#------------------------------------------------------------------------------ #$Date: 2010-01-30 14:59:17 +0100 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/7/7100265.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_7100265 _journal_name_full 'Chemical Communications' _journal_year 2005 _chemical_name_common ((Na(thf)2(Si(NCH2tBu)2C6H4))2) _chemical_formula_moiety 'C48 H84 N4 Na2 O4 Si2' _chemical_formula_sum 'C48 H84 N4 Na2 O4 Si2' _chemical_formula_weight 883.35 _symmetry_cell_setting monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.5047(4) _cell_length_b 12.1298(4) _cell_length_c 16.0628(4) _cell_angle_alpha 90 _cell_angle_beta 99.723(2) _cell_angle_gamma 90 _cell_volume 2785.48(14) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_wavelength 0.71073 _exptl_crystal_density_diffrn 1.053 _diffrn_ambient_temperature 223(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 Na Na -0.01791(11) -0.08793(13) -0.20362(9) 0.0732(5) Uani 1 1 d . . . Si Si 0.05652(7) 0.03069(8) -0.04517(6) 0.0590(4) Uani 1 1 d . . . O1 O 0.0843(3) -0.2055(4) -0.2547(3) 0.1331(15) Uani 1 1 d . . . O2 O -0.0674(3) 0.0142(3) -0.3270(2) 0.1090(12) Uani 1 1 d . . . N1 N 0.16498(19) 0.0224(2) 0.03302(18) 0.0584(7) Uani 1 1 d . . . N2 N 0.0610(2) 0.1783(2) -0.01991(18) 0.0613(8) Uani 1 1 d . . . C1 C 0.1663(2) 0.1046(3) 0.0928(2) 0.0580(9) Uani 1 1 d . . . C2 C 0.1054(3) 0.1949(3) 0.0619(2) 0.0596(9) Uani 1 1 d . . . C3 C 0.0972(3) 0.2837(3) 0.1157(2) 0.0701(10) Uani 1 1 d . . . H3 H 0.0581 0.3433 0.0962 0.084 Uiso 1 1 calc R . . C4 C 0.1464(3) 0.2844(4) 0.1979(3) 0.0795(11) Uani 1 1 d . . . H4 H 0.14 0.3443 0.2335 0.095 Uiso 1 1 calc R . . C5 C 0.2041(3) 0.1983(4) 0.2273(2) 0.0766(11) Uani 1 1 d . . . H5 H 0.2366 0.1996 0.2831 0.092 Uiso 1 1 calc R . . C6 C 0.2150(3) 0.1085(3) 0.1749(2) 0.0686(10) Uani 1 1 d . . . H6 H 0.2555 0.0505 0.1955 0.082 Uiso 1 1 calc R . . C7 C 0.2165(3) -0.0792(3) 0.0521(2) 0.0645(9) Uani 1 1 d . . . H7A H 0.1775 -0.1404 0.0265 0.077 Uiso 1 1 calc R . . H7B H 0.227 -0.0902 0.1134 0.077 Uiso 1 1 calc R . . C8 C 0.3112(3) -0.0856(4) 0.0220(3) 0.0821(12) Uani 1 1 d . . . C9 C 0.2953(4) -0.0712(6) -0.0745(4) 0.121(2) Uani 1 1 d . . . H9A H 0.2662 -0.0003 -0.0894 0.182 Uiso 1 1 calc R . . H9B H 0.2547 -0.1296 -0.1008 0.182 Uiso 1 1 calc R . . H9C H 0.3549 -0.0748 -0.0942 0.182 Uiso 1 1 calc R . . C10 C 0.3769(3) 0.0018(6) 0.0656(4) 0.1134(18) Uani 1 1 d . . . H10A H 0.3867 -0.01 0.1262 0.17 Uiso 1 1 calc R . . H10B H 0.3498 0.0742 0.0527 0.17 Uiso 1 1 calc R . . H10C H 0.4364 -0.0027 0.0458 0.17 Uiso 1 1 calc R . . C11 C 0.3511(4) -0.2021(5) 0.0438(4) 0.125(2) Uani 1 1 d . . . H11A H 0.3082 -0.2568 0.0153 0.188 Uiso 1 1 calc R . . H11B H 0.3591 -0.2135 0.1043 0.188 Uiso 1 1 calc R . . H11C H 0.4111 -0.2092 0.0253 0.188 Uiso 1 1 calc R . . C12 C -0.0057(3) 0.2570(3) -0.0628(2) 0.0657(10) Uani 1 1 d . . . H12A H -0.0311 0.2999 -0.0201 0.079 Uiso 1 1 calc R . . H12B H -0.0578 0.2163 -0.0959 0.079 Uiso 1 1 calc R . . C13 C 0.0337(3) 0.3383(4) -0.1224(3) 0.0811(12) Uani 1 1 d . . . C14 C 0.1076(4) 0.4117(5) -0.0727(4) 0.128(3) Uani 1 1 d . . . H14A H 0.0806 0.4525 -0.0308 0.193 Uiso 1 1 calc R . . H14B H 0.1306 0.463 -0.1108 0.193 Uiso 1 1 calc R . . H14C H 0.1589 0.3668 -0.0447 0.193 Uiso 1 1 calc R . . C15 C -0.0469(4) 0.4101(4) -0.1652(4) 0.113(2) Uani 1 1 d . . . H15A H -0.0236 0.4635 -0.2015 0.17 Uiso 1 1 calc R . . H15B H -0.0747 0.4484 -0.1226 0.17 Uiso 1 1 calc R . . H15C H -0.0937 0.364 -0.1988 0.17 Uiso 1 1 calc R . . C16 C 0.0752(5) 0.2720(6) -0.1882(4) 0.132(2) Uani 1 1 d . . . H16A H 0.0968 0.322 -0.2279 0.198 Uiso 1 1 calc R . . H16B H 0.0277 0.2235 -0.2183 0.198 Uiso 1 1 calc R . . H16C H 0.1274 0.2283 -0.1602 0.198 Uiso 1 1 calc R . . C17 C 0.1216(9) -0.1943(9) -0.3211(6) 0.209(5) Uani 1 1 d D A 1 H17A H 0.1764 -0.1459 -0.3096 0.251 Uiso 1 1 calc R A 1 H17B H 0.0766 -0.1622 -0.3671 0.251 Uiso 1 1 calc R A 1 C18 C 0.1489(10) -0.3037(9) -0.3439(8) 0.232(6) Uani 1 1 d D A 1 H18A H 0.2042 -0.3004 -0.3715 0.278 Uiso 1 1 calc R A 1 H18B H 0.0979 -0.3398 -0.382 0.278 Uiso 1 1 calc R A 1 C19 C 0.1698(11) -0.3625(9) -0.2634(8) 0.238(7) Uani 1 1 d D A 1 H19A H 0.1536 -0.4409 -0.2701 0.286 Uiso 1 1 calc R A 1 H19B H 0.2359 -0.3554 -0.2381 0.286 Uiso 1 1 calc R A 1 C20 C 0.1135(8) -0.3093(7) -0.2167(9) 0.223(6) Uani 1 1 d D A 1 H20A H 0.1475 -0.2973 -0.1593 0.267 Uiso 1 1 calc R A 1 H20B H 0.0586 -0.3548 -0.213 0.267 Uiso 1 1 calc R A 1 C21 C -0.1503(8) 0.0779(14) -0.3345(12) 0.131(7) Uani 0.58(2) 1 d PD A 1 H21A H -0.1539 0.1152 -0.281 0.157 Uiso 0.58(2) 1 calc PR A 1 H21B H -0.2055 0.0306 -0.3491 0.157 Uiso 0.58(2) 1 calc PR A 1 C22 C -0.1468(8) 0.1573(11) -0.3999(12) 0.112(5) Uani 0.58(2) 1 d PD A 1 H22A H -0.1891 0.1355 -0.4515 0.135 Uiso 0.58(2) 1 calc PR A 1 H22B H -0.1662 0.2298 -0.3823 0.135 Uiso 0.58(2) 1 calc PR A 1 C23 C -0.0548(8) 0.1621(9) -0.4153(8) 0.206(5) Uani 0.58(2) 1 d PD A 1 H23A H -0.0241 0.2295 -0.3909 0.248 Uiso 0.58(2) 1 calc PR A 1 H23B H -0.0541 0.1622 -0.4762 0.248 Uiso 0.58(2) 1 calc PR A 1 C24 C -0.0061(8) 0.0651(10) -0.3761(7) 0.209(5) Uani 0.58(2) 1 d PD A 1 H24A H 0.0084 0.0141 -0.4194 0.25 Uiso 0.58(2) 1 calc PR A 1 H24B H 0.0525 0.0866 -0.34 0.25 Uiso 0.58(2) 1 calc PR A 1 C21A C -0.131(3) 0.007(3) -0.396(2) 0.24(2) Uani 0.42(2) 1 d PD A 2 H21C H -0.1922 -0.0068 -0.3805 0.285 Uiso 0.42(2) 1 calc PR A 2 H21D H -0.1158 -0.0553 -0.4302 0.285 Uiso 0.42(2) 1 calc PR A 2 C22A C -0.1364(17) 0.105(2) -0.4466(15) 0.165(13) Uani 0.42(2) 1 d PD A 2 H22C H -0.139 0.0864 -0.5063 0.198 Uiso 0.42(2) 1 calc PR A 2 H22D H -0.1918 0.1481 -0.4404 0.198 Uiso 0.42(2) 1 calc PR A 2 C23A C -0.0548(8) 0.1621(9) -0.4153(8) 0.206(5) Uani 0.42(2) 1 d P A 2 H23C H -0.0641 0.219 -0.3742 0.248 Uiso 0.42(2) 1 calc PR A 2 H23D H -0.0246 0.1937 -0.46 0.248 Uiso 0.42(2) 1 calc PR A 2 C24A C -0.0061(8) 0.0651(10) -0.3761(7) 0.209(5) Uani 0.42(2) 1 d P A 2 H24C H 0.0084 0.0141 -0.4194 0.25 Uiso 0.42(2) 1 calc PR A 2 H24D H 0.0525 0.0866 -0.34 0.25 Uiso 0.42(2) 1 calc PR A 2 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 Na 0.0909(11) 0.0733(10) 0.0563(9) -0.0003(7) 0.0151(7) 0.0143(8) Si 0.0703(7) 0.0525(6) 0.0520(6) 0.0031(4) 0.0040(4) 0.0056(4) O1 0.141(3) 0.121(3) 0.147(4) -0.034(3) 0.052(3) 0.030(3) O2 0.154(3) 0.099(2) 0.072(2) 0.0171(17) 0.012(2) 0.024(2) N1 0.0631(17) 0.0546(17) 0.0567(16) 0.0028(13) 0.0078(13) 0.0096(13) N2 0.0746(18) 0.0479(16) 0.0576(17) 0.0072(13) 0.0003(13) 0.0045(13) C1 0.0594(19) 0.060(2) 0.0540(19) 0.0055(15) 0.0091(15) 0.0002(15) C2 0.071(2) 0.0492(19) 0.058(2) 0.0046(15) 0.0093(16) 0.0005(16) C3 0.087(3) 0.054(2) 0.069(2) -0.0002(17) 0.0104(19) 0.0043(18) C4 0.094(3) 0.073(3) 0.071(3) -0.013(2) 0.015(2) 0.003(2) C5 0.084(3) 0.086(3) 0.057(2) -0.008(2) 0.0044(18) -0.001(2) C6 0.066(2) 0.076(2) 0.061(2) 0.0055(18) 0.0049(17) 0.0076(18) C7 0.067(2) 0.063(2) 0.064(2) 0.0087(17) 0.0159(16) 0.0145(17) C8 0.076(3) 0.099(3) 0.076(3) 0.009(2) 0.028(2) 0.020(2) C9 0.119(4) 0.169(6) 0.087(3) 0.013(3) 0.049(3) 0.021(4) C10 0.070(3) 0.146(5) 0.133(5) -0.005(4) 0.043(3) -0.002(3) C11 0.121(4) 0.134(5) 0.127(4) 0.007(4) 0.042(4) 0.074(4) C12 0.067(2) 0.053(2) 0.073(2) 0.0128(17) 0.0005(17) 0.0002(16) C13 0.089(3) 0.070(2) 0.079(3) 0.030(2) -0.003(2) -0.007(2) C14 0.116(4) 0.123(4) 0.130(5) 0.066(4) -0.026(3) -0.052(4) C15 0.125(4) 0.076(3) 0.122(4) 0.042(3) -0.030(3) -0.009(3) C16 0.166(6) 0.138(5) 0.103(4) 0.044(4) 0.051(4) 0.009(4) C17 0.297(13) 0.208(10) 0.150(7) 0.031(7) 0.114(9) 0.103(9) C18 0.309(15) 0.169(10) 0.241(13) -0.003(9) 0.114(12) 0.065(10) C19 0.326(15) 0.161(8) 0.273(13) 0.095(9) 0.182(12) 0.111(10) C20 0.260(11) 0.106(6) 0.342(15) 0.057(7) 0.162(12) 0.077(7) C21 0.091(7) 0.150(11) 0.150(12) 0.092(10) 0.013(7) 0.043(7) C22 0.093(7) 0.105(8) 0.147(12) 0.057(8) 0.041(7) 0.028(6) C23 0.211(10) 0.199(10) 0.218(11) 0.120(9) 0.061(9) 0.051(9) C24 0.213(10) 0.252(11) 0.182(9) 0.090(8) 0.098(8) 0.109(9) C21A 0.27(3) 0.25(3) 0.15(2) 0.11(2) -0.11(2) -0.16(3) C22A 0.104(14) 0.27(3) 0.103(15) 0.091(18) -0.026(11) 0.005(17) C23A 0.211(10) 0.199(10) 0.218(11) 0.120(9) 0.061(9) 0.051(9) C24A 0.213(10) 0.252(11) 0.182(9) 0.090(8) 0.098(8) 0.109(9) 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 Na O1 2.306(4) . ? Na O2 2.345(4) . ? Na Si 2.9641(18) . ? Na C5 2.980(5) 3 ? Na C6 2.982(4) 3 ? Na C1 3.023(4) 3 ? Na C4 3.036(5) 3 ? Na C2 3.074(4) 3 ? Na C3 3.082(4) 3 ? Si N2 1.834(3) . ? Si N1 1.843(3) . ? Si Si 2.480(2) 3 ? O1 C17 1.282(9) . ? O1 C20 1.431(9) . ? O2 C21A 1.323(18) . ? O2 C21 1.419(10) . ? O2 C24 1.424(10) . ? N1 C1 1.382(4) . ? N1 C7 1.448(4) . ? N2 C2 1.377(4) . ? N2 C12 1.449(4) . ? C1 C6 1.387(5) . ? C1 C2 1.441(5) . ? C2 C3 1.399(5) . ? C3 C4 1.390(6) . ? C4 C5 1.370(6) . ? C5 C6 1.403(6) . ? C7 C8 1.533(6) . ? C8 C10 1.516(8) . ? C8 C9 1.538(7) . ? C8 C11 1.545(7) . ? C12 C13 1.550(5) . ? C13 C14 1.513(7) . ? C13 C15 1.526(6) . ? C13 C16 1.530(8) . ? C17 C18 1.450(10) . ? C18 C19 1.463(11) . ? C19 C20 1.362(10) . ? C21 C22 1.432(11) . ? C22 C23 1.399(11) . ? C23 C24 1.459(10) . ? C21A C22A 1.424(14) . ? _cod_database_code 7100265