#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200708.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_2200708 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first m459 _journal_page_last m461 _publ_section_title ; trans-Dichloro(meso-2,3,7,11,12-pentamethyl-3,7,11,17-tetra- azabicyclo[11.3.1]heptadeca-1(17),13,15-triene-\k^4^N^3,7,11,17^)rhodium(III) hexafluorphosphate ; loop_ _publ_author_name 'Blake, Alexander J.' 'Hyde, Timothy I.' 'Schr\"oder, Martin' _chemical_formula_moiety 'C18 H32 Cl2 N4 Rh 1+, P F6 1-' _chemical_formula_sum 'C18 H32 Cl2 F6 N4 P Rh' _chemical_formula_iupac '[Rh Cl2 (C18 H32 N4)] P F6' _chemical_formula_weight 623.26 _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 7.949(5) _cell_length_b 11.067(5) _cell_length_c 14.116(5) _cell_angle_alpha 74.22(5) _cell_angle_beta 86.26(5) _cell_angle_gamma 84.67(5) _cell_volume 1188.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.741 _diffrn_ambient_temperature 293(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 .09546(7) .23461(6) .21425(5) .0284(3) Uani d U 1 . . Rh Cl1 .2853(3) .1324(2) .33661(18) .0466(6) Uani d U 1 . . Cl Cl2 -.1108(3) .3363(2) .10132(18) .0469(6) Uani d U 1 . . Cl N3 .1235(9) .4127(7) .2420(6) .0413(16) Uani d U 1 . . N N7 .2980(8) .2396(7) .1060(6) .0447(17) Uani d U 1 . . N N11 .0066(9) .0580(7) .2113(6) .0420(16) Uani d U 1 . . N N17 -.0790(8) .2230(7) .3208(5) .0344(15) Uani d U 1 . . N C1 -.1075(11) .3213(8) .3597(7) .044(2) Uani d U 1 . . C C2 .0294(13) .4128(9) .3393(8) .052(2) Uani d U 1 . . C H2 -.0280 .4971 .3310 .062 Uiso calc R 1 . . H C2A .1309(17) .3866(11) .4284(9) .073(3) Uani d U 1 . . C H2A1 .2170 .4448 .4171 .110 Uiso calc R 1 . . H H2A2 .1827 .3021 .4421 .110 Uiso calc R 1 . . H H2A3 .0585 .3958 .4835 .110 Uiso calc R 1 . . H C3N .0398(14) .5275(9) .1698(9) .058(3) Uani d U 1 . . C H3N1 -.0781 .5166 .1674 .087 Uiso calc R 1 . . H H3N2 .0929 .5366 .1054 .087 Uiso calc R 1 . . H H3N3 .0520 .6015 .1910 .087 Uiso calc R 1 . . H C4 .3075(13) .4366(10) .2398(8) .056(2) Uani d U 1 . . C H4A .3626 .3728 .2923 .067 Uiso calc R 1 . . H H4B .3158 .5177 .2524 .067 Uiso calc R 1 . . H C5 .3994(12) .4356(10) .1433(9) .062(3) Uani d U 1 . . C H5A .3297 .4841 .0900 .074 Uiso calc R 1 . . H H5B .5029 .4772 .1387 .074 Uiso calc R 1 . . H C6 .4430(11) .3071(11) .1291(9) .059(3) Uani d U 1 . . C H6A .4940 .2545 .1884 .071 Uiso calc R 1 . . H H6B .5282 .3140 .0759 .071 Uiso calc R 1 . . H C7N .2509(13) .3016(11) .0029(7) .061(3) Uani d U 1 . . C H7NA .2014 .3853 -.0015 .091 Uiso calc R 1 . . H H7NB .1707 .2539 -.0163 .091 Uiso calc R 1 . . H H7NC .3501 .3055 -.0400 .091 Uiso calc R 1 . . H C8 .3750(12) .1091(10) .1117(9) .060(3) Uani d U 1 . . C H8A .4341 .0790 .1727 .072 Uiso calc R 1 . . H H8B .4592 .1146 .0581 .072 Uiso calc R 1 . . H C9 .2582(14) .0116(11) .1074(9) .067(3) Uani d U 1 . . C H9A .1843 .0470 .0529 .080 Uiso calc R 1 . . H H9B .3254 -.0597 .0933 .080 Uiso calc R 1 . . H C10 .1506(14) -.0353(9) .1994(9) .057(2) Uani d U 1 . . C H10A .1057 -.1131 .1977 .069 Uiso calc R 1 . . H H10B .2207 -.0535 .2561 .069 Uiso calc R 1 . . H C11N -.1140(14) .0651(10) .1309(9) .062(3) Uani d U 1 . . C H111 -.2084 .1242 .1355 .094 Uiso calc R 1 . . H H112 -.1536 -.0165 .1386 .094 Uiso calc R 1 . . H H113 -.0564 .0919 .0677 .094 Uiso calc R 1 . . H C12 -.0983(12) .0120(9) .3079(8) .049(2) Uani d U 1 . . C H12 -.1951 -.0266 .2919 .059 Uiso calc R 1 . . H C12A -.0088(14) -.0868(9) .3910(8) .061(3) Uani d U 1 . . C H121 .0367 -.1571 .3672 .091 Uiso calc R 1 . . H H122 -.0882 -.1151 .4450 .091 Uiso calc R 1 . . H H123 .0813 -.0503 .4128 .091 Uiso calc R 1 . . H C13 -.1693(10) .1245(9) .3439(7) .0420(19) Uani d U 1 . . C C14 -.3077(12) .1216(11) .4091(8) .062(3) Uani d U 1 . . C H14 -.3725 .0525 .4268 .074 Uiso calc R 1 . . H C15 -.3471(12) .2223(12) .4469(8) .061(3) Uani d U 1 . . C H15 -.4432 .2236 .4879 .074 Uiso calc R 1 . . H C16 -.2456(13) .3232(11) .4248(8) .060(3) Uani d U 1 . . C H16 -.2697 .3900 .4530 .072 Uiso calc R 1 . . H P .4075(3) .2810(2) .7110(2) .0533(7) Uani d DU 1 . . P F1 .3713(8) .4012(6) .7469(6) .102(3) Uani d DU 1 A . F F2 .483(3) .3606(9) .6136(8) .185(12) Uani d PDU .50 A 1 F F3 .5818(13) .2598(12) .7555(16) .196(12) Uani d PDU .50 A 1 F F4 .2326(15) .3034(14) .6664(16) .157(11) Uani d PDU .50 A 1 F F5 .332(3) .2024(9) .8085(8) .168(11) Uani d PDU .50 A 1 F F2' .450(3) .2057(11) .8163(7) .205(13) Uani d PDU .50 A 2 F F3' .2197(11) .2543(14) .7345(17) .155(11) Uani d PDU .50 A 2 F F4' .5934(10) .3083(14) .6880(15) .115(8) Uani d PDU .50 A 2 F F5' .364(3) .3566(13) .6064(6) .154(9) Uani d PDU .50 A 2 F F6 .4437(10) .1610(6) .6750(7) .137(4) Uani d DU 1 A . F 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 .0221(4) .0299(4) .0347(5) -.0043(3) .0019(3) -.0112(3) Cl1 .0393(12) .0457(13) .0563(16) .0019(10) -.0134(11) -.0153(12) Cl2 .0362(11) .0530(14) .0478(15) -.0005(10) -.0068(10) -.0072(11) N3 .042(4) .038(4) .046(4) -.010(3) .002(3) -.014(3) N7 .032(3) .057(4) .047(4) -.007(3) .013(3) -.018(4) N11 .042(4) .035(4) .053(4) -.003(3) -.008(3) -.017(3) N17 .024(3) .041(4) .040(4) -.006(3) .004(3) -.014(3) C1 .045(5) .038(5) .039(5) .010(3) .006(4) -.001(4) C2 .064(6) .039(5) .058(5) -.001(4) .007(4) -.026(4) C2A .099(9) .073(8) .058(6) -.028(7) .001(6) -.029(6) C3N .072(6) .034(5) .069(7) -.002(4) -.002(5) -.014(5) C4 .054(5) .055(6) .067(7) -.032(4) .000(4) -.022(5) C5 .044(5) .064(6) .080(8) -.028(5) .009(5) -.019(6) C6 .028(4) .079(6) .072(7) -.011(4) .007(4) -.023(6) C7N .052(6) .092(8) .035(5) -.002(5) .016(4) -.017(5) C8 .043(5) .070(6) .069(8) .015(4) .005(5) -.029(5) C9 .070(7) .065(6) .073(8) .015(5) .000(5) -.040(6) C10 .074(6) .031(5) .073(7) .008(4) -.009(5) -.026(5) C11N .063(6) .057(7) .071(7) -.010(5) -.028(5) -.017(6) C12 .042(5) .040(5) .063(6) -.019(4) -.011(4) -.003(4) C12A .075(7) .045(6) .059(7) -.011(5) -.011(5) -.002(5) C13 .032(4) .052(5) .036(5) -.011(3) .000(3) .000(4) C14 .039(5) .070(7) .067(8) -.012(4) .007(4) -.002(5) C15 .031(5) .095(7) .049(7) .001(4) .013(4) -.009(5) C16 .048(5) .077(7) .054(7) .014(4) .007(4) -.024(6) P .0528(15) .0430(15) .067(2) -.0049(11) .0085(13) -.0223(13) F1 .082(5) .090(5) .166(8) -.006(4) -.005(5) -.090(5) F2 .31(3) .105(12) .124(15) -.08(2) .128(17) -.024(11) F3 .101(10) .034(9) .44(4) -.004(7) -.145(16) -.013(14) F4 .116(14) .15(2) .25(3) .031(11) -.109(17) -.119(19) F5 .29(3) .169(14) .072(11) -.17(2) .051(12) -.035(9) F2' .26(3) .218(17) .069(8) .15(2) .036(12) .013(8) F3' .071(9) .105(15) .32(3) -.043(9) .093(15) -.131(19) F4' .046(6) .088(15) .22(2) -.011(7) .005(9) -.061(15) F5' .154(18) .211(16) .073(8) .087(18) -.026(11) -.027(8) F6 .124(6) .083(5) .234(10) -.029(4) .073(7) -.105(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 Cl1 . 2.345(3) yes Rh Cl2 . 2.349(3) yes Rh N3 . 2.145(7) yes Rh N7 . 2.140(7) yes Rh N11 . 2.150(7) yes Rh N17 . 1.964(7) yes N3 C4 . 1.507(12) ? N3 C2 . 1.521(13) ? N3 C3N . 1.524(12) ? N7 C7N . 1.486(13) ? N7 C8 . 1.499(12) ? N7 C6 . 1.528(12) ? N11 C10 . 1.501(12) ? N11 C11N . 1.514(12) ? N11 C12 . 1.539(13) ? N17 C13 . 1.316(11) ? N17 C1 . 1.342(11) ? C1 C16 . 1.387(13) ? C1 C2 . 1.516(14) ? C2 C2A . 1.485(16) ? C2 H2 . .9800 ? C2A H2A1 . .9600 ? C2A H2A2 . .9600 ? C2A H2A3 . .9600 ? C3N H3N1 . .9600 ? C3N H3N2 . .9600 ? C3N H3N3 . .9600 ? C4 C5 . 1.507(15) ? C4 H4A . .9700 ? C4 H4B . .9700 ? C5 C6 . 1.495(15) ? C5 H5A . .9700 ? C5 H5B . .9700 ? C6 H6A . .9700 ? C6 H6B . .9700 ? C7N H7NA . .9600 ? C7N H7NB . .9600 ? C7N H7NC . .9600 ? C8 C9 . 1.503(16) ? C8 H8A . .9700 ? C8 H8B . .9700 ? C9 C10 . 1.504(16) ? C9 H9A . .9700 ? C9 H9B . .9700 ? C10 H10A . .9700 ? C10 H10B . .9700 ? C11N H111 . .9600 ? C11N H112 . .9600 ? C11N H113 . .9600 ? C12 C13 . 1.518(14) ? C12 C12A . 1.531(14) ? C12 H12 . .9800 ? C12A H121 . .9600 ? C12A H122 . .9600 ? C12A H123 . .9600 ? C13 C14 . 1.385(14) ? C14 C15 . 1.364(16) ? C14 H14 . .9300 ? C15 C16 . 1.393(16) ? C15 H15 . .9300 ? C16 H16 . .9300 ? P F1 . 1.545(5) ? P F2 . 1.537(7) ? P F3 . 1.530(7) ? P F4 . 1.535(7) ? P F5 . 1.534(7) ? P F6 . 1.543(5) ? P F2' . 1.537(7) ? P F3' . 1.546(7) ? P F4' . 1.532(7) ? P F5' . 1.530(7) ? _cod_database_code 2200708