#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006430.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_2006430 _journal_name_full 'Acta Crystallographica' _journal_year 1997 _journal_volume C53 _journal_page_first 1061 _journal_page_last 1063 _publ_section_title ; Bis(carbazolate) Pentakis(tetrahydrofuran)barium Tetrahydrofuran Solvate ; loop_ _publ_author_name 'N\"ather, Christian' 'Hauck, Tim' 'Bock, Hans' _chemical_name_common Carbazole-barium-pentakis(THF)-THF _chemical_formula_moiety '2(C12 H8 N1) - , [Ba(C4 H8 O1)5] 2+ , C4 H8 O1' _chemical_formula_sum 'C48 H64 Ba N2 O6' _chemical_formula_weight 902.35 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 15.7566(9) _cell_length_b 15.9146(9) _cell_length_c 9.5363(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.854(5) _cell_angle_gamma 90.00 _cell_volume 2288.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _exptl_crystal_density_diffrn 1.309 _diffrn_ambient_temperature 200(2) _refine_ls_R_factor_obs .0233 _refine_ls_wR_factor_obs .0564 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol N1 .13719(13) -.0266(2) -.1227(2) .0457(4) Uani d . 1 . N C1 .0930(2) .0900(2) -.3039(3) .0497(6) Uani d . 1 . C H1 .0312(2) .0832(2) -.3179(3) .060 Uiso calc R 1 . H C2 .1231(2) .1527(2) -.3765(3) .0570(7) Uani d . 1 . C H2 .0817(2) .1898(2) -.4386(3) .068 Uiso calc R 1 . H C3 .2148(3) .1630(2) -.3604(3) .0587(7) Uani d . 1 . C H3 .2343(3) .2063(2) -.4122(3) .070 Uiso calc R 1 . H C4 .2758(2) .1099(2) -.2693(3) .0509(6) Uani d . 1 . C H4 .3372(2) .1162(2) -.2593(3) .061 Uiso calc R 1 . H C5 .24701(14) .0466(2) -.1915(2) .0402(5) Uani d . 1 . C C6 .15405(13) .0359(2) -.2087(2) .0404(4) Uani d . 1 . C C7 .2405(3) -.1201(2) .0589(4) .0619(8) Uani d . 1 . C H7 .1948(3) -.1496(2) .0849(4) .074 Uiso calc R 1 . H C8 .3290(3) -.1390(3) .1258(4) .0718(10) Uani d . 1 . C H8 .3435(3) -.1816(3) .1987(4) .086 Uiso calc R 1 . H C9 .3979(3) -.0968(3) .0883(5) .0697(10) Uani d . 1 . C H9 .4579(3) -.1110(3) .1360(5) .084 Uiso calc R 1 . H C10 .3786(2) -.0350(3) -.0171(4) .0570(6) Uani d . 1 . C H10 .4249(2) -.0066(3) -.0432(4) .068 Uiso calc R 1 . H C11 .28934(14) -.0145(2) -.0856(3) .0419(9) Uani d . 1 . C C12 .2197(2) -.0569(2) -.0470(3) .0447(5) Uani d . 1 . C Ba1 0 0 0 .03057(4) Uani d S 1 . Ba O1 .10277(13) -.0366(2) .2848(2) .0545(5) Uani d . 1 . O C21 .0768(2) -.0700(3) .4035(3) .0607(8) Uani d . 1 . C H21A .0224(2) -.1043(3) .3667(3) .073 Uiso calc R 1 . H H21B .0643(2) -.0240(3) .4645(3) .073 Uiso calc R 1 . H C22 .1519(3) -.1236(3) .4924(4) .0681(9) Uani d . 1 . C H22A .1446(3) -.1829(3) .4598(4) .082 Uiso calc R 1 . H H22B .1565(3) -.1208(3) .5980(4) .082 Uiso calc R 1 . H C23 .2319(2) -.0841(3) .4612(4) .0614(8) Uani d . 1 . C H23A .2642(2) -.1259(3) .4191(4) .074 Uiso calc R 1 . H H23B .2731(2) -.0608(3) .5519(4) .074 Uiso calc R 1 . H C24 .1941(2) -.0143(2) .3513(3) .0560(11) Uani d . 1 . C H24A .1986(2) .0407(2) .4015(3) .067 Uiso calc R 1 . H H24B .2265(2) -.0111(2) .2766(3) .067 Uiso calc R 1 . H O2 .1039(2) .1404(2) .1011(2) .0538(5) Uani d . 1 . O C31 .1906(2) .1606(2) .0892(3) .0543(6) Uani d . 1 . C H31A .1861(2) .1879(2) -.0060(3) .065 Uiso calc R 1 . H H31B .2272(2) .1092(2) .0975(3) .065 Uiso calc R 1 . H C32 .2309(3) .2203(3) .2152(4) .0682(10) Uani d . 1 . C H32A .2646(3) .1891(3) .3038(4) .082 Uiso calc R 1 . H H32B .2708(3) .2614(3) .1885(4) .082 Uiso calc R 1 . H C33 .1511(3) .2633(2) .2398(4) .0685(10) Uani d . 1 . C H33A .1632(3) .2839(2) .3417(4) .082 Uiso calc PR .70 1 H H33B .1304(3) .3106(2) .1709(4) .082 Uiso calc PR .70 1 H H33C .1520(3) .3240(2) .2171(4) .082 Uiso calc PR .30 2 H H33D .1518(3) .2574(2) .3435(4) .082 Uiso calc PR .30 2 H C34 .0876(4) .1939(4) .2097(6) .0625(12) Uani d P .70 1 C H34A .0934(4) .1616(4) .3007(6) .075 Uiso calc PR .70 1 H H34B .0265(4) .2163(4) .1752(6) .075 Uiso calc PR .70 1 H C34' .0643(6) .2208(7) .1355(11) .047(2) Uiso d P .30 2 C H34C .0190(6) .2105(7) .1870(11) .056 Uiso calc PR .30 2 H H34D .0382(6) .2547(7) .0464(11) .056 Uiso calc PR .30 2 H O3 0 -.1750(3) 0 .0861(15) Uani d S 1 . O C41 -.0269(5) -.3134(3) .0565(6) .091(2) Uani d . 1 . C H41A -.0906(5) -.3237(3) .0080(6) .109 Uiso calc PR .75 3 H H41B -.0044(5) -.3567(3) .1329(6) .109 Uiso calc PR .75 3 H H41C -.0731(5) -.3576(3) .0350(6) .109 Uiso calc PR .25 4 H H41D .0119(5) -.3200(3) .1581(6) .109 Uiso calc PR .25 4 H C42 -.0120(4) -.2265(3) .1207(5) .0608(10) Uani d P .75 3 C H42A -.0638(4) -.2072(3) .1509(5) .073 Uiso calc PR .75 3 H H42B .0415(4) -.2246(3) .2064(5) .073 Uiso calc PR .75 3 H C42' -.0621(11) -.2361(13) .032(2) .071(4) Uiso d P .25 4 C H42C -.0788(11) -.2173(13) .120(2) .085 Uiso calc PR .25 4 H H42D -.1168(11) -.2382(13) -.052(2) .085 Uiso calc PR .25 4 H O4 .5000 -.003(2) .5000 .355(10) Uiso d SD 1 . O C51 .4259(12) .0623(10) .4405(18) .215(7) Uiso d D 1 . C H51A .3638(12) .0491(10) .4081(18) .258 Uiso d R 1 . H H51B .4492(12) .0676(10) .3584(18) .258 Uiso d R 1 . H C52 .4566(10) .1503(14) .442(2) .146(7) Uiso d PD .50 5 C H52A .4426(10) .1389(14) .530(2) .175 Uiso d PR .50 5 H H52B .4243(10) .1992(14) .395(2) .175 Uiso d PR .50 5 H C52' .464(2) .136(2) .542(4) .259(19) Uiso d PD .50 6 C H52C .488(2) .170(2) .627(4) .311 Uiso d PR .50 6 H H52D .476(2) .163(2) .460(4) .311 Uiso d PR .50 6 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 N1 .0415(8) .0479(12) .0532(10) -.0075(7) .0223(7) -.0082(8) C1 .0440(10) .057(2) .0443(10) -.0021(10) .0067(8) -.0116(11) C2 .065(2) .053(2) .0451(11) .0010(13) .0041(11) -.0051(11) C3 .074(2) .052(2) .0493(12) -.0152(15) .0165(12) -.0026(12) C4 .0512(12) .051(2) .0536(12) -.0140(11) .0202(10) -.0067(12) C5 .0367(8) .0423(14) .0440(9) -.0073(8) .0155(7) -.0110(8) C6 .0381(8) .0452(11) .0406(8) -.0073(8) .0157(7) -.0138(9) C7 .084(2) .046(2) .067(2) .006(2) .040(2) .0049(14) C8 .100(3) .054(2) .063(2) .025(2) .025(2) .005(2) C9 .064(2) .064(2) .075(2) .022(2) .0116(15) -.006(2) C10 .0450(11) .052(2) .072(2) .0059(12) .0148(11) -.0088(15) C11 .0407(8) .037(3) .0516(9) .0011(7) .0198(7) -.0077(8) C12 .0501(11) .0402(12) .0501(11) -.0011(9) .0244(9) -.0064(10) Ba1 .03438(6) .02585(7) .03276(6) .000 .01179(4) .000 O1 .0538(9) .0656(13) .0407(7) .0133(10) .0086(7) .0132(9) C21 .065(2) .067(2) .0504(13) .014(2) .0166(12) .0070(13) C22 .087(2) .057(2) .0550(14) .017(2) .0121(14) .0165(15) C23 .065(2) .060(2) .0507(13) .0193(15) .0033(11) .0073(13) C24 .0643(13) .047(3) .0491(10) .0073(12) .0036(9) .0014(10) O2 .0653(11) .0389(11) .0570(10) -.0151(9) .0176(9) -.0145(9) C31 .067(2) .047(2) .0483(12) -.0153(13) .0148(11) -.0103(11) C32 .078(2) .067(2) .0540(14) -.029(2) .0099(14) -.017(2) C33 .104(3) .042(2) .0497(13) -.007(2) .006(2) -.0121(12) C34 .070(3) .057(3) .060(2) -.009(2) .018(2) -.021(2) O3 .114(3) .032(2) .137(4) .000 .074(3) .000 C41 .146(5) .041(2) .081(3) -.013(3) .027(3) .002(2) C42 .084(3) .035(2) .054(2) -.005(2) .006(2) .0005(15) 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 N1 C6 . 1.363(4) n N1 C12 . 1.379(4) n N1 Ba1 . 2.772(2) y C1 C2 . 1.374(5) n C1 C6 . 1.409(4) n C2 C3 . 1.417(5) n C3 C4 . 1.382(5) n C4 C5 . 1.402(4) n C5 C11 . 1.421(4) n C5 C6 . 1.436(3) n C7 C8 . 1.389(6) n C7 C12 . 1.395(5) n C8 C9 . 1.407(7) n C9 C10 . 1.376(6) n C10 C11 . 1.407(3) n C11 C12 . 1.425(3) n Ba1 N1 2 2.772(2) y Ba1 O2 . 2.773(2) y Ba1 O2 2 2.773(2) y Ba1 O3 . 2.785(4) y Ba1 O1 2 2.790(2) y Ba1 O1 . 2.790(2) y O1 C21 . 1.414(4) n O1 C24 . 1.439(4) n C21 C22 . 1.505(5) n C22 C23 . 1.514(6) n C23 C24 . 1.524(5) n O2 C34 . 1.420(5) n O2 C31 . 1.440(4) n O2 C34' . 1.500(11) n C31 C32 . 1.519(4) n C32 C33 . 1.509(7) n C33 C34 . 1.461(7) n C33 C34' . 1.590(10) n O3 C42 . 1.469(5) n O3 C42 2 1.469(5) n O3 C42' . 1.47(2) n O3 C42' 2 1.47(2) n C41 C42' . 1.34(2) n C41 C42 . 1.503(7) n C41 C41 2 1.552(12) n O4 O4 2_656 .00(7) n O4 C51 2_656 1.54(3) n O4 C51 . 1.54(3) n C51 C52 . 1.48(2) n C51 C52' . 1.53(3) n C51 O4 2_656 1.54(3) n C52 C52 2_656 1.50(2) n C52' C52' 2_656 1.56(3) n