Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name M.Lappert _publ_contact_author_address ; School of Chemistry & Molecular Science University of Sussex BRIGHTON BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Reactions between a sodium amide Na[N(SiMe3)R1] (R1 = SiMe3, SiMe2Ph or But) and a cyanoalkane RCN (R = Ad or But) ; _publ_requested_category FM loop_ _publ_author_name 'M. Lappert' 'Floria Antolini' 'Anthony G. Avent' 'P. B. Hitchcock' 'Alexei V. Khvostov' 'A. V. Protchenko' data_(1a)-jul1400 _database_code_depnum_ccdc_archive 'CCDC 271689' _audit_creation_date 2000-07-13T11:09:51-00:00 _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_name_common ((Na(NCAd)(Me3SiNSiMe3))2) _chemical_formula_moiety 'C34 H66 N4 Na2 Si4' _chemical_formula_sum 'C34 H66 N4 Na2 Si4' _chemical_formula_weight 689.25 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8840(4) _cell_length_b 9.9561(2) _cell_length_c 22.0449(8) _cell_angle_alpha 84.169(2) _cell_angle_beta 85.751(2) _cell_angle_gamma 81.851(2) _cell_volume 2132.41(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 33024 _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 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.186 _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 24257 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_unetI/netI 0.0438 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 7413 _reflns_number_gt 5957 _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 ; 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^)+(0.0770P)^2^+1.5911P] 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 7413 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.158 _refine_ls_wR_factor_gt 0.148 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.585 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.053 #----------------------------------------------------------------------------# # 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' 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 Na1 Na 0.36276(11) 0.36079(11) 0.25500(5) 0.0419(3) Uani 1 1 d . . . Na2 Na 0.14308(11) 0.60611(10) 0.25081(5) 0.0419(3) Uani 1 1 d . . . Si1 Si 0.23138(8) 0.43213(7) 0.38909(3) 0.0362(2) Uani 1 1 d . . . Si2 Si 0.39513(8) 0.64957(8) 0.32866(4) 0.0420(2) Uani 1 1 d . . . Si3 Si 0.32360(8) 0.49706(8) 0.11669(3) 0.0408(2) Uani 1 1 d . . . Si4 Si 0.07880(8) 0.36836(8) 0.16981(3) 0.0394(2) Uani 1 1 d . . . N1 N 0.3004(2) 0.5222(2) 0.32857(9) 0.0352(5) Uani 1 1 d . . . N2 N 0.2136(2) 0.4521(2) 0.17484(9) 0.0353(5) Uani 1 1 d . . . N3 N 0.5017(3) 0.1570(3) 0.22747(13) 0.0631(8) Uani 1 1 d . . . N4 N -0.0224(3) 0.7785(3) 0.28836(13) 0.0603(7) Uani 1 1 d . . . C1 C 0.3201(4) 0.4166(4) 0.46265(15) 0.0629(9) Uani 1 1 d . . . H1A H 0.4173 0.3825 0.4552 0.094 Uiso 1 1 calc R . . H1B H 0.278 0.3531 0.4927 0.094 Uiso 1 1 calc R . . H1C H 0.3113 0.5063 0.4784 0.094 Uiso 1 1 calc R . . C2 C 0.0478(3) 0.4976(3) 0.40961(15) 0.0545(8) Uani 1 1 d . . . H2A H -0.0049 0.5075 0.3731 0.082 Uiso 1 1 calc R . . H2B H 0.0427 0.5864 0.4258 0.082 Uiso 1 1 calc R . . H2C H 0.0099 0.4332 0.4406 0.082 Uiso 1 1 calc R . . C3 C 0.2296(3) 0.2513(3) 0.37027(14) 0.0471(7) Uani 1 1 d . . . H3A H 0.3231 0.2104 0.3591 0.071 Uiso 1 1 calc R . . H3B H 0.1719 0.2518 0.3359 0.071 Uiso 1 1 calc R . . H3C H 0.1928 0.198 0.406 0.071 Uiso 1 1 calc R . . C4 C 0.5840(3) 0.5916(4) 0.32096(19) 0.0697(10) Uani 1 1 d . . . H4A H 0.6049 0.5375 0.2859 0.105 Uiso 1 1 calc R . . H4B H 0.6128 0.5359 0.3582 0.105 Uiso 1 1 calc R . . H4C H 0.6332 0.6713 0.3147 0.105 Uiso 1 1 calc R . . C5 C 0.3569(4) 0.7811(3) 0.26196(16) 0.0656(10) Uani 1 1 d . . . H5A H 0.3707 0.7367 0.2239 0.098 Uiso 1 1 calc R . . H5B H 0.4184 0.8504 0.2607 0.098 Uiso 1 1 calc R . . H5C H 0.2617 0.8242 0.2667 0.098 Uiso 1 1 calc R . . C6 C 0.3636(4) 0.7516(4) 0.39666(16) 0.0657(10) Uani 1 1 d . . . H6A H 0.2656 0.7842 0.4022 0.099 Uiso 1 1 calc R . . H6B H 0.4149 0.8297 0.39 0.099 Uiso 1 1 calc R . . H6C H 0.3939 0.6942 0.4332 0.099 Uiso 1 1 calc R . . C7 C 0.3542(4) 0.3786(4) 0.05410(16) 0.0674(10) Uani 1 1 d . . . H7A H 0.381 0.2852 0.0719 0.101 Uiso 1 1 calc R . . H7B H 0.4274 0.4063 0.0251 0.101 Uiso 1 1 calc R . . H7C H 0.2699 0.3828 0.0327 0.101 Uiso 1 1 calc R . . C8 C 0.2729(5) 0.6721(4) 0.07878(19) 0.0791(12) Uani 1 1 d . . . H8A H 0.1813 0.6781 0.0637 0.119 Uiso 1 1 calc R . . H8B H 0.3386 0.6905 0.0445 0.119 Uiso 1 1 calc R . . H8C H 0.2724 0.7394 0.1083 0.119 Uiso 1 1 calc R . . C9 C 0.4998(3) 0.4973(4) 0.14340(15) 0.0568(8) Uani 1 1 d . . . H9A H 0.532 0.4076 0.1637 0.085 Uiso 1 1 calc R . . H9B H 0.4966 0.5667 0.1722 0.085 Uiso 1 1 calc R . . H9C H 0.5625 0.5179 0.1082 0.085 Uiso 1 1 calc R . . C10 C -0.0609(3) 0.4200(4) 0.22921(16) 0.0573(8) Uani 1 1 d . . . H10A H -0.0881 0.5188 0.2236 0.086 Uiso 1 1 calc R . . H10B H -0.0271 0.3947 0.2701 0.086 Uiso 1 1 calc R . . H10C H -0.14 0.3734 0.2248 0.086 Uiso 1 1 calc R . . C11 C 0.1221(4) 0.1788(3) 0.18493(17) 0.0604(9) Uani 1 1 d . . . H11A H 0.1942 0.1454 0.1551 0.091 Uiso 1 1 calc R . . H11B H 0.0404 0.1353 0.1814 0.091 Uiso 1 1 calc R . . H11C H 0.1542 0.1565 0.2262 0.091 Uiso 1 1 calc R . . C12 C -0.0068(4) 0.3992(4) 0.09516(16) 0.0644(9) Uani 1 1 d . . . H12A H -0.0314 0.4973 0.0851 0.097 Uiso 1 1 calc R . . H12B H -0.0897 0.3547 0.0988 0.097 Uiso 1 1 calc R . . H12C H 0.0561 0.3615 0.0628 0.097 Uiso 1 1 calc R . . C13 C 0.5662(3) 0.0955(3) 0.19149(14) 0.0475(7) Uani 1 1 d . . . C14 C 0.6520(3) 0.0192(3) 0.14561(13) 0.0409(6) Uani 1 1 d . . . C15 C 0.7564(3) -0.0871(3) 0.17701(14) 0.0539(8) Uani 1 1 d . . . H15A H 0.7088 -0.1522 0.2048 0.065 Uiso 1 1 calc R . . H15B H 0.8138 -0.0423 0.2015 0.065 Uiso 1 1 calc R . . C16 C 0.8463(3) -0.1629(4) 0.12877(15) 0.0564(8) Uani 1 1 d . . . H16 H 0.916 -0.2324 0.149 0.068 Uiso 1 1 calc R . . C17 C 0.7563(4) -0.2332(3) 0.09241(16) 0.0578(8) Uani 1 1 d . . . H17A H 0.709 -0.2986 0.1202 0.069 Uiso 1 1 calc R . . H17B H 0.8138 -0.2845 0.0615 0.069 Uiso 1 1 calc R . . C18 C 0.6506(3) -0.1278(3) 0.06073(14) 0.0536(8) Uani 1 1 d . . . H18 H 0.5928 -0.1749 0.0366 0.064 Uiso 1 1 calc R . . C19 C 0.5596(3) -0.0506(3) 0.10841(15) 0.0531(8) Uani 1 1 d . . . H19A H 0.5098 -0.1145 0.1359 0.064 Uiso 1 1 calc R . . H19B H 0.4916 0.0187 0.088 0.064 Uiso 1 1 calc R . . C20 C 0.7245(4) 0.1200(3) 0.10211(16) 0.0596(9) Uani 1 1 d . . . H20A H 0.6559 0.1895 0.0822 0.072 Uiso 1 1 calc R . . H20B H 0.7826 0.1672 0.1253 0.072 Uiso 1 1 calc R . . C21 C 0.8129(4) 0.0430(4) 0.05376(16) 0.0649(10) Uani 1 1 d . . . H21 H 0.8608 0.1081 0.0253 0.078 Uiso 1 1 calc R . . C22 C 0.7244(4) -0.0292(4) 0.01826(14) 0.0655(10) Uani 1 1 d . . . H22A H 0.7823 -0.0793 -0.0129 0.079 Uiso 1 1 calc R . . H22B H 0.6567 0.0387 -0.003 0.079 Uiso 1 1 calc R . . C23 C 0.9178(4) -0.0620(4) 0.08584(17) 0.0684(10) Uani 1 1 d . . . H23A H 0.9779 -0.1113 0.0551 0.082 Uiso 1 1 calc R . . H23B H 0.9757 -0.0153 0.1093 0.082 Uiso 1 1 calc R . . C24 C -0.0802(3) 0.8536(3) 0.32036(13) 0.0458(7) Uani 1 1 d . . . C25 C -0.1531(3) 0.9522(3) 0.36034(12) 0.0393(6) Uani 1 1 d . . . C26 C -0.1046(3) 0.9192(3) 0.42579(14) 0.0514(7) Uani 1 1 d . . . H26A H -0.0048 0.9222 0.4253 0.062 Uiso 1 1 calc R . . H26B H -0.1223 0.8263 0.4416 0.062 Uiso 1 1 calc R . . C27 C -0.1819(3) 1.0245(3) 0.46804(13) 0.0446(7) Uani 1 1 d . . . H27 H -0.1507 1.0034 0.5105 0.054 Uiso 1 1 calc R . . C28 C -0.1503(4) 1.1645(4) 0.44253(15) 0.0567(8) Uani 1 1 d . . . H28A H -0.1963 1.2335 0.4693 0.068 Uiso 1 1 calc R . . H28B H -0.0504 1.1668 0.4418 0.068 Uiso 1 1 calc R . . C29 C -0.1986(3) 1.1987(3) 0.37858(14) 0.0498(7) Uani 1 1 d . . . H29 H -0.1796 1.2925 0.3632 0.06 Uiso 1 1 calc R . . C30 C -0.1227(3) 1.0965(3) 0.33617(15) 0.0526(8) Uani 1 1 d . . . H30A H -0.0229 1.1002 0.335 0.063 Uiso 1 1 calc R . . H30B H -0.1534 1.1193 0.2942 0.063 Uiso 1 1 calc R . . C31 C -0.3074(3) 0.9468(3) 0.36176(15) 0.0490(7) Uani 1 1 d . . . H31A H -0.3271 0.8541 0.377 0.059 Uiso 1 1 calc R . . H31B H -0.3398 0.9681 0.32 0.059 Uiso 1 1 calc R . . C32 C -0.3825(3) 1.0514(3) 0.40402(14) 0.0459(7) Uani 1 1 d . . . H32 H -0.4834 1.0483 0.4052 0.055 Uiso 1 1 calc R . . C33 C -0.3326(3) 1.0173(3) 0.46794(14) 0.0539(8) Uani 1 1 d . . . H33A H -0.3832 1.0823 0.4955 0.065 Uiso 1 1 calc R . . H33B H -0.3511 0.9245 0.4835 0.065 Uiso 1 1 calc R . . C34 C -0.3519(3) 1.1926(3) 0.37854(16) 0.0559(8) Uani 1 1 d . . . H34A H -0.4028 1.262 0.4039 0.067 Uiso 1 1 calc R . . H34B H -0.382 1.2127 0.3364 0.067 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 Na1 0.0431(6) 0.0425(6) 0.0400(6) -0.0174(5) 0.0015(5) 0.0023(5) Na2 0.0485(6) 0.0379(6) 0.0378(6) -0.0131(4) 0.0017(5) 0.0038(5) Si1 0.0379(4) 0.0382(4) 0.0322(4) -0.0048(3) 0.0027(3) -0.0054(3) Si2 0.0465(5) 0.0402(4) 0.0433(4) -0.0189(3) 0.0134(3) -0.0170(3) Si3 0.0497(5) 0.0382(4) 0.0349(4) -0.0091(3) 0.0115(3) -0.0104(3) Si4 0.0430(4) 0.0396(4) 0.0374(4) -0.0054(3) -0.0002(3) -0.0115(3) N1 0.0415(12) 0.0358(12) 0.0308(11) -0.0112(9) 0.0054(9) -0.0122(10) N2 0.0403(12) 0.0349(11) 0.0318(11) -0.0097(9) 0.0060(9) -0.0089(9) N3 0.0663(19) 0.0646(18) 0.0537(17) -0.0162(14) 0.0014(14) 0.0122(15) N4 0.0642(18) 0.0606(17) 0.0528(16) -0.0196(14) -0.0056(14) 0.0149(14) C1 0.075(2) 0.068(2) 0.0456(19) -0.0053(16) -0.0118(17) -0.0079(18) C2 0.0515(18) 0.0589(19) 0.0477(18) -0.0014(14) 0.0160(14) -0.0007(15) C3 0.0456(17) 0.0418(15) 0.0534(18) -0.0016(13) 0.0030(14) -0.0097(13) C4 0.0477(19) 0.071(2) 0.097(3) -0.034(2) 0.0118(19) -0.0235(17) C5 0.090(3) 0.0467(18) 0.065(2) -0.0085(16) 0.0140(19) -0.0311(18) C6 0.081(3) 0.062(2) 0.064(2) -0.0339(17) 0.0175(18) -0.0326(19) C7 0.070(2) 0.087(3) 0.050(2) -0.0335(18) 0.0188(17) -0.022(2) C8 0.088(3) 0.059(2) 0.078(3) 0.0187(19) 0.022(2) -0.003(2) C9 0.0533(19) 0.064(2) 0.057(2) -0.0170(16) 0.0167(15) -0.0237(16) C10 0.0484(18) 0.065(2) 0.059(2) -0.0059(16) 0.0098(15) -0.0161(16) C11 0.070(2) 0.0449(17) 0.071(2) -0.0085(15) -0.0106(18) -0.0188(16) C12 0.063(2) 0.080(2) 0.055(2) -0.0016(17) -0.0124(17) -0.0221(19) C13 0.0497(17) 0.0466(16) 0.0442(17) -0.0085(13) -0.0025(14) 0.0032(14) C14 0.0443(16) 0.0404(15) 0.0387(15) -0.0125(12) 0.0072(12) -0.0064(12) C15 0.061(2) 0.0574(19) 0.0417(17) -0.0078(14) -0.0079(14) 0.0033(15) C16 0.056(2) 0.064(2) 0.0464(18) -0.0071(15) -0.0073(15) 0.0043(16) C17 0.069(2) 0.0426(17) 0.061(2) -0.0130(15) 0.0078(17) -0.0072(15) C18 0.0573(19) 0.0607(19) 0.0474(18) -0.0251(15) -0.0068(15) -0.0075(16) C19 0.0453(17) 0.063(2) 0.0547(19) -0.0214(15) -0.0004(14) -0.0088(15) C20 0.072(2) 0.0438(17) 0.064(2) -0.0087(15) 0.0156(17) -0.0173(16) C21 0.074(2) 0.058(2) 0.061(2) -0.0051(16) 0.0305(18) -0.0189(18) C22 0.077(2) 0.080(2) 0.0335(16) -0.0110(16) 0.0020(16) 0.0112(19) C23 0.0471(19) 0.096(3) 0.068(2) -0.024(2) 0.0105(17) -0.0225(19) C24 0.0453(16) 0.0491(17) 0.0417(16) -0.0089(13) -0.0045(13) 0.0024(13) C25 0.0382(15) 0.0417(15) 0.0395(15) -0.0134(12) 0.0028(12) -0.0063(12) C26 0.0480(18) 0.0570(18) 0.0486(18) -0.0090(14) -0.0090(14) 0.0011(14) C27 0.0475(16) 0.0523(17) 0.0349(15) -0.0086(12) -0.0041(12) -0.0059(13) C28 0.0543(19) 0.071(2) 0.0514(19) -0.0203(16) 0.0057(15) -0.0244(16) C29 0.0598(19) 0.0371(15) 0.0534(18) -0.0032(13) 0.0075(15) -0.0157(14) C30 0.060(2) 0.0491(17) 0.0494(18) -0.0087(14) 0.0103(15) -0.0125(15) C31 0.0445(17) 0.0488(17) 0.0563(19) -0.0142(14) -0.0077(14) -0.0066(13) C32 0.0294(14) 0.0548(17) 0.0545(18) -0.0131(14) 0.0028(12) -0.0065(12) C33 0.0561(19) 0.0597(19) 0.0476(18) -0.0077(14) 0.0101(15) -0.0189(15) C34 0.060(2) 0.0500(18) 0.0554(19) -0.0109(15) -0.0031(16) 0.0050(15) #----------------------------------------------------------------------------# # 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 Na1 N1 2.386(2) . ? Na1 N3 2.389(3) . ? Na1 N2 2.409(2) . ? Na2 N4 2.366(3) . ? Na2 N2 2.385(2) . ? Na2 N1 2.406(2) . ? Si1 N1 1.687(2) . ? Si1 C2 1.877(3) . ? Si1 C1 1.883(3) . ? Si1 C3 1.891(3) . ? Si2 N1 1.680(2) . ? Si2 C4 1.875(4) . ? Si2 C6 1.878(3) . ? Si2 C5 1.889(4) . ? Si3 N2 1.686(2) . ? Si3 C8 1.872(4) . ? Si3 C9 1.879(3) . ? Si3 C7 1.885(3) . ? Si4 N2 1.684(2) . ? Si4 C11 1.877(3) . ? Si4 C12 1.884(3) . ? Si4 C10 1.885(3) . ? N3 C13 1.151(4) . ? N4 C24 1.145(4) . ? C13 C14 1.471(4) . ? C14 C15 1.521(4) . ? C14 C20 1.532(4) . ? C14 C19 1.548(4) . ? C15 C16 1.524(4) . ? C16 C23 1.522(5) . ? C16 C17 1.522(5) . ? C17 C18 1.526(5) . ? C18 C22 1.512(5) . ? C18 C19 1.527(4) . ? C20 C21 1.525(4) . ? C21 C22 1.512(5) . ? C21 C23 1.523(6) . ? C24 C25 1.463(4) . ? C25 C31 1.532(4) . ? C25 C30 1.543(4) . ? C25 C26 1.543(4) . ? C26 C27 1.554(4) . ? C27 C33 1.502(4) . ? C27 C28 1.515(4) . ? C28 C29 1.513(5) . ? C29 C34 1.524(5) . ? C29 C30 1.531(4) . ? C31 C32 1.542(4) . ? C32 C33 1.517(4) . ? C32 C34 1.524(4) . ? 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 N1 Na1 N3 148.16(10) . . ? N1 Na1 N2 101.50(8) . . ? N3 Na1 N2 110.34(9) . . ? N4 Na2 N2 148.43(10) . . ? N4 Na2 N1 109.17(9) . . ? N2 Na2 N1 101.63(8) . . ? N1 Si1 C2 113.61(13) . . ? N1 Si1 C1 117.04(15) . . ? C2 Si1 C1 105.18(16) . . ? N1 Si1 C3 109.46(12) . . ? C2 Si1 C3 105.08(15) . . ? C1 Si1 C3 105.53(15) . . ? N1 Si2 C4 113.24(14) . . ? N1 Si2 C6 115.86(13) . . ? C4 Si2 C6 106.87(17) . . ? N1 Si2 C5 110.60(14) . . ? C4 Si2 C5 105.88(18) . . ? C6 Si2 C5 103.51(17) . . ? N2 Si3 C8 113.52(15) . . ? N2 Si3 C9 111.47(13) . . ? C8 Si3 C9 105.75(19) . . ? N2 Si3 C7 115.28(14) . . ? C8 Si3 C7 106.6(2) . . ? C9 Si3 C7 103.33(16) . . ? N2 Si4 C11 112.88(14) . . ? N2 Si4 C12 116.21(14) . . ? C11 Si4 C12 106.28(16) . . ? N2 Si4 C10 110.21(13) . . ? C11 Si4 C10 105.59(16) . . ? C12 Si4 C10 104.84(17) . . ? Si2 N1 Si1 128.15(13) . . ? Si2 N1 Na1 118.09(11) . . ? Si1 N1 Na1 104.28(10) . . ? Si2 N1 Na2 103.00(11) . . ? Si1 N1 Na2 114.10(11) . . ? Na1 N1 Na2 78.38(7) . . ? Si4 N2 Si3 126.08(13) . . ? Si4 N2 Na2 105.33(10) . . ? Si3 N2 Na2 118.98(11) . . ? Si4 N2 Na1 115.26(11) . . ? Si3 N2 Na1 103.00(11) . . ? Na2 N2 Na1 78.34(7) . . ? C13 N3 Na1 150.4(3) . . ? C24 N4 Na2 160.7(3) . . ? N3 C13 C14 178.3(4) . . ? C13 C14 C15 109.9(2) . . ? C13 C14 C20 108.5(2) . . ? C15 C14 C20 110.3(3) . . ? C13 C14 C19 109.2(2) . . ? C15 C14 C19 110.1(2) . . ? C20 C14 C19 108.7(3) . . ? C14 C15 C16 109.2(2) . . ? C23 C16 C17 109.3(3) . . ? C23 C16 C15 109.5(3) . . ? C17 C16 C15 108.9(3) . . ? C16 C17 C18 110.1(3) . . ? C22 C18 C17 109.0(3) . . ? C22 C18 C19 109.7(3) . . ? C17 C18 C19 109.7(3) . . ? C18 C19 C14 108.3(2) . . ? C21 C20 C14 109.3(2) . . ? C22 C21 C23 109.3(3) . . ? C22 C21 C20 109.9(3) . . ? C23 C21 C20 108.4(3) . . ? C21 C22 C18 110.4(3) . . ? C16 C23 C21 110.3(3) . . ? N4 C24 C25 178.7(4) . . ? C24 C25 C31 109.9(2) . . ? C24 C25 C30 109.2(2) . . ? C31 C25 C30 109.7(2) . . ? C24 C25 C26 110.0(2) . . ? C31 C25 C26 109.1(2) . . ? C30 C25 C26 108.9(2) . . ? C25 C26 C27 109.8(2) . . ? C33 C27 C28 110.5(3) . . ? C33 C27 C26 108.4(2) . . ? C28 C27 C26 107.8(2) . . ? C29 C28 C27 110.6(2) . . ? C28 C29 C34 110.4(3) . . ? C28 C29 C30 109.8(3) . . ? C34 C29 C30 108.8(3) . . ? C29 C30 C25 108.8(2) . . ? C25 C31 C32 109.2(2) . . ? C33 C32 C34 110.3(3) . . ? C33 C32 C31 109.4(3) . . ? C34 C32 C31 108.3(3) . . ? C27 C33 C32 110.9(2) . . ? C32 C34 C29 109.7(3) . . ? #===END data_(1b)-aug2500 _database_code_depnum_ccdc_archive 'CCDC 271690' _audit_creation_date 2000-08-30T17:32:16-00:00 _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_name_common ((Na(N(SiMe3)2)(NCtBu))2) _chemical_formula_moiety 'C22 H54 N4 Na2 Si4' _chemical_formula_sum 'C22 H54 N4 Na2 Si4' _chemical_formula_weight 533.03 _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 14.4173(5) _cell_length_b 11.7327(3) _cell_length_c 22.1248(5) _cell_angle_alpha 90 _cell_angle_beta 106.847(1) _cell_angle_gamma 90 _cell_volume 3581.87(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 16859 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 0.988 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.205 _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 28309 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_unetI/netI 0.0665 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 8493 _reflns_number_gt 5448 _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 ; The C19 tBu group is disordered 0.66:0.34 over two orientations and C-C and C...C distance constraints were applied to it. 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^)+(0.1294P)^2^+3.1685P] 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 8493 _refine_ls_number_parameters 317 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1866 _refine_ls_wR_factor_gt 0.1475 _refine_ls_goodness_of_fit_ref 0.787 _refine_ls_restrained_S_all 0.8 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.417 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.049 #----------------------------------------------------------------------------# # 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' 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 Na1 Na 1.01606(8) -0.00532(8) 0.25115(4) 0.0368(3) Uani 1 1 d . . . Na2 Na 1.02939(8) 0.25542(8) 0.26021(4) 0.0399(3) Uani 1 1 d . . . Si1 Si 0.82221(5) 0.16415(6) 0.16990(3) 0.03321(19) Uani 1 1 d . . . Si2 Si 0.98492(5) 0.10675(6) 0.11538(3) 0.03297(19) Uani 1 1 d . . . Si3 Si 1.05328(6) 0.08441(6) 0.39369(3) 0.03308(19) Uani 1 1 d . . . Si4 Si 1.22381(6) 0.13378(7) 0.34495(3) 0.0390(2) Uani 1 1 d . . . N1 N 1.10519(16) 0.11208(17) 0.33618(9) 0.0313(5) Uani 1 1 d . . . N2 N 0.93933(16) 0.13795(17) 0.17554(9) 0.0313(5) Uani 1 1 d . . . N5 N 0.9637(2) -0.1951(2) 0.21510(13) 0.0577(7) Uani 1 1 d . . . N6 N 1.0500(3) 0.4424(2) 0.30535(14) 0.0682(9) Uani 1 1 d . . . C1 C 0.8129(3) 0.2575(3) 0.23747(14) 0.0499(8) Uani 1 1 d . . . H1A H 0.8486 0.3286 0.2373 0.075 Uiso 1 1 calc R . . H1B H 0.8407 0.2174 0.2775 0.075 Uiso 1 1 calc R . . H1C H 0.7447 0.2749 0.2326 0.075 Uiso 1 1 calc R . . C2 C 0.7517(2) 0.0310(3) 0.17439(16) 0.0514(8) Uani 1 1 d . . . H2A H 0.7859 -0.0127 0.212 0.077 Uiso 1 1 calc R . . H2B H 0.7454 -0.0153 0.1365 0.077 Uiso 1 1 calc R . . H2C H 0.6872 0.0518 0.177 0.077 Uiso 1 1 calc R . . C3 C 0.7507(2) 0.2414(3) 0.09640(14) 0.0484(7) Uani 1 1 d . . . H3A H 0.7844 0.312 0.0918 0.073 Uiso 1 1 calc R . . H3B H 0.6861 0.2597 0.0998 0.073 Uiso 1 1 calc R . . H3C H 0.7446 0.1927 0.0595 0.073 Uiso 1 1 calc R . . C4 C 1.0301(3) 0.2344(3) 0.08161(16) 0.0618(9) Uani 1 1 d . . . H4A H 1.0756 0.277 0.1157 0.093 Uiso 1 1 calc R . . H4B H 0.9753 0.2835 0.0606 0.093 Uiso 1 1 calc R . . H4C H 1.0632 0.2095 0.0509 0.093 Uiso 1 1 calc R . . C5 C 1.0922(2) 0.0077(3) 0.14197(14) 0.0499(7) Uani 1 1 d . . . H5A H 1.073 -0.0613 0.1603 0.075 Uiso 1 1 calc R . . H5B H 1.1446 0.046 0.1738 0.075 Uiso 1 1 calc R . . H5C H 1.1146 -0.0131 0.1057 0.075 Uiso 1 1 calc R . . C6 C 0.8981(2) 0.0301(3) 0.04729(14) 0.0534(8) Uani 1 1 d . . . H6A H 0.8728 -0.0377 0.063 0.08 Uiso 1 1 calc R . . H6B H 0.9321 0.0072 0.0167 0.08 Uiso 1 1 calc R . . H6C H 0.8443 0.081 0.0267 0.08 Uiso 1 1 calc R . . C7 C 0.9390(2) -0.0012(2) 0.36125(13) 0.0448(7) Uani 1 1 d . . . H7A H 0.9541 -0.0714 0.342 0.067 Uiso 1 1 calc R . . H7B H 0.8919 0.0438 0.3293 0.067 Uiso 1 1 calc R . . H7C H 0.9116 -0.0206 0.3956 0.067 Uiso 1 1 calc R . . C8 C 1.1296(3) -0.0007(3) 0.46264(14) 0.0533(8) Uani 1 1 d . . . H8A H 1.1515 -0.0709 0.4471 0.08 Uiso 1 1 calc R . . H8B H 1.0909 -0.0198 0.4911 0.08 Uiso 1 1 calc R . . H8C H 1.1859 0.0446 0.4855 0.08 Uiso 1 1 calc R . . C9 C 1.0160(3) 0.2159(3) 0.42936(14) 0.0506(8) Uani 1 1 d . . . H9A H 0.9759 0.2643 0.3957 0.076 Uiso 1 1 calc R . . H9B H 1.0739 0.2582 0.4528 0.076 Uiso 1 1 calc R . . H9C H 0.9787 0.1939 0.4582 0.076 Uiso 1 1 calc R . . C10 C 1.2925(3) 0.2079(4) 0.41961(16) 0.0724(11) Uani 1 1 d . . . H10A H 1.2593 0.2789 0.424 0.109 Uiso 1 1 calc R . . H10B H 1.3582 0.2251 0.418 0.109 Uiso 1 1 calc R . . H10C H 1.2958 0.1583 0.4558 0.109 Uiso 1 1 calc R . . C11 C 1.2892(3) -0.0011(4) 0.3381(3) 0.0875(14) Uani 1 1 d . . . H11A H 1.2544 -0.041 0.2992 0.131 Uiso 1 1 calc R . . H11B H 1.2926 -0.05 0.3746 0.131 Uiso 1 1 calc R . . H11C H 1.355 0.017 0.3369 0.131 Uiso 1 1 calc R . . C12 C 1.2407(3) 0.2306(3) 0.28108(16) 0.0652(10) Uani 1 1 d . . . H12A H 1.207 0.1985 0.2396 0.098 Uiso 1 1 calc R . . H12B H 1.3099 0.2378 0.2851 0.098 Uiso 1 1 calc R . . H12C H 1.2138 0.306 0.2853 0.098 Uiso 1 1 calc R . . C13 C 0.9229(2) -0.2584(2) 0.17840(14) 0.0438(7) Uani 1 1 d . . . C14 C 0.8691(2) -0.3399(2) 0.12966(13) 0.0448(7) Uani 1 1 d . . . C15 C 0.9219(4) -0.3546(5) 0.0808(2) 0.1055(18) Uani 1 1 d . . . H15A H 0.8866 -0.4088 0.0486 0.158 Uiso 1 1 calc R . . H15B H 0.9873 -0.3837 0.101 0.158 Uiso 1 1 calc R . . H15C H 0.9263 -0.2809 0.061 0.158 Uiso 1 1 calc R . . C16 C 0.7687(3) -0.2879(4) 0.09835(18) 0.0732(11) Uani 1 1 d . . . H16A H 0.7311 -0.3398 0.0656 0.11 Uiso 1 1 calc R . . H16B H 0.7763 -0.2145 0.0792 0.11 Uiso 1 1 calc R . . H16C H 0.7346 -0.2764 0.1303 0.11 Uiso 1 1 calc R . . C17 C 0.8560(5) -0.4477(3) 0.1627(2) 0.111(2) Uani 1 1 d . . . H17A H 0.821 -0.5036 0.1314 0.166 Uiso 1 1 calc R . . H17B H 0.8189 -0.4315 0.1924 0.166 Uiso 1 1 calc R . . H17C H 0.9197 -0.4785 0.1857 0.166 Uiso 1 1 calc R . . C18 C 1.0697(2) 0.5113(3) 0.34251(15) 0.0526(8) Uani 1 1 d . A . C19 C 1.0950(2) 0.6006(3) 0.39218(15) 0.0520(8) Uani 1 1 d D . . C20 C 1.1496(9) 0.5460(8) 0.4507(4) 0.133(6) Uani 0.656(15) 1 d PD A 1 H20A H 1.1675 0.603 0.4845 0.199 Uiso 0.656(15) 1 calc PR A 1 H20B H 1.2083 0.5114 0.445 0.199 Uiso 0.656(15) 1 calc PR A 1 H20C H 1.1096 0.4868 0.4621 0.199 Uiso 0.656(15) 1 calc PR A 1 C21 C 1.1611(7) 0.6896(7) 0.3685(6) 0.094(4) Uani 0.656(15) 1 d PD A 1 H21A H 1.1224 0.7266 0.3297 0.141 Uiso 0.656(15) 1 calc PR A 1 H21B H 1.2157 0.6494 0.3602 0.141 Uiso 0.656(15) 1 calc PR A 1 H21C H 1.1857 0.7474 0.4012 0.141 Uiso 0.656(15) 1 calc PR A 1 C22 C 1.0048(5) 0.6627(8) 0.3918(5) 0.068(2) Uani 0.656(15) 1 d PD A 1 H22A H 0.9753 0.6951 0.3498 0.103 Uiso 0.656(15) 1 calc PR A 1 H22B H 1.0206 0.7242 0.4231 0.103 Uiso 0.656(15) 1 calc PR A 1 H22C H 0.9592 0.6098 0.4023 0.103 Uiso 0.656(15) 1 calc PR A 1 C20A C 1.0818(18) 0.5436(12) 0.4552(7) 0.103(8) Uani 0.344(15) 1 d PD A 2 H20D H 1.0981 0.5996 0.4896 0.154 Uiso 0.344(15) 1 calc PR A 2 H20E H 1.125 0.4776 0.467 0.154 Uiso 0.344(15) 1 calc PR A 2 H20F H 1.0145 0.519 0.4476 0.154 Uiso 0.344(15) 1 calc PR A 2 C21A C 1.1997(7) 0.6372(13) 0.4091(7) 0.066(4) Uani 0.344(15) 1 d PD A 2 H21D H 1.2117 0.696 0.4419 0.099 Uiso 0.344(15) 1 calc PR A 2 H21E H 1.2138 0.6679 0.3715 0.099 Uiso 0.344(15) 1 calc PR A 2 H21F H 1.2416 0.5714 0.4248 0.099 Uiso 0.344(15) 1 calc PR A 2 C22A C 1.0265(11) 0.6998(12) 0.3761(11) 0.088(8) Uani 0.344(15) 1 d PD A 2 H22D H 1.0455 0.7572 0.4097 0.131 Uiso 0.344(15) 1 calc PR A 2 H22E H 0.9605 0.6737 0.3722 0.131 Uiso 0.344(15) 1 calc PR A 2 H22F H 1.0289 0.7335 0.3361 0.131 Uiso 0.344(15) 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 Na1 0.0476(6) 0.0282(5) 0.0291(5) -0.0024(4) 0.0026(4) -0.0026(4) Na2 0.0548(7) 0.0276(5) 0.0311(5) -0.0031(4) 0.0029(5) -0.0015(5) Si1 0.0383(4) 0.0304(4) 0.0304(4) 0.0028(3) 0.0092(3) 0.0042(3) Si2 0.0364(4) 0.0382(4) 0.0239(3) -0.0027(3) 0.0080(3) -0.0053(3) Si3 0.0432(4) 0.0299(4) 0.0246(3) 0.0006(3) 0.0073(3) -0.0012(3) Si4 0.0364(4) 0.0418(4) 0.0363(4) -0.0085(3) 0.0064(3) -0.0035(3) N1 0.0345(12) 0.0309(11) 0.0259(10) -0.0020(8) 0.0047(8) -0.0037(9) N2 0.0367(12) 0.0320(11) 0.0229(10) -0.0012(8) 0.0049(8) 0.0007(9) N5 0.0640(18) 0.0406(14) 0.0576(16) -0.0071(12) 0.0002(13) -0.0103(13) N6 0.092(2) 0.0402(15) 0.0637(18) -0.0149(13) 0.0094(16) 0.0006(15) C1 0.063(2) 0.0447(16) 0.0456(16) 0.0003(12) 0.0215(14) 0.0148(15) C2 0.0429(18) 0.0457(17) 0.066(2) 0.0073(14) 0.0171(15) -0.0019(14) C3 0.0500(18) 0.0499(17) 0.0415(15) 0.0094(13) 0.0072(13) 0.0109(14) C4 0.071(2) 0.062(2) 0.0561(19) 0.0120(16) 0.0252(17) -0.0148(18) C5 0.0487(18) 0.0622(19) 0.0405(15) -0.0041(13) 0.0155(13) 0.0086(15) C6 0.0518(19) 0.072(2) 0.0362(15) -0.0196(14) 0.0123(13) -0.0078(16) C7 0.0529(18) 0.0443(16) 0.0393(15) 0.0018(12) 0.0167(13) -0.0092(13) C8 0.067(2) 0.0519(18) 0.0363(15) 0.0108(13) 0.0071(14) -0.0025(16) C9 0.067(2) 0.0450(17) 0.0427(16) -0.0067(13) 0.0211(15) -0.0017(15) C10 0.053(2) 0.106(3) 0.0507(19) -0.026(2) 0.0042(16) -0.027(2) C11 0.060(3) 0.070(3) 0.134(4) -0.016(3) 0.031(3) 0.016(2) C12 0.058(2) 0.083(3) 0.059(2) -0.0018(18) 0.0240(17) -0.0247(19) C13 0.0483(18) 0.0349(14) 0.0448(15) -0.0008(12) 0.0083(13) -0.0082(13) C14 0.0532(18) 0.0378(14) 0.0412(15) -0.0082(12) 0.0101(13) -0.0106(13) C15 0.090(4) 0.149(5) 0.092(3) -0.053(3) 0.049(3) -0.024(3) C16 0.065(2) 0.078(3) 0.065(2) -0.0206(19) -0.0012(18) -0.012(2) C17 0.173(6) 0.048(2) 0.086(3) 0.001(2) 0.000(3) -0.044(3) C18 0.056(2) 0.0354(15) 0.0602(19) -0.0066(14) 0.0067(15) 0.0052(14) C19 0.0437(18) 0.0413(16) 0.0607(19) -0.0171(14) -0.0013(14) 0.0027(13) C20 0.158(11) 0.094(6) 0.083(7) -0.037(5) -0.066(7) 0.048(8) C21 0.092(6) 0.074(5) 0.134(9) -0.046(6) 0.061(6) -0.036(5) C22 0.053(4) 0.060(6) 0.088(5) -0.032(4) 0.014(3) 0.002(4) C20A 0.20(2) 0.054(8) 0.053(8) -0.014(6) 0.043(12) 0.010(12) C21A 0.059(7) 0.071(8) 0.061(8) -0.013(6) 0.008(5) -0.004(6) C22A 0.067(10) 0.031(8) 0.132(17) -0.032(8) -0.022(10) 0.012(7) #----------------------------------------------------------------------------# # 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 Na1 N1 2.385(2) . ? Na1 N2 2.403(2) . ? Na1 N5 2.412(3) . ? Na2 N2 2.384(2) . ? Na2 N6 2.393(3) . ? Na2 N1 2.405(2) . ? Si1 N2 1.685(2) . ? Si1 C2 1.881(3) . ? Si1 C3 1.886(3) . ? Si1 C1 1.889(3) . ? Si2 N2 1.687(2) . ? Si2 C4 1.873(3) . ? Si2 C6 1.885(3) . ? Si2 C5 1.887(3) . ? Si3 N1 1.684(2) . ? Si3 C9 1.882(3) . ? Si3 C7 1.885(3) . ? Si3 C8 1.887(3) . ? Si4 N1 1.684(2) . ? Si4 C11 1.871(4) . ? Si4 C10 1.875(3) . ? Si4 C12 1.883(3) . ? N5 C13 1.131(4) . ? N6 C18 1.129(4) . ? C13 C14 1.481(4) . ? C14 C17 1.500(5) . ? C14 C15 1.501(5) . ? C14 C16 1.538(5) . ? C18 C19 1.485(4) . ? C19 C20 1.455(8) . ? C19 C22 1.488(7) . ? C19 C22A 1.501(10) . ? 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 N1 Na1 N2 100.32(8) . . ? N1 Na1 N5 147.12(9) . . ? N2 Na1 N5 112.25(9) . . ? N2 Na2 N6 146.23(10) . . ? N2 Na2 N1 100.29(8) . . ? N6 Na2 N1 111.91(9) . . ? N2 Si1 C2 112.93(13) . . ? N2 Si1 C3 115.91(13) . . ? C2 Si1 C3 106.03(15) . . ? N2 Si1 C1 110.26(13) . . ? C2 Si1 C1 106.04(15) . . ? C3 Si1 C1 104.92(14) . . ? N2 Si2 C4 113.68(14) . . ? N2 Si2 C6 114.46(13) . . ? C4 Si2 C6 106.85(16) . . ? N2 Si2 C5 111.05(12) . . ? C4 Si2 C5 105.57(17) . . ? C6 Si2 C5 104.46(15) . . ? N1 Si3 C9 113.73(12) . . ? N1 Si3 C7 110.23(11) . . ? C9 Si3 C7 105.80(15) . . ? N1 Si3 C8 115.49(14) . . ? C9 Si3 C8 105.38(14) . . ? C7 Si3 C8 105.43(14) . . ? N1 Si4 C11 112.46(16) . . ? N1 Si4 C10 115.52(15) . . ? C11 Si4 C10 108.3(2) . . ? N1 Si4 C12 110.63(14) . . ? C11 Si4 C12 105.8(2) . . ? C10 Si4 C12 103.38(18) . . ? Si4 N1 Si3 126.94(12) . . ? Si4 N1 Na1 118.39(11) . . ? Si3 N1 Na1 103.22(10) . . ? Si4 N1 Na2 102.44(10) . . ? Si3 N1 Na2 116.83(11) . . ? Na1 N1 Na2 79.67(7) . . ? Si1 N2 Si2 126.33(12) . . ? Si1 N2 Na2 104.99(10) . . ? Si2 N2 Na2 119.83(11) . . ? Si1 N2 Na1 115.37(11) . . ? Si2 N2 Na1 101.04(10) . . ? Na2 N2 Na1 79.71(7) . . ? C13 N5 Na1 153.0(2) . . ? C18 N6 Na2 159.2(3) . . ? N5 C13 C14 179.1(3) . . ? C13 C14 C17 107.6(3) . . ? C13 C14 C15 109.3(3) . . ? C17 C14 C15 114.5(4) . . ? C13 C14 C16 107.3(3) . . ? C17 C14 C16 108.6(3) . . ? C15 C14 C16 109.2(3) . . ? N6 C18 C19 178.9(4) . . ? C20 C19 C18 107.6(4) . . ? C20 C19 C22 117.8(7) . . ? C18 C19 C22 108.4(5) . . ? C20 C19 C22A 134.5(10) . . ? C18 C19 C22A 111.6(9) . . ? #===END data_(2a)-jun2500 _database_code_depnum_ccdc_archive 'CCDC 271691' _audit_creation_date 2000-06-21T11:06:04-00:00 _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_name_common ((Na(AdCN)(N(SiMe3)(SiMe2Ph)))2) _chemical_formula_moiety 'C44 H70 N4 Na2 Si4' _chemical_formula_sum 'C44 H70 N4 Na2 Si4' _chemical_formula_weight 813.38 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3261(7) _cell_length_b 11.1180(12) _cell_length_c 11.9940(10) _cell_angle_alpha 117.513(4) _cell_angle_beta 92.062(5) _cell_angle_gamma 100.720(5) _cell_volume 1188.14(18) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28349 _cell_measurement_theta_min 3.638 _cell_measurement_theta_max 27.878 _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 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.177 _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 13439 _diffrn_reflns_av_R_equivalents 0.0963 _diffrn_reflns_av_unetI/netI 0.0842 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 27.97 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.96 _diffrn_measured_fraction_theta_max 0.96 _reflns_number_total 5493 _reflns_number_gt 4248 _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 ; 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^)+(0.0477P)^2^+1.6178P] 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 5493 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.095 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2046 _refine_ls_wR_factor_gt 0.1934 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.406 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.067 #----------------------------------------------------------------------------# # 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' 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 -0.09283(12) 0.88795(13) 0.02099(13) 0.0377(3) Uani 1 1 d . . . Si1 Si 0.22485(9) 0.87713(9) 0.02666(8) 0.0331(2) Uani 1 1 d . . . Si2 Si 0.08880(9) 0.79273(9) -0.23711(8) 0.0350(2) Uani 1 1 d . . . N1 N 0.1087(3) 0.8738(3) -0.0774(2) 0.0323(6) Uani 1 1 d . . . N2 N -0.2686(3) 0.6893(3) -0.0342(3) 0.0494(8) Uani 1 1 d . . . C1 C 0.3257(4) 0.7413(4) -0.0362(4) 0.0479(9) Uani 1 1 d . . . H1A H 0.2659 0.6488 -0.0827 0.072 Uiso 1 1 calc R . . H1B H 0.381 0.7465 0.0347 0.072 Uiso 1 1 calc R . . H1C H 0.383 0.7579 -0.0934 0.072 Uiso 1 1 calc R . . C2 C 0.3527(3) 1.0469(4) 0.1120(4) 0.0447(8) Uani 1 1 d . . . H2A H 0.3076 1.1241 0.1478 0.067 Uiso 1 1 calc R . . H2B H 0.4095 1.0579 0.0522 0.067 Uiso 1 1 calc R . . H2C H 0.4074 1.047 0.1806 0.067 Uiso 1 1 calc R . . C3 C 0.1412(3) 0.8454(4) 0.1528(3) 0.0355(7) Uani 1 1 d . . . C4 C 0.0409(3) 0.7256(4) 0.1158(4) 0.0433(8) Uani 1 1 d . . . H4 H 0.0137 0.6629 0.028 0.052 Uiso 1 1 calc R . . C5 C -0.0203(4) 0.6956(4) 0.2047(4) 0.0523(10) Uani 1 1 d . . . H5 H -0.0883 0.6134 0.1768 0.063 Uiso 1 1 calc R . . C6 C 0.0168(4) 0.7839(5) 0.3317(4) 0.0495(9) Uani 1 1 d . . . H6 H -0.0246 0.7625 0.3918 0.059 Uiso 1 1 calc R . . C7 C 0.1149(4) 0.9045(4) 0.3727(4) 0.0467(8) Uani 1 1 d . . . H7 H 0.1404 0.9668 0.4608 0.056 Uiso 1 1 calc R . . C8 C 0.1763(3) 0.9338(4) 0.2831(3) 0.0393(7) Uani 1 1 d . . . H8 H 0.244 1.0164 0.3119 0.047 Uiso 1 1 calc R . . C9 C 0.1696(5) 0.9115(5) -0.2997(4) 0.0671(12) Uani 1 1 d . . . H9A H 0.1403 0.9992 -0.2594 0.101 Uiso 1 1 calc R . . H9B H 0.1439 0.8664 -0.3918 0.101 Uiso 1 1 calc R . . H9C H 0.2666 0.9306 -0.2804 0.101 Uiso 1 1 calc R . . C10 C 0.1517(5) 0.6287(5) -0.3201(4) 0.0700(14) Uani 1 1 d . . . H10A H 0.1116 0.5622 -0.292 0.105 Uiso 1 1 calc R . . H10B H 0.2487 0.651 -0.2995 0.105 Uiso 1 1 calc R . . H10C H 0.1274 0.5877 -0.4121 0.105 Uiso 1 1 calc R . . C11 C -0.0921(4) 0.7383(5) -0.3047(4) 0.0543(10) Uani 1 1 d . . . H11A H -0.14 0.6749 -0.2764 0.081 Uiso 1 1 calc R . . H11B H -0.101 0.6908 -0.3977 0.081 Uiso 1 1 calc R . . H11C H -0.1297 0.8208 -0.2754 0.081 Uiso 1 1 calc R . . C12 C -0.3342(3) 0.5900(4) -0.1148(3) 0.0388(7) Uani 1 1 d . . . C13 C -0.4159(3) 0.4640(3) -0.2222(3) 0.0342(7) Uani 1 1 d . . . C14 C -0.5306(3) 0.3955(3) -0.1762(3) 0.0371(7) Uani 1 1 d . . . H14A H -0.4939 0.3695 -0.1152 0.044 Uiso 1 1 calc R . . H14B H -0.5868 0.462 -0.1328 0.044 Uiso 1 1 calc R . . C15 C -0.6142(3) 0.2658(3) -0.2907(3) 0.0398(7) Uani 1 1 d . . . H15 H -0.6883 0.2208 -0.2614 0.048 Uiso 1 1 calc R . . C16 C -0.6723(3) 0.3068(4) -0.3832(3) 0.0441(8) Uani 1 1 d . . . H16A H -0.7291 0.3728 -0.3407 0.053 Uiso 1 1 calc R . . H16B H -0.728 0.2231 -0.4567 0.053 Uiso 1 1 calc R . . C17 C -0.5589(4) 0.3748(4) -0.4288(4) 0.0499(9) Uani 1 1 d . . . H17 H -0.5972 0.4009 -0.4901 0.06 Uiso 1 1 calc R . . C18 C -0.4749(4) 0.5055(4) -0.3158(3) 0.0438(8) Uani 1 1 d . . . H18A H -0.5308 0.5726 -0.2731 0.053 Uiso 1 1 calc R . . H18B H -0.4023 0.5506 -0.3452 0.053 Uiso 1 1 calc R . . C19 C -0.3277(3) 0.3601(4) -0.2884(4) 0.0448(8) Uani 1 1 d . . . H19A H -0.253 0.4039 -0.3169 0.054 Uiso 1 1 calc R . . H19B H -0.2903 0.3329 -0.2286 0.054 Uiso 1 1 calc R . . C20 C -0.4138(4) 0.2321(4) -0.4023(4) 0.0549(10) Uani 1 1 d . . . H20 H -0.3578 0.1643 -0.4466 0.066 Uiso 1 1 calc R . . C21 C -0.5274(4) 0.1630(4) -0.3568(4) 0.0526(10) Uani 1 1 d . . . H21A H -0.5817 0.0781 -0.4301 0.063 Uiso 1 1 calc R . . H21B H -0.4901 0.1355 -0.2971 0.063 Uiso 1 1 calc R . . C22 C -0.4721(4) 0.2728(5) -0.4946(4) 0.0636(12) Uani 1 1 d . . . H22A H -0.526 0.1887 -0.569 0.076 Uiso 1 1 calc R . . H22B H -0.3993 0.3164 -0.525 0.076 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 Na 0.0369(7) 0.0283(6) 0.0485(8) 0.0192(6) 0.0074(5) 0.0059(5) Si1 0.0350(5) 0.0313(5) 0.0363(5) 0.0180(4) 0.0058(3) 0.0101(4) Si2 0.0397(5) 0.0333(5) 0.0351(5) 0.0176(4) 0.0067(4) 0.0115(4) N1 0.0353(13) 0.0301(13) 0.0374(14) 0.0195(11) 0.0060(11) 0.0116(11) N2 0.0472(17) 0.0412(17) 0.0534(19) 0.0223(15) -0.0011(14) -0.0022(14) C1 0.051(2) 0.050(2) 0.050(2) 0.0258(18) 0.0067(16) 0.0241(17) C2 0.0402(18) 0.045(2) 0.049(2) 0.0239(17) 0.0049(15) 0.0033(15) C3 0.0353(16) 0.0381(17) 0.0397(17) 0.0227(14) 0.0057(13) 0.0119(13) C4 0.0416(18) 0.044(2) 0.047(2) 0.0256(17) 0.0012(15) 0.0055(15) C5 0.043(2) 0.056(2) 0.066(3) 0.041(2) 0.0030(18) -0.0010(17) C6 0.0443(19) 0.067(3) 0.056(2) 0.043(2) 0.0131(17) 0.0157(18) C7 0.047(2) 0.057(2) 0.0424(19) 0.0274(18) 0.0091(15) 0.0164(17) C8 0.0408(17) 0.0401(18) 0.0411(18) 0.0230(15) 0.0037(14) 0.0092(14) C9 0.079(3) 0.074(3) 0.054(2) 0.042(2) 0.013(2) -0.001(2) C10 0.090(3) 0.067(3) 0.043(2) 0.008(2) 0.002(2) 0.047(3) C11 0.051(2) 0.061(3) 0.046(2) 0.0211(19) -0.0017(17) 0.0148(19) C12 0.0374(17) 0.0360(18) 0.0460(19) 0.0245(16) 0.0020(14) 0.0020(14) C13 0.0369(16) 0.0295(16) 0.0363(16) 0.0168(13) 0.0015(13) 0.0053(13) C14 0.0440(18) 0.0308(16) 0.0380(17) 0.0185(14) 0.0041(14) 0.0069(14) C15 0.0389(17) 0.0301(16) 0.0462(19) 0.0168(15) 0.0059(14) 0.0022(13) C16 0.0349(17) 0.046(2) 0.0446(19) 0.0177(16) 0.0002(14) 0.0047(15) C17 0.046(2) 0.064(3) 0.043(2) 0.0318(19) -0.0012(16) 0.0028(18) C18 0.0456(19) 0.045(2) 0.049(2) 0.0323(18) 0.0033(16) 0.0050(16) C19 0.0344(17) 0.0395(19) 0.052(2) 0.0148(16) 0.0026(15) 0.0105(14) C20 0.043(2) 0.043(2) 0.057(2) 0.0049(18) 0.0087(17) 0.0148(17) C21 0.051(2) 0.0276(17) 0.067(3) 0.0134(17) -0.0007(18) 0.0084(15) C22 0.052(2) 0.075(3) 0.037(2) 0.010(2) 0.0085(17) -0.001(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 Na N2 2.384(3) . ? Na N1 2.423(3) . ? Na N1 2.453(3) 2_575 ? Si1 N1 1.683(3) . ? Si1 C1 1.877(4) . ? Si1 C2 1.882(4) . ? Si1 C3 1.906(3) . ? Si1 Na 3.4138(15) 2_575 ? Si2 N1 1.683(3) . ? Si2 C11 1.879(4) . ? Si2 C10 1.883(4) . ? Si2 C9 1.885(4) . ? N1 Na 2.453(3) 2_575 ? N2 C12 1.140(4) . ? C3 C8 1.396(5) . ? C3 C4 1.397(5) . ? C4 C5 1.395(5) . ? C5 C6 1.367(6) . ? C6 C7 1.384(6) . ? C7 C8 1.399(5) . ? C12 C13 1.465(5) . ? C13 C18 1.542(4) . ? C13 C14 1.545(4) . ? C13 C19 1.547(5) . ? C14 C15 1.527(5) . ? C15 C16 1.523(5) . ? C15 C21 1.527(5) . ? C16 C17 1.530(5) . ? C17 C22 1.521(6) . ? C17 C18 1.526(5) . ? C19 C20 1.526(5) . ? C20 C22 1.520(6) . ? C20 C21 1.537(6) . ? 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 N2 Na N1 122.77(11) . . ? N2 Na N1 128.43(11) . 2_575 ? N1 Na N1 101.15(9) . 2_575 ? N1 Si1 C1 117.36(15) . . ? N1 Si1 C2 114.09(15) . . ? C1 Si1 C2 104.30(18) . . ? N1 Si1 C3 109.57(13) . . ? C1 Si1 C3 103.41(16) . . ? C2 Si1 C3 107.15(16) . . ? N1 Si2 C11 111.09(16) . . ? N1 Si2 C10 117.56(17) . . ? C11 Si2 C10 104.3(2) . . ? N1 Si2 C9 111.74(18) . . ? C11 Si2 C9 105.3(2) . . ? C10 Si2 C9 105.9(2) . . ? Si1 N1 Si2 130.09(16) . . ? Si1 N1 Na 105.75(12) . . ? Si2 N1 Na 116.55(13) . . ? Si1 N1 Na 109.89(13) . 2_575 ? Si2 N1 Na 103.40(12) . 2_575 ? Na N1 Na 78.85(9) . 2_575 ? C12 N2 Na 145.9(3) . . ? C8 C3 C4 116.5(3) . . ? C8 C3 Si1 123.9(3) . . ? C4 C3 Si1 119.5(3) . . ? C5 C4 C3 121.7(4) . . ? C6 C5 C4 120.4(4) . . ? C5 C6 C7 119.9(3) . . ? C6 C7 C8 119.4(4) . . ? C3 C8 C7 122.1(3) . . ? N2 C12 C13 177.7(4) . . ? C12 C13 C18 108.4(3) . . ? C12 C13 C14 110.6(3) . . ? C18 C13 C14 109.2(3) . . ? C12 C13 C19 109.2(3) . . ? C18 C13 C19 110.0(3) . . ? C14 C13 C19 109.5(3) . . ? C15 C14 C13 109.0(3) . . ? C16 C15 C21 109.6(3) . . ? C16 C15 C14 109.6(3) . . ? C21 C15 C14 109.7(3) . . ? C15 C16 C17 109.4(3) . . ? C22 C17 C18 109.6(3) . . ? C22 C17 C16 109.7(3) . . ? C18 C17 C16 109.7(3) . . ? C17 C18 C13 108.8(3) . . ? C20 C19 C13 108.2(3) . . ? C22 C20 C19 110.5(4) . . ? C22 C20 C21 109.4(3) . . ? C19 C20 C21 109.6(3) . . ? C15 C21 C20 109.2(3) . . ? C20 C22 C17 109.6(3) . . ? #===END data_(2b)-feb1000 _database_code_depnum_ccdc_archive 'CCDC 271692' _audit_creation_date 2000-02-04T15:51:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ((Na(tBuCN)(Me3SiNSiMe2Ph))2) _chemical_formula_moiety 'C32 H58 N4 Na2 Si4' _chemical_formula_sum 'C32 H58 N4 Na2 Si4' _chemical_formula_weight 657.16 _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 10.9961(3) _cell_length_b 10.9755(2) _cell_length_c 17.7283(5) _cell_angle_alpha 90 _cell_angle_beta 105.666(1) _cell_angle_gamma 90 _cell_volume 2060.11(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10080 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 30.034 _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 0.3 _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.19 _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 19890 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.71 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 5976 _reflns_number_gt 4918 _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 ; 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^)+(0.0516P)^2^+0.5492P] 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 5976 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.327 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.043 #----------------------------------------------------------------------------# # 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' 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 -0.58873(5) -0.04140(5) 0.04897(3) 0.03199(13) Uani 1 1 d . . . Si1 Si -0.26835(3) -0.03568(3) 0.135663(19) 0.02667(9) Uani 1 1 d . . . Si2 Si -0.38351(3) -0.24866(3) 0.02993(2) 0.02846(9) Uani 1 1 d . . . N1 N -0.37077(9) -0.10177(9) 0.05866(6) 0.0270(2) Uani 1 1 d . . . N2 N -0.68111(14) -0.04567(14) 0.15627(8) 0.0487(3) Uani 1 1 d . . . C1 C -0.34215(15) 0.01607(15) 0.21448(8) 0.0410(3) Uani 1 1 d . . . H1A H -0.4168 0.0658 0.1911 0.061 Uiso 1 1 calc R . . H1B H -0.2809 0.0646 0.2533 0.061 Uiso 1 1 calc R . . H1C H -0.3671 -0.0552 0.2401 0.061 Uiso 1 1 calc R . . C2 C -0.12765(14) -0.12825(14) 0.18990(9) 0.0429(3) Uani 1 1 d . . . H2A H -0.083 -0.1589 0.1528 0.064 Uiso 1 1 calc R . . H2B H -0.1562 -0.1971 0.2159 0.064 Uiso 1 1 calc R . . H2C H -0.0705 -0.077 0.2292 0.064 Uiso 1 1 calc R . . C3 C -0.19555(11) 0.10331(11) 0.10026(7) 0.0282(2) Uani 1 1 d . . . C4 C -0.19161(14) 0.22034(12) 0.13186(8) 0.0366(3) Uani 1 1 d . . . H4 H -0.2282 0.2342 0.1739 0.044 Uiso 1 1 calc R . . C5 C -0.13528(16) 0.31737(13) 0.10323(10) 0.0452(3) Uani 1 1 d . . . H5 H -0.1348 0.3962 0.1254 0.054 Uiso 1 1 calc R . . C6 C -0.08036(15) 0.29932(15) 0.04288(9) 0.0462(4) Uani 1 1 d . . . H6 H -0.0422 0.3655 0.0233 0.055 Uiso 1 1 calc R . . C7 C -0.08109(14) 0.18470(15) 0.01100(9) 0.0420(3) Uani 1 1 d . . . H7 H -0.0424 0.1715 -0.0302 0.05 Uiso 1 1 calc R . . C8 C -0.13836(13) 0.08841(12) 0.03911(8) 0.0338(3) Uani 1 1 d . . . H8 H -0.1388 0.0101 0.0162 0.041 Uiso 1 1 calc R . . C9 C -0.23435(17) -0.34000(16) 0.04802(12) 0.0575(5) Uani 1 1 d . . . H9A H -0.1912 -0.3397 0.1042 0.086 Uiso 1 1 calc R . . H9B H -0.179 -0.304 0.019 0.086 Uiso 1 1 calc R . . H9C H -0.2548 -0.424 0.0304 0.086 Uiso 1 1 calc R . . C10 C -0.45459(18) -0.25887(16) -0.07874(10) 0.0525(4) Uani 1 1 d . . . H10A H -0.5341 -0.2133 -0.0932 0.079 Uiso 1 1 calc R . . H10B H -0.4709 -0.3444 -0.0939 0.079 Uiso 1 1 calc R . . H10C H -0.3958 -0.2242 -0.1058 0.079 Uiso 1 1 calc R . . C11 C -0.4922(3) -0.33666(18) 0.07525(16) 0.0814(8) Uani 1 1 d . . . H11A H -0.5721 -0.2925 0.0673 0.122 Uiso 1 1 calc R . . H11B H -0.4528 -0.3463 0.1315 0.122 Uiso 1 1 calc R . . H11C H -0.5084 -0.4171 0.0506 0.122 Uiso 1 1 calc R . . C12 C -0.70811(13) 0.00363(13) 0.20587(8) 0.0347(3) Uani 1 1 d . . . C13 C -0.74129(12) 0.07204(13) 0.26933(8) 0.0327(3) Uani 1 1 d . . . C14 C -0.76606(18) -0.01811(16) 0.32901(10) 0.0506(4) Uani 1 1 d . . . H14A H -0.7882 0.0266 0.3713 0.076 Uiso 1 1 calc R . . H14B H -0.69 -0.0668 0.3508 0.076 Uiso 1 1 calc R . . H14C H -0.836 -0.072 0.3033 0.076 Uiso 1 1 calc R . . C15 C -0.85975(16) 0.14761(17) 0.23265(11) 0.0528(4) Uani 1 1 d . . . H15A H -0.8833 0.1944 0.2736 0.079 Uiso 1 1 calc R . . H15B H -0.9293 0.0931 0.2071 0.079 Uiso 1 1 calc R . . H15C H -0.8424 0.2037 0.1938 0.079 Uiso 1 1 calc R . . C16 C -0.62981(17) 0.15611(19) 0.30611(12) 0.0606(5) Uani 1 1 d . . . H16A H -0.6489 0.2035 0.3484 0.091 Uiso 1 1 calc R . . H16B H -0.6154 0.2116 0.2661 0.091 Uiso 1 1 calc R . . H16C H -0.5539 0.107 0.3274 0.091 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 Na 0.0331(3) 0.0367(3) 0.0296(3) 0.0075(2) 0.0143(2) 0.0074(2) Si1 0.02832(16) 0.02590(16) 0.02508(16) 0.00326(12) 0.00600(12) 0.00251(12) Si2 0.03339(18) 0.02304(16) 0.03149(18) 0.00092(12) 0.01310(13) 0.00184(12) N1 0.0285(5) 0.0241(5) 0.0282(5) 0.0027(4) 0.0072(4) 0.0041(4) N2 0.0533(8) 0.0613(9) 0.0378(7) -0.0042(6) 0.0230(6) -0.0056(6) C1 0.0496(8) 0.0467(8) 0.0299(6) -0.0013(6) 0.0161(6) -0.0026(6) C2 0.0377(7) 0.0382(7) 0.0450(8) 0.0097(6) -0.0024(6) 0.0053(6) C3 0.0280(5) 0.0274(6) 0.0277(6) 0.0019(4) 0.0049(4) 0.0013(4) C4 0.0443(7) 0.0311(6) 0.0350(7) -0.0016(5) 0.0118(5) 0.0000(5) C5 0.0577(9) 0.0291(7) 0.0479(8) -0.0020(6) 0.0127(7) -0.0065(6) C6 0.0524(9) 0.0404(8) 0.0449(8) 0.0092(6) 0.0116(7) -0.0101(7) C7 0.0445(8) 0.0486(8) 0.0363(7) 0.0051(6) 0.0166(6) -0.0044(6) C8 0.0373(6) 0.0330(6) 0.0317(6) -0.0007(5) 0.0102(5) 0.0003(5) C9 0.0560(10) 0.0430(9) 0.0649(11) -0.0085(8) 0.0012(8) 0.0242(7) C10 0.0636(10) 0.0454(9) 0.0402(8) -0.0112(7) -0.0001(7) 0.0142(7) C11 0.1201(19) 0.0465(10) 0.1078(18) -0.0159(11) 0.0828(16) -0.0322(11) C12 0.0328(6) 0.0418(7) 0.0314(6) 0.0004(5) 0.0118(5) -0.0085(5) C13 0.0320(6) 0.0355(6) 0.0315(6) -0.0048(5) 0.0099(5) -0.0058(5) C14 0.0668(11) 0.0523(9) 0.0418(8) 0.0038(7) 0.0305(8) 0.0040(8) C15 0.0469(9) 0.0514(9) 0.0579(10) -0.0001(8) 0.0105(7) 0.0066(7) C16 0.0511(9) 0.0659(12) 0.0598(11) -0.0233(9) 0.0061(8) -0.0208(8) #----------------------------------------------------------------------------# # 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 N2 2.3867(14) . ? Na N1 2.4185(11) 3_455 ? Na N1 2.4475(11) . ? Si1 N1 1.6816(11) . ? Si1 C1 1.8831(14) . ? Si1 C2 1.8833(14) . ? Si1 C3 1.9061(13) . ? Si2 N1 1.6851(11) . ? Si2 C9 1.8746(16) . ? Si2 C10 1.8766(17) . ? Si2 C11 1.8776(18) . ? N1 Na 2.4186(11) 3_455 ? N2 C12 1.1380(18) . ? C3 C4 1.3972(18) . ? C3 C8 1.4019(18) . ? C4 C5 1.395(2) . ? C5 C6 1.378(2) . ? C6 C7 1.378(2) . ? C7 C8 1.3898(19) . ? C8 Na 3.0298(14) 3_455 ? C12 C13 1.4778(19) . ? C13 C14 1.526(2) . ? C13 C16 1.532(2) . ? C13 C15 1.533(2) . ? 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 N2 Na N1 127.89(5) . 3_455 ? N2 Na N1 123.93(5) . . ? N1 Na N1 101.50(3) 3_455 . ? N1 Si1 C1 113.84(6) . . ? N1 Si1 C2 117.36(6) . . ? C1 Si1 C2 104.07(7) . . ? N1 Si1 C3 109.06(5) . . ? C1 Si1 C3 107.84(6) . . ? C2 Si1 C3 103.87(6) . . ? N1 Si2 C9 117.54(7) . . ? N1 Si2 C10 110.18(7) . . ? C9 Si2 C10 104.26(8) . . ? N1 Si2 C11 111.93(7) . . ? C9 Si2 C11 106.28(11) . . ? C10 Si2 C11 105.77(11) . . ? Si1 N1 Si2 129.85(6) . . ? Si1 N1 Na 107.49(5) . 3_455 ? Si2 N1 Na 113.62(5) . 3_455 ? Si1 N1 Na 111.63(5) . . ? Si2 N1 Na 103.76(5) . . ? Na N1 Na 78.50(3) 3_455 . ? C12 N2 Na 149.60(13) . . ? C4 C3 C8 116.45(12) . . ? C4 C3 Si1 125.03(10) . . ? C8 C3 Si1 118.50(9) . . ? C5 C4 C3 121.65(13) . . ? C6 C5 C4 120.25(14) . . ? C5 C6 C7 119.64(14) . . ? C6 C7 C8 120.01(14) . . ? C7 C8 C3 122.00(13) . . ? C7 C8 Na 115.24(9) . 3_455 ? C3 C8 Na 80.20(7) . 3_455 ? N2 C12 C13 177.80(15) . . ? C12 C13 C14 108.99(12) . . ? C12 C13 C16 107.24(12) . . ? C14 C13 C16 111.56(14) . . ? C12 C13 C15 107.95(12) . . ? C14 C13 C15 110.77(13) . . ? C16 C13 C15 110.19(14) . . ? #===END data_(3)-feb1605 _database_code_depnum_ccdc_archive 'CCDC 271693' _audit_creation_date 2005-02-16T12:26:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H54 N3 Na3 Si3' _chemical_formula_sum 'C21 H54 N3 Na3 Si3' _chemical_formula_weight 501.91 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6622(2) _cell_length_b 12.3995(3) _cell_length_c 15.4351(4) _cell_angle_alpha 78.751(2) _cell_angle_beta 80.164(1) _cell_angle_gamma 86.661(1) _cell_volume 1601.55(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 21747 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.201 _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_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.594181E-1 _diffrn_orient_matrix_ub_12 0.91358E-2 _diffrn_orient_matrix_ub_13 -0.623905E-1 _diffrn_orient_matrix_ub_21 0.667906E-1 _diffrn_orient_matrix_ub_22 0.558722E-1 _diffrn_orient_matrix_ub_23 0.133309E-1 _diffrn_orient_matrix_ub_31 0.757999E-1 _diffrn_orient_matrix_ub_32 -0.596726E-1 _diffrn_orient_matrix_ub_33 0.202997E-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 0.0433 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_number 28337 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 26.06 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 6290 _reflns_number_gt 5261 _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-86 (Sheldrick, 1986)' _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 ; *************************************************************************** In one ligand (N3) there is unresolved end-for-end disorder with partial Si/C occupancy for Si3 and C18, and bonds and angles involving this ligand are unreliable. *************************************************************************** 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^)+(0.0721P)^2^+1.2196P] 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 6290 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.049 _refine_ls_wR_factor_ref 0.1428 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.612 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.051 #----------------------------------------------------------------------------# # 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' 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 Si1 Si 0.44539(7) 0.24384(6) 0.48487(4) 0.03363(17) Uani 1 1 d . A 1 Si2 Si 0.97572(7) 0.53325(5) 0.18425(4) 0.03191(17) Uani 1 1 d . A 1 Si3 Si 0.62745(10) 0.11787(7) 0.13531(6) 0.0294(3) Uani 0.598(3) 1 d P A 1 Na1 Na 0.68943(11) 0.13367(8) 0.34027(6) 0.0386(2) Uani 1 1 d . A 1 Na2 Na 0.70644(11) 0.41604(8) 0.34873(6) 0.0428(2) Uani 1 1 d . A 1 Na3 Na 0.80816(11) 0.33105(7) 0.13680(6) 0.0349(2) Uani 1 1 d . A 1 N1 N 0.6399(2) 0.24895(16) 0.45118(11) 0.0308(4) Uani 1 1 d . A 1 N2 N 0.7894(2) 0.49596(14) 0.19629(12) 0.0285(4) Uani 1 1 d . A 1 N3 N 0.7699(2) 0.13919(14) 0.18534(12) 0.0309(4) Uani 1 1 d . A 1 C1 C 0.3528(3) 0.2374(3) 0.38522(18) 0.0521(7) Uani 1 1 d . A 1 H1A H 0.3868 0.2995 0.3371 0.078 Uiso 1 1 calc R A 1 H1B H 0.2384 0.2409 0.4017 0.078 Uiso 1 1 calc R A 1 H1C H 0.3845 0.1682 0.3646 0.078 Uiso 1 1 calc R A 1 C2 C 0.3490(3) 0.3667(3) 0.5300(2) 0.0571(7) Uani 1 1 d . A 1 H2A H 0.3926 0.3747 0.5829 0.086 Uiso 1 1 calc R A 1 H2B H 0.2358 0.3559 0.5465 0.086 Uiso 1 1 calc R A 1 H2C H 0.3685 0.4332 0.4839 0.086 Uiso 1 1 calc R A 1 C3 C 0.3668(3) 0.1201(2) 0.56924(18) 0.0514(7) Uani 1 1 d . A 1 H3A H 0.4092 0.1166 0.6247 0.077 Uiso 1 1 calc R A 1 H3B H 0.3983 0.0532 0.5451 0.077 Uiso 1 1 calc R A 1 H3C H 0.2522 0.1262 0.5818 0.077 Uiso 1 1 calc R A 1 C4 C 0.7532(2) 0.23196(18) 0.51427(13) 0.0291(5) Uani 1 1 d . A 1 C5 C 0.9001(3) 0.3001(4) 0.4719(2) 0.0734(11) Uani 1 1 d . A 1 H5A H 0.8697 0.3781 0.458 0.11 Uiso 1 1 calc R A 1 H5B H 0.9491 0.2756 0.4167 0.11 Uiso 1 1 calc R A 1 H5C H 0.9748 0.2897 0.5141 0.11 Uiso 1 1 calc R A 1 C6 C 0.8024(5) 0.1096(3) 0.5356(3) 0.0784(11) Uani 1 1 d . A 1 H6A H 0.7099 0.0659 0.5632 0.118 Uiso 1 1 calc R A 1 H6B H 0.8783 0.0997 0.577 0.118 Uiso 1 1 calc R A 1 H6C H 0.8502 0.0853 0.4801 0.118 Uiso 1 1 calc R A 1 C7 C 0.6940(4) 0.2688(3) 0.6038(2) 0.0666(9) Uani 1 1 d . A 1 H7A H 0.6633 0.3469 0.5925 0.1 Uiso 1 1 calc R A 1 H7B H 0.7776 0.2573 0.6404 0.1 Uiso 1 1 calc R A 1 H7C H 0.6033 0.2255 0.6355 0.1 Uiso 1 1 calc R A 1 C8 C 1.0216(3) 0.6115(3) 0.2680(2) 0.0546(7) Uani 1 1 d . A 1 H8A H 0.9607 0.6809 0.2635 0.082 Uiso 1 1 calc R A 1 H8B H 1.1337 0.6269 0.2561 0.082 Uiso 1 1 calc R A 1 H8C H 0.9944 0.5678 0.3283 0.082 Uiso 1 1 calc R A 1 C9 C 1.0977(3) 0.4046(2) 0.20031(19) 0.0439(6) Uani 1 1 d . A 1 H9A H 1.0798 0.359 0.158 0.066 Uiso 1 1 calc R A 1 H9B H 1.069 0.3641 0.2617 0.066 Uiso 1 1 calc R A 1 H9C H 1.2087 0.4231 0.1897 0.066 Uiso 1 1 calc R A 1 C10 C 1.0672(3) 0.6113(2) 0.0722(2) 0.0522(7) Uani 1 1 d . A 1 H10A H 1.0472 0.5739 0.025 0.078 Uiso 1 1 calc R A 1 H10B H 1.1805 0.6148 0.0703 0.078 Uiso 1 1 calc R A 1 H10C H 1.0216 0.6861 0.0628 0.078 Uiso 1 1 calc R A 1 C11 C 0.6622(2) 0.57248(14) 0.16914(13) 0.0189(4) Uani 1 1 d . A 1 C12 C 0.5014(3) 0.5306(2) 0.2258(2) 0.0510(7) Uani 1 1 d . A 1 H12A H 0.4873 0.4546 0.2201 0.077 Uiso 1 1 calc R A 1 H12B H 0.4158 0.5775 0.2038 0.077 Uiso 1 1 calc R A 1 H12C H 0.5006 0.5337 0.2888 0.077 Uiso 1 1 calc R A 1 C13 C 0.6760(4) 0.6927(2) 0.1807(2) 0.0575(8) Uani 1 1 d . A 1 H13A H 0.6867 0.6935 0.2427 0.086 Uiso 1 1 calc R A 1 H13B H 0.5817 0.7352 0.1663 0.086 Uiso 1 1 calc R A 1 H13C H 0.7682 0.7254 0.1403 0.086 Uiso 1 1 calc R A 1 C14 C 0.6467(4) 0.5763(3) 0.06895(19) 0.0564(7) Uani 1 1 d . A 1 H14A H 0.6374 0.5013 0.0592 0.085 Uiso 1 1 calc R A 1 H14B H 0.7399 0.6097 0.03 0.085 Uiso 1 1 calc R A 1 H14C H 0.5533 0.6202 0.0551 0.085 Uiso 1 1 calc R A 1 C15 C 0.6778(5) 0.1014(3) 0.0246(3) 0.0813(11) Uani 1 1 d . A 1 H15A H 0.7444 0.1618 -0.0092 0.122 Uiso 1 1 calc R A 1 H15B H 0.5824 0.1021 -0.0017 0.122 Uiso 1 1 calc R A 1 H15C H 0.7348 0.0312 0.0225 0.122 Uiso 1 1 calc R A 1 C16 C 0.5030(4) 0.2347(3) 0.1324(2) 0.0575(8) Uani 1 1 d . A 1 H16A H 0.4701 0.2485 0.1933 0.086 Uiso 1 1 calc R A 1 H16B H 0.4105 0.2224 0.1072 0.086 Uiso 1 1 calc R A 1 H16C H 0.5588 0.2984 0.0952 0.086 Uiso 1 1 calc R A 1 C17 C 0.5109(4) 0.0086(3) 0.1919(2) 0.0637(8) Uani 1 1 d . A 1 H17A H 0.4811 0.015 0.2548 0.096 Uiso 1 1 calc R A 1 H17B H 0.5694 -0.0608 0.188 0.096 Uiso 1 1 calc R A 1 H17C H 0.4163 0.0099 0.1647 0.096 Uiso 1 1 calc R A 1 C18 C 0.93168(13) 0.07545(8) 0.17916(7) 0.0304(4) Uani 0.598(3) 1 d P A 1 C19 C 1.0580(4) 0.1257(2) 0.0880(2) 0.0577(8) Uani 1 1 d . A 1 H19A H 1.0139 0.121 0.0345 0.086 Uiso 1 1 calc R A 1 H19B H 1.1567 0.0829 0.0879 0.086 Uiso 1 1 calc R A 1 H19C H 1.0775 0.2028 0.088 0.086 Uiso 1 1 calc R A 1 C20 C 1.0129(3) 0.0845(3) 0.2666(2) 0.0660(9) Uani 1 1 d . A 1 H20A H 0.9415 0.0557 0.3217 0.099 Uiso 1 1 calc R A 1 H20B H 1.0338 0.1616 0.2653 0.099 Uiso 1 1 calc R A 1 H20C H 1.1116 0.0415 0.2647 0.099 Uiso 1 1 calc R A 1 C21 C 0.9201(5) -0.0592(3) 0.1791(2) 0.0724(10) Uani 1 1 d . A 1 H21A H 0.8734 -0.0686 0.1276 0.109 Uiso 1 1 calc R A 1 H21B H 0.8549 -0.0944 0.2345 0.109 Uiso 1 1 calc R A 1 H21C H 1.0255 -0.0932 0.1751 0.109 Uiso 1 1 calc R A 1 C3X C 0.62745(10) 0.11787(7) 0.13531(6) 0.0294(3) Uani 0.402(3) 1 d P A 2 Si18 Si 0.93168(13) 0.07545(8) 0.17916(7) 0.0304(4) Uani 0.402(3) 1 d P 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 Si1 0.0293(3) 0.0436(4) 0.0259(3) -0.0052(3) 0.0009(2) -0.0043(3) Si2 0.0301(3) 0.0308(3) 0.0351(3) -0.0076(3) -0.0031(3) -0.0050(2) Si3 0.0364(5) 0.0267(5) 0.0267(5) -0.0087(3) -0.0053(3) -0.0004(3) Na1 0.0442(5) 0.0448(5) 0.0267(5) -0.0101(4) -0.0012(4) -0.0016(4) Na2 0.0411(5) 0.0473(6) 0.0337(5) 0.0037(4) -0.0003(4) -0.0044(4) Na3 0.0423(5) 0.0246(4) 0.0377(5) -0.0069(4) -0.0046(4) -0.0027(4) N1 0.0298(9) 0.0399(10) 0.0218(9) -0.0040(8) -0.0034(7) -0.0018(8) N2 0.0307(9) 0.0228(8) 0.0303(9) -0.0029(7) -0.0022(7) -0.0025(7) N3 0.0420(10) 0.0255(9) 0.0263(9) -0.0087(7) -0.0040(8) -0.0016(8) C1 0.0331(13) 0.084(2) 0.0377(14) -0.0068(14) -0.0064(11) -0.0063(13) C2 0.0420(15) 0.0618(18) 0.0658(19) -0.0196(15) 0.0026(13) 0.0047(13) C3 0.0466(15) 0.0597(17) 0.0424(15) -0.0014(13) 0.0033(12) -0.0146(13) C4 0.0291(11) 0.0386(12) 0.0209(10) -0.0052(9) -0.0082(8) 0.0003(9) C5 0.0391(16) 0.120(3) 0.0575(19) 0.0067(19) -0.0179(14) -0.0219(17) C6 0.102(3) 0.071(2) 0.073(2) -0.0138(18) -0.053(2) 0.026(2) C7 0.0580(18) 0.105(3) 0.0461(17) -0.0295(17) -0.0138(14) -0.0102(18) C8 0.0402(14) 0.0689(19) 0.0643(18) -0.0334(15) -0.0100(13) -0.0037(13) C9 0.0282(12) 0.0468(14) 0.0563(16) -0.0085(12) -0.0077(11) 0.0009(10) C10 0.0495(16) 0.0466(15) 0.0568(17) -0.0026(13) -0.0025(13) -0.0122(12) C11 0.0187(9) 0.0128(8) 0.0253(9) -0.0034(7) -0.0050(7) 0.0025(7) C12 0.0316(13) 0.0511(16) 0.0689(19) -0.0096(14) -0.0086(12) 0.0067(11) C13 0.0538(17) 0.0354(14) 0.084(2) -0.0118(14) -0.0153(15) 0.0030(12) C14 0.0640(18) 0.0569(17) 0.0486(16) -0.0028(13) -0.0235(14) 0.0145(14) C15 0.072(2) 0.069(2) 0.098(3) -0.034(2) 0.021(2) -0.0107(18) C16 0.0582(18) 0.0660(19) 0.0509(17) 0.0008(14) -0.0277(14) -0.0086(14) C17 0.079(2) 0.0546(18) 0.0569(18) -0.0074(14) -0.0179(16) 0.0160(16) C18 0.0364(6) 0.0239(6) 0.0299(6) -0.0066(4) -0.0019(4) 0.0030(4) C19 0.076(2) 0.0489(16) 0.0518(17) -0.0174(13) -0.0170(15) 0.0165(15) C20 0.0412(15) 0.071(2) 0.067(2) 0.0184(16) 0.0005(14) 0.0167(14) C21 0.084(2) 0.066(2) 0.066(2) -0.0267(17) 0.0148(18) -0.0259(18) C3X 0.0364(5) 0.0267(5) 0.0267(5) -0.0087(3) -0.0053(3) -0.0004(3) Si18 0.0364(6) 0.0239(6) 0.0299(6) -0.0066(4) -0.0019(4) 0.0030(4) #----------------------------------------------------------------------------# # 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 Si1 N1 1.6777(19) . ? Si1 C1 1.869(3) . ? Si1 C3 1.885(3) . ? Si1 C2 1.889(3) . ? Si2 N2 1.6744(18) . ? Si2 C9 1.860(3) . ? Si2 C8 1.865(3) . ? Si2 C10 1.877(3) . ? Si3 N3 1.623(2) . ? Si3 C17 1.736(4) . ? Si3 C15 1.738(4) . ? Si3 C16 1.752(3) . ? Na1 N3 2.363(2) . ? Na1 N1 2.406(2) . ? Na2 N2 2.373(2) . ? Na2 N1 2.382(2) . ? Na3 N3 2.3753(19) . ? Na3 N2 2.3861(19) . ? N1 C4 1.475(3) . ? N2 C11 1.474(2) . ? N3 C18 1.566(2) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 C7 1.535(4) . ? C4 C6 1.540(4) . ? C4 C5 1.545(4) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C13 1.549(3) . ? C11 C14 1.566(3) . ? C11 C12 1.570(3) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C20 1.650(4) . ? C18 C19 1.666(3) . ? C18 C21 1.679(3) . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? 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 N1 Si1 C1 107.65(10) . . ? N1 Si1 C3 117.64(12) . . ? C1 Si1 C3 103.44(13) . . ? N1 Si1 C2 116.17(12) . . ? C1 Si1 C2 105.35(14) . . ? C3 Si1 C2 105.23(14) . . ? N2 Si2 C9 107.10(10) . . ? N2 Si2 C8 116.15(11) . . ? C9 Si2 C8 104.85(13) . . ? N2 Si2 C10 117.82(11) . . ? C9 Si2 C10 103.97(13) . . ? C8 Si2 C10 105.57(14) . . ? N3 Si3 C17 114.13(13) . . ? N3 Si3 C15 116.64(16) . . ? C17 Si3 C15 107.37(17) . . ? N3 Si3 C16 106.98(12) . . ? C17 Si3 C16 105.39(15) . . ? C15 Si3 C16 105.40(18) . . ? N3 Na1 N1 142.39(8) . . ? N2 Na2 N1 144.92(8) . . ? N3 Na3 N2 139.96(7) . . ? C4 N1 Si1 122.85(14) . . ? C4 N1 Na2 106.71(13) . . ? Si1 N1 Na2 110.41(9) . . ? C4 N1 Na1 114.09(13) . . ? Si1 N1 Na1 104.00(9) . . ? Na2 N1 Na1 95.40(7) . . ? C11 N2 Si2 123.32(13) . . ? C11 N2 Na2 106.36(12) . . ? Si2 N2 Na2 108.31(9) . . ? C11 N2 Na3 114.09(12) . . ? Si2 N2 Na3 104.02(9) . . ? Na2 N2 Na3 97.69(7) . . ? C18 N3 Si3 124.86(12) . . ? C18 N3 Na1 104.22(10) . . ? Si3 N3 Na1 112.67(10) . . ? C18 N3 Na3 110.12(10) . . ? Si3 N3 Na3 102.59(9) . . ? Na1 N3 Na3 99.63(7) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C7 114.9(2) . . ? N1 C4 C6 110.4(2) . . ? C7 C4 C6 107.4(2) . . ? N1 C4 C5 109.36(19) . . ? C7 C4 C5 105.5(2) . . ? C6 C4 C5 109.0(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C13 115.63(18) . . ? N2 C11 C14 111.35(17) . . ? C13 C11 C14 107.2(2) . . ? N2 C11 C12 109.50(16) . . ? C13 C11 C12 106.66(19) . . ? C14 C11 C12 106.0(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si3 C16 H16A 109.5 . . ? Si3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C20 109.12(14) . . ? N3 C18 C19 113.15(14) . . ? C20 C18 C19 107.16(16) . . ? N3 C18 C21 114.28(17) . . ? C20 C18 C21 106.58(19) . . ? C19 C18 C21 106.12(16) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? #===END data_(4a)-apr2900 _database_code_depnum_ccdc_archive 'CCDC 271694' _audit_creation_date 2000-04-28T16:18:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ((NaC(Ph)(adamantane))6).2(C6H6) _chemical_formula_moiety 'C102 H120 N6 Na6, 2(C6 H6)' _chemical_formula_sum 'C114 H132 N6 Na6' _chemical_formula_weight 1724.2 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P-31c _symmetry_space_group_name_Hall '-P 3 2c' _symmetry_Int_Tables_number 163 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-y, -x, -z+1/2' '-x+y, -x, z' 'x, x-y, -z+1/2' '-x+y, y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'y, x, z-1/2' 'x-y, x, -z' '-x, -x+y, z-1/2' 'x-y, -y, z-1/2' _cell_length_a 15.9031(2) _cell_length_b 15.9031(2) _cell_length_c 23.5014(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 5147.40(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 39596 _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 yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.086 _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 83203 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 22.99 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 2390 _reflns_number_gt 2049 _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 ; The diffraction was weak and did not extend to higher angle. A final difference map showed low electron density which may be another unresolved molecule of benzene solvate disordered about a 3-fold axis. 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^)+(0.1415P)^2^+8.2531P] 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 2390 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2604 _refine_ls_wR_factor_gt 0.2514 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.611 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.084 #----------------------------------------------------------------------------# # 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' 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 0.52120(11) 0.32832(10) 0.29484(6) 0.0324(5) Uani 1 1 d . . . N N 0.6643(2) 0.4853(2) 0.30587(13) 0.0308(8) Uani 1 1 d . . . C1 C 0.6431(3) 0.5328(3) 0.33974(15) 0.0283(9) Uani 1 1 d . . . C2 C 0.5419(3) 0.4834(3) 0.36678(16) 0.0329(10) Uani 1 1 d . . . C3 C 0.5242(3) 0.4299(3) 0.41644(19) 0.0444(11) Uani 1 1 d . . . H3 H 0.5769 0.4305 0.4359 0.053 Uiso 1 1 calc R . . C4 C 0.4306(4) 0.3754(4) 0.4383(2) 0.0550(13) Uani 1 1 d . . . H4 H 0.4203 0.3397 0.4725 0.066 Uiso 1 1 calc R . . C5 C 0.3543(4) 0.3728(3) 0.4113(2) 0.0588(14) Uani 1 1 d . . . H5 H 0.2908 0.3359 0.4266 0.071 Uiso 1 1 calc R . . C6 C 0.3695(3) 0.4244(4) 0.3610(3) 0.0625(15) Uani 1 1 d . . . H6 H 0.316 0.4219 0.3414 0.075 Uiso 1 1 calc R . . C7 C 0.4628(3) 0.4797(3) 0.3395(2) 0.0455(11) Uani 1 1 d . . . H7 H 0.4727 0.5156 0.3054 0.055 Uiso 1 1 calc R . . C8 C 0.7106(3) 0.6405(3) 0.35725(16) 0.0303(9) Uani 1 1 d . . . C9 C 0.8149(3) 0.6757(3) 0.33821(18) 0.0337(10) Uani 1 1 d . . . H9A H 0.8161 0.667 0.2966 0.04 Uiso 1 1 calc R . . H9B H 0.839 0.636 0.3569 0.04 Uiso 1 1 calc R . . C10 C 0.8817(3) 0.7826(3) 0.3532(2) 0.0427(11) Uani 1 1 d . . . H10 H 0.9492 0.8034 0.3401 0.051 Uiso 1 1 calc R . . C11 C 0.8817(3) 0.7952(3) 0.4173(2) 0.0547(13) Uani 1 1 d . . . H11A H 0.925 0.8643 0.4274 0.066 Uiso 1 1 calc R . . H11B H 0.9063 0.7562 0.4363 0.066 Uiso 1 1 calc R . . C12 C 0.7788(4) 0.7622(4) 0.4371(2) 0.0589(14) Uani 1 1 d . . . H12 H 0.7784 0.7701 0.4793 0.071 Uiso 1 1 calc R . . C13 C 0.7117(4) 0.6559(3) 0.42137(18) 0.0495(12) Uani 1 1 d . . . H13A H 0.7338 0.6152 0.4409 0.059 Uiso 1 1 calc R . . H13B H 0.645 0.6352 0.4346 0.059 Uiso 1 1 calc R . . C14 C 0.6760(3) 0.7047(3) 0.3281(2) 0.0495(12) Uani 1 1 d . . . H14A H 0.6759 0.6967 0.2863 0.059 Uiso 1 1 calc R . . H14B H 0.6088 0.684 0.3402 0.059 Uiso 1 1 calc R . . C15 C 0.7431(4) 0.8121(3) 0.3437(3) 0.0627(15) Uani 1 1 d . . . H15 H 0.7193 0.8528 0.325 0.075 Uiso 1 1 calc R . . C16 C 0.7424(4) 0.8232(4) 0.4083(3) 0.0745(19) Uani 1 1 d . . . H16A H 0.7845 0.8923 0.4189 0.089 Uiso 1 1 calc R . . H16B H 0.6756 0.8023 0.4214 0.089 Uiso 1 1 calc R . . C17 C 0.8460(3) 0.8445(3) 0.3237(2) 0.0532(12) Uani 1 1 d . . . H17A H 0.8894 0.9139 0.3332 0.064 Uiso 1 1 calc R . . H17B H 0.8468 0.8369 0.2819 0.064 Uiso 1 1 calc R . . C18 C 0.2876(5) 0.5668(4) 0.4521(2) 0.0684(15) Uani 1 1 d . . . H18 H 0.2563 0.498 0.4521 0.082 Uiso 1 1 calc R . . C19 C 0.3880(5) 0.6218(5) 0.4521(2) 0.0703(16) Uani 1 1 d . . . H19 H 0.4256 0.5904 0.4521 0.084 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 Na 0.0342(9) 0.0257(8) 0.0343(9) 0.0026(6) 0.0049(6) 0.0126(7) N 0.0312(18) 0.0310(18) 0.0316(17) -0.0034(13) 0.0022(14) 0.0167(15) C1 0.026(2) 0.031(2) 0.0293(19) 0.0021(16) 0.0004(15) 0.0152(17) C2 0.030(2) 0.027(2) 0.040(2) -0.0076(17) 0.0054(17) 0.0130(17) C3 0.038(2) 0.043(3) 0.046(3) 0.002(2) 0.0089(19) 0.015(2) C4 0.052(3) 0.046(3) 0.057(3) 0.005(2) 0.023(2) 0.017(2) C5 0.038(3) 0.040(3) 0.090(4) -0.003(3) 0.027(3) 0.013(2) C6 0.028(2) 0.059(3) 0.098(4) -0.008(3) -0.004(3) 0.020(2) C7 0.033(2) 0.050(3) 0.051(3) -0.001(2) 0.0014(19) 0.019(2) C8 0.029(2) 0.029(2) 0.034(2) -0.0031(16) 0.0022(16) 0.0149(17) C9 0.028(2) 0.032(2) 0.040(2) -0.0051(17) 0.0006(16) 0.0145(18) C10 0.029(2) 0.034(2) 0.061(3) -0.008(2) 0.0042(19) 0.0130(19) C11 0.047(3) 0.038(3) 0.066(3) -0.021(2) -0.013(2) 0.012(2) C12 0.060(3) 0.045(3) 0.055(3) -0.023(2) 0.010(2) 0.014(2) C13 0.051(3) 0.040(3) 0.044(2) -0.012(2) 0.010(2) 0.012(2) C14 0.032(2) 0.033(2) 0.087(3) 0.000(2) -0.006(2) 0.018(2) C15 0.044(3) 0.030(2) 0.118(5) -0.001(3) -0.006(3) 0.021(2) C16 0.042(3) 0.039(3) 0.129(5) -0.032(3) 0.024(3) 0.011(2) C17 0.044(3) 0.031(2) 0.074(3) 0.003(2) 0.004(2) 0.011(2) C18 0.078(4) 0.058(3) 0.064(4) 0.002(3) -0.002(3) 0.030(3) C19 0.079(4) 0.079(4) 0.064(4) -0.004(3) -0.006(3) 0.048(4) #----------------------------------------------------------------------------# # 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 N 2.339(3) 2_655 ? Na N 2.375(3) 3_665 ? Na N 2.408(3) . ? N C1 1.253(5) . ? N Na 2.339(3) 4_665 ? N Na 2.375(3) 3_665 ? C1 C2 1.533(5) . ? C1 C8 1.555(5) . ? C2 C7 1.386(6) . ? C2 C3 1.387(6) . ? C3 C4 1.393(6) . ? C4 C5 1.352(8) . ? C5 C6 1.389(8) . ? C6 C7 1.389(7) . ? C8 C13 1.526(6) . ? C8 C9 1.528(5) . ? C8 C14 1.543(6) . ? C9 C10 1.528(6) . ? C10 C11 1.520(7) . ? C10 C17 1.526(6) . ? C11 C12 1.521(7) . ? C12 C16 1.514(9) . ? C12 C13 1.527(6) . ? C14 C15 1.539(6) . ? C15 C17 1.524(7) . ? C15 C16 1.530(9) . ? C18 C19 1.365(8) 4_565 ? C18 C19 1.385(8) . ? C19 C18 1.365(8) 2_665 ? 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 Na N 100.36(10) 2_655 3_665 ? N Na N 125.46(14) 2_655 . ? N Na N 95.63(11) 3_665 . ? C1 N Na 131.0(3) . 4_665 ? C1 N Na 133.9(3) . 3_665 ? Na N Na 79.47(10) 4_665 3_665 ? C1 N Na 107.1(2) . . ? Na N Na 112.16(14) 4_665 . ? Na N Na 83.63(11) 3_665 . ? N C1 C2 119.0(3) . . ? N C1 C8 125.9(3) . . ? C2 C1 C8 115.1(3) . . ? C7 C2 C3 117.5(4) . . ? C7 C2 C1 121.9(4) . . ? C3 C2 C1 120.1(4) . . ? C2 C3 C4 121.2(4) . . ? C5 C4 C3 120.6(5) . . ? C4 C5 C6 119.6(4) . . ? C5 C6 C7 119.9(5) . . ? C2 C7 C6 121.2(4) . . ? C13 C8 C9 107.9(3) . . ? C13 C8 C14 108.2(4) . . ? C9 C8 C14 108.0(3) . . ? C13 C8 C1 112.6(3) . . ? C9 C8 C1 110.6(3) . . ? C14 C8 C1 109.5(3) . . ? C8 C9 C10 111.4(3) . . ? C11 C10 C17 109.9(4) . . ? C11 C10 C9 109.2(4) . . ? C17 C10 C9 109.7(4) . . ? C10 C11 C12 109.3(4) . . ? C16 C12 C11 109.4(4) . . ? C16 C12 C13 108.8(4) . . ? C11 C12 C13 110.0(4) . . ? C8 C13 C12 111.3(4) . . ? C15 C14 C8 110.5(4) . . ? C17 C15 C16 109.6(4) . . ? C17 C15 C14 109.5(4) . . ? C16 C15 C14 108.9(4) . . ? C12 C16 C15 110.1(4) . . ? C15 C17 C10 109.0(4) . . ? C19 C18 C19 119.8(6) 4_565 . ? C18 C19 C18 120.2(6) 2_665 . ? #===END data_(3b)-apr405 _database_code_depnum_ccdc_archive 'CCDC 271695' _audit_creation_date 2005-04-04T11:26:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H81 N6 Na3 Si3' _chemical_formula_sum 'C36 H81 N6 Na3 Si3' _chemical_formula_weight 751.31 _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 11.1936(2) _cell_length_b 11.7449(2) _cell_length_c 39.5782(5) _cell_angle_alpha 90 _cell_angle_beta 92.796(1) _cell_angle_gamma 90 _cell_volume 5197.06(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 301422 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 25.682 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 0.96 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.143 _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_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.94798E-2 _diffrn_orient_matrix_ub_12 0.800574E-1 _diffrn_orient_matrix_ub_13 0.80435E-2 _diffrn_orient_matrix_ub_21 0.3442E-2 _diffrn_orient_matrix_ub_22 0.280112E-1 _diffrn_orient_matrix_ub_23 -0.237926E-1 _diffrn_orient_matrix_ub_31 -0.888728E-1 _diffrn_orient_matrix_ub_32 -0.74546E-2 _diffrn_orient_matrix_ub_33 -0.30213E-2 _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 0.1072 _diffrn_reflns_av_unetI/netI 0.0534 _diffrn_reflns_number 56295 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 25.78 _diffrn_reflns_theta_full 25.78 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _reflns_number_total 9802 _reflns_number_gt 7530 _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-86 (Sheldrick, 1986)' _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 ; For all three N(tBu)(SiMe3) ligands there is unresolved end-for-end disorder with partial occupancies refined for C1/Si1 etc. All dimensions for these ligands are therefore misleading . 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^)+(0.1164P)^2^+4.0523P] 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 9802 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0895 _refine_ls_wR_factor_ref 0.2552 _refine_ls_wR_factor_gt 0.2381 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.507 _refine_diff_density_min -0.293 _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' 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 Na1 Na 0.14257(13) 0.38109(13) 0.17248(4) 0.0700(4) Uani 1 1 d . . . Na2 Na 0.15736(11) 0.23384(10) 0.09259(3) 0.0540(3) Uani 1 1 d . . . Na3 Na 0.36372(11) 0.47379(11) 0.11206(3) 0.0574(3) Uani 1 1 d . . . N1 N 0.0408(3) 0.2290(2) 0.14163(8) 0.0649(8) Uani 1 1 d . . . N2 N 0.3064(2) 0.3464(2) 0.06682(6) 0.0521(6) Uani 1 1 d . . . N3 N 0.3079(3) 0.5109(3) 0.16826(7) 0.0664(8) Uani 1 1 d . . . N4 N 0.0483(4) 0.4185(5) 0.22537(11) 0.1147(15) Uani 1 1 d . . . N5 N 0.1217(3) 0.0749(3) 0.05325(9) 0.0793(9) Uani 1 1 d . . . N6 N 0.5251(4) 0.6029(3) 0.09824(10) 0.0997(13) Uani 1 1 d . . . C2 C -0.0155(6) 0.1100(6) 0.19699(16) 0.142(3) Uani 1 1 d . . . H2A H -0.0152 0.1833 0.2088 0.213 Uiso 1 1 calc R A 1 H2B H 0.0224 0.0521 0.2118 0.213 Uiso 1 1 calc R A 1 H2C H -0.0981 0.0876 0.191 0.213 Uiso 1 1 calc R A 1 C3 C 0.2077(4) 0.1262(4) 0.17918(13) 0.0936(14) Uani 1 1 d . . . H3A H 0.2206 0.1967 0.1921 0.14 Uiso 1 1 calc R B 1 H3B H 0.2627 0.1236 0.1607 0.14 Uiso 1 1 calc R B 1 H3C H 0.2224 0.0606 0.1941 0.14 Uiso 1 1 calc R B 1 C4 C 0.0570(7) 0.0023(5) 0.14249(19) 0.148(3) Uani 1 1 d . . . H4A H 0.1017 0.0096 0.1219 0.221 Uiso 1 1 calc R C 1 H4B H -0.026 -0.0187 0.1364 0.221 Uiso 1 1 calc R C 1 H4C H 0.0938 -0.0567 0.1571 0.221 Uiso 1 1 calc R C 1 C5 C -0.1889(6) 0.1515(6) 0.11706(19) 0.145(3) Uani 1 1 d . . . H5A H -0.1491 0.1021 0.1011 0.218 Uiso 1 1 calc R D 1 H5B H -0.2603 0.1853 0.1058 0.218 Uiso 1 1 calc R D 1 H5C H -0.2122 0.1065 0.1365 0.218 Uiso 1 1 calc R D 1 C6 C -0.1696(5) 0.3452(7) 0.15855(19) 0.149(3) Uani 1 1 d . . . H6A H -0.1178 0.4077 0.1667 0.223 Uiso 1 1 calc R E 1 H6B H -0.1935 0.2995 0.1778 0.223 Uiso 1 1 calc R E 1 H6C H -0.2411 0.3765 0.1466 0.223 Uiso 1 1 calc R E 1 C7 C -0.0881(4) 0.3507(4) 0.09382(13) 0.0924(14) Uani 1 1 d . . . H7A H -0.0347 0.4153 0.0988 0.139 Uiso 1 1 calc R F 1 H7B H -0.1689 0.3788 0.088 0.139 Uiso 1 1 calc R F 1 H7C H -0.0588 0.3075 0.0747 0.139 Uiso 1 1 calc R F 1 C9 C 0.1793(4) 0.5219(4) 0.05831(12) 0.0851(12) Uani 1 1 d . . . H9A H 0.1221 0.4884 0.0734 0.128 Uiso 1 1 calc R G 1 H9B H 0.1361 0.5681 0.0411 0.128 Uiso 1 1 calc R G 1 H9C H 0.2359 0.5701 0.0714 0.128 Uiso 1 1 calc R G 1 C10 C 0.1545(4) 0.3598(4) 0.01635(11) 0.0913(13) Uani 1 1 d . . . H10A H 0.0974 0.3199 0.0301 0.137 Uiso 1 1 calc R H 1 H10B H 0.1942 0.3049 0.002 0.137 Uiso 1 1 calc R H 1 H10C H 0.1118 0.4163 0.0021 0.137 Uiso 1 1 calc R H 1 C11 C 0.3401(4) 0.4861(5) 0.01731(12) 0.0999(15) Uani 1 1 d . . . H11A H 0.4003 0.5261 0.0317 0.15 Uiso 1 1 calc R I 1 H11B H 0.2958 0.5413 0.003 0.15 Uiso 1 1 calc R I 1 H11C H 0.3798 0.431 0.003 0.15 Uiso 1 1 calc R I 1 C12 C 0.4257(4) 0.1530(3) 0.09332(12) 0.0811(11) Uani 1 1 d . . . H12A H 0.3486 0.1134 0.0935 0.122 Uiso 1 1 calc R J 1 H12B H 0.4426 0.1894 0.1153 0.122 Uiso 1 1 calc R J 1 H12C H 0.489 0.098 0.089 0.122 Uiso 1 1 calc R J 1 C13 C 0.5674(4) 0.3285(4) 0.06269(12) 0.0835(12) Uani 1 1 d . . . H13A H 0.5712 0.3881 0.0454 0.125 Uiso 1 1 calc R K 1 H13B H 0.6287 0.2708 0.0589 0.125 Uiso 1 1 calc R K 1 H13C H 0.5817 0.3622 0.0852 0.125 Uiso 1 1 calc R K 1 C14 C 0.4155(5) 0.1822(5) 0.01959(14) 0.1083(17) Uani 1 1 d . . . H14A H 0.3381 0.144 0.0162 0.162 Uiso 1 1 calc R L 1 H14B H 0.4797 0.1254 0.0203 0.162 Uiso 1 1 calc R L 1 H14C H 0.4267 0.2352 0.0009 0.162 Uiso 1 1 calc R L 1 C16 C 0.3771(5) 0.4265(5) 0.22620(12) 0.1055(16) Uani 1 1 d . . . H16A H 0.3129 0.3706 0.2226 0.158 Uiso 1 1 calc R M 1 H16B H 0.3506 0.4873 0.2411 0.158 Uiso 1 1 calc R M 1 H16C H 0.4478 0.3891 0.2367 0.158 Uiso 1 1 calc R M 1 C17 C 0.4791(4) 0.3682(4) 0.17232(11) 0.0846(12) Uani 1 1 d . . . H17A H 0.4208 0.3075 0.1673 0.127 Uiso 1 1 calc R N 1 H17B H 0.5432 0.3391 0.1877 0.127 Uiso 1 1 calc R N 1 H17C H 0.513 0.3938 0.1513 0.127 Uiso 1 1 calc R N 1 C18 C 0.5129(4) 0.5682(6) 0.19729(14) 0.1112(18) Uani 1 1 d . . . H18A H 0.534 0.6018 0.1757 0.167 Uiso 1 1 calc R O 1 H18B H 0.5831 0.53 0.2078 0.167 Uiso 1 1 calc R O 1 H18C H 0.4861 0.6282 0.2123 0.167 Uiso 1 1 calc R O 1 C19 C 0.3239(6) 0.7509(4) 0.14873(17) 0.1199(19) Uani 1 1 d . . . H19A H 0.3398 0.7253 0.1258 0.18 Uiso 1 1 calc R P 1 H19B H 0.3996 0.7701 0.1609 0.18 Uiso 1 1 calc R P 1 H19C H 0.2722 0.8182 0.1475 0.18 Uiso 1 1 calc R P 1 C20 C 0.2263(6) 0.6953(6) 0.21286(17) 0.142(3) Uani 1 1 d . . . H20A H 0.1875 0.6378 0.2265 0.213 Uiso 1 1 calc R Q 1 H20B H 0.1752 0.7629 0.2107 0.213 Uiso 1 1 calc R Q 1 H20C H 0.3035 0.7163 0.2239 0.213 Uiso 1 1 calc R Q 1 C21 C 0.0978(4) 0.6309(4) 0.15073(16) 0.1057(17) Uani 1 1 d . . . H21A H 0.0518 0.5712 0.1615 0.159 Uiso 1 1 calc R R 1 H21B H 0.1032 0.6135 0.1266 0.159 Uiso 1 1 calc R R 1 H21C H 0.0579 0.7044 0.1533 0.159 Uiso 1 1 calc R R 1 C22 C -0.0168(4) 0.4534(4) 0.24380(11) 0.0818(12) Uani 1 1 d . . . C23 C -0.1026(3) 0.4990(4) 0.26739(10) 0.0731(10) Uani 1 1 d . . . C24 C -0.1518(6) 0.6107(5) 0.25330(19) 0.131(2) Uani 1 1 d . . . H24A H -0.209 0.6423 0.2688 0.196 Uiso 1 1 calc R . . H24B H -0.1923 0.5973 0.2311 0.196 Uiso 1 1 calc R . . H24C H -0.086 0.6646 0.2509 0.196 Uiso 1 1 calc R . . C25 C -0.0372(5) 0.5172(6) 0.30111(14) 0.124(2) Uani 1 1 d . . . H25A H -0.0924 0.5485 0.3172 0.185 Uiso 1 1 calc R . . H25B H 0.029 0.5705 0.2985 0.185 Uiso 1 1 calc R . . H25C H -0.0055 0.4443 0.3096 0.185 Uiso 1 1 calc R . . C26 C -0.2046(4) 0.4126(5) 0.26965(15) 0.1108(17) Uani 1 1 d . . . H26A H -0.2635 0.4413 0.2851 0.166 Uiso 1 1 calc R . . H26B H -0.1723 0.34 0.2782 0.166 Uiso 1 1 calc R . . H26C H -0.2432 0.4012 0.2471 0.166 Uiso 1 1 calc R . . C27 C 0.1499(3) -0.0048(3) 0.03975(9) 0.0619(8) Uani 1 1 d . . . C28 C 0.1858(4) -0.1093(3) 0.02182(11) 0.0715(10) Uani 1 1 d . . . C29 C 0.0825(4) -0.1938(4) 0.02313(17) 0.1096(18) Uani 1 1 d . . . H29A H 0.103 -0.2637 0.0112 0.164 Uiso 1 1 calc R . . H29B H 0.0103 -0.1602 0.0123 0.164 Uiso 1 1 calc R . . H29C H 0.068 -0.2118 0.0468 0.164 Uiso 1 1 calc R . . C30 C 0.3010(4) -0.1543(4) 0.03958(14) 0.0970(14) Uani 1 1 d . . . H30A H 0.3268 -0.2234 0.0281 0.145 Uiso 1 1 calc R . . H30B H 0.2862 -0.172 0.0632 0.145 Uiso 1 1 calc R . . H30C H 0.3637 -0.0963 0.0388 0.145 Uiso 1 1 calc R . . C31 C 0.2079(5) -0.0766(5) -0.01504(12) 0.1041(16) Uani 1 1 d . . . H31A H 0.2311 -0.1445 -0.0275 0.156 Uiso 1 1 calc R . . H31B H 0.2722 -0.02 -0.0153 0.156 Uiso 1 1 calc R . . H31C H 0.1346 -0.0445 -0.0257 0.156 Uiso 1 1 calc R . . C32 C 0.6029(4) 0.6657(3) 0.09988(10) 0.0723(10) Uani 1 1 d . . . C33 C 0.7005(4) 0.7466(3) 0.10257(10) 0.0752(11) Uani 1 1 d . . . C34 C 0.7430(6) 0.7592(6) 0.13891(14) 0.137(3) Uani 1 1 d . . . H34A H 0.8081 0.815 0.1406 0.205 Uiso 1 1 calc R . . H34B H 0.7719 0.6856 0.1476 0.205 Uiso 1 1 calc R . . H34C H 0.6767 0.7853 0.1522 0.205 Uiso 1 1 calc R . . C35 C 0.6519(8) 0.8584(5) 0.0889(3) 0.206(5) Uani 1 1 d . . . H35A H 0.7155 0.9159 0.0901 0.309 Uiso 1 1 calc R . . H35B H 0.5858 0.8834 0.1024 0.309 Uiso 1 1 calc R . . H35C H 0.6231 0.8484 0.0653 0.309 Uiso 1 1 calc R . . C36 C 0.8034(6) 0.7058(9) 0.0824(2) 0.189(4) Uani 1 1 d . . . H36A H 0.8682 0.762 0.084 0.283 Uiso 1 1 calc R . . H36B H 0.7761 0.6963 0.0587 0.283 Uiso 1 1 calc R . . H36C H 0.8326 0.6328 0.0915 0.283 Uiso 1 1 calc R . . C1 C 0.05929(18) 0.12192(17) 0.16239(5) 0.0769(8) Uani 0.588(5) 1 d P S 1 C8 C 0.2511(2) 0.4219(2) 0.04022(6) 0.0678(10) Uani 0.795(5) 1 d P T 1 C15 C 0.4099(2) 0.4795(3) 0.19086(6) 0.0830(11) Uani 0.759(6) 1 d P U 1 Si1 Si -0.09166(11) 0.25884(12) 0.13077(4) 0.0598(5) Uani 0.588(5) 1 d P S 1 Si2 Si 0.41960(10) 0.26194(10) 0.05996(3) 0.0571(4) Uani 0.795(5) 1 d P T 1 Si3 Si 0.25001(12) 0.63761(11) 0.17105(4) 0.0718(5) Uani 0.759(6) 1 d P U 1 Si1A Si 0.05929(18) 0.12192(17) 0.16239(5) 0.0769(8) Uani 0.412(5) 1 d P S 2 Si2A Si 0.2511(2) 0.4219(2) 0.04022(6) 0.0678(10) Uani 0.205(5) 1 d P T 2 Si3A Si 0.4099(2) 0.4795(3) 0.19086(6) 0.0830(11) Uani 0.241(6) 1 d P U 2 C1A C -0.09166(11) 0.25884(12) 0.13077(4) 0.0598(5) Uani 0.412(5) 1 d P S 2 C8A C 0.41960(10) 0.26194(10) 0.05996(3) 0.0571(4) Uani 0.205(5) 1 d P T 2 C15A C 0.25001(12) 0.63761(11) 0.17105(4) 0.0718(5) Uani 0.241(6) 1 d P U 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 Na1 0.0633(8) 0.0804(10) 0.0676(8) -0.0191(7) 0.0155(7) -0.0202(7) Na2 0.0554(7) 0.0484(7) 0.0595(7) -0.0078(5) 0.0156(6) -0.0109(5) Na3 0.0629(8) 0.0549(7) 0.0544(7) -0.0083(5) 0.0018(6) -0.0162(6) N1 0.0654(17) 0.0637(17) 0.0679(17) -0.0098(14) 0.0253(14) -0.0276(14) N2 0.0552(15) 0.0527(14) 0.0494(13) -0.0048(11) 0.0124(11) -0.0158(12) N3 0.0675(18) 0.0741(19) 0.0579(16) -0.0202(14) 0.0072(13) -0.0227(15) N4 0.103(3) 0.146(4) 0.099(3) -0.032(3) 0.043(3) -0.024(3) N5 0.072(2) 0.068(2) 0.099(2) -0.0260(18) 0.0138(18) -0.0132(16) N6 0.109(3) 0.093(3) 0.099(3) -0.025(2) 0.023(2) -0.049(2) C2 0.142(5) 0.165(6) 0.119(5) 0.075(4) 0.014(4) 0.016(5) C3 0.068(3) 0.099(3) 0.113(3) 0.042(3) -0.009(2) -0.003(2) C4 0.185(7) 0.090(4) 0.166(6) 0.047(4) -0.010(5) 0.022(4) C5 0.118(5) 0.138(5) 0.173(6) 0.031(5) -0.069(4) -0.015(4) C6 0.075(3) 0.202(7) 0.167(6) -0.024(6) -0.010(4) 0.034(4) C7 0.060(2) 0.089(3) 0.128(4) 0.040(3) -0.006(2) -0.009(2) C9 0.079(3) 0.067(2) 0.108(3) 0.024(2) -0.008(2) 0.002(2) C10 0.089(3) 0.116(4) 0.068(2) 0.010(2) -0.006(2) -0.021(3) C11 0.091(3) 0.122(4) 0.087(3) 0.034(3) 0.007(2) -0.017(3) C12 0.073(3) 0.059(2) 0.112(3) -0.003(2) 0.008(2) 0.0091(19) C13 0.073(3) 0.087(3) 0.091(3) -0.002(2) 0.008(2) -0.005(2) C14 0.090(3) 0.122(4) 0.115(4) -0.034(3) 0.026(3) -0.023(3) C16 0.104(4) 0.128(4) 0.083(3) 0.010(3) -0.014(3) -0.026(3) C17 0.070(3) 0.101(3) 0.082(3) 0.008(2) -0.005(2) 0.011(2) C18 0.079(3) 0.154(5) 0.098(3) 0.027(3) -0.018(3) -0.022(3) C19 0.142(5) 0.072(3) 0.147(5) 0.002(3) 0.024(4) 0.016(3) C20 0.154(6) 0.121(5) 0.154(6) -0.060(4) 0.044(5) -0.012(4) C21 0.076(3) 0.084(3) 0.157(5) -0.031(3) -0.002(3) 0.017(2) C22 0.077(3) 0.096(3) 0.074(2) -0.012(2) 0.018(2) -0.012(2) C23 0.057(2) 0.084(3) 0.080(2) -0.004(2) 0.0120(18) -0.0022(19) C24 0.112(4) 0.102(4) 0.179(6) 0.025(4) 0.010(4) 0.015(3) C25 0.104(4) 0.171(6) 0.096(4) -0.040(4) 0.002(3) 0.016(4) C26 0.077(3) 0.124(4) 0.135(4) -0.005(3) 0.039(3) -0.011(3) C27 0.065(2) 0.0468(18) 0.073(2) -0.0092(16) 0.0009(17) -0.0046(15) C28 0.072(2) 0.0468(18) 0.095(3) -0.0151(18) -0.008(2) 0.0064(17) C29 0.092(3) 0.054(2) 0.179(5) -0.022(3) -0.019(3) -0.006(2) C30 0.082(3) 0.080(3) 0.126(4) 0.005(3) -0.014(3) 0.015(2) C31 0.132(4) 0.098(3) 0.081(3) -0.026(3) -0.003(3) 0.027(3) C32 0.082(3) 0.065(2) 0.071(2) -0.0132(18) 0.0143(19) -0.018(2) C33 0.077(2) 0.074(2) 0.075(2) -0.0001(19) 0.0063(19) -0.031(2) C34 0.128(5) 0.185(7) 0.096(4) -0.020(4) 0.001(3) -0.080(5) C35 0.214(9) 0.084(4) 0.308(12) 0.064(6) -0.108(9) -0.069(5) C36 0.124(5) 0.277(11) 0.172(7) -0.072(7) 0.069(5) -0.067(6) C1 0.0703(13) 0.0742(13) 0.0867(14) 0.0321(10) 0.0097(10) -0.0159(9) C8 0.0692(17) 0.0838(18) 0.0500(13) 0.0114(11) -0.0008(10) -0.0230(13) C15 0.0797(18) 0.113(2) 0.0548(14) 0.0013(13) -0.0073(11) -0.0396(15) Si1 0.0410(8) 0.0683(9) 0.0705(9) -0.0013(6) 0.0054(6) -0.0140(6) Si2 0.0512(7) 0.0589(7) 0.0626(7) -0.0099(5) 0.0146(5) -0.0075(5) Si3 0.0711(9) 0.0633(8) 0.0819(9) -0.0267(6) 0.0117(6) -0.0076(6) Si1A 0.0703(13) 0.0742(13) 0.0867(14) 0.0321(10) 0.0097(10) -0.0159(9) Si2A 0.0692(17) 0.0838(18) 0.0500(13) 0.0114(11) -0.0008(10) -0.0230(13) Si3A 0.0797(18) 0.113(2) 0.0548(14) 0.0013(13) -0.0073(11) -0.0396(15) C1A 0.0410(8) 0.0683(9) 0.0705(9) -0.0013(6) 0.0054(6) -0.0140(6) C8A 0.0512(7) 0.0589(7) 0.0626(7) -0.0099(5) 0.0146(5) -0.0075(5) C15A 0.0711(9) 0.0633(8) 0.0819(9) -0.0267(6) 0.0117(6) -0.0076(6) #----------------------------------------------------------------------------# # 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 Na1 N3 2.410(3) . ? Na1 N1 2.417(3) . ? Na1 N4 2.430(4) . ? Na2 N1 2.391(3) . ? Na2 N2 2.395(3) . ? Na2 N5 2.452(3) . ? Na3 N3 2.380(3) . ? Na3 N2 2.397(3) . ? Na3 N6 2.441(4) . ? N1 C1 1.511(4) . ? N1 Si1 1.564(3) . ? N2 C8 1.488(4) . ? N2 Si2 1.642(3) . ? N3 C15 1.463(4) . ? N3 Si3 1.629(3) . ? N4 C22 1.133(5) . ? N5 C27 1.130(4) . ? N6 C32 1.141(5) . ? C2 C1 1.645(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C1 1.759(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C1 1.610(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 Si1 1.735(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 Si1 1.759(7) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 Si1 1.819(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C8 1.611(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C8 1.579(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C8 1.573(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Si2 1.838(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Si2 1.829(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Si2 1.850(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 C15 1.590(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C15 1.703(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C15 1.565(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 Si3 1.818(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 Si3 1.819(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 Si3 1.850(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.473(6) . ? C23 C25 1.506(7) . ? C23 C24 1.518(7) . ? C23 C26 1.533(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.483(5) . ? C28 C29 1.526(6) . ? C28 C30 1.532(6) . ? C28 C31 1.540(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.448(5) . ? C33 C34 1.500(7) . ? C33 C36 1.510(8) . ? C33 C35 1.511(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 N3 Na1 N1 140.99(11) . . ? N3 Na1 N4 108.22(14) . . ? N1 Na1 N4 110.79(14) . . ? N1 Na2 N2 141.04(10) . . ? N1 Na2 N5 114.77(11) . . ? N2 Na2 N5 104.18(11) . . ? N3 Na3 N2 137.72(10) . . ? N3 Na3 N6 109.06(12) . . ? N2 Na3 N6 113.22(12) . . ? C1 N1 Si1 116.03(18) . . ? C1 N1 Na2 113.31(18) . . ? Si1 N1 Na2 108.61(17) . . ? C1 N1 Na1 106.95(18) . . ? Si1 N1 Na1 112.98(17) . . ? Na2 N1 Na1 97.48(10) . . ? C8 N2 Si2 122.75(19) . . ? C8 N2 Na2 110.81(17) . . ? Si2 N2 Na2 107.22(13) . . ? C8 N2 Na3 104.10(17) . . ? Si2 N2 Na3 108.67(13) . . ? Na2 N2 Na3 101.12(10) . . ? C15 N3 Si3 119.4(2) . . ? C15 N3 Na3 107.00(19) . . ? Si3 N3 Na3 110.76(17) . . ? C15 N3 Na1 112.1(2) . . ? Si3 N3 Na1 105.30(15) . . ? Na3 N3 Na1 100.74(10) . . ? C22 N4 Na1 160.1(5) . . ? C27 N5 Na2 152.9(3) . . ? C32 N6 Na3 163.8(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 C23 179.2(5) . . ? C22 C23 C25 108.0(4) . . ? C22 C23 C24 108.5(4) . . ? C25 C23 C24 110.8(5) . . ? C22 C23 C26 107.9(4) . . ? C25 C23 C26 111.9(4) . . ? C24 C23 C26 109.6(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 C28 179.5(5) . . ? C27 C28 C29 107.4(3) . . ? C27 C28 C30 107.9(3) . . ? C29 C28 C30 112.5(4) . . ? C27 C28 C31 107.8(3) . . ? C29 C28 C31 110.6(4) . . ? C30 C28 C31 110.5(4) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N6 C32 C33 178.8(5) . . ? C32 C33 C34 109.8(4) . . ? C32 C33 C36 110.2(5) . . ? C34 C33 C36 108.9(5) . . ? C32 C33 C35 106.6(4) . . ? C34 C33 C35 110.4(5) . . ? C36 C33 C35 110.9(7) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N1 C1 C4 117.5(3) . . ? N1 C1 C2 117.5(3) . . ? C4 C1 C2 109.7(4) . . ? N1 C1 C3 106.5(2) . . ? C4 C1 C3 101.7(3) . . ? C2 C1 C3 101.4(3) . . ? N2 C8 C11 116.1(3) . . ? N2 C8 C10 113.4(3) . . ? C11 C8 C10 108.1(3) . . ? N2 C8 C9 108.6(2) . . ? C11 C8 C9 104.5(3) . . ? C10 C8 C9 105.1(3) . . ? N3 C15 C18 118.5(3) . . ? N3 C15 C16 115.5(3) . . ? C18 C15 C16 108.5(3) . . ? N3 C15 C17 106.7(2) . . ? C18 C15 C17 103.6(3) . . ? C16 C15 C17 102.0(3) . . ? N1 Si1 C5 119.7(3) . . ? N1 Si1 C6 116.8(2) . . ? C5 Si1 C6 107.0(4) . . ? N1 Si1 C7 107.24(18) . . ? C5 Si1 C7 102.6(3) . . ? C6 Si1 C7 101.0(3) . . ? N2 Si2 C13 115.81(18) . . ? N2 Si2 C12 107.68(17) . . ? C13 Si2 C12 104.7(2) . . ? N2 Si2 C14 117.5(2) . . ? C13 Si2 C14 104.6(2) . . ? C12 Si2 C14 105.5(2) . . ? N3 Si3 C19 116.3(2) . . ? N3 Si3 C20 118.6(3) . . ? C19 Si3 C20 105.0(3) . . ? N3 Si3 C21 107.02(19) . . ? C19 Si3 C21 104.5(3) . . ? C20 Si3 C21 103.9(3) . . ? #===END data_(5a)-jul2400 _database_code_depnum_ccdc_archive 'CCDC 271696' _audit_creation_date 2000-07-19T14:45:43-00:00 _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_name_common (((AdCN)Li(ME3SiNSiMe3))2) _chemical_formula_moiety 'C34 H66 Li2 N4 Si4' _chemical_formula_sum 'C34 H66 Li2 N4 Si4' _chemical_formula_weight 657.15 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7259(3) _cell_length_b 16.8180(5) _cell_length_c 20.6515(6) _cell_angle_alpha 105.254(2) _cell_angle_beta 98.168(2) _cell_angle_gamma 100.003(2) _cell_volume 4116.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17343 _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 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.06 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.171 _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 35502 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_unetI/netI 0.0641 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 25.09 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _reflns_number_total 14367 _reflns_number_gt 10072 _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 ; In one of the two independent molecules, one adamantyl group (on C25b) is disordered equally over two orientation related by a 60 degree rotation. The atoms of this group were resolved but left isotropic. 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^)+(0.0497P)^2^+2.2604P] 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 14367 _refine_ls_number_parameters 779 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.13 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.382 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.048 #----------------------------------------------------------------------------# # 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' Li Li -0.0003 0.0001 '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' 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 Li1 Li -0.1360(3) 0.6304(3) 0.3770(2) 0.0315(10) Uani 1 1 d . A 1 Li2 Li -0.3269(3) 0.6437(3) 0.3679(2) 0.0329(10) Uani 1 1 d . A 1 N1 N -0.19034(16) 0.73831(12) 0.40574(10) 0.0261(4) Uani 1 1 d . A 1 N2 N -0.27397(16) 0.53612(12) 0.33607(10) 0.0252(4) Uani 1 1 d . A 1 N3 N 0.00644(17) 0.58514(14) 0.37626(11) 0.0365(5) Uani 1 1 d . A 1 N4 N -0.47099(18) 0.67832(15) 0.38148(12) 0.0397(6) Uani 1 1 d . A 1 Si1 Si -0.20261(6) 0.80459(5) 0.35665(4) 0.03158(18) Uani 1 1 d . A 1 Si2 Si -0.14843(5) 0.77592(4) 0.49205(3) 0.02776(17) Uani 1 1 d . A 1 Si3 Si -0.27400(6) 0.50091(4) 0.25127(3) 0.02918(17) Uani 1 1 d . A 1 Si4 Si -0.30927(5) 0.47209(4) 0.38466(3) 0.02737(16) Uani 1 1 d . A 1 C1 C -0.3073(3) 0.7518(2) 0.27519(14) 0.0525(8) Uani 1 1 d . A 1 H1A H -0.3773 0.7313 0.2865 0.079 Uiso 1 1 calc R A 1 H1B H -0.2836 0.704 0.2472 0.079 Uiso 1 1 calc R A 1 H1C H -0.3155 0.7925 0.2496 0.079 Uiso 1 1 calc R A 1 C2 C -0.2506(3) 0.90186(19) 0.39774(15) 0.0501(8) Uani 1 1 d . A 1 H2A H -0.3186 0.8854 0.4127 0.075 Uiso 1 1 calc R A 1 H2B H -0.2629 0.9332 0.3646 0.075 Uiso 1 1 calc R A 1 H2C H -0.1951 0.9377 0.4374 0.075 Uiso 1 1 calc R A 1 C3 C -0.0728(3) 0.8414(2) 0.32948(18) 0.0588(9) Uani 1 1 d . A 1 H3A H -0.0449 0.7923 0.3077 0.088 Uiso 1 1 calc R A 1 H3B H -0.0189 0.8778 0.3697 0.088 Uiso 1 1 calc R A 1 H3C H -0.0868 0.8731 0.2968 0.088 Uiso 1 1 calc R A 1 C4 C -0.0451(2) 0.87900(18) 0.52471(15) 0.0447(7) Uani 1 1 d . A 1 H4A H -0.0747 0.9225 0.5094 0.067 Uiso 1 1 calc R A 1 H4B H 0.0213 0.8723 0.5069 0.067 Uiso 1 1 calc R A 1 H4C H -0.0279 0.896 0.5749 0.067 Uiso 1 1 calc R A 1 C5 C -0.2632(2) 0.79125(19) 0.53906(13) 0.0420(7) Uani 1 1 d . A 1 H5A H -0.3008 0.8314 0.5241 0.063 Uiso 1 1 calc R A 1 H5B H -0.2339 0.8134 0.5884 0.063 Uiso 1 1 calc R A 1 H5C H -0.3146 0.737 0.5292 0.063 Uiso 1 1 calc R A 1 C6 C -0.0828(2) 0.69813(17) 0.52467(13) 0.0357(6) Uani 1 1 d . A 1 H6A H -0.0219 0.6876 0.502 0.054 Uiso 1 1 calc R A 1 H6B H -0.1365 0.6449 0.5148 0.054 Uiso 1 1 calc R A 1 H6C H -0.056 0.7213 0.5742 0.054 Uiso 1 1 calc R A 1 C7 C -0.4042(2) 0.5016(2) 0.19630(14) 0.0450(7) Uani 1 1 d . A 1 H7A H -0.4204 0.5577 0.2103 0.068 Uiso 1 1 calc R A 1 H7B H -0.4636 0.4596 0.2016 0.068 Uiso 1 1 calc R A 1 H7C H -0.3967 0.4877 0.1483 0.068 Uiso 1 1 calc R A 1 C8 C -0.1618(2) 0.5688(2) 0.22634(14) 0.0441(7) Uani 1 1 d . A 1 H8A H -0.0915 0.5704 0.2537 0.066 Uiso 1 1 calc R A 1 H8B H -0.174 0.6262 0.2347 0.066 Uiso 1 1 calc R A 1 H8C H -0.1615 0.545 0.1777 0.066 Uiso 1 1 calc R A 1 C9 C -0.2511(3) 0.39095(19) 0.22048(15) 0.0528(8) Uani 1 1 d . A 1 H9A H -0.1836 0.3869 0.2476 0.079 Uiso 1 1 calc R A 1 H9B H -0.2454 0.3782 0.1722 0.079 Uiso 1 1 calc R A 1 H9C H -0.3123 0.3504 0.2256 0.079 Uiso 1 1 calc R A 1 C10 C -0.1903(2) 0.43854(19) 0.42624(14) 0.0405(7) Uani 1 1 d . A 1 H10A H -0.1327 0.4886 0.4512 0.061 Uiso 1 1 calc R A 1 H10B H -0.1624 0.4012 0.391 0.061 Uiso 1 1 calc R A 1 H10C H -0.2136 0.4084 0.4582 0.061 Uiso 1 1 calc R A 1 C11 C -0.4132(2) 0.37136(18) 0.33918(15) 0.0454(7) Uani 1 1 d . A 1 H11A H -0.4781 0.3845 0.3163 0.068 Uiso 1 1 calc R A 1 H11B H -0.4332 0.3422 0.3725 0.068 Uiso 1 1 calc R A 1 H11C H -0.3826 0.3348 0.305 0.068 Uiso 1 1 calc R A 1 C12 C -0.3719(2) 0.52892(18) 0.45557(13) 0.0373(6) Uani 1 1 d . A 1 H12A H -0.4346 0.5475 0.4359 0.056 Uiso 1 1 calc R A 1 H12B H -0.3178 0.5782 0.486 0.056 Uiso 1 1 calc R A 1 H12C H -0.3958 0.4906 0.4817 0.056 Uiso 1 1 calc R A 1 C13 C 0.0604(2) 0.54062(16) 0.35592(12) 0.0295(6) Uani 1 1 d . A 1 C14 C 0.12797(18) 0.48330(15) 0.32553(12) 0.0245(5) Uani 1 1 d . A 1 C15 C 0.0664(2) 0.39125(17) 0.30981(17) 0.0467(8) Uani 1 1 d . A 1 H15A H -0.0041 0.3812 0.2783 0.056 Uiso 1 1 calc R A 1 H15B H 0.0516 0.3796 0.3526 0.056 Uiso 1 1 calc R A 1 C16 C 0.1370(2) 0.33245(18) 0.27647(17) 0.0502(8) Uani 1 1 d . A 1 H16 H 0.0976 0.2722 0.2653 0.06 Uiso 1 1 calc R A 1 C17 C 0.2444(2) 0.34756(19) 0.32542(15) 0.0446(7) Uani 1 1 d . A 1 H17A H 0.2307 0.3355 0.3682 0.054 Uiso 1 1 calc R A 1 H17B H 0.2892 0.3093 0.3044 0.054 Uiso 1 1 calc R A 1 C18 C 0.3039(2) 0.43767(18) 0.34118(14) 0.0405(7) Uani 1 1 d . A 1 H18 H 0.3747 0.4472 0.3733 0.049 Uiso 1 1 calc R A 1 C19 C 0.2353(2) 0.49628(19) 0.37530(14) 0.0403(7) Uani 1 1 d . A 1 H19A H 0.2755 0.5558 0.3878 0.048 Uiso 1 1 calc R A 1 H19B H 0.2202 0.4836 0.4177 0.048 Uiso 1 1 calc R A 1 C20 C 0.1501(3) 0.50160(19) 0.25967(14) 0.0442(7) Uani 1 1 d . A 1 H20A H 0.1889 0.5612 0.2699 0.053 Uiso 1 1 calc R A 1 H20B H 0.0804 0.4925 0.2276 0.053 Uiso 1 1 calc R A 1 C21 C 0.2196(3) 0.4425(2) 0.22703(15) 0.0485(8) Uani 1 1 d . A 1 H21 H 0.2349 0.4545 0.184 0.058 Uiso 1 1 calc R A 1 C22 C 0.1588(3) 0.3522(2) 0.21037(15) 0.0580(10) Uani 1 1 d . A 1 H22A H 0.2022 0.3139 0.1877 0.07 Uiso 1 1 calc R A 1 H22B H 0.0889 0.343 0.1785 0.07 Uiso 1 1 calc R A 1 C23 C 0.3261(2) 0.4566(2) 0.27629(17) 0.0511(8) Uani 1 1 d . A 1 H23A H 0.3663 0.516 0.2872 0.061 Uiso 1 1 calc R A 1 H23B H 0.3717 0.4194 0.2547 0.061 Uiso 1 1 calc R A 1 C24 C -0.5268(2) 0.71716(16) 0.40711(13) 0.0318(6) Uani 1 1 d . A 1 C25 C -0.59870(19) 0.76661(15) 0.44197(12) 0.0257(5) Uani 1 1 d . A 1 C26 C -0.5506(2) 0.86162(17) 0.45638(16) 0.0420(7) Uani 1 1 d . A 1 H26A H -0.4768 0.8773 0.4853 0.05 Uiso 1 1 calc R A 1 H26B H -0.545 0.8748 0.4128 0.05 Uiso 1 1 calc R A 1 C27 C -0.6261(2) 0.91179(17) 0.49365(17) 0.0457(8) Uani 1 1 d . A 1 H27 H -0.5958 0.9737 0.5036 0.055 Uiso 1 1 calc R A 1 C28 C -0.7396(2) 0.88806(18) 0.44856(15) 0.0412(7) Uani 1 1 d . A 1 H28A H -0.7874 0.9217 0.4717 0.049 Uiso 1 1 calc R A 1 H28B H -0.7352 0.9004 0.4046 0.049 Uiso 1 1 calc R A 1 C29 C -0.7863(2) 0.79455(17) 0.43537(14) 0.0375(6) Uani 1 1 d . A 1 H29 H -0.8611 0.7788 0.4066 0.045 Uiso 1 1 calc R A 1 C30 C -0.7126(2) 0.74415(18) 0.39700(14) 0.0395(7) Uani 1 1 d . A 1 H30A H -0.7436 0.6828 0.3859 0.047 Uiso 1 1 calc R A 1 H30B H -0.7081 0.7578 0.3536 0.047 Uiso 1 1 calc R A 1 C31 C -0.6049(2) 0.74705(18) 0.51002(13) 0.0373(6) Uani 1 1 d . A 1 H31A H -0.6342 0.6859 0.5013 0.045 Uiso 1 1 calc R A 1 H31B H -0.5312 0.7623 0.539 0.045 Uiso 1 1 calc R A 1 C32 C -0.6788(2) 0.79774(19) 0.54667(14) 0.0440(7) Uani 1 1 d . A 1 H32 H -0.6836 0.7849 0.5909 0.053 Uiso 1 1 calc R A 1 C33 C -0.6327(3) 0.8911(2) 0.56089(15) 0.0534(9) Uani 1 1 d . A 1 H33A H -0.5592 0.9071 0.5902 0.064 Uiso 1 1 calc R A 1 H33B H -0.6798 0.924 0.5856 0.064 Uiso 1 1 calc R A 1 C34 C -0.7915(2) 0.77403(19) 0.50206(15) 0.0439(7) Uani 1 1 d . A 1 H34A H -0.8219 0.7129 0.4925 0.053 Uiso 1 1 calc R A 1 H34B H -0.8401 0.8055 0.5265 0.053 Uiso 1 1 calc R A 1 Li1B Li 0.1466(3) 0.8596(3) 0.1266(2) 0.0342(10) Uani 1 1 d . B 2 Li2B Li 0.3433(3) 0.8717(3) 0.1316(2) 0.0329(10) Uani 1 1 d . B 2 N1B N 0.22372(16) 0.76391(12) 0.09563(10) 0.0265(5) Uani 1 1 d . B 2 N2B N 0.26495(16) 0.96647(12) 0.16307(10) 0.0286(5) Uani 1 1 d . B 2 N3B N -0.02103(19) 0.83044(16) 0.10534(12) 0.0447(6) Uani 1 1 d . B 2 N4B N 0.50975(18) 0.91059(15) 0.14294(12) 0.0421(6) Uani 1 1 d . B 2 Si1B Si 0.22429(5) 0.72654(4) 0.01082(3) 0.02759(17) Uani 1 1 d . B 2 Si2B Si 0.20080(6) 0.69859(4) 0.14526(4) 0.02971(17) Uani 1 1 d . B 2 Si3B Si 0.24419(6) 1.02661(5) 0.11023(4) 0.03375(18) Uani 1 1 d . B 2 Si4B Si 0.30370(6) 1.00568(5) 0.24957(4) 0.03202(18) Uani 1 1 d . B 2 C1B C 0.2695(2) 0.62402(17) -0.01545(14) 0.0391(7) Uani 1 1 d . B 2 H1B1 H 0.3407 0.6293 0.0126 0.059 Uiso 1 1 calc R B 2 H1B2 H 0.275 0.6107 -0.0638 0.059 Uiso 1 1 calc R B 2 H1B3 H 0.2163 0.5787 -0.0088 0.059 Uiso 1 1 calc R B 2 C2B C 0.0882(2) 0.7074(2) -0.04643(14) 0.0442(7) Uani 1 1 d . B 2 H2B1 H 0.0349 0.667 -0.0344 0.066 Uiso 1 1 calc R B 2 H2B2 H 0.0941 0.6844 -0.0942 0.066 Uiso 1 1 calc R B 2 H2B3 H 0.0644 0.7608 -0.0406 0.066 Uiso 1 1 calc R B 2 C3B C 0.3208(2) 0.80444(18) -0.01609(14) 0.0388(7) Uani 1 1 d . B 2 H3B1 H 0.3934 0.8165 0.0124 0.058 Uiso 1 1 calc R B 2 H3B2 H 0.2948 0.8569 -0.0105 0.058 Uiso 1 1 calc R B 2 H3B3 H 0.3243 0.7805 -0.0642 0.058 Uiso 1 1 calc R B 2 C4B C 0.3302(2) 0.6754(2) 0.18480(16) 0.0473(7) Uani 1 1 d . B 2 H4B1 H 0.3666 0.6495 0.1486 0.071 Uiso 1 1 calc R B 2 H4B2 H 0.3131 0.6364 0.2116 0.071 Uiso 1 1 calc R B 2 H4B3 H 0.3784 0.7281 0.2148 0.071 Uiso 1 1 calc R B 2 C5B C 0.1037(2) 0.59385(18) 0.10090(15) 0.0473(7) Uani 1 1 d . B 2 H5B1 H 0.131 0.5634 0.0618 0.071 Uiso 1 1 calc R B 2 H5B2 H 0.032 0.6033 0.0848 0.071 Uiso 1 1 calc R B 2 H5B3 H 0.0975 0.5603 0.133 0.071 Uiso 1 1 calc R B 2 C6B C 0.1362(2) 0.74793(19) 0.21761(14) 0.0440(7) Uani 1 1 d . B 2 H6B1 H 0.182 0.8034 0.2441 0.066 Uiso 1 1 calc R B 2 H6B2 H 0.1287 0.7114 0.2474 0.066 Uiso 1 1 calc R B 2 H6B3 H 0.0641 0.7547 0.1991 0.066 Uiso 1 1 calc R B 2 C7B C 0.3675(3) 1.0608(2) 0.07579(17) 0.0553(8) Uani 1 1 d . B 2 H7B1 H 0.4277 1.0927 0.1139 0.083 Uiso 1 1 calc R B 2 H7B2 H 0.351 1.0966 0.0469 0.083 Uiso 1 1 calc R B 2 H7B3 H 0.3881 1.0109 0.0485 0.083 Uiso 1 1 calc R B 2 C8B C 0.1338(2) 0.9665(2) 0.03373(15) 0.0479(8) Uani 1 1 d . B 2 H8B1 H 0.0671 0.9471 0.0491 0.072 Uiso 1 1 calc R B 2 H8B2 H 0.1568 0.9176 0.0068 0.072 Uiso 1 1 calc R B 2 H8B3 H 0.1197 1.0034 0.0054 0.072 Uiso 1 1 calc R B 2 C9B C 0.1984(3) 1.12606(19) 0.14827(17) 0.0576(9) Uani 1 1 d . B 2 H9B1 H 0.1337 1.1122 0.1673 0.086 Uiso 1 1 calc R B 2 H9B2 H 0.1807 1.1529 0.1126 0.086 Uiso 1 1 calc R B 2 H9B3 H 0.2568 1.1649 0.1847 0.086 Uiso 1 1 calc R B 2 C10B C 0.3897(3) 1.11624(19) 0.28305(17) 0.0565(9) Uani 1 1 d . B 2 H10D H 0.3507 1.1548 0.2667 0.085 Uiso 1 1 calc R B 2 H10E H 0.4584 1.1179 0.2666 0.085 Uiso 1 1 calc R B 2 H10F H 0.4049 1.1337 0.3332 0.085 Uiso 1 1 calc R B 2 C11B C 0.1844(3) 1.0062(2) 0.29374(16) 0.0535(8) Uani 1 1 d . B 2 H11D H 0.1374 1.0398 0.2769 0.08 Uiso 1 1 calc R B 2 H11E H 0.2106 1.031 0.3432 0.08 Uiso 1 1 calc R B 2 H11F H 0.143 0.9482 0.2842 0.08 Uiso 1 1 calc R B 2 C12B C 0.3888(2) 0.94030(19) 0.28512(14) 0.0427(7) Uani 1 1 d . B 2 H12D H 0.3492 0.8811 0.2701 0.064 Uiso 1 1 calc R B 2 H12E H 0.4042 0.961 0.3353 0.064 Uiso 1 1 calc R B 2 H12F H 0.4575 0.9447 0.2686 0.064 Uiso 1 1 calc R B 2 C13B C -0.1056(2) 0.78907(18) 0.08015(14) 0.0363(6) Uani 1 1 d . B 2 C14B C -0.21273(19) 0.73244(16) 0.04733(12) 0.0290(6) Uani 1 1 d . B 2 C15B C -0.3046(2) 0.77315(16) 0.07279(14) 0.0337(6) Uani 1 1 d . B 2 H15C H -0.2949 0.7854 0.1231 0.04 Uiso 1 1 calc R B 2 H15D H -0.3021 0.8271 0.0616 0.04 Uiso 1 1 calc R B 2 C16B C -0.4141(2) 0.71284(16) 0.03851(13) 0.0329(6) Uani 1 1 d . B 2 H16B H -0.4737 0.7393 0.055 0.039 Uiso 1 1 calc R B 2 C17B C -0.4183(2) 0.63029(17) 0.05669(14) 0.0384(6) Uani 1 1 d . B 2 H17C H -0.4089 0.6416 0.1069 0.046 Uiso 1 1 calc R B 2 H17D H -0.4899 0.5914 0.0352 0.046 Uiso 1 1 calc R B 2 C18B C -0.3280(2) 0.58976(17) 0.03112(14) 0.0381(6) Uani 1 1 d . B 2 H18B H -0.3312 0.5354 0.0427 0.046 Uiso 1 1 calc R B 2 C19B C -0.2175(2) 0.64883(17) 0.06552(14) 0.0371(6) Uani 1 1 d . B 2 H19C H -0.1587 0.6222 0.0496 0.045 Uiso 1 1 calc R B 2 H19D H -0.2072 0.66 0.1158 0.045 Uiso 1 1 calc R B 2 C20B C -0.2281(2) 0.71451(19) -0.03090(13) 0.0390(7) Uani 1 1 d . B 2 H20C H -0.2251 0.768 -0.0429 0.047 Uiso 1 1 calc R B 2 H20D H -0.1692 0.6886 -0.0477 0.047 Uiso 1 1 calc R B 2 C21B C -0.3387(2) 0.65427(18) -0.06442(13) 0.0370(6) Uani 1 1 d . B 2 H21B H -0.3492 0.6422 -0.1153 0.044 Uiso 1 1 calc R B 2 C22B C -0.4290(2) 0.69550(17) -0.03898(14) 0.0373(6) Uani 1 1 d . B 2 H22C H -0.4263 0.7491 -0.0507 0.045 Uiso 1 1 calc R B 2 H22D H -0.5009 0.6576 -0.0615 0.045 Uiso 1 1 calc R B 2 C23B C -0.3424(2) 0.57187(18) -0.04625(14) 0.0424(7) Uani 1 1 d . B 2 H23C H -0.4131 0.5322 -0.0689 0.051 Uiso 1 1 calc R B 2 H23D H -0.2837 0.5454 -0.0627 0.051 Uiso 1 1 calc R B 2 C24B C 0.5915(2) 0.95845(17) 0.16238(13) 0.0343(6) Uani 1 1 d . B 2 C25B C 0.69407(19) 1.02202(16) 0.18952(12) 0.0282(5) Uiso 0.5 1 d P B 2 C26B C 0.7142(4) 1.0499(3) 0.2689(3) 0.0357(12) Uiso 0.5 1 d P B 2 H26C H 0.6516 1.0716 0.2842 0.043 Uiso 0.5 1 calc PR B 2 H26D H 0.7201 1.0005 0.2855 0.043 Uiso 0.5 1 calc PR B 2 C27B C 0.8187(6) 1.1189(5) 0.2999(4) 0.045(2) Uiso 0.5 1 d P B 2 H27B H 0.8315 1.1371 0.351 0.054 Uiso 0.5 1 calc PR B 2 C28B C 0.6854(4) 1.1027(3) 0.1659(3) 0.0376(13) Uiso 0.5 1 d P B 2 H28C H 0.6756 1.0879 0.1154 0.045 Uiso 0.5 1 calc PR B 2 H28D H 0.6212 1.1236 0.1794 0.045 Uiso 0.5 1 calc PR B 2 C29B C 0.7898(6) 1.1728(5) 0.1992(4) 0.045(2) Uiso 0.5 1 d P B 2 H29B H 0.785 1.2244 0.1846 0.054 Uiso 0.5 1 calc PR B 2 C30B C 0.7920(4) 0.9889(3) 0.1667(3) 0.0368(12) Uiso 0.5 1 d P B 2 H30C H 0.7847 0.9786 0.1166 0.044 Uiso 0.5 1 calc PR B 2 H30D H 0.7923 0.9343 0.1764 0.044 Uiso 0.5 1 calc PR B 2 C31B C 0.9134(7) 1.0593(6) 0.2080(5) 0.052(3) Uiso 0.5 1 d P B 2 H31C H 0.9793 1.0383 0.1966 0.063 Uiso 0.5 1 calc PR B 2 C32B C 0.9133(6) 1.0834(5) 0.2741(4) 0.050(2) Uiso 0.5 1 d P B 2 H32A H 0.9809 1.127 0.2965 0.059 Uiso 0.5 1 calc PR B 2 H32B H 0.9186 1.0342 0.2912 0.059 Uiso 0.5 1 calc PR B 2 C33B C 0.8857(7) 1.1329(5) 0.1723(4) 0.051(2) Uiso 0.5 1 d P B 2 H33C H 0.952 1.1783 0.1823 0.061 Uiso 0.5 1 calc PR B 2 H33D H 0.8651 1.1076 0.122 0.061 Uiso 0.5 1 calc PR B 2 C34B C 0.8102(7) 1.1929(5) 0.2717(4) 0.046(2) Uiso 0.5 1 d P B 2 H34C H 0.7511 1.2184 0.2886 0.056 Uiso 0.5 1 calc PR B 2 H34D H 0.879 1.2362 0.2903 0.056 Uiso 0.5 1 calc PR B 2 C25C C 0.69407(19) 1.02202(16) 0.18952(12) 0.0282(5) Uiso 0.5 1 d P C 3 C26C C 0.7724(5) 0.9877(4) 0.2332(3) 0.0447(14) Uiso 0.5 1 d P C 3 H26E H 0.7862 0.9347 0.2048 0.054 Uiso 0.5 1 calc PR C 3 H26F H 0.7395 0.9752 0.2711 0.054 Uiso 0.5 1 calc PR C 3 C27C C 0.8816(7) 1.0548(5) 0.2630(4) 0.053(2) Uiso 0.5 1 d P C 3 H27C H 0.9389 1.0352 0.2892 0.064 Uiso 0.5 1 calc PR C 3 C28C C 0.6705(5) 1.1020(4) 0.2336(3) 0.0473(15) Uiso 0.5 1 d P C 3 H28E H 0.637 1.0896 0.2712 0.057 Uiso 0.5 1 calc PR C 3 H28F H 0.6186 1.1232 0.2056 0.057 Uiso 0.5 1 calc PR C 3 C29C C 0.7789(6) 1.1713(5) 0.2642(4) 0.050(2) Uiso 0.5 1 d P C 3 H29C H 0.767 1.2256 0.293 0.06 Uiso 0.5 1 calc PR C 3 C30C C 0.7425(4) 1.0382(4) 0.1294(3) 0.0411(13) Uiso 0.5 1 d P C 3 H30E H 0.6911 1.0587 0.1005 0.049 Uiso 0.5 1 calc PR C 3 H30F H 0.7565 0.9853 0.1009 0.049 Uiso 0.5 1 calc PR C 3 C31C C 0.8514(7) 1.1062(5) 0.1590(4) 0.058(2) Uiso 0.5 1 d P C 3 H31D H 0.8859 1.1178 0.1208 0.07 Uiso 0.5 1 calc PR C 3 C32C C 0.9092(7) 1.0686(6) 0.1922(4) 0.047(2) Uiso 0.5 1 d P C 3 H32C H 0.9856 1.1006 0.2023 0.057 Uiso 0.5 1 calc PR C 3 H32D H 0.9063 1.0122 0.1607 0.057 Uiso 0.5 1 calc PR C 3 C33C C 0.8270(7) 1.1814(5) 0.1989(4) 0.045(2) Uiso 0.5 1 d P C 3 H33E H 0.7739 1.1999 0.1695 0.054 Uiso 0.5 1 calc PR C 3 H33F H 0.8944 1.2265 0.2145 0.054 Uiso 0.5 1 calc PR C 3 C34C C 0.8540(7) 1.1334(5) 0.3029(4) 0.050(2) Uiso 0.5 1 d P C 3 H34E H 0.8208 1.1208 0.3407 0.06 Uiso 0.5 1 calc PR C 3 H34F H 0.9226 1.1763 0.3239 0.06 Uiso 0.5 1 calc PR C 3 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 Li1 0.033(2) 0.028(2) 0.036(2) 0.0079(19) 0.0112(19) 0.0129(19) Li2 0.031(2) 0.031(2) 0.036(2) 0.0032(19) 0.0068(18) 0.0131(19) N1 0.0319(11) 0.0221(11) 0.0264(11) 0.0069(9) 0.0082(9) 0.0096(9) N2 0.0298(11) 0.0231(11) 0.0244(11) 0.0069(9) 0.0063(8) 0.0095(9) N3 0.0304(12) 0.0387(14) 0.0400(13) 0.0069(11) 0.0076(10) 0.0134(11) N4 0.0351(13) 0.0376(14) 0.0463(14) 0.0072(11) 0.0096(11) 0.0147(11) Si1 0.0422(4) 0.0273(4) 0.0317(4) 0.0119(3) 0.0140(3) 0.0141(3) Si2 0.0289(4) 0.0267(4) 0.0265(4) 0.0051(3) 0.0050(3) 0.0077(3) Si3 0.0374(4) 0.0276(4) 0.0237(4) 0.0059(3) 0.0059(3) 0.0127(3) Si4 0.0272(4) 0.0269(4) 0.0297(4) 0.0106(3) 0.0061(3) 0.0065(3) C1 0.074(2) 0.053(2) 0.0354(17) 0.0178(15) 0.0047(15) 0.0251(17) C2 0.075(2) 0.0423(18) 0.0437(18) 0.0165(14) 0.0190(16) 0.0308(17) C3 0.063(2) 0.062(2) 0.070(2) 0.0380(19) 0.0337(18) 0.0202(18) C4 0.0437(17) 0.0334(17) 0.0484(18) 0.0058(13) -0.0031(13) 0.0056(13) C5 0.0442(17) 0.0499(19) 0.0307(15) 0.0039(13) 0.0098(13) 0.0177(14) C6 0.0352(15) 0.0384(16) 0.0340(15) 0.0119(12) 0.0054(12) 0.0089(12) C7 0.0451(17) 0.053(2) 0.0315(16) 0.0099(14) -0.0010(13) 0.0084(15) C8 0.0445(17) 0.060(2) 0.0350(16) 0.0199(14) 0.0131(13) 0.0181(15) C9 0.086(2) 0.0403(18) 0.0389(17) 0.0074(14) 0.0199(16) 0.0322(17) C10 0.0404(16) 0.0449(18) 0.0467(17) 0.0257(14) 0.0120(13) 0.0153(14) C11 0.0419(17) 0.0374(17) 0.0545(19) 0.0148(14) 0.0085(14) 0.0010(13) C12 0.0329(15) 0.0478(18) 0.0339(15) 0.0148(13) 0.0112(12) 0.0082(13) C13 0.0273(13) 0.0313(15) 0.0290(14) 0.0082(11) 0.0043(11) 0.0067(12) C14 0.0232(12) 0.0221(13) 0.0286(13) 0.0052(10) 0.0079(10) 0.0075(10) C15 0.0325(15) 0.0300(16) 0.075(2) 0.0107(15) 0.0150(15) 0.0042(13) C16 0.0399(17) 0.0204(15) 0.082(2) 0.0022(15) 0.0158(16) 0.0021(13) C17 0.0544(19) 0.0446(18) 0.0511(18) 0.0243(15) 0.0219(15) 0.0283(15) C18 0.0295(14) 0.0460(18) 0.0404(16) 0.0019(13) -0.0004(12) 0.0170(13) C19 0.0356(15) 0.0429(17) 0.0366(16) 0.0007(13) 0.0016(12) 0.0150(13) C20 0.064(2) 0.0480(19) 0.0380(16) 0.0220(14) 0.0233(14) 0.0343(16) C21 0.072(2) 0.057(2) 0.0372(17) 0.0234(15) 0.0303(16) 0.0393(18) C22 0.060(2) 0.060(2) 0.0382(18) -0.0163(15) -0.0103(15) 0.0338(18) C23 0.0451(18) 0.0418(18) 0.075(2) 0.0150(16) 0.0350(17) 0.0156(15) C24 0.0284(14) 0.0284(14) 0.0376(15) 0.0081(12) 0.0055(12) 0.0077(12) C25 0.0245(13) 0.0216(13) 0.0317(14) 0.0061(11) 0.0077(10) 0.0078(10) C26 0.0301(14) 0.0291(15) 0.072(2) 0.0182(14) 0.0204(14) 0.0068(12) C27 0.0355(16) 0.0157(14) 0.083(2) 0.0066(14) 0.0185(15) 0.0041(12) C28 0.0408(16) 0.0387(17) 0.0561(19) 0.0218(14) 0.0183(14) 0.0217(14) C29 0.0237(13) 0.0353(16) 0.0474(17) 0.0043(13) -0.0008(12) 0.0092(12) C30 0.0346(15) 0.0382(17) 0.0387(16) 0.0000(13) -0.0011(12) 0.0136(13) C31 0.0416(16) 0.0383(16) 0.0378(16) 0.0151(13) 0.0084(12) 0.0175(13) C32 0.0535(18) 0.056(2) 0.0347(16) 0.0182(14) 0.0195(14) 0.0268(16) C33 0.0432(18) 0.054(2) 0.0457(18) -0.0143(15) -0.0028(14) 0.0190(15) C34 0.0351(16) 0.0396(17) 0.066(2) 0.0200(15) 0.0241(15) 0.0143(13) Li1B 0.032(2) 0.029(2) 0.038(2) 0.0044(19) 0.0063(19) 0.0063(19) Li2B 0.027(2) 0.025(2) 0.044(3) 0.0075(19) 0.0039(19) 0.0069(18) N1B 0.0278(11) 0.0227(11) 0.0277(11) 0.0067(9) 0.0049(9) 0.0040(9) N2B 0.0291(11) 0.0217(11) 0.0330(12) 0.0071(9) 0.0040(9) 0.0038(9) N3B 0.0307(13) 0.0474(16) 0.0495(15) 0.0107(12) -0.0004(11) 0.0037(12) N4B 0.0306(13) 0.0426(15) 0.0486(15) 0.0086(12) 0.0079(11) 0.0032(12) Si1B 0.0273(4) 0.0271(4) 0.0273(4) 0.0059(3) 0.0035(3) 0.0078(3) Si2B 0.0301(4) 0.0278(4) 0.0319(4) 0.0112(3) 0.0053(3) 0.0051(3) Si3B 0.0392(4) 0.0270(4) 0.0382(4) 0.0128(3) 0.0074(3) 0.0111(3) Si4B 0.0320(4) 0.0276(4) 0.0317(4) 0.0044(3) 0.0011(3) 0.0050(3) C1B 0.0422(16) 0.0349(16) 0.0407(16) 0.0071(13) 0.0124(13) 0.0127(13) C2B 0.0358(16) 0.056(2) 0.0348(16) 0.0055(14) -0.0011(12) 0.0136(14) C3B 0.0436(16) 0.0438(17) 0.0337(15) 0.0156(13) 0.0088(12) 0.0148(14) C4B 0.0473(18) 0.053(2) 0.0534(19) 0.0309(16) 0.0106(14) 0.0178(15) C5B 0.0550(19) 0.0356(17) 0.0495(19) 0.0176(14) 0.0097(15) -0.0018(14) C6B 0.0470(17) 0.0515(19) 0.0371(16) 0.0168(14) 0.0136(13) 0.0100(14) C7B 0.0524(19) 0.055(2) 0.069(2) 0.0361(18) 0.0156(17) 0.0093(16) C8B 0.0519(18) 0.052(2) 0.0430(17) 0.0209(15) -0.0003(14) 0.0180(15) C9B 0.082(2) 0.0388(19) 0.061(2) 0.0201(16) 0.0154(18) 0.0291(18) C10B 0.060(2) 0.0342(18) 0.057(2) 0.0029(15) -0.0104(16) -0.0029(15) C11B 0.0543(19) 0.062(2) 0.0472(19) 0.0107(16) 0.0173(15) 0.0220(17) C12B 0.0416(16) 0.0460(18) 0.0404(17) 0.0161(14) 0.0037(13) 0.0076(14) C13B 0.0333(16) 0.0376(16) 0.0378(16) 0.0130(13) 0.0036(12) 0.0068(13) C14B 0.0227(13) 0.0318(15) 0.0300(14) 0.0089(11) 0.0019(10) 0.0021(11) C15B 0.0341(14) 0.0269(15) 0.0373(15) 0.0050(12) 0.0073(12) 0.0060(11) C16B 0.0263(13) 0.0287(15) 0.0424(16) 0.0062(12) 0.0090(11) 0.0077(11) C17B 0.0353(15) 0.0361(16) 0.0436(17) 0.0139(13) 0.0110(12) 0.0019(12) C18B 0.0427(16) 0.0270(15) 0.0482(17) 0.0176(13) 0.0054(13) 0.0097(12) C19B 0.0353(15) 0.0402(17) 0.0397(16) 0.0164(13) 0.0038(12) 0.0144(13) C20B 0.0311(15) 0.0533(19) 0.0338(15) 0.0170(13) 0.0073(12) 0.0056(13) C21B 0.0347(15) 0.0462(18) 0.0264(14) 0.0080(12) 0.0035(11) 0.0056(13) C22B 0.0286(14) 0.0331(16) 0.0479(17) 0.0152(13) -0.0033(12) 0.0041(12) C23B 0.0380(16) 0.0342(16) 0.0470(18) -0.0009(13) 0.0055(13) 0.0094(13) C24B 0.0304(15) 0.0348(16) 0.0345(15) 0.0070(12) 0.0048(12) 0.0051(13) #----------------------------------------------------------------------------# # 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 Li1 N1 2.028(4) . ? Li1 N2 2.054(5) . ? Li1 N3 2.084(4) . ? Li2 N2 2.021(4) . ? Li2 N1 2.040(5) . ? Li2 N4 2.052(4) . ? N1 Si2 1.697(2) . ? N1 Si1 1.704(2) . ? N2 Si3 1.6945(19) . ? N2 Si4 1.702(2) . ? N3 C13 1.142(3) . ? N4 C24 1.139(3) . ? Si1 C3 1.876(3) . ? Si1 C2 1.879(3) . ? Si1 C1 1.887(3) . ? Si2 C4 1.879(3) . ? Si2 C6 1.883(3) . ? Si2 C5 1.882(3) . ? Si3 C7 1.874(3) . ? Si3 C9 1.879(3) . ? Si3 C8 1.887(3) . ? Si4 C10 1.879(3) . ? Si4 C11 1.880(3) . ? Si4 C12 1.885(2) . ? C13 C14 1.478(3) . ? C14 C20 1.524(3) . ? C14 C19 1.533(3) . ? C14 C15 1.536(4) . ? C15 C16 1.544(4) . ? C16 C17 1.519(4) . ? C16 C22 1.538(5) . ? C17 C18 1.499(4) . ? C18 C23 1.510(4) . ? C18 C19 1.530(3) . ? C20 C21 1.532(3) . ? C21 C22 1.505(5) . ? C21 C23 1.516(4) . ? C24 C25 1.477(3) . ? C25 C30 1.533(3) . ? C25 C31 1.535(3) . ? C25 C26 1.541(3) . ? C26 C27 1.542(4) . ? C27 C28 1.528(4) . ? C27 C33 1.527(4) . ? C28 C29 1.518(4) . ? C29 C34 1.513(4) . ? C29 C30 1.535(3) . ? C31 C32 1.525(3) . ? C32 C33 1.512(4) . ? C32 C34 1.516(4) . ? Li1B N2B 2.023(5) . ? Li1B N1B 2.037(4) . ? Li1B N3B 2.059(5) . ? Li2B N2B 2.037(4) . ? Li2B N1B 2.041(5) . ? Li2B N4B 2.065(5) . ? N1B Si1B 1.700(2) . ? N1B Si2B 1.705(2) . ? N2B Si3B 1.696(2) . ? N2B Si4B 1.699(2) . ? N3B C13B 1.141(3) . ? N4B C24B 1.145(3) . ? Si1B C2B 1.878(3) . ? Si1B C1B 1.881(3) . ? Si1B C3B 1.885(3) . ? Si2B C6B 1.879(3) . ? Si2B C5B 1.882(3) . ? Si2B C4B 1.882(3) . ? Si3B C7B 1.875(3) . ? Si3B C8B 1.878(3) . ? Si3B C9B 1.880(3) . ? Si4B C12B 1.880(3) . ? Si4B C10B 1.880(3) . ? Si4B C11B 1.879(3) . ? C13B C14B 1.474(4) . ? C14B C20B 1.540(3) . ? C14B C15B 1.541(3) . ? C14B C19B 1.542(4) . ? C15B C16B 1.523(3) . ? C16B C17B 1.525(4) . ? C16B C22B 1.527(4) . ? C17B C18B 1.523(4) . ? C18B C23B 1.524(4) . ? C18B C19B 1.526(4) . ? C20B C21B 1.531(4) . ? C21B C23B 1.523(4) . ? C21B C22B 1.528(4) . ? C24B C25B 1.467(4) . ? C25B C30B 1.534(5) . ? C25B C26B 1.552(6) . ? C25B C28B 1.574(6) . ? C26B C27B 1.535(9) . ? C27B C34B 1.521(11) . ? C27B C32B 1.534(10) . ? C28B C29B 1.549(9) . ? C29B C34B 1.419(10) . ? C29B C33B 1.591(10) . ? C30B C31B 1.725(10) . ? C31B C32B 1.318(11) . ? C31B C33B 1.661(11) . ? C26C C27C 1.558(10) . ? C27C C34C 1.490(11) . ? C27C C32C 1.616(11) . ? C28C C29C 1.570(10) . ? C29C C34C 1.492(11) . ? C29C C33C 1.593(10) . ? C30C C31C 1.562(10) . ? C31C C32C 1.287(11) . ? C31C C33C 1.428(10) . ? 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 N1 Li1 N2 105.10(19) . . ? N1 Li1 N3 142.1(2) . . ? N2 Li1 N3 112.8(2) . . ? N2 Li2 N1 105.87(19) . . ? N2 Li2 N4 138.0(2) . . ? N1 Li2 N4 115.7(2) . . ? Si2 N1 Si1 121.44(12) . . ? Si2 N1 Li1 105.59(15) . . ? Si1 N1 Li1 124.09(16) . . ? Si2 N1 Li2 117.75(16) . . ? Si1 N1 Li2 104.66(16) . . ? Li1 N1 Li2 74.55(18) . . ? Si3 N2 Si4 124.10(12) . . ? Si3 N2 Li2 116.42(16) . . ? Si4 N2 Li2 109.08(15) . . ? Si3 N2 Li1 105.68(15) . . ? Si4 N2 Li1 116.70(16) . . ? Li2 N2 Li1 74.42(17) . . ? C13 N3 Li1 155.7(2) . . ? C24 N4 Li2 156.8(3) . . ? N1 Si1 C3 113.06(13) . . ? N1 Si1 C2 114.72(11) . . ? C3 Si1 C2 106.84(15) . . ? N1 Si1 C1 111.61(12) . . ? C3 Si1 C1 106.03(16) . . ? C2 Si1 C1 103.80(14) . . ? N1 Si2 C4 115.76(12) . . ? N1 Si2 C6 109.88(11) . . ? C4 Si2 C6 105.56(13) . . ? N1 Si2 C5 113.33(11) . . ? C4 Si2 C5 105.88(13) . . ? C6 Si2 C5 105.68(13) . . ? N2 Si3 C7 112.74(11) . . ? N2 Si3 C9 115.29(12) . . ? C7 Si3 C9 105.94(15) . . ? N2 Si3 C8 111.53(12) . . ? C7 Si3 C8 106.29(13) . . ? C9 Si3 C8 104.29(14) . . ? N2 Si4 C10 113.19(11) . . ? N2 Si4 C11 116.08(12) . . ? C10 Si4 C11 105.29(13) . . ? N2 Si4 C12 109.93(11) . . ? C10 Si4 C12 106.97(12) . . ? C11 Si4 C12 104.67(13) . . ? N3 C13 C14 176.7(3) . . ? C13 C14 C20 108.0(2) . . ? C13 C14 C19 110.9(2) . . ? C20 C14 C19 110.4(2) . . ? C13 C14 C15 109.4(2) . . ? C20 C14 C15 110.1(2) . . ? C19 C14 C15 108.1(2) . . ? C14 C15 C16 108.6(2) . . ? C17 C16 C22 109.5(2) . . ? C17 C16 C15 109.7(2) . . ? C22 C16 C15 108.7(2) . . ? C18 C17 C16 109.5(2) . . ? C17 C18 C23 110.2(2) . . ? C17 C18 C19 109.4(2) . . ? C23 C18 C19 109.8(2) . . ? C18 C19 C14 109.2(2) . . ? C14 C20 C21 108.9(2) . . ? C22 C21 C23 109.6(2) . . ? C22 C21 C20 109.4(3) . . ? C23 C21 C20 109.8(2) . . ? C21 C22 C16 109.8(2) . . ? C21 C23 C18 109.8(2) . . ? N4 C24 C25 178.4(3) . . ? C24 C25 C30 110.6(2) . . ? C24 C25 C31 108.4(2) . . ? C30 C25 C31 110.3(2) . . ? C24 C25 C26 109.4(2) . . ? C30 C25 C26 108.8(2) . . ? C31 C25 C26 109.3(2) . . ? C27 C26 C25 108.4(2) . . ? C28 C27 C33 109.8(2) . . ? C28 C27 C26 109.8(2) . . ? C33 C27 C26 109.1(2) . . ? C29 C28 C27 109.0(2) . . ? C34 C29 C28 110.7(2) . . ? C34 C29 C30 109.4(2) . . ? C28 C29 C30 108.6(2) . . ? C25 C30 C29 109.4(2) . . ? C32 C31 C25 109.0(2) . . ? C33 C32 C34 109.3(2) . . ? C33 C32 C31 109.7(2) . . ? C34 C32 C31 109.6(2) . . ? C32 C33 C27 109.9(2) . . ? C29 C34 C32 110.3(2) . . ? N2B Li1B N1B 105.9(2) . . ? N2B Li1B N3B 136.2(2) . . ? N1B Li1B N3B 117.5(2) . . ? N2B Li2B N1B 105.19(19) . . ? N2B Li2B N4B 114.8(2) . . ? N1B Li2B N4B 140.0(2) . . ? Si1B N1B Si2B 122.28(12) . . ? Si1B N1B Li1B 118.37(16) . . ? Si2B N1B Li1B 106.93(16) . . ? Si1B N1B Li2B 105.52(16) . . ? Si2B N1B Li2B 120.32(16) . . ? Li1B N1B Li2B 74.28(18) . . ? Si3B N2B Si4B 124.02(12) . . ? Si3B N2B Li1B 106.82(16) . . ? Si4B N2B Li1B 116.56(16) . . ? Si3B N2B Li2B 117.00(16) . . ? Si4B N2B Li2B 107.57(16) . . ? Li1B N2B Li2B 74.65(18) . . ? C13B N3B Li1B 155.7(3) . . ? C24B N4B Li2B 154.5(2) . . ? N1B Si1B C2B 114.00(11) . . ? N1B Si1B C1B 115.22(11) . . ? C2B Si1B C1B 104.85(13) . . ? N1B Si1B C3B 110.27(11) . . ? C2B Si1B C3B 106.40(13) . . ? C1B Si1B C3B 105.37(12) . . ? N1B Si2B C6B 110.73(12) . . ? N1B Si2B C5B 115.53(12) . . ? C6B Si2B C5B 103.74(14) . . ? N1B Si2B C4B 112.25(12) . . ? C6B Si2B C4B 106.95(13) . . ? C5B Si2B C4B 106.98(14) . . ? N2B Si3B C7B 113.43(12) . . ? N2B Si3B C8B 110.70(12) . . ? C7B Si3B C8B 106.27(15) . . ? N2B Si3B C9B 115.61(12) . . ? C7B Si3B C9B 105.64(15) . . ? C8B Si3B C9B 104.38(14) . . ? N2B Si4B C12B 111.18(12) . . ? N2B Si4B C10B 115.91(13) . . ? C12B Si4B C10B 104.27(14) . . ? N2B Si4B C11B 112.45(13) . . ? C12B Si4B C11B 106.40(14) . . ? C10B Si4B C11B 105.88(15) . . ? N3B C13B C14B 177.5(3) . . ? C13B C14B C20B 109.4(2) . . ? C13B C14B C15B 110.6(2) . . ? C20B C14B C15B 109.3(2) . . ? C13B C14B C19B 108.9(2) . . ? C20B C14B C19B 109.5(2) . . ? C15B C14B C19B 109.1(2) . . ? C16B C15B C14B 109.3(2) . . ? C15B C16B C17B 109.7(2) . . ? C15B C16B C22B 109.4(2) . . ? C17B C16B C22B 109.9(2) . . ? C18B C17B C16B 109.3(2) . . ? C23B C18B C17B 110.0(2) . . ? C23B C18B C19B 109.5(2) . . ? C17B C18B C19B 109.8(2) . . ? C18B C19B C14B 109.0(2) . . ? C21B C20B C14B 108.9(2) . . ? C23B C21B C20B 109.6(2) . . ? C23B C21B C22B 109.9(2) . . ? C20B C21B C22B 109.4(2) . . ? C16B C22B C21B 109.4(2) . . ? C18B C23B C21B 109.5(2) . . ? N4B C24B C25B 177.5(3) . . ? C24B C25B C30B 112.6(3) . . ? C24B C25B C26B 109.1(3) . . ? C30B C25B C26B 108.8(3) . . ? C24B C25B C28B 109.8(3) . . ? C30B C25B C28B 109.2(3) . . ? C26B C25B C28B 107.2(3) . . ? C27B C26B C25B 111.2(4) . . ? C34B C27B C32B 106.4(6) . . ? C34B C27B C26B 108.7(6) . . ? C32B C27B C26B 107.8(6) . . ? C29B C28B C25B 110.0(4) . . ? C34B C29B C28B 111.6(7) . . ? C34B C29B C33B 108.3(6) . . ? C28B C29B C33B 104.9(6) . . ? C25B C30B C31B 111.7(4) . . ? C32B C31B C33B 110.8(7) . . ? C32B C31B C30B 108.4(7) . . ? C33B C31B C30B 93.8(6) . . ? C31B C32B C27B 120.2(7) . . ? C29B C33B C31B 112.3(6) . . ? C29B C34B C27B 115.3(7) . . ? C34C C27C C26C 106.8(6) . . ? C34C C27C C32C 108.0(6) . . ? C26C C27C C32C 98.7(6) . . ? C34C C29C C28C 106.3(7) . . ? C34C C29C C33C 107.4(6) . . ? C28C C29C C33C 104.4(6) . . ? C32C C31C C33C 115.9(8) . . ? C32C C31C C30C 102.0(7) . . ? C33C C31C C30C 108.0(7) . . ? C31C C32C C27C 120.3(7) . . ? C31C C33C C29C 114.2(6) . . ? C29C C34C C27C 116.4(7) . . ? #===END #===END data_(4b)-jul1705 _database_code_depnum_ccdc_archive 'CCDC 283660' _audit_creation_date 2005-07-19T14:26:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C66 H84 N6 Na6' _chemical_formula_sum 'C66 H84 N6 Na6' _chemical_formula_weight 1099.33 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8309(5) _cell_length_b 12.2435(5) _cell_length_c 12.8840(6) _cell_angle_alpha 99.552(2) _cell_angle_beta 106.080(2) _cell_angle_gamma 108.896(2) _cell_volume 1628.15(12) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34411 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_diffrn 1.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.1 _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_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.949425E-1 _diffrn_orient_matrix_ub_12 -0.389631E-1 _diffrn_orient_matrix_ub_13 -0.224882E-1 _diffrn_orient_matrix_ub_21 0.95638E-2 _diffrn_orient_matrix_ub_22 -0.621321E-1 _diffrn_orient_matrix_ub_23 0.39318E-1 _diffrn_orient_matrix_ub_31 0.47868E-2 _diffrn_orient_matrix_ub_32 0.520959E-1 _diffrn_orient_matrix_ub_33 0.709465E-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 0.0518 _diffrn_reflns_av_unetI/netI 0.0367 _diffrn_reflns_number 21553 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.4 _diffrn_reflns_theta_max 26.13 _diffrn_reflns_theta_full 26.13 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 6343 _reflns_number_gt 5254 _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-86 (Sheldrick, 1986)' _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 ; 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^)+(0.0570P)^2^+0.6126P] 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 6343 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.252 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.038 #----------------------------------------------------------------------------# # 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' 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 Na1 Na 0.56865(6) 0.57809(6) 0.36694(6) 0.03950(18) Uani 1 1 d . . . Na2 Na 0.64390(6) 0.39760(6) 0.48099(5) 0.03703(18) Uani 1 1 d . . . Na3 Na 0.71131(6) 0.60965(6) 0.68571(5) 0.03459(17) Uani 1 1 d . . . N1 N 0.48285(13) 0.36114(13) 0.31002(11) 0.0340(3) Uani 1 1 d . . . N2 N 0.75305(12) 0.60549(13) 0.51309(12) 0.0345(3) Uani 1 1 d . . . N3 N 0.62855(13) 0.39827(12) 0.65618(12) 0.0344(3) Uani 1 1 d . . . C1 C 0.44901(14) 0.28887(14) 0.21554(13) 0.0301(3) Uani 1 1 d . . . C2 C 0.34873(15) 0.29548(14) 0.11470(13) 0.0302(3) Uani 1 1 d . . . C3 C 0.38399(17) 0.37222(17) 0.05025(15) 0.0414(4) Uani 1 1 d . . . H3 H 0.472 0.4152 0.0645 0.05 Uiso 1 1 calc R . . C4 C 0.2930(2) 0.3868(2) -0.03401(17) 0.0505(5) Uani 1 1 d . . . H4 H 0.3191 0.4393 -0.0771 0.061 Uiso 1 1 calc R . . C5 C 0.16461(19) 0.3257(2) -0.05601(16) 0.0487(5) Uani 1 1 d . . . H5 H 0.1023 0.3354 -0.1144 0.058 Uiso 1 1 calc R . . C6 C 0.12760(17) 0.25056(18) 0.00740(15) 0.0441(4) Uani 1 1 d . . . H6 H 0.0393 0.2093 -0.0065 0.053 Uiso 1 1 calc R . . C7 C 0.21817(16) 0.23470(16) 0.09131(14) 0.0364(4) Uani 1 1 d . . . H7 H 0.1911 0.1816 0.1337 0.044 Uiso 1 1 calc R . . C8 C 0.50002(19) 0.18937(17) 0.18759(15) 0.0434(4) Uani 1 1 d . . . C9 C 0.3914(3) 0.0666(2) 0.1434(3) 0.0979(11) Uani 1 1 d . . . H9A H 0.3257 0.0642 0.0761 0.147 Uiso 1 1 calc R . . H9B H 0.3544 0.0511 0.2013 0.147 Uiso 1 1 calc R . . H9C H 0.424 0.0049 0.1241 0.147 Uiso 1 1 calc R . . C10 C 0.6037(3) 0.1954(2) 0.2916(2) 0.0773(8) Uani 1 1 d . . . H10A H 0.6738 0.2748 0.3181 0.116 Uiso 1 1 calc R . . H10B H 0.636 0.1332 0.2729 0.116 Uiso 1 1 calc R . . H10C H 0.5683 0.1819 0.3509 0.116 Uiso 1 1 calc R . . C11 C 0.5624(3) 0.2106(3) 0.0993(2) 0.0838(9) Uani 1 1 d . . . H11A H 0.6322 0.2904 0.1275 0.126 Uiso 1 1 calc R . . H11B H 0.4986 0.2062 0.0296 0.126 Uiso 1 1 calc R . . H11C H 0.5964 0.149 0.0842 0.126 Uiso 1 1 calc R . . C12 C 0.86347(14) 0.67844(14) 0.52939(13) 0.0299(3) Uani 1 1 d . . . C13 C 0.94011(14) 0.77499(15) 0.64207(14) 0.0328(4) Uani 1 1 d . . . C14 C 1.02510(16) 0.75655(17) 0.72998(15) 0.0402(4) Uani 1 1 d . . . H14 H 1.0402 0.6847 0.7183 0.048 Uiso 1 1 calc R . . C15 C 1.08795(18) 0.8419(2) 0.83443(16) 0.0516(5) Uani 1 1 d . . . H15 H 1.1456 0.8279 0.8933 0.062 Uiso 1 1 calc R . . C16 C 1.0671(2) 0.94678(19) 0.85308(18) 0.0545(5) Uani 1 1 d . . . H16 H 1.1104 1.0052 0.9244 0.065 Uiso 1 1 calc R . . C17 C 0.9833(2) 0.96609(18) 0.76767(18) 0.0528(5) Uani 1 1 d . . . H17 H 0.9684 1.0381 0.7801 0.063 Uiso 1 1 calc R . . C18 C 0.92010(17) 0.88104(16) 0.66316(16) 0.0425(4) Uani 1 1 d . . . H18 H 0.8621 0.8956 0.605 0.051 Uiso 1 1 calc R . . C19 C 0.93256(15) 0.68297(16) 0.44207(14) 0.0355(4) Uani 1 1 d . . . C20 C 0.9535(2) 0.8011(2) 0.41035(18) 0.0507(5) Uani 1 1 d . . . H20A H 0.8709 0.8068 0.3783 0.076 Uiso 1 1 calc R . . H20B H 0.9957 0.8033 0.3547 0.076 Uiso 1 1 calc R . . H20C H 1.0074 0.869 0.4777 0.076 Uiso 1 1 calc R . . C21 C 0.8527(2) 0.5765(2) 0.33728(16) 0.0563(5) Uani 1 1 d . . . H21A H 0.7686 0.5788 0.3042 0.084 Uiso 1 1 calc R . . H21B H 0.8425 0.5013 0.3579 0.084 Uiso 1 1 calc R . . H21C H 0.8959 0.5812 0.2823 0.084 Uiso 1 1 calc R . . C22 C 1.06338(17) 0.67722(19) 0.49255(17) 0.0446(4) Uani 1 1 d . . . H22A H 1.0519 0.6019 0.5132 0.067 Uiso 1 1 calc R . . H22B H 1.1161 0.7455 0.5598 0.067 Uiso 1 1 calc R . . H22C H 1.1057 0.6807 0.437 0.067 Uiso 1 1 calc R . . C23 C 0.63375(15) 0.32678(14) 0.71470(13) 0.0292(3) Uani 1 1 d . . . C24 C 0.51033(15) 0.22674(14) 0.70560(14) 0.0319(3) Uani 1 1 d . . . C25 C 0.45230(16) 0.23475(16) 0.78508(15) 0.0387(4) Uani 1 1 d . . . H25 H 0.4939 0.301 0.851 0.046 Uiso 1 1 calc R . . C26 C 0.33408(18) 0.14754(18) 0.77012(18) 0.0474(5) Uani 1 1 d . . . H26 H 0.2958 0.1552 0.8253 0.057 Uiso 1 1 calc R . . C27 C 0.27284(18) 0.05052(17) 0.67557(19) 0.0498(5) Uani 1 1 d . . . H27 H 0.1932 -0.0098 0.6659 0.06 Uiso 1 1 calc R . . C28 C 0.32786(19) 0.04169(18) 0.59511(19) 0.0530(5) Uani 1 1 d . . . H28 H 0.2853 -0.0243 0.529 0.064 Uiso 1 1 calc R . . C29 C 0.44548(18) 0.12881(16) 0.60990(16) 0.0445(4) Uani 1 1 d . . . H29 H 0.4822 0.1213 0.5536 0.053 Uiso 1 1 calc R . . C30 C 0.75949(16) 0.32580(16) 0.79498(15) 0.0359(4) Uani 1 1 d . . . C31 C 0.87241(17) 0.44041(18) 0.80987(18) 0.0462(5) Uani 1 1 d . . . H31A H 0.8768 0.4462 0.736 0.069 Uiso 1 1 calc R . . H31B H 0.9519 0.4377 0.8565 0.069 Uiso 1 1 calc R . . H31C H 0.8608 0.5107 0.8466 0.069 Uiso 1 1 calc R . . C32 C 0.77778(19) 0.21465(18) 0.7403(2) 0.0515(5) Uani 1 1 d . . . H32A H 0.7053 0.1419 0.7314 0.077 Uiso 1 1 calc R . . H32B H 0.8569 0.2125 0.7882 0.077 Uiso 1 1 calc R . . H32C H 0.7828 0.2186 0.6662 0.077 Uiso 1 1 calc R . . C33 C 0.75399(19) 0.3182(2) 0.91100(16) 0.0509(5) Uani 1 1 d . . . H33A H 0.6817 0.2453 0.9024 0.076 Uiso 1 1 calc R . . H33B H 0.7431 0.389 0.9476 0.076 Uiso 1 1 calc R . . H33C H 0.8336 0.3154 0.9573 0.076 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 Na1 0.0262(3) 0.0395(4) 0.0460(4) 0.0154(3) 0.0077(3) 0.0071(3) Na2 0.0371(4) 0.0360(4) 0.0287(3) 0.0069(3) 0.0058(3) 0.0089(3) Na3 0.0291(3) 0.0337(4) 0.0326(3) 0.0048(3) 0.0110(3) 0.0040(3) N1 0.0283(7) 0.0355(7) 0.0314(7) 0.0063(6) 0.0072(6) 0.0084(6) N2 0.0249(7) 0.0371(8) 0.0348(7) 0.0118(6) 0.0081(6) 0.0049(6) N3 0.0347(7) 0.0347(8) 0.0331(7) 0.0129(6) 0.0118(6) 0.0111(6) C1 0.0241(8) 0.0299(8) 0.0311(8) 0.0084(7) 0.0076(6) 0.0057(6) C2 0.0275(8) 0.0303(8) 0.0278(8) 0.0025(6) 0.0070(6) 0.0099(7) C3 0.0325(9) 0.0498(11) 0.0426(10) 0.0188(8) 0.0131(8) 0.0143(8) C4 0.0517(12) 0.0622(13) 0.0476(11) 0.0293(10) 0.0191(9) 0.0264(10) C5 0.0426(11) 0.0665(13) 0.0389(10) 0.0152(9) 0.0071(8) 0.0297(10) C6 0.0274(9) 0.0547(11) 0.0383(10) 0.0023(8) 0.0047(7) 0.0126(8) C7 0.0300(8) 0.0377(9) 0.0317(8) 0.0050(7) 0.0072(7) 0.0065(7) C8 0.0474(11) 0.0418(10) 0.0377(9) 0.0054(8) 0.0064(8) 0.0234(9) C9 0.0816(19) 0.0338(12) 0.156(3) 0.0001(15) 0.025(2) 0.0219(13) C10 0.102(2) 0.0798(17) 0.0551(14) 0.0095(12) 0.0029(13) 0.0670(17) C11 0.102(2) 0.120(2) 0.0765(17) 0.0347(17) 0.0488(16) 0.084(2) C12 0.0252(8) 0.0313(8) 0.0307(8) 0.0138(7) 0.0071(6) 0.0080(7) C13 0.0225(7) 0.0335(9) 0.0357(9) 0.0126(7) 0.0103(7) 0.0012(7) C14 0.0335(9) 0.0434(10) 0.0370(9) 0.0128(8) 0.0085(7) 0.0091(8) C15 0.0358(10) 0.0657(14) 0.0360(10) 0.0114(9) 0.0035(8) 0.0075(9) C16 0.0458(11) 0.0472(12) 0.0444(11) -0.0011(9) 0.0116(9) -0.0035(9) C17 0.0566(12) 0.0346(10) 0.0574(13) 0.0065(9) 0.0229(10) 0.0065(9) C18 0.0386(10) 0.0377(10) 0.0450(10) 0.0126(8) 0.0121(8) 0.0089(8) C19 0.0277(8) 0.0428(10) 0.0359(9) 0.0174(7) 0.0122(7) 0.0097(7) C20 0.0494(11) 0.0647(13) 0.0618(13) 0.0424(11) 0.0318(10) 0.0295(10) C21 0.0462(11) 0.0704(14) 0.0378(10) 0.0063(10) 0.0174(9) 0.0070(10) C22 0.0385(10) 0.0548(12) 0.0514(11) 0.0238(9) 0.0213(9) 0.0227(9) C23 0.0291(8) 0.0298(8) 0.0297(8) 0.0072(7) 0.0124(6) 0.0116(7) C24 0.0294(8) 0.0297(8) 0.0375(9) 0.0143(7) 0.0099(7) 0.0118(7) C25 0.0306(9) 0.0408(10) 0.0437(10) 0.0138(8) 0.0140(7) 0.0108(7) C26 0.0351(10) 0.0523(12) 0.0627(13) 0.0266(10) 0.0236(9) 0.0165(9) C27 0.0307(9) 0.0398(10) 0.0764(14) 0.0258(10) 0.0140(9) 0.0099(8) C28 0.0436(11) 0.0344(10) 0.0615(13) 0.0059(9) 0.0059(10) 0.0055(9) C29 0.0441(10) 0.0375(10) 0.0455(10) 0.0084(8) 0.0145(8) 0.0106(8) C30 0.0284(8) 0.0386(9) 0.0442(10) 0.0170(8) 0.0134(7) 0.0145(7) C31 0.0275(9) 0.0463(11) 0.0614(12) 0.0179(9) 0.0121(8) 0.0121(8) C32 0.0434(11) 0.0453(11) 0.0798(15) 0.0243(10) 0.0287(10) 0.0255(9) C33 0.0402(10) 0.0690(13) 0.0445(11) 0.0266(10) 0.0088(8) 0.0225(10) #----------------------------------------------------------------------------# # 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 Na1 N2 2.3362(15) . ? Na1 N3 2.3868(15) 2_666 ? Na1 N1 2.4122(15) . ? Na1 Na2 3.0761(10) . ? Na1 Na3 3.1656(9) 2_666 ? Na2 N3 2.3129(15) . ? Na2 N1 2.3409(15) . ? Na2 N2 2.3544(15) . ? Na2 Na3 3.0909(9) . ? Na3 N3 2.3721(15) . ? Na3 N2 2.4041(15) . ? Na3 N1 2.4503(15) 2_666 ? Na3 Na1 3.1656(9) 2_666 ? N1 C1 1.252(2) . ? N1 Na3 2.4503(15) 2_666 ? N2 C12 1.256(2) . ? N3 C23 1.252(2) . ? N3 Na1 2.3868(15) 2_666 ? C1 C2 1.531(2) . ? C1 C8 1.559(2) . ? C2 C3 1.394(2) . ? C2 C7 1.398(2) . ? C3 C4 1.382(3) . ? C3 H3 0.95 . ? C4 C5 1.380(3) . ? C4 H4 0.95 . ? C5 C6 1.376(3) . ? C5 H5 0.95 . ? C6 C7 1.385(2) . ? C6 H6 0.95 . ? C7 H7 0.95 . ? C8 C9 1.515(3) . ? C8 C10 1.518(3) . ? C8 C11 1.532(3) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C13 1.528(2) . ? C12 C19 1.561(2) . ? C13 C18 1.390(3) . ? C13 C14 1.395(2) . ? C14 C15 1.390(3) . ? C14 H14 0.95 . ? C15 C16 1.380(3) . ? C15 H15 0.95 . ? C16 C17 1.373(3) . ? C16 H16 0.95 . ? C17 C18 1.389(3) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? C19 C21 1.525(3) . ? C19 C20 1.530(3) . ? C19 C22 1.533(2) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C24 1.531(2) . ? C23 C30 1.564(2) . ? C24 C25 1.389(2) . ? C24 C29 1.391(2) . ? C25 C26 1.396(2) . ? C25 H25 0.95 . ? C26 C27 1.376(3) . ? C26 H26 0.95 . ? C27 C28 1.376(3) . ? C27 H27 0.95 . ? C28 C29 1.391(3) . ? C28 H28 0.95 . ? C29 H29 0.95 . ? C30 C33 1.531(3) . ? C30 C31 1.531(2) . ? C30 C32 1.534(3) . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? 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 N2 Na1 N3 138.59(6) . 2_666 ? N2 Na1 N1 96.69(5) . . ? N3 Na1 N1 97.46(5) 2_666 . ? N2 Na1 Na2 49.28(4) . . ? N3 Na1 Na2 123.61(4) 2_666 . ? N1 Na1 Na2 48.67(4) . . ? N2 Na1 Na3 126.48(4) . 2_666 ? N3 Na1 Na3 48.10(4) 2_666 2_666 ? N1 Na1 Na3 49.91(4) . 2_666 ? Na2 Na1 Na3 82.60(2) . 2_666 ? N3 Na2 N1 128.91(6) . . ? N3 Na2 N2 99.24(5) . . ? N1 Na2 N2 98.17(5) . . ? N3 Na2 Na1 118.07(4) . . ? N1 Na2 Na1 50.69(4) . . ? N2 Na2 Na1 48.76(4) . . ? N3 Na2 Na3 49.55(4) . . ? N1 Na2 Na3 121.20(4) . . ? N2 Na2 Na3 50.20(4) . . ? Na1 Na2 Na3 78.04(2) . . ? N3 Na3 N2 96.21(5) . . ? N3 Na3 N1 96.82(5) . 2_666 ? N2 Na3 N1 116.84(5) . 2_666 ? N3 Na3 Na2 47.90(4) . . ? N2 Na3 Na2 48.79(4) . . ? N1 Na3 Na2 109.81(4) 2_666 . ? N3 Na3 Na1 48.50(4) . 2_666 ? N2 Na3 Na1 109.16(4) . 2_666 ? N1 Na3 Na1 48.86(4) 2_666 2_666 ? Na2 Na3 Na1 71.21(2) . 2_666 ? C1 N1 Na2 131.31(12) . . ? C1 N1 Na1 130.12(12) . . ? Na2 N1 Na1 80.64(5) . . ? C1 N1 Na3 104.41(10) . 2_666 ? Na2 N1 Na3 118.61(6) . 2_666 ? Na1 N1 Na3 81.24(5) . 2_666 ? C12 N2 Na1 124.75(11) . . ? C12 N2 Na2 138.70(12) . . ? Na1 N2 Na2 81.96(5) . . ? C12 N2 Na3 111.74(11) . . ? Na1 N2 Na3 109.98(6) . . ? Na2 N2 Na3 81.01(5) . . ? C23 N3 Na2 132.56(11) . . ? C23 N3 Na3 137.01(12) . . ? Na2 N3 Na3 82.55(5) . . ? C23 N3 Na1 107.05(11) . 2_666 ? Na2 N3 Na1 101.62(6) . 2_666 ? Na3 N3 Na1 83.39(5) . 2_666 ? N1 C1 C2 119.25(14) . . ? N1 C1 C8 126.25(15) . . ? C2 C1 C8 114.50(13) . . ? C3 C2 C7 117.47(15) . . ? C3 C2 C1 121.05(14) . . ? C7 C2 C1 121.14(15) . . ? C4 C3 C2 121.11(17) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 120.52(18) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 119.37(17) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 120.42(17) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C2 121.10(17) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C9 C8 C10 110.6(2) . . ? C9 C8 C11 109.4(2) . . ? C10 C8 C11 106.3(2) . . ? C9 C8 C1 110.08(17) . . ? C10 C8 C1 110.07(15) . . ? C11 C8 C1 110.29(16) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 119.61(14) . . ? N2 C12 C19 125.73(15) . . ? C13 C12 C19 114.64(13) . . ? C18 C13 C14 117.60(16) . . ? C18 C13 C12 120.71(15) . . ? C14 C13 C12 121.51(15) . . ? C15 C14 C13 120.92(18) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 120.39(19) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.45(19) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.4(2) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 121.24(18) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? C21 C19 C20 110.02(16) . . ? C21 C19 C22 108.51(16) . . ? C20 C19 C22 108.22(15) . . ? C21 C19 C12 110.08(14) . . ? C20 C19 C12 109.54(15) . . ? C22 C19 C12 110.44(13) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 C24 119.63(14) . . ? N3 C23 C30 125.15(14) . . ? C24 C23 C30 115.14(13) . . ? C25 C24 C29 117.37(16) . . ? C25 C24 C23 122.35(15) . . ? C29 C24 C23 119.98(15) . . ? C24 C25 C26 121.39(17) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C27 C26 C25 120.11(18) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 119.43(18) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 120.43(19) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C24 121.26(18) . . ? C28 C29 H29 119.4 . . ? C24 C29 H29 119.4 . . ? C33 C30 C31 108.81(16) . . ? C33 C30 C32 108.34(16) . . ? C31 C30 C32 110.13(15) . . ? C33 C30 C23 112.51(14) . . ? C31 C30 C23 109.41(14) . . ? C32 C30 C23 107.62(15) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ?