#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2012026.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_2012026 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2001 _journal_volume 57 _journal_page_first 702 _journal_page_last 703 _publ_section_title ; \m-Oxo-bis[(\h^5^-1,2-dicarbaundecaborato)bis(N,N-dimethylacetamidinato) tantalum] dichloromethane hemisolvate ; _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _publ_author_name "Goeta, Andr\`es E." 'Hughes, Andrew K.' 'Malget, John M.' _chemical_formula_moiety 'C20 H58 B18 N8 O Ta2 , 0.5C H2 Cl2' _chemical_formula_sum 'C20.5 H59 B18 Cl N8 O Ta2' _[local]_cod_chemical_formula_sum_orig 'C20.50 H59 B18 Cl N8 O Ta2' _chemical_formula_iupac '[Ta2 O (C2 B9 H11)2 (C4 H9 N2)4] , 0.5C H2 Cl2' _chemical_formula_weight 1025.69 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.414(3) _cell_length_b 10.769(3) _cell_length_c 17.863(5) _cell_angle_alpha 90 _cell_angle_beta 93.303(6) _cell_angle_gamma 90 _cell_volume 2192.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _exptl_crystal_density_diffrn 1.554 _diffrn_ambient_temperature 150(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 C1A -.0730(8) .3083(8) .1802(5) .0332(17) Uani d . 1 . . C H1A .0137 .3076 .1920 .040 Uiso calc R 1 . . H C2A -.1586(7) .2868(7) .2444(5) .0336(17) Uani d . 1 . . C H2A -.1277 .2729 .2973 .040 Uiso calc R 1 . . H TaA -.12318(2) .51696(3) .235286(16) .02870(8) Uani d . 1 . . Ta B4A -.1295(8) .4024(9) .1140(6) .038(2) Uani d . 1 . . B H4A -.0767 .4653 .0790 .046 Uiso calc R 1 . . H B5A -.1197(10) .2407(10) .0969(6) .042(2) Uani d . 1 . . B H5A -.0629 .2010 .0538 .051 Uiso calc R 1 . . H B6A -.1345(10) .1637(10) .1843(6) .046(2) Uani d . 1 . . B H6A -.0879 .0749 .1994 .055 Uiso calc R 1 . . H B7A -.2769(10) .1989(11) .2129(7) .052(3) Uani d . 1 . . B H7A -.3254 .1309 .2470 .063 Uiso calc R 1 . . H B8A -.2822(8) .3601(10) .2291(6) .043(2) Uani d . 1 . . B H8A -.3375 .3924 .2752 .051 Uiso calc R 1 . . H B9A -.2704(8) .4365(10) .1411(6) .039(2) Uani d . 1 . . B H9A -.3199 .5227 .1240 .047 Uiso calc R 1 . . H B10A -.2505(10) .3215(10) .0734(6) .044(3) Uani d . 1 . . B H10A -.2813 .3353 .0134 .053 Uiso calc R 1 . . H B11A -.2575(11) .1754(11) .1168(6) .052(3) Uani d . 1 . . B H11A -.2944 .0919 .0865 .063 Uiso calc R 1 . . H B12A -.3490(9) .2961(10) .1431(7) .048(3) Uani d . 1 . . B H12A -.4462 .2934 .1303 .058 Uiso calc R 1 . . H N1A -.2063(5) .5866(6) .3110(4) .0355(15) Uani d . 1 . . N C3A -.2782(6) .6204(8) .3613(5) .0366(18) Uani d . 1 . . C C4A -.3103(7) .5348(9) .4230(5) .049(2) Uani d . 1 . . C H4A1 -.2826 .4507 .4125 .074 Uiso calc R 1 . . H H4A2 -.3957 .5339 .4260 .074 Uiso calc R 1 . . H H4A3 -.2734 .5637 .4707 .074 Uiso calc R 1 . . H N2A -.3222(6) .7322(7) .3610(5) .0476(19) Uani d . 1 . . N C5A -.4113(8) .7723(9) .4141(6) .052(3) Uani d . 1 . . C H5A1 -.4795 .7170 .4091 .079 Uiso calc R 1 . . H H5A2 -.4360 .8576 .4024 .079 Uiso calc R 1 . . H H5A3 -.3769 .7685 .4656 .079 Uiso calc R 1 . . H C6A -.2883(9) .8237(9) .3042(6) .054(2) Uani d . 1 . . C H6A1 -.2257 .7889 .2753 .080 Uiso calc R 1 . . H H6A2 -.2602 .8998 .3294 .080 Uiso calc R 1 . . H H6A3 -.3565 .8430 .2704 .080 Uiso calc R 1 . . H N3A -.0867(6) .6596(7) .1824(5) .0410(17) Uani d . 1 . . N C7A -.0746(8) .7447(9) .1302(5) .044(2) Uani d . 1 . . C C8A -.1663(10) .7564(13) .0671(7) .071(3) Uani d . 1 . . C H8A1 -.2243 .6898 .0708 .106 Uiso calc R 1 . . H H8A2 -.1292 .7499 .0191 .106 Uiso calc R 1 . . H H8A3 -.2054 .8371 .0701 .106 Uiso calc R 1 . . H N4A .0170(7) .8239(7) .1370(4) .0478(19) Uani d . 1 . . N C9A .0369(10) .9218(11) .0832(6) .067(3) Uani d . 1 . . C H9A1 -.0378 .9450 .0573 .101 Uiso calc R 1 . . H H9A2 .0911 .8920 .0465 .101 Uiso calc R 1 . . H H9A3 .0709 .9943 .1095 .101 Uiso calc R 1 . . H C10A .1015(9) .8145(10) .1998(6) .054(3) Uani d . 1 . . C H1A1 .1148 .7268 .2123 .082 Uiso calc R 1 . . H H1A2 .0716 .8576 .2430 .082 Uiso calc R 1 . . H H1A3 .1756 .8526 .1867 .082 Uiso calc R 1 . . H O1 .0213(4) .4767(6) .2862(3) .0365(14) Uani d . 1 . . O C1B .0807(6) .6582(7) .3969(5) .0325(17) Uani d . 1 . . C H1B .0192 .6801 .3569 .039 Uiso calc R 1 . . H C2B .0695(6) .5361(8) .4452(4) .0317(16) Uani d . 1 . . C H2B .0010 .4790 .4364 .038 Uiso calc R 1 . . H TaB .17936(2) .48489(3) .331441(15) .02563(7) Uani d . 1 . . Ta B4B .2228(7) .6943(8) .3848(5) .0271(17) Uani d . 1 . . B H4B .2557 .7457 .3357 .033 Uiso calc R 1 . . H B5B .1388(8) .7777(8) .4510(5) .0328(19) Uani d . 1 . . B H5B .1178 .8788 .4438 .039 Uiso calc R 1 . . H B6B .0377(8) .6775(9) .4857(6) .040(2) Uani d . 1 . . B H6B -.0512 .7103 .5006 .048 Uiso calc R 1 . . H B7B .1146(8) .5579(10) .5361(5) .038(2) Uani d . 1 . . B H7B .0773 .5113 .5855 .045 Uiso calc R 1 . . H B8B .1987(7) .4748(9) .4723(4) .0319(17) Uani d . 1 . . B H8B .2156 .3740 .4840 .038 Uiso calc R 1 . . H B9B .3036(7) .5770(8) .4350(5) .0285(18) Uani d . 1 . . B H9B .3942 .5471 .4219 .034 Uiso calc R 1 . . H B10B .2825(7) .7262(8) .4759(5) .0304(18) Uani d . 1 . . B H10B .3576 .7923 .4859 .036 Uiso calc R 1 . . H B11B .1636(8) .7138(9) .5390(6) .040(2) Uani d . 1 . . B H11B .1604 .7708 .5913 .047 Uiso calc R 1 . . H B12B .2668(8) .5888(9) .5297(6) .038(2) Uani d . 1 . . B H12B .3326 .5639 .5763 .045 Uiso calc R 1 . . H N1B .2222(6) .3181(6) .3383(4) .0373(15) Uani d . 1 . . N C3B .2489(7) .1997(8) .3463(5) .0386(19) Uani d . 1 . . C C4B .1524(8) .1068(9) .3386(6) .052(2) Uani d . 1 . . C H4B1 .1538 .0545 .3835 .079 Uiso calc R 1 . . H H4B2 .1630 .0547 .2945 .079 Uiso calc R 1 . . H H4B3 .0768 .1499 .3327 .079 Uiso calc R 1 . . H N2B .3569(6) .1652(7) .3604(5) .0450(18) Uani d . 1 . . N C5B .3932(9) .0381(9) .3676(7) .067(3) Uani d . 1 . . C H5B1 .3243 -.0147 .3728 .100 Uiso calc R 1 . . H H5B2 .4469 .0290 .4121 .100 Uiso calc R 1 . . H H5B3 .4333 .0134 .3229 .100 Uiso calc R 1 . . H C6B .4538(7) .2565(9) .3611(7) .055(3) Uani d . 1 . . C H6B1 .4453 .3159 .4019 .083 Uiso calc R 1 . . H H6B2 .4512 .3009 .3131 .083 Uiso calc R 1 . . H H6B3 .5290 .2131 .3685 .083 Uiso calc R 1 . . H N3B .2642(5) .5332(6) .2491(3) .0338(14) Uani d . 1 . . N C7B .3439(6) .5639(8) .2044(5) .0353(17) Uani d . 1 . . C C8B .4616(7) .6033(12) .2364(6) .058(3) Uani d . 1 . . C H8B1 .4611 .6053 .2912 .087 Uiso calc R 1 . . H H8B2 .4799 .6862 .2177 .087 Uiso calc R 1 . . H H8B3 .5212 .5442 .2213 .087 Uiso calc R 1 . . H N4B .3213(6) .5667(8) .1314(4) .0451(18) Uani d . 1 . . N C9B .4117(9) .5870(15) .0789(5) .077(4) Uani d . 1 . . C H9B1 .4593 .6589 .0949 .115 Uiso calc R 1 . . H H9B2 .3750 .6023 .0288 .115 Uiso calc R 1 . . H H9B3 .4619 .5132 .0775 .115 Uiso calc R 1 . . H C10B .2081(7) .5310(11) .0991(5) .056(2) Uani d . 1 . . C H1B1 .1516 .5289 .1383 .083 Uiso calc R 1 . . H H1B2 .2134 .4485 .0764 .083 Uiso calc R 1 . . H H1B3 .1822 .5913 .0605 .083 Uiso calc R 1 . . H Cl1 .4259(6) .9397(6) .1466(4) .087(2) Uani d PD .50 . . Cl C11 .3818(11) 1.0709(10) .0995(7) .053(5) Uani d PD .50 . . C H111 .3402 1.0458 .0518 .063 Uiso calc PR .50 . . H H112 .4527 1.1176 .0868 .063 Uiso calc PR .50 . . H Cl2 .2922(4) 1.1695(6) .1456(3) .0652(15) Uani d PD .50 . . 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 C1A .039(4) .034(4) .027(4) .005(3) .001(3) -.008(3) C2A .041(4) .030(4) .030(4) -.008(3) -.002(3) .004(3) TaA .02339(13) .03408(17) .02845(15) -.00003(10) -.00009(10) -.00364(12) B4A .042(5) .038(5) .033(5) .000(4) -.002(4) -.002(4) B5A .048(6) .044(6) .034(6) -.009(4) -.003(4) -.007(4) B6A .061(6) .036(5) .039(6) -.007(5) -.003(5) -.005(4) B7A .052(6) .052(7) .054(7) -.019(5) .011(5) -.008(5) B8A .028(4) .047(6) .054(7) -.009(4) .010(4) -.005(5) B9A .028(4) .051(6) .037(5) -.009(4) -.007(4) .006(4) B10A .057(6) .046(6) .028(5) -.016(5) -.013(5) .001(4) B11A .067(7) .055(7) .034(6) -.020(6) -.008(5) -.010(5) B12A .038(5) .049(6) .056(7) -.013(4) -.010(5) -.003(5) N1A .027(3) .041(4) .039(4) .005(3) .003(3) -.009(3) C3A .027(4) .039(4) .043(5) .003(3) -.010(3) .001(4) C4A .047(5) .043(5) .058(6) .008(4) .010(4) .014(4) N2A .042(4) .049(5) .051(5) -.002(3) -.004(3) -.012(4) C5A .047(5) .034(5) .079(8) -.003(4) .027(5) -.022(5) C6A .061(6) .036(5) .065(7) -.004(4) .016(5) .009(5) N3A .041(4) .042(4) .039(5) -.005(3) -.001(3) -.004(3) C7A .047(5) .047(5) .037(5) .001(4) .004(4) .001(4) C8A .057(7) .092(9) .062(8) -.001(6) -.006(6) .016(7) N4A .067(5) .035(4) .042(5) .002(3) .009(4) .007(3) C9A .082(7) .065(7) .057(7) -.004(6) .022(6) .034(6) C10A .057(6) .045(6) .059(7) -.018(5) -.013(5) .008(5) O1 .023(2) .050(4) .035(3) .002(2) -.0056(19) -.013(3) C1B .030(4) .029(4) .038(5) .008(3) -.001(3) -.007(3) C2B .024(3) .039(4) .032(4) -.004(3) .001(3) -.004(3) TaB .02190(12) .02607(14) .02867(15) .00134(10) -.00085(10) -.00454(11) B4B .032(4) .028(4) .021(4) -.006(3) .002(3) -.001(3) B5B .040(5) .028(4) .030(5) .005(3) .005(4) -.005(4) B6B .033(5) .043(5) .045(6) .005(4) .010(4) -.004(4) B7B .035(4) .053(6) .025(4) -.011(4) .002(3) .001(4) B8B .035(4) .032(4) .028(4) -.010(4) -.002(3) .001(4) B9B .022(4) .028(4) .035(5) -.001(3) -.009(3) -.003(3) B10B .031(4) .029(4) .032(5) -.001(3) .005(4) -.003(4) B11B .038(5) .041(5) .040(6) -.007(4) .010(4) .001(4) B12B .037(5) .036(5) .039(5) -.007(4) -.003(4) .004(4) N1B .040(4) .032(4) .040(4) -.003(3) .001(3) -.006(3) C3B .043(5) .035(4) .038(5) -.005(3) .007(4) -.006(4) C4B .046(5) .039(5) .073(7) -.016(4) .004(5) -.001(5) N2B .040(4) .033(4) .062(5) .006(3) .001(4) .001(3) C5B .068(6) .038(5) .095(9) .021(5) .010(6) .017(6) C6B .031(4) .043(5) .092(8) .002(4) -.004(5) .005(5) N3B .031(3) .040(4) .030(3) -.001(3) .004(2) -.006(3) C7B .031(4) .041(4) .035(4) .012(3) .007(3) .001(3) C8B .035(5) .092(8) .048(6) -.005(5) .000(4) .011(6) N4B .035(3) .073(5) .027(4) .012(3) .000(3) .000(3) C9B .050(6) .155(13) .027(5) .029(7) .013(4) .017(6) C10B .048(5) .075(7) .042(5) .002(5) -.007(4) -.003(5) Cl1 .103(5) .074(4) .078(4) -.004(4) -.035(4) .002(3) C11 .055(10) .070(12) .033(9) -.053(10) .005(8) -.009(8) Cl2 .047(3) .090(4) .060(3) -.013(3) .013(2) .002(3) 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 C1A C2A . 1.565(12) ? C1A B4A . 1.660(13) ? C1A B6A . 1.712(13) ? C1A B5A . 1.714(13) ? C1A TaA . 2.531(8) ? C1A H1A . 1.0001 ? C2A B8A . 1.626(13) ? C2A B7A . 1.717(13) ? C2A B6A . 1.737(13) ? C2A TaA . 2.518(8) ? C2A H2A . 1.0001 ? TaA N1A . 1.855(6) ? TaA N3A . 1.862(8) ? TaA O1 . 1.887(5) ? TaA B9A . 2.466(9) ? TaA B8A . 2.477(9) ? TaA B4A . 2.491(10) ? B4A B9A . 1.746(14) ? B4A B10A . 1.754(13) ? B4A B5A . 1.772(14) ? B4A H4A . 1.1200 ? B5A B10A . 1.758(16) ? B5A B11A . 1.778(16) ? B5A B6A . 1.785(16) ? B5A H5A . 1.1200 ? B6A B7A . 1.772(17) ? B6A B11A . 1.801(15) ? B6A H6A . 1.1200 ? B7A B11A . 1.761(17) ? B7A B8A . 1.762(16) ? B7A B12A . 1.792(17) ? B7A H7A . 1.1200 ? B8A B9A . 1.787(15) ? B8A B12A . 1.812(15) ? B8A H8A . 1.1200 ? B9A B10A . 1.753(15) ? B9A B12A . 1.760(14) ? B9A H9A . 1.1200 ? B10A B12A . 1.746(16) ? B10A B11A . 1.758(16) ? B10A H10A . 1.1200 ? B11A B12A . 1.748(18) ? B11A H11A . 1.1200 ? B12A H12A . 1.1200 ? N1A C3A . 1.303(10) ? C3A N2A . 1.305(11) ? C3A C4A . 1.499(12) ? C4A H4A1 . .9800 ? C4A H4A2 . .9800 ? C4A H4A3 . .9800 ? N2A C6A . 1.481(13) ? N2A C5A . 1.494(11) ? C5A H5A1 . .9800 ? C5A H5A2 . .9800 ? C5A H5A3 . .9800 ? C6A H6A1 . .9800 ? C6A H6A2 . .9800 ? C6A H6A3 . .9800 ? N3A C7A . 1.320(12) ? C7A N4A . 1.349(12) ? C7A C8A . 1.499(14) ? C8A H8A1 . .9800 ? C8A H8A2 . .9800 ? C8A H8A3 . .9800 ? N4A C10A . 1.440(12) ? N4A C9A . 1.453(12) ? C9A H9A1 . .9800 ? C9A H9A2 . .9800 ? C9A H9A3 . .9800 ? C10A H1A1 . .9800 ? C10A H1A2 . .9800 ? C10A H1A3 . .9800 ? O1 TaB . 1.936(4) ? C1B C2B . 1.582(11) ? C1B B4B . 1.694(11) ? C1B B6B . 1.701(13) ? C1B B5B . 1.720(12) ? C1B TaB . 2.504(7) ? C1B H1B . 1.0001 ? C2B B8B . 1.663(11) ? C2B B7B . 1.691(11) ? C2B B6B . 1.733(12) ? C2B TaB . 2.510(7) ? C2B H2B . 1.0001 ? TaB N1B . 1.863(7) ? TaB N3B . 1.881(6) ? TaB B9B . 2.473(8) ? TaB B4B . 2.487(8) ? TaB B8B . 2.515(8) ? B4B B10B . 1.761(12) ? B4B B9B . 1.777(12) ? B4B B5B . 1.805(12) ? B4B H4B . 1.1200 ? B5B B6B . 1.722(14) ? B5B B11B . 1.724(14) ? B5B B10B . 1.764(12) ? B5B H5B . 1.1200 ? B6B B11B . 1.722(14) ? B6B B7B . 1.774(14) ? B6B H6B . 1.1200 ? B7B B11B . 1.770(14) ? B7B B8B . 1.774(13) ? B7B B12B . 1.779(12) ? B7B H7B . 1.1200 ? B8B B12B . 1.752(12) ? B8B B9B . 1.783(12) ? B8B H8B . 1.1200 ? B9B B12B . 1.771(14) ? B9B B10B . 1.788(12) ? B9B H9B . 1.1200 ? B10B B12B . 1.780(13) ? B10B B11B . 1.819(13) ? B10B H10B . 1.1200 ? B11B B12B . 1.803(14) ? B11B H11B . 1.1200 ? B12B H12B . 1.1200 ? N1B C3B . 1.318(11) ? C3B N2B . 1.298(11) ? C3B C4B . 1.489(11) ? C4B H4B1 . .9800 ? C4B H4B2 . .9800 ? C4B H4B3 . .9800 ? N2B C5B . 1.433(11) ? N2B C6B . 1.480(11) ? C5B H5B1 . .9800 ? C5B H5B2 . .9800 ? C5B H5B3 . .9800 ? C6B H6B1 . .9800 ? C6B H6B2 . .9800 ? C6B H6B3 . .9800 ? N3B C7B . 1.288(9) ? C7B N4B . 1.315(10) ? C7B C8B . 1.491(12) ? C8B H8B1 . .9800 ? C8B H8B2 . .9800 ? C8B H8B3 . .9800 ? N4B C10B . 1.436(11) ? N4B C9B . 1.450(11) ? C9B H9B1 . .9800 ? C9B H9B2 . .9800 ? C9B H9B3 . .9800 ? C10B H1B1 . .9800 ? C10B H1B2 . .9800 ? C10B H1B3 . .9800 ? Cl1 C11 . 1.705(9) ? C11 Cl2 . 1.718(9) ? C11 H111 . .9900 ? C11 H112 . .9900 ? _cod_database_code 2012026