#------------------------------------------------------------------------------ #$Date: 2008-11-20 19:58:43 +0000 (Thu, 20 Nov 2008) $ #$Revision: 481 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008477.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_2008477 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1999 _journal_volume 55 _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 '[Rh(C3 H9 P)4 ] +, C12 H8 B O4 -' _chemical_formula_sum 'C24 H44 B O4 P4 Rh' _chemical_formula_weight 634.19 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7315(9) _cell_length_b 29.559(3) _cell_length_c 10.8716(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.541(2) _cell_angle_gamma 90.00 _cell_volume 3052.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _exptl_crystal_density_diffrn 1.380 _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 .42773(2) .107004(7) .06683(2) .02030(7) Uani d . 1 . . Rh P1 .39257(8) .15620(3) -.10186(7) .02619(18) Uani d . 1 . . P C1 .4492(4) .21367(11) -.0596(3) .0418(9) Uani d . 1 . . C H1A .5523 .2151 -.0411 .063 Uiso calc R 1 . . H H1B .4151 .2230 .0150 .063 Uiso calc R 1 . . H H1C .4108 .2340 -.1299 .063 Uiso calc R 1 . . H C2 .4607(4) .14796(13) -.2443(3) .0437(9) Uani d . 1 . . C H2A .4283 .1188 -.2825 .066 Uiso calc R 1 . . H H2B .5639 .1484 -.2224 .066 Uiso calc R 1 . . H H2C .4265 .1723 -.3044 .066 Uiso calc R 1 . . H C3 .2058(3) .16666(11) -.1649(3) .0341(7) Uani d . 1 . . C H3A .1583 .1715 -.0952 .051 Uiso calc R 1 . . H H3B .1641 .1405 -.2146 .051 Uiso calc R 1 . . H H3C .1948 .1936 -.2187 .051 Uiso calc R 1 . . H P2 .39223(8) .08559(3) .26064(7) .02512(17) Uani d . 1 . . P C4 .4666(3) .03536(11) .3500(3) .0361(8) Uani d . 1 . . C H4A .4377 .0082 .2993 .054 Uiso calc R 1 . . H H4B .4322 .0336 .4282 .054 Uiso calc R 1 . . H H4C .5695 .0375 .3703 .054 Uiso calc R 1 . . H C5 .2056(3) .07970(11) .2614(3) .0351(7) Uani d . 1 . . C H5A .1681 .0526 .2140 .053 Uiso calc R 1 . . H H5B .1544 .1064 .2220 .053 Uiso calc R 1 . . H H5C .1942 .0770 .3484 .053 Uiso calc R 1 . . H C6 .4416(3) .12955(11) .3802(3) .0368(8) Uani d . 1 . . C H6A .4068 .1589 .3446 .055 Uiso calc R 1 . . H H6B .5444 .1306 .4077 .055 Uiso calc R 1 . . H H6C .4001 .1227 .4526 .055 Uiso calc R 1 . . H P3 .64992(8) .13495(3) .15020(8) .02654(18) Uani d . 1 . . P C7 .7616(3) .13842(11) .0352(3) .0387(8) Uani d . 1 . . C H7A .7552 .1101 -.0123 .058 Uiso calc R 1 . . H H7B .8594 .1435 .0793 .058 Uiso calc R 1 . . H H7C .7300 .1635 -.0229 .058 Uiso calc R 1 . . H C8 .6848(3) .18958(11) .2304(4) .0415(9) Uani d . 1 . . C H8A .6312 .1917 .2968 .062 Uiso calc R 1 . . H H8B .6564 .2141 .1695 .062 Uiso calc R 1 . . H H8C .7856 .1922 .2680 .062 Uiso calc R 1 . . H C9 .7590(3) .09676(10) .2634(3) .0326(7) Uani d . 1 . . C H9A .7540 .0662 .2280 .049 Uiso calc R 1 . . H H9B .7246 .0964 .3417 .049 Uiso calc R 1 . . H H9C .8568 .1073 .2812 .049 Uiso calc R 1 . . H P4 .26658(8) .05619(3) -.03910(7) .02582(17) Uani d . 1 . . P C10 .2858(3) -.00139(10) .0248(3) .0371(8) Uani d . 1 . . C H10A .2672 -.0014 .1098 .056 Uiso calc R 1 . . H H10B .3819 -.0121 .0283 .056 Uiso calc R 1 . . H H10C .2187 -.0214 -.0296 .056 Uiso calc R 1 . . H C11 .0752(3) .06267(12) -.0669(3) .0382(8) Uani d . 1 . . C H11A .0479 .0683 .0133 .057 Uiso calc R 1 . . H H11B .0296 .0349 -.1051 .057 Uiso calc R 1 . . H H11C .0456 .0882 -.1240 .057 Uiso calc R 1 . . H C12 .2886(3) .04377(12) -.1983(3) .0371(8) Uani d . 1 . . C H12A .3878 .0372 -.1960 .056 Uiso calc R 1 . . H H12B .2587 .0700 -.2528 .056 Uiso calc R 1 . . H H12C .2310 .0175 -.2315 .056 Uiso calc R 1 . . H B 1.0733(4) .16617(12) -.5108(3) .0280(7) Uani d . 1 . . B O1 .9496(2) .17554(7) -.45725(19) .0302(5) Uani d . 1 . . O O2 1.1069(2) .11760(7) -.48110(19) .0299(5) Uani d . 1 . . O C13 .9029(3) .13501(10) -.4237(3) .0271(7) Uani d . 1 . . C C14 .9957(3) .10035(10) -.4406(3) .0264(6) Uani d . 1 . . C C15 .9668(3) .05593(11) -.4203(3) .0326(7) Uani d . 1 . . C H15 1.0287 .0324 -.4334 .039 Uiso calc R 1 . . H C16 .8426(4) .04635(12) -.3794(3) .0402(8) Uani d . 1 . . C H16 .8191 .0159 -.3653 .048 Uiso calc R 1 . . H C17 .7541(4) .08091(12) -.3595(3) .0400(8) Uani d . 1 . . C H17 .6716 .0738 -.3302 .048 Uiso calc R 1 . . H C18 .7833(3) .12591(11) -.3815(3) .0333(7) Uani d . 1 . . C H18 .7222 .1495 -.3676 .040 Uiso calc R 1 . . H O3 1.0431(2) .17346(7) -.64990(19) .0284(5) Uani d . 1 . . O O4 1.1935(2) .19614(7) -.4604(2) .0332(5) Uani d . 1 . . O C19 1.1416(3) .20279(10) -.6730(3) .0280(7) Uani d . 1 . . C C20 1.2306(3) .21627(10) -.5605(3) .0317(7) Uani d . 1 . . C C21 1.3390(3) .24599(11) -.5601(4) .0444(9) Uani d . 1 . . C H21 1.4003 .2551 -.4838 .053 Uiso calc R 1 . . H C22 1.3554(4) .26234(13) -.6775(5) .0597(12) Uani d . 1 . . C H22 1.4289 .2832 -.6804 .072 Uiso calc R 1 . . H C23 1.2686(5) .24902(13) -.7872(5) .0560(11) Uani d . 1 . . C H23 1.2824 .2609 -.8649 .067 Uiso calc R 1 . . H C24 1.1590(4) .21808(11) -.7878(4) .0423(9) Uani d . 1 . . C H24 1.0995 .2082 -.8643 .051 Uiso calc 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 Rh .02009(11) .02040(12) .01960(11) -.00137(9) .00252(8) .00088(9) P1 .0249(4) .0289(4) .0254(4) .0029(3) .0070(3) .0070(3) C1 .0386(19) .0297(18) .055(2) -.0011(15) .0044(17) .0134(16) C2 .042(2) .062(3) .0308(18) .0126(18) .0156(16) .0127(17) C3 .0298(17) .0406(19) .0330(18) .0080(14) .0091(14) .0091(15) P2 .0296(4) .0237(4) .0225(4) .0031(3) .0066(3) .0016(3) C4 .0405(19) .0338(18) .0345(18) .0053(15) .0096(15) .0090(14) C5 .0347(18) .0397(19) .0359(18) .0012(15) .0188(15) .0010(15) C6 .0410(19) .040(2) .0270(17) .0039(16) .0021(14) -.0081(14) P3 .0224(4) .0226(4) .0324(4) -.0019(3) .0010(3) -.0007(3) C7 .0261(16) .0360(19) .055(2) -.0024(14) .0123(15) .0071(16) C8 .0339(18) .0266(18) .058(2) -.0031(14) -.0040(17) -.0092(16) C9 .0302(16) .0299(18) .0335(17) .0014(13) -.0027(14) -.0026(13) P4 .0216(4) .0268(4) .0278(4) -.0020(3) .0028(3) -.0034(3) C10 .0372(18) .0282(17) .044(2) -.0052(14) .0049(16) -.0048(15) C11 .0227(15) .048(2) .0412(19) -.0050(15) .0003(14) .0009(17) C12 .0351(18) .041(2) .0321(18) .0036(15) .0015(14) -.0100(15) B .0279(18) .0280(19) .0278(18) .0019(14) .0054(14) -.0022(15) O1 .0340(12) .0239(11) .0362(12) .0011(9) .0154(10) .0003(9) O2 .0325(12) .0268(12) .0323(12) .0039(9) .0114(9) .0008(9) C13 .0333(17) .0262(16) .0214(15) -.0013(13) .0053(13) -.0012(12) C14 .0307(16) .0260(16) .0211(14) -.0016(13) .0027(12) -.0033(12) C15 .0387(18) .0263(17) .0278(17) .0009(14) -.0041(14) -.0014(13) C16 .045(2) .0317(19) .041(2) -.0123(16) .0022(16) .0061(15) C17 .0347(18) .046(2) .0386(19) -.0107(16) .0072(15) .0024(16) C18 .0325(17) .0366(18) .0312(17) -.0044(14) .0078(14) -.0009(14) O3 .0243(10) .0309(12) .0301(11) -.0037(9) .0060(9) .0022(9) O4 .0333(12) .0323(12) .0318(12) -.0037(10) .0022(10) -.0007(10) C19 .0246(15) .0260(16) .0353(18) .0059(13) .0103(13) .0033(13) C20 .0251(16) .0219(16) .051(2) .0039(12) .0135(15) .0002(14) C21 .0315(18) .0274(18) .074(3) -.0034(14) .0117(18) -.0104(18) C22 .047(2) .032(2) .111(4) -.0049(18) .043(3) .002(2) C23 .067(3) .037(2) .081(3) .011(2) .051(3) .016(2) C24 .047(2) .036(2) .049(2) .0142(16) .0215(18) .0096(16) 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 P4 . 2.2929(8) yes Rh P2 . 2.2969(8) yes Rh P1 . 2.3071(8) yes Rh P3 . 2.3083(8) yes P1 C1 . 1.814(3) no P1 C3 . 1.824(3) no P1 C2 . 1.829(3) no P2 C5 . 1.826(3) no P2 C6 . 1.827(3) no P2 C4 . 1.835(3) no P3 C7 . 1.828(3) no P3 C9 . 1.830(3) no P3 C8 . 1.832(3) no P4 C12 . 1.827(3) no P4 C11 . 1.831(3) no P4 C10 . 1.832(3) no B O1 . 1.472(4) yes B O4 . 1.475(4) yes B O2 . 1.492(4) yes B O3 . 1.492(4) yes O1 C13 . 1.359(3) no O2 C14 . 1.353(3) no C13 C18 . 1.368(4) no C13 C14 . 1.404(4) no C14 C15 . 1.371(4) no C15 C16 . 1.405(5) no C16 C17 . 1.383(5) no C17 C18 . 1.392(5) no O3 C19 . 1.356(3) no O4 C20 . 1.357(4) no C19 C24 . 1.372(4) no C19 C20 . 1.395(4) no C20 C21 . 1.372(4) no C21 C22 . 1.406(6) no C22 C23 . 1.362(6) no C23 C24 . 1.404(5) no