#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008478.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_2008478 _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 '[RhH2 (C3 H9 P)4 +, C12 H8 B O4 -' _chemical_formula_sum 'C24 H46 B O4 P4 Rh' _chemical_formula_weight 636.21 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.4442(7) _cell_length_b 18.7746(10) _cell_length_c 24.5809(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6204.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _exptl_crystal_density_diffrn 1.362 _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 .36617(4) .62184(3) .57450(2) .02152(16) Uani d D 1 A . Rh H1 .405(5) .570(3) .534(2) .015(18) Uiso d D 1 . . H H2 .270(5) .622(5) .544(3) .05(3) Uiso d D 1 . . H P1 .28342(15) .52706(11) .61314(9) .0294(5) Uani d . 1 . . P C1 .3184(7) .4889(5) .6787(4) .049(3) Uani d . 1 . . C H1A .3875 .4724 .6771 .073 Uiso calc R 1 . . H H1B .2746 .4486 .6870 .073 Uiso calc R 1 . . H H1C .3117 .5252 .7071 .073 Uiso calc R 1 . . H C2 .1500(6) .5394(5) .6217(4) .045(2) Uani d . 1 . . C H2A .1200 .4949 .6346 .068 Uiso calc R 1 . . H H2B .1202 .5527 .5868 .068 Uiso calc R 1 . . H H2C .1378 .5772 .6484 .068 Uiso calc R 1 . . H C3 .2849(8) .4490(5) .5699(5) .065(3) Uani d . 1 . . C H3A .2605 .4618 .5336 .097 Uiso calc R 1 . . H H3B .2420 .4122 .5855 .097 Uiso calc R 1 . . H H3C .3531 .4309 .5670 .097 Uiso calc R 1 . . H P2 .29859(14) .70846(11) .63282(8) .0254(4) Uani d . 1 . . P C4 .2772(7) .6825(6) .7031(3) .046(2) Uani d . 1 . . C H4A .3380 .6615 .7181 .069 Uiso calc R 1 . . H H4B .2232 .6475 .7046 .069 Uiso calc R 1 . . H H4C .2588 .7246 .7244 .069 Uiso calc R 1 . . H C5 .1768(6) .7429(5) .6131(4) .038(2) Uani d . 1 . . C H5A .1567 .7805 .6385 .057 Uiso calc R 1 . . H H5B .1278 .7043 .6140 .057 Uiso calc R 1 . . H H5C .1805 .7625 .5762 .057 Uiso calc R 1 . . H C6 .3676(7) .7909(5) .6419(5) .061(3) Uani d . 1 . . C H6A .3315 .8221 .6670 .091 Uiso calc R 1 . . H H6B .3752 .8147 .6067 .091 Uiso calc R 1 . . H H6C .4335 .7802 .6569 .091 Uiso calc R 1 . . H P3 .52546(14) .60889(12) .61387(8) .0275(5) Uani d . 1 . . P C7 .5525(13) .5525(11) .6695(8) .055(6) Uani d P .573(12) A 1 C H7A .6211 .5606 .6815 .083 Uiso calc PR .573(12) A 1 H H7B .5446 .5027 .6584 .083 Uiso calc PR .573(12) A 1 H H7C .5068 .5630 .6995 .083 Uiso calc PR .573(12) A 1 H C8 .5856(11) .6928(9) .6420(7) .046(4) Uani d P .573(12) A 1 C H8A .5492 .7085 .6744 .068 Uiso calc PR .573(12) A 1 H H8B .5838 .7304 .6144 .068 Uiso calc PR .573(12) A 1 H H8C .6548 .6827 .6518 .068 Uiso calc PR .573(12) A 1 H C9 .6229(11) .5839(10) .5657(6) .044(4) Uani d P .573(12) A 1 C H9A .6265 .6195 .5366 .066 Uiso calc PR .573(12) A 1 H H9B .6074 .5372 .5500 .066 Uiso calc PR .573(12) A 1 H H9C .6869 .5816 .5847 .066 Uiso calc PR .573(12) A 1 H C7X .5381(15) .6084(11) .6878(8) .034(5) Uani d P .427(12) A 2 C H7X1 .5181 .6549 .7023 .051 Uiso calc PR .427(12) A 2 H H7X2 .6075 .5989 .6975 .051 Uiso calc PR .427(12) A 2 H H7X3 .4954 .5712 .7031 .051 Uiso calc PR .427(12) A 2 H C8X .6267(15) .6573(13) .5929(10) .054(7) Uani d P .427(12) A 2 C H8X1 .6147 .7080 .5997 .082 Uiso calc PR .427(12) A 2 H H8X2 .6375 .6495 .5539 .082 Uiso calc PR .427(12) A 2 H H8X3 .6856 .6419 .6132 .082 Uiso calc PR .427(12) A 2 H C9X .5689(15) .5145(11) .5981(9) .041(6) Uani d P .427(12) A 2 C H9X1 .6334 .5060 .6155 .062 Uiso calc PR .427(12) A 2 H H9X2 .5755 .5086 .5587 .062 Uiso calc PR .427(12) A 2 H H9X3 .5202 .4803 .6121 .062 Uiso calc PR .427(12) A 2 H P4 .40559(15) .69890(16) .50491(9) .0432(7) Uani d . 1 . . P C10 .5033(8) .7660(7) .5106(5) .081(5) Uani d . 1 A . C H10A .4863 .7997 .5396 .122 Uiso calc R 1 . . H H10B .5094 .7917 .4760 .122 Uiso calc R 1 . . H H10C .5666 .7428 .5192 .122 Uiso calc R 1 . . H C11 .4432(9) .6540(8) .4432(4) .088(5) Uani d . 1 A . C H11A .4536 .6892 .4143 .132 Uiso calc R 1 . . H H11B .3911 .6205 .4321 .132 Uiso calc R 1 . . H H11C .5052 .6279 .4497 .132 Uiso calc R 1 . . H C12 .3030(7) .7516(7) .4795(4) .063(3) Uani d . 1 A . C H12A .2859 .7883 .5062 .095 Uiso calc R 1 . . H H12B .2453 .7207 .4734 .095 Uiso calc R 1 . . H H12C .3223 .7742 .4452 .095 Uiso calc R 1 . . H B .0872(7) .1616(5) .8347(3) .0265(18) Uani d . 1 . . B O1 .1247(4) .0948(3) .8105(2) .0296(12) Uani d . 1 . . O O2 .0613(4) .1412(3) .8921(2) .0283(12) Uani d . 1 . . O C13 .1283(5) .0454(4) .8508(3) .0280(16) Uani d . 1 . . C C14 .0920(5) .0742(4) .8994(3) .0234(15) Uani d . 1 . . C C15 .0896(6) .0341(5) .9464(3) .0325(18) Uani d . 1 . . C H15 .0650 .0534 .9794 .039 Uiso calc R 1 . . H C16 .1245(6) -.0360(5) .9437(4) .041(2) Uani d . 1 . . C H16 .1235 -.0649 .9754 .049 Uiso calc R 1 . . H C17 .1605(7) -.0638(5) .8954(4) .043(2) Uani d . 1 . . C H17 .1841 -.1115 .8945 .052 Uiso calc R 1 . . H C18 .1627(6) -.0232(5) .8483(3) .0351(19) Uani d . 1 . . C H18 .1874 -.0424 .8152 .042 Uiso calc R 1 . . H O3 .0002(4) .1898(3) .8047(2) .0294(12) Uani d . 1 . . O O4 .1614(4) .2194(3) .8339(2) .0313(12) Uani d . 1 . . O C19 .0227(6) .2585(4) .7912(3) .0295(17) Uani d . 1 . . C C20 .1189(6) .2750(4) .8076(3) .0303(17) Uani d . 1 . . C C21 .1603(8) .3405(5) .7979(4) .045(2) Uani d . 1 . . C H21 .2263 .3512 .8090 .054 Uiso calc R 1 . . H C22 .1015(9) .3911(5) .7709(4) .056(3) Uani d . 1 . . C H22 .1270 .4375 .7644 .067 Uiso calc R 1 . . H C23 .0072(9) .3739(6) .7538(4) .060(3) Uani d . 1 . . C H23 -.0310 .4087 .7351 .071 Uiso calc R 1 . . H C24 -.0341(7) .3070(5) .7632(3) .040(2) Uani d . 1 . . C H24 -.0991 .2954 .7508 .048 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 .0186(2) .0287(3) .0172(3) .0006(2) -.0014(2) .0018(2) P1 .0238(9) .0218(10) .0427(12) -.0006(8) -.0051(9) .0038(9) C1 .043(5) .044(6) .060(6) -.009(4) -.006(5) .021(5) C2 .026(4) .044(6) .066(6) -.012(4) -.008(4) .009(5) C3 .066(7) .031(5) .097(9) .006(5) -.013(7) -.023(6) P2 .0221(9) .0221(10) .0321(10) .0036(8) -.0034(8) -.0003(8) C4 .051(5) .061(7) .026(4) .023(5) -.009(4) -.013(4) C5 .026(4) .045(5) .043(5) .020(4) .004(4) .008(4) C6 .044(5) .033(5) .105(9) -.009(5) .014(6) -.029(6) P3 .0212(9) .0346(12) .0266(10) .0062(8) -.0025(7) .0056(9) C7 .041(9) .064(14) .062(12) .010(9) -.008(8) .044(11) C8 .025(7) .054(11) .058(11) -.005(7) -.006(7) -.009(9) C9 .029(7) .059(11) .045(9) .015(7) .006(7) -.001(8) C7X .040(11) .030(12) .032(10) .006(9) -.017(8) .001(8) C8X .024(10) .064(16) .075(17) .010(11) -.013(11) .034(14) C9X .032(10) .044(13) .048(13) .010(9) .001(9) -.016(10) P4 .0223(9) .0799(19) .0275(11) .0009(11) -.0007(9) .0294(12) C10 .048(6) .126(12) .070(8) -.031(7) -.008(5) .074(8) C11 .057(7) .177(16) .029(5) .036(8) .015(5) .031(7) C12 .031(4) .100(9) .059(6) .008(6) .007(4) .055(7) B .029(4) .031(5) .019(4) .006(4) .004(3) -.003(4) O1 .042(3) .026(3) .022(3) .001(2) .006(2) .002(2) O2 .035(3) .031(3) .019(2) .002(2) .004(2) -.004(2) C13 .022(3) .035(4) .026(4) .001(3) -.001(3) .000(3) C14 .018(3) .024(4) .028(4) -.003(3) -.001(3) .001(3) C15 .031(4) .041(5) .026(4) -.002(4) .001(3) .000(4) C16 .040(5) .048(5) .035(4) -.002(4) .000(4) .015(4) C17 .047(5) .035(5) .048(5) .013(4) .000(4) .010(4) C18 .037(4) .036(5) .032(4) .004(4) .004(4) -.001(4) O3 .027(3) .028(3) .033(3) -.002(2) -.002(2) -.002(2) O4 .028(3) .033(3) .033(3) -.004(2) -.002(2) .003(2) C19 .034(4) .028(4) .026(4) .006(3) .008(3) -.004(3) C20 .037(4) .029(4) .025(4) .002(4) .004(3) -.006(3) C21 .061(6) .034(5) .041(5) -.011(5) .000(4) -.004(4) C22 .081(8) .022(5) .065(7) .011(5) .015(6) .005(4) C23 .084(8) .050(6) .045(5) .044(6) .012(5) .012(5) C24 .041(5) .046(6) .033(5) .014(4) .002(4) .005(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 Rh H1 . 1.48(5) yes Rh H2 . 1.49(5) yes Rh P4 . 2.302(2) yes Rh P1 . 2.304(2) yes Rh P2 . 2.351(2) yes Rh P3 . 2.363(2) yes P1 C3 . 1.811(10) no P1 C2 . 1.821(8) no P1 C1 . 1.824(9) no P2 C4 . 1.817(9) no P2 C6 . 1.818(9) no P2 C5 . 1.826(7) no P3 C8X . 1.71(2) no P3 C7 . 1.767(15) no P3 C7X . 1.824(19) no P3 C9 . 1.826(14) no P3 C8 . 1.901(16) no P3 C9X . 1.91(2) no P4 C11 . 1.807(12) no P4 C12 . 1.808(9) no P4 C10 . 1.826(11) no B O4 . 1.475(10) yes B O1 . 1.476(10) yes B O3 . 1.482(10) yes B O2 . 1.502(10) yes O1 C13 . 1.357(9) no O2 C14 . 1.337(9) no C13 C18 . 1.371(11) no C13 C14 . 1.398(10) no C14 C15 . 1.379(10) no C15 C16 . 1.399(12) no C16 C17 . 1.385(13) no C17 C18 . 1.386(12) no O3 C19 . 1.365(9) no O4 C20 . 1.355(9) no C19 C24 . 1.373(11) no C19 C20 . 1.390(11) no C20 C21 . 1.371(12) no C21 C22 . 1.403(14) no C22 C23 . 1.374(16) no C23 C24 . 1.392(14) no