#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/69/2006986.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_2006986 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1998 _journal_volume 54 _journal_page_first 225 _journal_page_last 227 _publ_section_title ; A Dinuclear Tungsten(III) Complex Containing a Tungsten--Tungsten Triple Bond with an Asymmetric Arrangement of Ligands: [W~2~Cl~3~(OCMe~3~)~3~(NHMe~2~)~2~] ; loop_ _publ_author_name 'Malcolm H. Chisholm' 'Kirsten Folting' 'De-Dong Wu' _chemical_formula_moiety 'C16 H41 Cl3 N2 O3 W2' _chemical_formula_sum 'C16 H41 Cl3 N2 O3 W2' _chemical_formula_iupac '[W2 Cl3 (C4 H9 O)3 (C2 H7 N)2]' _chemical_formula_weight 783.56 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a b' _symmetry_space_group_name_Hall '-P 2bc -2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y, -z-1/2' '-x-1/2, y-1/2, -z' 'x, y-1/2, -z-1/2' _cell_length_a 13.705(2) _cell_length_b 32.939(4) _cell_length_c 11.6224(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5246.6(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.984 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .039 _refine_ls_wR_factor_obs .0844 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 W1 .52855(2) .156113(10) .81412(3) .02776(12) Uani d . 1 . W W2 .53847(2) .092733(11) .72875(3) .03035(12) Uani d . 1 . W Cl3 .6067(2) .20302(6) .6872(2) .0348(5) Uani d . 1 . Cl N4 .6807(5) .1534(2) .8875(6) .032(2) Uani d . 1 . N C5 .6979(7) .1861(3) .9709(9) .044(2) Uani d . 1 . C C6 .7694(6) .1496(3) .8111(9) .036(2) Uani d . 1 . C O7 .4939(4) .1496(2) .9700(5) .0347(15) Uani d . 1 . O C8 .4668(7) .1303(3) 1.0735(8) .040(2) Uani d . 1 . C C9 .4843(7) .1599(4) 1.1701(9) .048(3) Uani d . 1 . C C10 .3569(7) .1201(3) 1.0683(9) .044(2) Uani d . 1 . C C11 .5265(8) .0920(3) 1.0906(9) .052(3) Uani d . 1 . C O12 .4042(4) .1720(2) .7548(5) .0315(14) Uani d . 1 . O C13 .3501(6) .2091(3) .7747(8) .034(2) Uani d . 1 . C C14 .4023(7) .2363(3) .8574(9) .045(2) Uani d . 1 . C C15 .2511(7) .1969(3) .8208(8) .041(2) Uani d . 1 . C C16 .3393(7) .2295(3) .6574(9) .045(2) Uani d . 1 . C Cl17 .6512(2) .09890(7) .5760(2) .0376(5) Uani d . 1 . Cl Cl18 .3983(2) .06180(7) .8072(2) .0437(6) Uani d . 1 . Cl N19 .4296(6) .1079(3) .5870(7) .040(2) Uani d . 1 . N C20 .3976(8) .0709(4) .5250(9) .054(3) Uani d . 1 . C C21 .4506(7) .1405(3) .5031(8) .043(2) Uani d . 1 . C O22 .6322(4) .0691(2) .8292(5) .0329(14) Uani d . 1 . O C23 .6766(7) .0285(3) .8259(8) .040(2) Uani d . 1 . C C24 .7832(7) .0353(3) .7995(9) .048(3) Uani d . 1 . C C25 .6640(8) .0099(3) .9434(9) .049(3) Uani d . 1 . C C26 .6300(8) .0022(3) .7333(9) .046(2) Uani d . 1 . C H1 .6818 .1288 .9336 .028 Uiso d . 1 . H H2 .7558 .1806 1.0129 .043 Uiso d . 1 . H H3 .7030 .2107 .9314 .043 Uiso d . 1 . H H4 .6440 .1871 1.0235 .043 Uiso d . 1 . H H5 .8255 .1446 .8554 .035 Uiso d . 1 . H H6 .7593 .1284 .7572 .035 Uiso d . 1 . H H7 .7769 .1747 .7702 .035 Uiso d . 1 . H H8 .5524 .1655 1.1732 .046 Uiso d . 1 . H H9 .4493 .1840 1.1562 .046 Uiso d . 1 . H H10 .4640 .1481 1.2406 .046 Uiso d . 1 . H H11 .3228 .1423 1.0377 .042 Uiso d . 1 . H H12 .3492 .0968 1.0215 .042 Uiso d . 1 . H H13 .3345 .1143 1.1442 .042 Uiso d . 1 . H H14 .5065 .0790 1.1581 .046 Uiso d . 1 . H H15 .5170 .0753 1.0256 .046 Uiso d . 1 . H H16 .5931 .0998 1.0958 .046 Uiso d . 1 . H H17 .4241 .2213 .9229 .043 Uiso d . 1 . H H18 .4578 .2485 .8214 .043 Uiso d . 1 . H H19 .3596 .2574 .8830 .043 Uiso d . 1 . H H20 .2155 .2203 .8406 .039 Uiso d . 1 . H H21 .2169 .1818 .7638 .039 Uiso d . 1 . H H22 .2598 .1802 .8873 .039 Uiso d . 1 . H H23 .4025 .2343 .6261 .043 Uiso d . 1 . H H24 .3040 .2121 .6073 .043 Uiso d . 1 . H H25 .3059 .2543 .6667 .043 Uiso d . 1 . H H26 .3723 .1178 .6283 .038 Uiso d . 1 . H H27 .3400 .0771 .4819 .052 Uiso d . 1 . H H28 .4474 .0624 .4758 .052 Uiso d . 1 . H H29 .3825 .0503 .5796 .052 Uiso d . 1 . H H30 .4721 .1646 .5419 .041 Uiso d . 1 . H H31 .5011 .1318 .4526 .041 Uiso d . 1 . H H32 .3940 .1469 .4596 .041 Uiso d . 1 . H H33 .8162 .0095 .7956 .045 Uiso d . 1 . H H34 .7899 .0483 .7264 .045 Uiso d . 1 . H H35 .8127 .0513 .8569 .045 Uiso d . 1 . H H36 .5972 .0039 .9576 .044 Uiso d . 1 . H H37 .7008 -.0148 .9488 .044 Uiso d . 1 . H H38 .6870 .0281 1.0014 .044 Uiso d . 1 . H H39 .5646 -.0030 .7503 .044 Uiso d . 1 . H H40 .6360 .0152 .6604 .044 Uiso d . 1 . H H41 .6651 -.0233 .7292 .044 Uiso d . 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 W1 .0292(2) .0289(2) .0252(2) .00000(14) .00027(15) -.00006(14) W2 .0357(2) .0290(2) .0263(2) -.0007(2) -.00023(15) -.0006(2) Cl3 .0361(11) .0348(11) .0335(11) -.0004(9) .0039(10) .0046(9) N4 .037(4) .032(4) .025(4) -.003(3) .004(3) .011(3) C5 .044(5) .044(6) .042(6) .000(4) -.012(5) -.005(5) C6 .036(5) .030(5) .043(5) -.002(4) .000(4) -.001(4) O7 .037(3) .048(4) .019(3) -.004(3) .003(3) .001(3) C8 .049(6) .041(6) .031(5) -.001(4) -.002(5) .007(4) C9 .036(5) .073(8) .035(6) -.001(5) -.006(4) .001(5) C10 .045(6) .055(6) .032(5) -.001(5) .001(5) .002(5) C11 .053(6) .058(7) .046(6) .014(5) .001(5) .012(5) O12 .026(3) .040(3) .028(3) -.002(2) -.003(3) .004(3) C13 .035(4) .033(5) .035(5) .007(4) -.003(4) -.003(4) C14 .040(5) .042(5) .054(6) .005(4) -.004(5) .002(5) C15 .041(5) .047(5) .035(5) .002(4) -.002(4) -.005(5) C16 .043(5) .052(6) .040(6) .013(5) .005(5) .009(5) Cl17 .0416(12) .0426(13) .0287(11) .0026(10) .0020(9) -.0008(10) Cl18 .0478(13) .0457(14) .0377(13) -.0137(11) .0030(11) -.0013(11) N19 .037(4) .049(5) .035(5) .006(4) -.004(4) -.001(4) C20 .058(6) .069(7) .035(6) -.009(6) -.009(5) -.013(5) C21 .045(5) .056(6) .029(5) .007(5) -.003(4) .002(5) O22 .037(3) .032(3) .030(3) .005(3) -.001(3) .004(3) C23 .055(6) .030(5) .036(5) .007(4) -.001(5) -.003(4) C24 .051(6) .051(6) .043(6) .014(5) .006(5) -.001(5) C25 .052(6) .046(6) .048(6) .010(5) .003(5) .010(5) C26 .064(6) .032(5) .042(6) .003(5) .008(5) -.001(5) 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 W1 O7 . 1.885(6) yes W1 O12 . 1.911(6) yes W1 N4 . 2.255(7) yes W1 W2 . 2.3155(5) yes W1 Cl3 . 2.390(2) yes W2 O22 . 1.903(6) yes W2 N19 . 2.278(8) yes W2 Cl18 . 2.358(2) yes W2 Cl17 . 2.363(2) yes N4 C5 . 1.467(12) ? N4 C6 . 1.511(11) ? O7 C8 . 1.411(11) ? C8 C9 . 1.507(14) ? C8 C11 . 1.517(14) ? C8 C10 . 1.544(14) ? O12 C13 . 1.449(10) ? C13 C14 . 1.495(13) ? C13 C15 . 1.512(13) ? C13 C16 . 1.527(13) ? N19 C21 . 1.478(13) ? N19 C20 . 1.483(13) ? O22 C23 . 1.468(10) ? C23 C25 . 1.508(14) ? C23 C24 . 1.509(14) ? C23 C26 . 1.523(14) ? _cod_database_code 2006986