6) no C42 C43 . 1.377(6) no C43 C44 . 1.390(5) no C45 C46 . 1.392(5) no C45 C50 . 1.393(5) no C46 C47 . 1.387(5) no C47 C48 . 1.377(6) no C48 C49 . 1.388(6) no C49 C50 . 1.391(5) no C51 C52 . 1.529(5) no B O3 . 1.477(5) yes B O1 . 1.482(5) yes B O2 . 1.483(5) yes B O4 . 1.485(5) yes O1 C53 . 1.364(4) no O2 C54 . 1.358(4) no C53 C58 . 1.372(5) no C53 C54 . 1.390(5) no C54 C55 . 1.374(5) no C55 C56 . 1.401(6) no C56 C57 . 1.372(6) no C57 C58 . 1.398(6) no O3 C59 . 1.362(5) no O4 C60 . 1.361(4) no C59 C64 . 1.373(5) no C59 C60 . 1.394(5) no C60 C61 . 1.379(5) no C61 C62 . 1.401(6) no C62 C63 . 1.376(6) no C63 C64 . 1.400(6) no C65 Cl3 . 1.715(5) no C65 Cl4 . 1.723(5) no