Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Barbara Gehrhus' _publ_contact_author_address ; Department of Chemistry University of Sussex Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email B.GEHRHUS@SUSSEX.AC.UK _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-. ; _publ_requested_category FM loop_ _publ_author_name 'Barbara Gehrhus' 'Floria Antolini' 'P. B. Hitchcock' 'M. Lappert' data_2b-(feb701) _database_code_depnum_ccdc_archive 'CCDC 273243' _audit_creation_date 2001-02-08T17:59:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _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 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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_reflns_used 9720 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 15100 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_unetI/netI 0.057 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 5086 _reflns_number_gt 3587 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There is some residual density in the region of the thf and Et2O ligands suggesting perhaps some slight mixing of the ligands. However this could not be successfully modelled and only an ordered structure was refined. The high R factor reflects this problem. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1704P)^2^+3.2953P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5086 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1247 _refine_ls_R_factor_gt 0.0926 _refine_ls_wR_factor_ref 0.2905 _refine_ls_wR_factor_gt 0.26 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.785 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Si N1 106.72(14) . . ? O1 Si N2 100.71(15) . . ? N1 Si N2 87.08(15) . . ? O1 Si Na 115.82(10) . 3_675 ? N1 Si Na 114.27(11) . 3_675 ? N2 Si Na 127.61(12) . 3_675 ? O1 Na O3 119.67(16) . . ? O1 Na O2 98.21(13) . . ? O3 Na O2 86.90(15) . . ? O1 Na Si 129.37(9) . 3_675 ? O3 Na Si 98.10(13) . 3_675 ? O2 Na Si 117.52(11) . 3_675 ? C25 O1 Si 122.3(3) . . ? C25 O1 Na 124.4(2) . . ? Si O1 Na 111.84(14) . . ? C17 O2 C20 106.1(6) . . ? C17 O2 Na 131.1(4) . . ? C20 O2 Na 122.2(4) . . ? C23 O3 C21 104.1(8) . . ? C23 O3 Na 143.9(7) . . ? C21 O3 Na 111.5(6) . . ? C1 N1 C7 120.2(3) . . ? C1 N1 Si 114.3(3) . . ? C7 N1 Si 124.0(3) . . ? C2 N2 C12 120.6(3) . . ? C2 N2 Si 113.8(3) . . ? C12 N2 Si 123.4(3) . . ? C6 C1 N1 128.5(4) . . ? C6 C1 C2 119.5(4) . . ? N1 C1 C2 112.1(3) . . ? C3 C2 N2 128.2(4) . . ? C3 C2 C1 119.4(4) . . ? N2 C2 C1 112.3(3) . . ? C2 C3 C4 119.7(4) . . ? C5 C4 C3 120.7(4) . . ? C4 C5 C6 120.8(4) . . ? C5 C6 C1 119.9(5) . . ? N1 C7 C8 117.8(3) . . ? C9 C8 C11 109.3(4) . . ? C9 C8 C10 108.9(4) . . ? C11 C8 C10 110.4(4) . . ? C9 C8 C7 112.5(4) . . ? C11 C8 C7 106.9(4) . . ? C10 C8 C7 108.8(4) . . ? N2 C12 C13 117.2(4) . . ? C16 C13 C12 111.1(4) . . ? C16 C13 C14 110.3(5) . . ? C12 C13 C14 106.3(5) . . ? C16 C13 C15 108.1(5) . . ? C12 C13 C15 110.9(4) . . ? C14 C13 C15 110.2(5) . . ? O2 C17 C18 103.6(8) . . ? C19 C18 C17 116.6(10) . . ? C18 C19 C20 98.3(9) . . ? O2 C20 C19 106.9(9) . . ? C22 C21 O3 117.8(13) . . ? O3 C23 C24 100.7(8) . . ? #===END data_4-(may2104) _database_code_depnum_ccdc_archive 'CCDC 273245' _audit_creation_date 2004-06-09T09:46:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C16 H32 Na1 O4), (C48 H78 N6 Si3)' _chemical_formula_sum 'C64 H110 N6 Na1 O4 Si3' _chemical_formula_weight 1134.84 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m' _symmetry_space_group_name_Hall '-P 6c' _symmetry_Int_Tables_number 176 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' 'y, -x+y, z+1/2' '-x+y, -x, z' 'x-y, x, z+1/2' '-x, -y, -z' 'x, y, -z-1/2' 'y, -x+y, -z' '-y, x-y, -z-1/2' 'x-y, x, -z' '-x+y, -x, -z-1/2' _cell_length_a 15.0206(17) _cell_length_b 15.0206(17) _cell_length_c 16.8690(16) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3296.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5214 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1242 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.11842E-2 _diffrn_orient_matrix_ub_12 0.375712E-1 _diffrn_orient_matrix_ub_13 0.485652E-1 _diffrn_orient_matrix_ub_21 0.410815E-1 _diffrn_orient_matrix_ub_22 -0.252486E-1 _diffrn_orient_matrix_ub_23 0.291243E-1 _diffrn_orient_matrix_ub_31 0.649661E-1 _diffrn_orient_matrix_ub_32 0.621337E-1 _diffrn_orient_matrix_ub_33 -0.175316E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_unetI/netI 0.0609 _diffrn_reflns_number 4420 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 22.94 _diffrn_reflns_theta_full 22.94 _diffrn_measured_fraction_theta_full 0.923 _diffrn_measured_fraction_theta_max 0.923 _reflns_number_total 1467 _reflns_number_gt 1079 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The structure is obviously disordered as the thf ligands coordinated to Na along the 3-fold axis overlap with the next cation along the axis. Either the cations along the chain alternate between [Na(thf)5] and [Na(thf)3], or are all [Na(thf)4] with the trigonal pyramids aligned; in either case the arrangement is then disordered so as to average the structure. These thf ligands are of course also disordered about the 3-fold axis. Hydrogen atoms for all the thf ligands were omitted. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1703P)^2^+13.4496P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1467 _refine_ls_number_parameters 120 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1611 _refine_ls_R_factor_gt 0.1278 _refine_ls_wR_factor_ref 0.3658 _refine_ls_wR_factor_gt 0.3434 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.031 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.095 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.7659(2) 0.3568(2) 0.25 0.0392(10) Uani 1 2 d S . . Na Na 0 0 0.25 0.140(5) Uani 1 6 d S . . O1 O 0.0879(11) 0.1692(12) 0.25 0.154(6) Uani 1 2 d S . . O2 O 0 0 0.1132(15) 0.094(8) Uani 0.5 3 d SPD . . N N 0.8639(5) 0.3893(4) 0.1775(4) 0.0438(17) Uani 1 1 d . . . C1 C 0.9633(6) 0.4473(6) 0.2093(5) 0.046(2) Uani 1 1 d . . . C2 C 1.0550(6) 0.5050(6) 0.1671(5) 0.051(2) Uani 1 1 d . . . H2 H 1.0555 0.506 0.1108 0.061 Uiso 1 1 calc R . . C3 C 1.1463(6) 0.5611(7) 0.2105(5) 0.065(3) Uani 1 1 d . . . H3 H 1.2094 0.5999 0.1829 0.078 Uiso 1 1 calc R . . C4 C 0.8438(6) 0.3708(6) 0.0921(4) 0.048(2) Uani 1 1 d . . . H4A H 0.8949 0.4331 0.0635 0.057 Uiso 1 1 calc R . . H4B H 0.7752 0.3621 0.081 0.057 Uiso 1 1 calc R . . C5 C 0.8470(7) 0.2765(7) 0.0566(5) 0.061(2) Uani 1 1 d . . . C6 C 0.9558(7) 0.3002(8) 0.0452(6) 0.074(3) Uani 1 1 d . . . H6A H 0.9901 0.3137 0.0968 0.111 Uiso 1 1 calc R . . H6B H 0.9924 0.361 0.0113 0.111 Uiso 1 1 calc R . . H6C H 0.9559 0.2414 0.0201 0.111 Uiso 1 1 calc R . . C7 C 0.7912(7) 0.1837(7) 0.1107(5) 0.056(2) Uani 1 1 d . . . H7A H 0.7197 0.1673 0.1174 0.084 Uiso 1 1 calc R . . H7B H 0.8253 0.1993 0.1625 0.084 Uiso 1 1 calc R . . H7C H 0.7924 0.1248 0.0871 0.084 Uiso 1 1 calc R . . C8 C 0.7930(7) 0.2561(7) -0.0220(5) 0.064(3) Uani 1 1 d . . . H8A H 0.7221 0.2407 -0.0137 0.096 Uiso 1 1 calc R . . H8B H 0.7926 0.1975 -0.0477 0.096 Uiso 1 1 calc R . . H8C H 0.8291 0.317 -0.0558 0.096 Uiso 1 1 calc R . . C9 C 0.197(3) 0.208(3) 0.2133(19) 0.154(13) Uiso 0.5 1 d P . . C10 C 0.256(2) 0.313(2) 0.25 0.156(9) Uiso 1 2 d S . . C11 C 0.183(3) 0.356(3) 0.25 0.175(11) Uiso 1 2 d S . . C12 C 0.073(2) 0.259(2) 0.25 0.139(8) Uiso 1 2 d S . . C13 C 0.073(4) 0.079(4) 0.065(3) 0.19(3) Uiso 0.33 1 d PD . . C14 C -0.005(10) 0.056(6) -0.001(5) 0.133(17) Uiso 0.33 1 d PD . . 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 0.0348(17) 0.0388(18) 0.0454(17) 0 0 0.0195(15) Na 0.132(7) 0.132(7) 0.154(13) 0 0 0.066(4) O1 0.095(11) 0.113(11) 0.230(18) 0 0 0.033(9) O2 0.107(12) 0.107(12) 0.069(15) 0 0 0.054(6) N 0.037(4) 0.038(4) 0.055(4) 0.001(3) 0.003(3) 0.017(3) C1 0.036(5) 0.037(4) 0.067(5) -0.002(3) 0.002(3) 0.019(4) C2 0.032(4) 0.038(5) 0.072(6) 0.007(4) 0.007(4) 0.010(4) C3 0.033(5) 0.058(6) 0.088(6) 0.014(4) 0.009(4) 0.011(4) C4 0.048(5) 0.047(5) 0.046(4) 0.004(3) 0.002(3) 0.023(4) C5 0.051(5) 0.052(5) 0.074(6) -0.010(4) 0.012(4) 0.021(4) C6 0.054(6) 0.076(7) 0.096(7) -0.019(5) 0.017(5) 0.034(5) C7 0.057(5) 0.060(6) 0.056(5) -0.004(4) 0.003(4) 0.033(5) C8 0.072(6) 0.053(5) 0.049(5) -0.001(4) 0.007(4) 0.017(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N 1.784(6) . ? Si Si 2.338(5) 3_655 ? Na O1 2.202(16) . ? Na O2 2.31(3) . ? O1 C12 1.47(3) . ? O1 C9 1.56(4) . ? O2 C13 1.41(2) . ? N C1 1.405(10) . ? N C4 1.469(9) . ? C1 C1 1.373(15) 8_556 ? C1 C2 1.401(11) . ? C2 C3 1.403(12) . ? C3 C3 1.333(18) 8_556 ? C4 C5 1.560(11) . ? C5 C6 1.500(12) . ? C5 C8 1.503(12) . ? C5 C7 1.519(12) . ? C9 C10 1.50(4) . ? C10 C11 1.53(4) . ? C11 C12 1.56(4) . ? C13 C14 1.53(2) . ? C14 C14 1.52(6) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Si N 86.6(4) 8_556 . ? N Si Si 131.6(2) . 5_665 ? N Si Si 126.1(2) . 3_655 ? Si Si Si 60 5_665 3_655 ? O1 Na O1 120 5 3 ? O1 Na O2 90 5 . ? O2 Na O2 180 8_556 . ? C12 O1 C9 105.3(19) . . ? C12 O1 Na 141.3(14) . . ? C9 O1 Na 110.2(17) . . ? C13 O2 C13 90(4) . 5 ? C13 O2 Na 125(3) . . ? C1 N C4 123.0(6) . . ? C1 N Si 112.5(5) . . ? C4 N Si 123.9(5) . . ? C1 C1 C2 120.5(5) 8_556 . ? C1 C1 N 112.5(4) 8_556 . ? C2 C1 N 127.0(7) . . ? C1 C2 C3 118.0(8) . . ? C3 C3 C2 121.4(5) 8_556 . ? N C4 C5 116.8(7) . . ? C6 C5 C8 110.4(8) . . ? C6 C5 C7 109.3(8) . . ? C8 C5 C7 110.4(7) . . ? C6 C5 C4 110.9(7) . . ? C8 C5 C4 105.3(7) . . ? C7 C5 C4 110.4(7) . . ? C10 C9 O1 101(3) . . ? C9 C10 C11 105(3) . . ? C10 C11 C12 105(3) . . ? O1 C12 C11 106(2) . . ? C14 C13 O2 111(5) 9 . ? C13 C14 C14 102(6) 11 5 ? #===END data_5-(may3502) _database_code_depnum_ccdc_archive 'CCDC 273246' _audit_creation_date 2002-05-31T14:11:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _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 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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_reflns_used 12808 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 23.534 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.12 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_unetI/netI 0.0505 _diffrn_reflns_number 13206 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.34 _diffrn_reflns_theta_max 23.54 _diffrn_reflns_theta_full 23.54 _diffrn_measured_fraction_theta_full 0.947 _diffrn_measured_fraction_theta_max 0.947 _reflns_number_total 3922 _reflns_number_gt 3325 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The crystals do not diffract well at higher angle (essentially nothing above 20 degrees theta with M0 radiation). Data sets were collected on two different crystals and both showed the same problem. The thf groups show large ADPs and were refined with C-C bond length constraints (SADI). In one thf group disorder was resolved. M1 ia a dummy atom of zero occupancy fixed at the C1 to C6 ring centroid, and assumed to have the same esd as a ring carbon atom when calculating distances and angles. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1464P)^2^+1.9638P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3922 _refine_ls_number_parameters 290 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2537 _refine_ls_wR_factor_gt 0.2394 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.356 _refine_diff_density_min -0.29 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Na O2 98.59(17) . . ? O1 Na Si 116.29(14) . . ? O2 Na Si 118.99(11) . . ? N2 Si N1 84.73(13) . . ? N2 Si Si 99.54(11) . 3 ? N1 Si Si 99.07(10) . 3 ? N2 Si Na 131.13(10) . . ? N1 Si Na 134.76(10) . . ? Si Si Na 100.12(6) 3 . ? C17 O1 C20 108.1(6) . . ? C17 O1 Na 128.1(5) . . ? C20 O1 Na 123.7(5) . . ? C21A O2 C24 88.4(17) . . ? C21 O2 C24 108.4(6) . . ? C21A O2 Na 138.5(8) . . ? C21 O2 Na 119.6(6) . . ? C24 O2 Na 124.5(5) . . ? C1 N1 C7 121.4(3) . . ? C1 N1 Si 110.1(2) . . ? C7 N1 Si 122.8(2) . . ? C2 N2 C12 121.6(3) . . ? C2 N2 Si 110.3(2) . . ? C12 N2 Si 122.9(2) . . ? N1 C1 C6 129.0(3) . . ? N1 C1 C2 111.9(3) . . ? C6 C1 C2 119.0(3) . . ? N2 C2 C3 128.8(3) . . ? N2 C2 C1 112.2(3) . . ? C3 C2 C1 118.9(3) . . ? C4 C3 C2 120.5(4) . . ? C5 C4 C3 120.5(4) . . ? C4 C5 C6 120.6(4) . . ? C1 C6 C5 120.4(4) . . ? N1 C7 C8 115.8(3) . . ? C10 C8 C7 110.3(4) . . ? C10 C8 C9 111.2(5) . . ? C7 C8 C9 108.8(4) . . ? C10 C8 C11 110.7(5) . . ? C7 C8 C11 107.2(4) . . ? C9 C8 C11 108.6(4) . . ? N2 C12 C13 115.3(3) . . ? C14 C13 C15 108.8(4) . . ? C14 C13 C16 110.4(5) . . ? C15 C13 C16 110.5(5) . . ? C14 C13 C12 110.5(4) . . ? C15 C13 C12 107.9(4) . . ? C16 C13 C12 108.8(4) . . ? O1 C17 C18 106.6(9) . . ? C17 C18 C19 104.3(9) . . ? C20 C19 C18 101.6(9) . . ? C19 C20 O1 110.1(8) . . ? O2 C21 C22 107.0(9) . . ? C23 C22 C21 108.2(9) . . ? C22 C23 C24 107.2(8) . . ? O2 C24 C23 106.7(7) . . ? O2 C21A C22A 112.9(15) . . ? #===END