#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4062449.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_4062449 _journal_name_full 'Organometallics' _journal_year 2003 _chemical_formula_sum 'C22 H31 N O2 Si W ' _chemical_formula_moiety 'C22 H31 N O2 Si W ' _chemical_formula_weight 553.43 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,-y,1/2+z 1/2+x,1/2+y,z 1/2+x,1/2-y,1/2+z _cell_length_a 10.610(1) _cell_length_b 15.180(1) _cell_length_c 13.4861(9) _cell_angle_alpha 90 _cell_angle_beta 94.782(5) _cell_angle_gamma 90 _cell_volume 2164.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.2 _exptl_crystal_density_diffrn 1.698 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.015(2) 0.16382(1) 0.501(2) 0.01501(7) Uani 1.00 d . . . Si1 Si 0.237(2) 0.1391(1) 0.462(2) 0.0192(5) Uani 1.00 d . . . O1 O -0.156(3) 0.1426(5) 0.304(2) 0.033(2) Uani 1.00 d . . . O2 O 0.059(3) -0.0341(4) 0.454(2) 0.032(1) Uani 1.00 d . . . N1 N 0.315(3) 0.2537(5) 0.464(2) 0.024(1) Uani 1.00 d . . . C1 C -0.087(3) 0.1500(5) 0.376(2) 0.020(2) Uani 1.00 d . . . C2 C 0.046(3) 0.0413(5) 0.469(2) 0.020(1) Uani 1.00 d . . . C3 C 0.354(3) 0.0722(6) 0.543(2) 0.031(2) Uani 1.00 d . . . C4 C 0.260(3) 0.1034(7) 0.331(2) 0.031(2) Uani 1.00 d . . . C5 C 0.090(3) 0.2805(5) 0.419(2) 0.019(2) Uani 1.00 d . . . C6 C 0.001(3) 0.3385(6) 0.371(2) 0.025(3) Uani 1.00 d . . . C7 C 0.027(3) 0.4200(6) 0.333(2) 0.031(2) Uani 1.00 d . . . C8 C 0.152(3) 0.4486(6) 0.339(2) 0.032(2) Uani 1.00 d . . . C9 C 0.245(3) 0.3945(6) 0.383(2) 0.031(2) Uani 1.00 d . . . C10 C 0.212(3) 0.3129(7) 0.420(2) 0.023(2) Uani 1.00 d . . . C11 C 0.356(3) 0.2824(6) 0.569(2) 0.026(2) Uani 1.00 d . . . C12 C 0.430(3) 0.2592(6) 0.407(2) 0.033(2) Uani 1.00 d . . . C13 C -0.150(3) 0.1528(5) 0.601(2) 0.020(2) Uani 1.00 d . . . C14 C -0.126(3) 0.2439(5) 0.590(2) 0.020(2) Uani 1.00 d . . . C15 C -0.004(3) 0.2645(5) 0.637(2) 0.022(2) Uani 1.00 d . . . C16 C 0.048(3) 0.1842(6) 0.679(2) 0.019(2) Uani 1.00 d . . . C17 C -0.043(3) 0.1147(5) 0.656(2) 0.020(1) Uani 1.00 d . . . C18 C -0.271(3) 0.1058(7) 0.572(2) 0.030(2) Uani 1.00 d . . . C19 C -0.222(3) 0.3088(7) 0.548(2) 0.029(2) Uani 1.00 d . . . C20 C 0.048(3) 0.3551(9) 0.650(2) 0.026(2) Uani 1.00 d . . . C21 C 0.164(3) 0.1731(6) 0.749(2) 0.023(2) Uani 1.00 d . . . C22 C -0.025(3) 0.0216(6) 0.694(2) 0.031(2) Uani 1.00 d . . . H1 H 0.3244 0.0113 0.5311 0.0379 Uiso 1.00 calc . . . H2 H 0.4247 0.0849 0.5240 0.0379 Uiso 1.00 calc . . . H3 H 0.3354 0.0865 0.6094 0.0379 Uiso 1.00 calc . . . H4 H 0.2132 0.0461 0.3204 0.0385 Uiso 1.00 calc . . . H5 H 0.2060 0.1436 0.2859 0.0385 Uiso 1.00 calc . . . H6 H 0.3355 0.1023 0.3221 0.0385 Uiso 1.00 calc . . . H7 H -0.0980 0.3192 0.3618 0.0299 Uiso 1.00 calc . . . H8 H -0.0520 0.4559 0.3036 0.0376 Uiso 1.00 calc . . . H9 H 0.1601 0.5047 0.3141 0.0389 Uiso 1.00 calc . . . H10 H 0.3185 0.4127 0.3881 0.0368 Uiso 1.00 calc . . . H11 H 0.4080 0.2444 0.5967 0.0310 Uiso 1.00 calc . . . H12 H 0.3740 0.3411 0.5687 0.0310 Uiso 1.00 calc . . . H13 H 0.2727 0.2795 0.6081 0.0310 Uiso 1.00 calc . . . H14 H 0.4827 0.2213 0.4362 0.0390 Uiso 1.00 calc . . . H15 H 0.3985 0.2420 0.3394 0.0390 Uiso 1.00 calc . . . H16 H 0.4498 0.3182 0.4081 0.0390 Uiso 1.00 calc . . . H17 H -0.3396 0.1447 0.5357 0.0369 Uiso 1.00 calc . . . H18 H -0.2662 0.0566 0.5307 0.0369 Uiso 1.00 calc . . . H19 H -0.3190 0.0856 0.6295 0.0369 Uiso 1.00 calc . . . H20 H -0.1963 0.3663 0.5490 0.0340 Uiso 1.00 calc . . . H21 H -0.2618 0.2936 0.4822 0.0340 Uiso 1.00 calc . . . H22 H -0.3039 0.3101 0.5880 0.0340 Uiso 1.00 calc . . . H23 H 0.1199 0.3533 0.6816 0.0356 Uiso 1.00 calc . . . H24 H 0.0400 0.3835 0.5860 0.0356 Uiso 1.00 calc . . . H25 H -0.0153 0.3903 0.6887 0.0356 Uiso 1.00 calc . . . H26 H 0.1282 0.1575 0.8130 0.0283 Uiso 1.00 calc . . . H27 H 0.2036 0.1278 0.7251 0.0283 Uiso 1.00 calc . . . H28 H 0.1969 0.2269 0.7525 0.0283 Uiso 1.00 calc . . . H29 H -0.1082 -0.0133 0.6697 0.0371 Uiso 1.00 calc . . . H30 H 0.0372 -0.0026 0.6698 0.0371 Uiso 1.00 calc . . . H31 H -0.0300 0.0216 0.7639 0.0371 Uiso 1.00 calc . . . 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 0.0127(1) 0.0152(1) 0.0168(1) -0.0005(2) -0.00028(8) 0.0000(2) Si1 0.0131(9) 0.0186(9) 0.0259(10) 0.0023(8) 0.0013(8) -0.0001(8) O1 0.034(4) 0.034(3) 0.027(3) 0.004(3) -0.015(2) -0.013(3) O2 0.037(4) 0.021(2) 0.040(3) 0.004(3) 0.008(3) -0.003(2) N1 0.023(3) 0.017(2) 0.032(3) 0.001(2) 0.004(2) 0.002(2) C1 0.014(4) 0.021(3) 0.025(3) 0.003(3) -0.006(2) -0.006(3) C2 0.014(3) 0.017(2) 0.027(4) 0.000(3) -0.003(2) 0.004(2) C3 0.018(4) 0.024(4) 0.049(5) 0.005(3) -0.005(3) 0.014(3) C4 0.022(4) 0.039(4) 0.032(3) -0.002(3) 0.008(3) -0.017(3) C5 0.019(3) 0.016(3) 0.021(3) -0.002(2) 0.000(3) 0.000(2) C6 0.020(6) 0.027(5) 0.027(6) 0.006(3) -0.004(4) 0.004(3) C7 0.043(4) 0.028(4) 0.022(4) -0.005(4) 0.001(3) -0.001(3) C8 0.041(4) 0.022(4) 0.034(4) 0.002(3) 0.004(3) 0.008(3) C9 0.020(4) 0.031(4) 0.042(5) -0.005(3) 0.010(3) 0.007(3) C10 0.017(3) 0.028(3) 0.023(4) -0.002(3) -0.002(3) -0.002(3) C11 0.011(4) 0.030(4) 0.036(4) 0.004(3) -0.007(3) -0.005(3) C12 0.022(4) 0.029(4) 0.051(5) 0.004(3) 0.016(3) 0.002(4) C13 0.016(3) 0.026(3) 0.019(4) -0.002(2) 0.007(2) -0.006(3) C14 0.018(3) 0.024(3) 0.018(3) 0.008(2) 0.005(2) -0.001(2) C15 0.019(3) 0.022(3) 0.026(4) 0.000(3) 0.005(3) -0.004(3) C16 0.011(3) 0.029(3) 0.018(3) 0.002(2) -0.002(2) 0.000(3) C17 0.023(3) 0.022(3) 0.015(2) 0.000(2) 0.005(2) -0.003(2) C18 0.021(4) 0.039(5) 0.030(4) -0.012(4) -0.007(3) 0.005(4) C19 0.026(5) 0.026(4) 0.034(5) 0.015(4) 0.002(4) 0.003(4) C20 0.023(5) 0.026(4) 0.028(5) -0.007(4) -0.001(4) -0.004(4) C21 0.013(3) 0.043(5) 0.011(3) 0.006(3) -0.002(2) -0.003(3) C22 0.047(5) 0.022(3) 0.024(4) -0.009(3) 0.014(3) 0.005(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 SI1 2.487(3) . . yes W1 C1 1.937(9) . . yes W1 C2 1.943(8) . . yes W1 C5 2.263(8) . . yes W1 C13 2.302(9) . . yes W1 C14 2.335(7) . . yes W1 C15 2.406(8) . . yes W1 C16 2.413(8) . . yes W1 C17 2.342(7) . . yes SI1 N1 1.925(8) . . yes SI1 C3 1.878(9) . . yes SI1 C4 1.882(9) . . yes O1 C1 1.18(1) . . yes O2 C2 1.17(1) . . yes N1 C10 1.50(1) . . yes N1 C11 1.50(1) . . yes N1 C12 1.50(1) . . yes C5 C6 1.41(1) . . yes C5 C10 1.39(1) . . yes C6 C7 1.37(2) . . yes C7 C8 1.40(2) . . yes C8 C9 1.38(1) . . yes C9 C10 1.39(1) . . yes C13 C14 1.42(1) . . yes C13 C17 1.42(1) . . yes C13 C18 1.49(1) . . yes C14 C15 1.42(1) . . yes C14 C19 1.50(1) . . yes C15 C16 1.43(1) . . yes C15 C20 1.49(1) . . yes C16 C17 1.44(1) . . yes C16 C21 1.50(1) . . yes C17 C22 1.51(1) . . yes