#------------------------------------------------------------------------------ #$Date: 2010-01-30 14:59:17 +0100 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/7/7100263.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_7100263 _journal_name_full 'Chemical Communications' _journal_year 2005 _publ_section_title ; Crystalline Na-Si(NN) derivatives [Si(NN) = Si{(NCH2tBu)2C6H4-1,2}]: the silylenoid [Si(NN)OMe]-, the dianion [(NN)Si-Si(NN)]2-, and the radical anion c-[Si(NN)]3-. ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Barbara Gehrhus' 'Floria Antolini' 'P. B. Hitchcock' 'M. Lappert' _chemical_formula_moiety 'C50 H94 N4 Na2 O6 Si2' _chemical_formula_structural 'C50 H94 N4 Na2 O6 Si2' _chemical_formula_sum 'C50 H94 N4 Na2 O6 Si2' _chemical_formula_weight 949.45 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0924(4) _cell_length_b 11.3065(5) _cell_length_c 21.7705(8) _cell_angle_alpha 90 _cell_angle_beta 102.275(2) _cell_angle_gamma 90 _cell_volume 2908.47(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_wavelength 0.71073 _exptl_crystal_density_diffrn 1.084 _diffrn_ambient_temperature 173(2) 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.37297(9) 0.86726(9) 0.04340(5) 0.0382(4) Uani 1 1 d . . . Na Na 0.63477(12) 0.89234(13) 0.01784(7) 0.0438(5) Uani 1 1 d . . . O1 O 0.4903(2) 0.7816(2) 0.04038(13) 0.0455(7) Uani 1 1 d . . . O2 O 0.7687(3) 0.8638(3) 0.11447(17) 0.0731(10) Uani 1 1 d . . . O3 O 0.7686(4) 0.8030(4) -0.0322(2) 0.1000(15) Uani 1 1 d . . . N1 N 0.2512(2) 0.7771(3) 0.01448(14) 0.0390(8) Uani 1 1 d . . . N2 N 0.3539(3) 0.8331(3) 0.12148(15) 0.0408(8) Uani 1 1 d . . . C1 C 0.2092(3) 0.7187(3) 0.06136(19) 0.0412(9) Uani 1 1 d . . . C2 C 0.2690(3) 0.7504(4) 0.12273(19) 0.0426(9) Uani 1 1 d . . . C3 C 0.2392(4) 0.6990(4) 0.1747(2) 0.0559(11) Uani 1 1 d . . . H3 H 0.2789 0.7191 0.2158 0.067 Uiso 1 1 calc R . . C4 C 0.1501(5) 0.6173(5) 0.1662(3) 0.0711(15) Uani 1 1 d . . . H4 H 0.1304 0.5812 0.2018 0.085 Uiso 1 1 calc R . . C5 C 0.0914(4) 0.5889(5) 0.1073(3) 0.0733(15) Uani 1 1 d . . . H5 H 0.0301 0.5347 0.1024 0.088 Uiso 1 1 calc R . . C6 C 0.1202(4) 0.6382(4) 0.0545(2) 0.0580(12) Uani 1 1 d . . . H6 H 0.0793 0.6172 0.0137 0.07 Uiso 1 1 calc R . . C7 C 0.1833(3) 0.7833(4) -0.04966(19) 0.0472(10) Uani 1 1 d . . . H7A H 0.1839 0.8664 -0.064 0.057 Uiso 1 1 calc R . . H7B H 0.1042 0.7636 -0.0481 0.057 Uiso 1 1 calc R . . C8 C 0.2184(4) 0.7041(4) -0.0999(2) 0.0538(11) Uani 1 1 d . . . C9 C 0.2322(5) 0.5756(4) -0.0799(3) 0.0726(15) Uani 1 1 d . . . H9A H 0.2912 0.569 -0.0415 0.109 Uiso 1 1 calc R . . H9B H 0.2537 0.5288 -0.1134 0.109 Uiso 1 1 calc R . . H9C H 0.1604 0.5458 -0.0719 0.109 Uiso 1 1 calc R . . C10 C 0.3305(4) 0.7491(5) -0.1124(2) 0.0702(14) Uani 1 1 d . . . H10A H 0.3514 0.7022 -0.1461 0.105 Uiso 1 1 calc R . . H10B H 0.3896 0.7416 -0.0741 0.105 Uiso 1 1 calc R . . H10C H 0.3226 0.8323 -0.1251 0.105 Uiso 1 1 calc R . . C11 C 0.1252(5) 0.7143(6) -0.1591(2) 0.0835(18) Uani 1 1 d . . . H11A H 0.0539 0.6848 -0.1504 0.125 Uiso 1 1 calc R . . H11B H 0.1457 0.6673 -0.1928 0.125 Uiso 1 1 calc R . . H11C H 0.1162 0.7973 -0.1721 0.125 Uiso 1 1 calc R . . C12 C 0.4378(4) 0.8610(4) 0.1787(2) 0.0537(11) Uani 1 1 d . . . H12A H 0.5132 0.8637 0.1678 0.064 Uiso 1 1 calc R . . H12B H 0.439 0.7951 0.2087 0.064 Uiso 1 1 calc R . . C13 C 0.4216(5) 0.9763(4) 0.2125(2) 0.0719(15) Uani 1 1 d . . . C14 C 0.5146(7) 0.9782(7) 0.2734(3) 0.118(3) Uani 1 1 d . . . H14A H 0.5075 1.0506 0.2971 0.176 Uiso 1 1 calc R . . H14B H 0.5892 0.9761 0.2627 0.176 Uiso 1 1 calc R . . H14C H 0.5059 0.9091 0.2992 0.176 Uiso 1 1 calc R . . C15 C 0.3027(7) 0.9806(6) 0.2287(3) 0.099(2) Uani 1 1 d . . . H15A H 0.2444 0.9781 0.1898 0.148 Uiso 1 1 calc R . . H15B H 0.295 1.0539 0.2515 0.148 Uiso 1 1 calc R . . H15C H 0.2935 0.9125 0.255 0.148 Uiso 1 1 calc R . . C16 C 0.4331(6) 1.0828(5) 0.1720(3) 0.0854(19) Uani 1 1 d . . . H16A H 0.5073 1.0811 0.1607 0.128 Uiso 1 1 calc R . . H16B H 0.4261 1.1554 0.1955 0.128 Uiso 1 1 calc R . . H16C H 0.3735 1.0808 0.1337 0.128 Uiso 1 1 calc R . . C17 C 0.7784(10) 0.9160(10) 0.1713(4) 0.157(4) Uani 1 1 d . . . H17A H 0.704 0.9206 0.1834 0.188 Uiso 1 1 calc R . . H17B H 0.81 0.9968 0.1713 0.188 Uiso 1 1 calc R . . C18 C 0.855(2) 0.8392(13) 0.2133(6) 0.44(2) Uani 1 1 d . . . H18A H 0.9289 0.8799 0.2255 0.53 Uiso 1 1 calc R . . H18B H 0.8253 0.8286 0.252 0.53 Uiso 1 1 calc R . . C19 C 0.8717(8) 0.7389(9) 0.1927(4) 0.140(3) Uani 1 1 d . . . H19A H 0.8186 0.6791 0.2029 0.168 Uiso 1 1 calc R . . H19B H 0.9506 0.7119 0.208 0.168 Uiso 1 1 calc R . . C20 C 0.8471(12) 0.7685(10) 0.1236(5) 0.217(8) Uani 1 1 d . . . H20A H 0.9176 0.7919 0.1105 0.261 Uiso 1 1 calc R . . H20B H 0.8145 0.6991 0.0984 0.261 Uiso 1 1 calc R . . C21 C 0.8766(10) 0.8743(13) -0.0229(8) 0.224(8) Uani 1 1 d . . . H21A H 0.8798 0.9258 0.0143 0.269 Uiso 1 1 calc R . . H21B H 0.941 0.8186 -0.0125 0.269 Uiso 1 1 calc R . . C22 C 0.8935(8) 0.9461(9) -0.0730(6) 0.156(4) Uani 1 1 d . . . H22A H 0.8286 0.9991 -0.0859 0.234 Uiso 1 1 calc R . . H22B H 0.9013 0.896 -0.1086 0.234 Uiso 1 1 calc R . . H22C H 0.9625 0.9931 -0.0595 0.234 Uiso 1 1 calc R . . C23 C 0.7922(9) 0.7038(9) -0.0615(6) 0.166(5) Uani 1 1 d . . . H23A H 0.8543 0.658 -0.035 0.2 Uiso 1 1 calc R . . H23B H 0.8122 0.7218 -0.1023 0.2 Uiso 1 1 calc R . . C24 C 0.6799(6) 0.6393(6) -0.0703(4) 0.104(2) Uani 1 1 d . . . H24A H 0.6207 0.6866 -0.097 0.156 Uiso 1 1 calc R . . H24B H 0.6606 0.6269 -0.0293 0.156 Uiso 1 1 calc R . . H24C H 0.6858 0.5625 -0.0903 0.156 Uiso 1 1 calc R . . C25 C 0.5020(4) 0.6628(4) 0.0631(2) 0.0593(12) Uani 1 1 d . . . H25A H 0.4448 0.647 0.0879 0.089 Uiso 1 1 calc R . . H25B H 0.5777 0.6519 0.0895 0.089 Uiso 1 1 calc R . . H25C H 0.4915 0.6081 0.0274 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0406(6) 0.0351(6) 0.0404(6) 0.0035(4) 0.0121(4) -0.0018(4) Na 0.0391(8) 0.0398(8) 0.0518(9) 0.0096(7) 0.0078(7) -0.0010(6) O1 0.0375(14) 0.0412(15) 0.0583(17) 0.0092(13) 0.0113(12) 0.0001(11) O2 0.070(2) 0.071(2) 0.065(2) 0.0034(18) -0.0150(17) 0.0147(18) O3 0.125(4) 0.086(3) 0.085(3) -0.008(2) 0.012(3) 0.049(3) N1 0.0360(16) 0.0410(18) 0.0396(17) 0.0043(14) 0.0075(14) 0.0045(14) N2 0.0436(17) 0.0380(17) 0.0406(17) 0.0035(14) 0.0081(14) -0.0039(14) C1 0.0327(19) 0.042(2) 0.050(2) 0.0066(18) 0.0128(17) 0.0035(16) C2 0.038(2) 0.044(2) 0.048(2) 0.0076(18) 0.0129(17) 0.0014(17) C3 0.062(3) 0.054(3) 0.055(3) 0.012(2) 0.020(2) -0.003(2) C4 0.072(3) 0.079(4) 0.068(3) 0.025(3) 0.028(3) -0.013(3) C5 0.055(3) 0.077(3) 0.092(4) 0.012(3) 0.025(3) -0.026(3) C6 0.038(2) 0.067(3) 0.068(3) 0.006(2) 0.009(2) -0.010(2) C7 0.038(2) 0.057(2) 0.046(2) 0.0005(19) 0.0067(17) 0.0047(19) C8 0.047(2) 0.066(3) 0.048(2) -0.012(2) 0.0086(19) -0.004(2) C9 0.070(3) 0.055(3) 0.091(4) -0.023(3) 0.014(3) -0.009(3) C10 0.064(3) 0.094(4) 0.060(3) -0.023(3) 0.029(2) -0.010(3) C11 0.069(3) 0.126(5) 0.050(3) -0.020(3) -0.001(2) 0.001(3) C12 0.061(3) 0.052(3) 0.044(2) 0.0055(19) 0.003(2) -0.007(2) C13 0.114(4) 0.056(3) 0.044(3) -0.001(2) 0.011(3) -0.022(3) C14 0.178(8) 0.113(6) 0.048(3) -0.008(3) -0.008(4) -0.050(5) C15 0.153(6) 0.071(4) 0.087(4) -0.014(3) 0.060(4) -0.003(4) C16 0.141(5) 0.053(3) 0.061(3) -0.003(3) 0.019(3) -0.031(3) C17 0.201(10) 0.158(8) 0.089(5) -0.010(5) -0.019(6) 0.091(8) C18 0.82(5) 0.190(13) 0.164(12) -0.087(10) -0.25(2) 0.31(2) C19 0.141(7) 0.140(8) 0.131(8) 0.048(6) 0.010(6) 0.041(6) C20 0.284(15) 0.197(11) 0.116(7) -0.039(7) -0.079(9) 0.158(11) C21 0.156(10) 0.196(13) 0.38(2) 0.106(13) 0.186(13) 0.048(9) C22 0.116(7) 0.114(7) 0.242(13) 0.023(8) 0.047(8) 0.004(6) C23 0.144(9) 0.125(8) 0.213(12) -0.011(8) -0.001(8) 0.064(7) C24 0.105(5) 0.082(4) 0.120(6) 0.026(4) 0.013(4) -0.005(4) C25 0.049(2) 0.049(2) 0.083(3) 0.014(2) 0.019(2) 0.010(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si O1 1.731(3) . ? Si N1 1.792(3) . ? Si N2 1.805(3) . ? Si Na 3.0201(18) 3_675 ? Na O1 2.286(3) . ? Na O3 2.361(5) . ? Na O2 2.388(4) . ? O1 C25 1.428(5) . ? O2 C17 1.354(9) . ? O2 C20 1.421(9) . ? O3 C23 1.351(10) . ? O3 C21 1.511(13) . ? N1 C1 1.398(5) . ? N1 C7 1.463(5) . ? N2 C2 1.393(5) . ? N2 C12 1.464(5) . ? C1 C6 1.393(6) . ? C1 C2 1.423(6) . ? C2 C3 1.385(6) . ? C3 C4 1.401(7) . ? C4 C5 1.366(8) . ? C5 C6 1.387(7) . ? C7 C8 1.541(6) . ? C8 C9 1.516(7) . ? C8 C11 1.526(6) . ? C8 C10 1.526(7) . ? C12 C13 1.529(7) . ? C13 C16 1.517(7) . ? C13 C14 1.546(8) . ? C13 C15 1.552(9) . ? C17 C18 1.445(13) . ? C18 C19 1.252(13) . ? C19 C20 1.508(13) . ? C21 C22 1.410(14) . ? C23 C24 1.518(12) . ? _cod_database_code 7100263