Supplementary information (ESI) for Dalton Trans. This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_name 'M. F. Lappert' _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK loop_ _publ_author_name M.F.Lappert P.B.Hitchcock L.Bourget-Merle P.G.Merle data_(1)-mar4200 _database_code_depnum_ccdc_archive 'CCDC 668981' _audit_creation_date 2000-03-31T09:46:11-00:00 _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 mar4200 _chemical_formula_moiety 'C36 H68 Li2 N2 Si4' _chemical_formula_structural 'C36 H68 LI2 N2 SI4' _chemical_formula_sum 'C36 H68 Li2 N2 Si4' _chemical_formula_weight 655.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.9148(5) _cell_length_b 12.7201(3) _cell_length_c 19.5483(5) _cell_angle_alpha 90 _cell_angle_beta 115.9990(10) _cell_angle_gamma 90 _cell_volume 4003.83(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 27721 _cell_measurement_theta_min 1.018 _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 0.2 _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.174 _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_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 36327 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.8 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 9493 _reflns_number_gt 7317 _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 hydrogen atoms on C2 and C20 were refined; other H atoms were in riding mode. 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^)+(0.0512P)^2^+2.6140P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9493 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.458 _refine_diff_density_min -0.313 _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 0.1974(2) 0.7214(3) -0.0189(2) 0.0333(7) Uani 1 1 d . . . Li2 Li 0.2995(2) 0.8421(3) -0.0195(2) 0.0378(8) Uani 1 1 d . . . Si1 Si 0.33968(4) 0.63727(5) -0.08096(3) 0.03309(14) Uani 1 1 d . . . Si2 Si 0.20420(4) 0.46818(4) 0.08319(3) 0.03121(14) Uani 1 1 d . . . Si3 Si 0.17194(3) 0.93567(4) 0.05016(3) 0.02726(13) Uani 1 1 d . . . Si4 Si 0.30313(4) 1.05348(5) -0.06929(3) 0.03359(14) Uani 1 1 d . . . N1 N 0.30805(10) 0.68608(13) -0.01656(9) 0.0287(4) Uani 1 1 d . . . N2 N 0.19240(10) 0.87887(12) -0.01883(9) 0.0263(3) Uani 1 1 d . . . C1 C 0.30933(12) 0.62695(14) 0.04452(11) 0.0262(4) Uani 1 1 d . . . C2 C 0.24295(13) 0.56366(15) 0.03333(11) 0.0297(4) Uani 1 1 d . . . H2 H 0.2048(15) 0.5555(18) -0.0194(14) 0.039(6) Uiso 1 1 d . . . C3 C 0.32385(18) 0.4923(2) -0.09497(17) 0.0568(7) Uani 1 1 d . . . H3C H 0.2646 0.4761 -0.1144 0.085 Uiso 1 1 calc R . . H3B H 0.3547 0.4564 -0.0462 0.085 Uiso 1 1 calc R . . H3A H 0.3439 0.4683 -0.1316 0.085 Uiso 1 1 calc R . . C4 C 0.45207(15) 0.6644(2) -0.05464(14) 0.0473(6) Uani 1 1 d . . . H4C H 0.487 0.6265 -0.0078 0.071 Uiso 1 1 calc R . . H4B H 0.4627 0.7401 -0.0465 0.071 Uiso 1 1 calc R . . H4A H 0.4652 0.6409 -0.0959 0.071 Uiso 1 1 calc R . . C5 C 0.28066(18) 0.7041(2) -0.17452(14) 0.0569(7) Uani 1 1 d . . . H5C H 0.3011 0.6797 -0.2108 0.085 Uiso 1 1 calc R . . H5B H 0.2884 0.7803 -0.1679 0.085 Uiso 1 1 calc R . . H5A H 0.2215 0.6872 -0.194 0.085 Uiso 1 1 calc R . . C6 C 0.11489(17) 0.4026(2) 0.00315(15) 0.0543(7) Uani 1 1 d . . . H6C H 0.0731 0.4554 -0.0257 0.081 Uiso 1 1 calc R . . H6B H 0.0902 0.3502 0.0238 0.081 Uiso 1 1 calc R . . H6A H 0.1347 0.3678 -0.0305 0.081 Uiso 1 1 calc R . . C7 C 0.16192(15) 0.5296(2) 0.14571(14) 0.0446(6) Uani 1 1 d . . . H7C H 0.2054 0.5717 0.1852 0.067 Uiso 1 1 calc R . . H7B H 0.1433 0.4745 0.1697 0.067 Uiso 1 1 calc R . . H7A H 0.1149 0.5751 0.1151 0.067 Uiso 1 1 calc R . . C8 C 0.27850(15) 0.36091(17) 0.13685(13) 0.0409(5) Uani 1 1 d . . . H8C H 0.2921 0.3194 0.1016 0.061 Uiso 1 1 calc R . . H8B H 0.2529 0.3153 0.1611 0.061 Uiso 1 1 calc R . . H8A H 0.3294 0.3919 0.176 0.061 Uiso 1 1 calc R . . C9 C 0.38521(12) 0.63988(14) 0.12253(11) 0.0266(4) Uani 1 1 d . . . C10 C 0.43165(13) 0.74348(15) 0.12757(11) 0.0290(4) Uani 1 1 d . . . H10B H 0.4476 0.7469 0.0851 0.035 Uiso 1 1 calc R . . H10A H 0.3942 0.8034 0.1221 0.035 Uiso 1 1 calc R . . C11 C 0.50972(13) 0.75329(15) 0.20329(12) 0.0315(4) Uani 1 1 d . . . H11 H 0.5381 0.8214 0.2044 0.038 Uiso 1 1 calc R . . C12 C 0.56850(13) 0.66225(16) 0.21063(13) 0.0344(5) Uani 1 1 d . . . H12B H 0.6194 0.6681 0.2592 0.041 Uiso 1 1 calc R . . H12A H 0.5848 0.6647 0.1684 0.041 Uiso 1 1 calc R . . C13 C 0.52421(13) 0.55819(15) 0.20829(12) 0.0324(4) Uani 1 1 d . . . H13 H 0.5626 0.4984 0.2138 0.039 Uiso 1 1 calc R . . C14 C 0.49959(14) 0.55546(17) 0.27403(12) 0.0364(5) Uani 1 1 d . . . H14B H 0.5499 0.5613 0.3231 0.044 Uiso 1 1 calc R . . H14A H 0.472 0.4878 0.2735 0.044 Uiso 1 1 calc R . . C15 C 0.44027(13) 0.64689(16) 0.26593(11) 0.0326(4) Uani 1 1 d . . . H15 H 0.4239 0.6444 0.3087 0.039 Uiso 1 1 calc R . . C16 C 0.36237(13) 0.63705(16) 0.18975(11) 0.0304(4) Uani 1 1 d . . . H16B H 0.3238 0.6955 0.1847 0.036 Uiso 1 1 calc R . . H16A H 0.3337 0.5702 0.1887 0.036 Uiso 1 1 calc R . . C17 C 0.44639(12) 0.54812(15) 0.13230(11) 0.0290(4) Uani 1 1 d . . . H17B H 0.4187 0.4802 0.1306 0.035 Uiso 1 1 calc R . . H17A H 0.4625 0.5492 0.0899 0.035 Uiso 1 1 calc R . . C18 C 0.48464(14) 0.75090(16) 0.26890(12) 0.0347(5) Uani 1 1 d . . . H18A H 0.5346 0.7573 0.3182 0.042 Uiso 1 1 calc R . . H18B H 0.4472 0.8106 0.2642 0.042 Uiso 1 1 calc R . . C19 C 0.16463(12) 0.90771(15) -0.09501(11) 0.0266(4) Uani 1 1 d . . . C20 C 0.21024(14) 0.96940(17) -0.11928(12) 0.0339(4) Uani 1 1 d . . . H20 H 0.1900(15) 0.9754(19) -0.1729(14) 0.043(7) Uiso 1 1 d . . . C21 C 0.11383(14) 1.06292(17) 0.01956(13) 0.0379(5) Uani 1 1 d . . . H21C H 0.0586 1.0496 -0.0218 0.057 Uiso 1 1 calc R . . H21B H 0.1443 1.1109 0.0017 0.057 Uiso 1 1 calc R . . H21A H 0.1082 1.0947 0.0627 0.057 Uiso 1 1 calc R . . C22 C 0.26995(14) 0.9659(2) 0.13786(13) 0.0465(6) Uani 1 1 d . . . H22C H 0.3023 1.0185 0.1257 0.07 Uiso 1 1 calc R . . H22B H 0.3028 0.9016 0.1561 0.07 Uiso 1 1 calc R . . H22A H 0.2558 0.9936 0.1775 0.07 Uiso 1 1 calc R . . C23 C 0.11432(15) 0.8425(2) 0.08432(14) 0.0444(6) Uani 1 1 d . . . H23C H 0.1087 0.8737 0.1277 0.067 Uiso 1 1 calc R . . H23B H 0.1451 0.7762 0.1 0.067 Uiso 1 1 calc R . . H23A H 0.059 0.829 0.0431 0.067 Uiso 1 1 calc R . . C24 C 0.28437(18) 1.1736(2) -0.02479(18) 0.0578(7) Uani 1 1 d . . . H24C H 0.2423 1.2172 -0.0641 0.087 Uiso 1 1 calc R . . H24B H 0.3362 1.2135 0.0003 0.087 Uiso 1 1 calc R . . H24A H 0.2648 1.1533 0.0129 0.087 Uiso 1 1 calc R . . C25 C 0.39433(14) 0.98337(19) 0.00674(14) 0.0438(5) Uani 1 1 d . . . H25C H 0.3785 0.9559 0.0454 0.066 Uiso 1 1 calc R . . H25B H 0.4407 1.0326 0.0305 0.066 Uiso 1 1 calc R . . H25A H 0.4112 0.925 -0.0161 0.066 Uiso 1 1 calc R . . C26 C 0.33711(18) 1.0952(2) -0.14285(16) 0.0563(7) Uani 1 1 d . . . H26C H 0.3507 1.0329 -0.1647 0.084 Uiso 1 1 calc R . . H26B H 0.3863 1.1402 -0.1193 0.084 Uiso 1 1 calc R . . H26A H 0.2922 1.1343 -0.1832 0.084 Uiso 1 1 calc R . . C27 C 0.08078(12) 0.85919(15) -0.15329(11) 0.0277(4) Uani 1 1 d . . . C28 C 0.07286(13) 0.74200(16) -0.13598(12) 0.0315(4) Uani 1 1 d . . . H28B H 0.1187 0.7016 -0.1387 0.038 Uiso 1 1 calc R . . H28A H 0.0781 0.7355 -0.0836 0.038 Uiso 1 1 calc R . . C29 C -0.01039(14) 0.69528(17) -0.19221(13) 0.0391(5) Uani 1 1 d . . . H29 H -0.0131 0.6196 -0.1795 0.047 Uiso 1 1 calc R . . C30 C -0.08080(14) 0.75583(19) -0.18566(14) 0.0431(5) Uani 1 1 d . . . H30A H -0.1351 0.7261 -0.2214 0.052 Uiso 1 1 calc R . . H30B H -0.0758 0.7492 -0.1334 0.052 Uiso 1 1 calc R . . C31 C -0.07607(13) 0.87170(18) -0.20436(13) 0.0394(5) Uani 1 1 d . . . H31 H -0.1221 0.9114 -0.2002 0.047 Uiso 1 1 calc R . . C32 C -0.08529(15) 0.8799(2) -0.28599(14) 0.0469(6) Uani 1 1 d . . . H32B H -0.1394 0.8503 -0.322 0.056 Uiso 1 1 calc R . . H32A H -0.0835 0.9547 -0.2994 0.056 Uiso 1 1 calc R . . C33 C -0.01465(14) 0.8195(2) -0.29210(12) 0.0421(5) Uani 1 1 d . . . H33 H -0.0202 0.8254 -0.3451 0.05 Uiso 1 1 calc R . . C34 C 0.06849(13) 0.86674(18) -0.23632(11) 0.0350(5) Uani 1 1 d . . . H34B H 0.0708 0.9415 -0.2495 0.042 Uiso 1 1 calc R . . H34A H 0.1143 0.8292 -0.2412 0.042 Uiso 1 1 calc R . . C35 C 0.00783(13) 0.91743(16) -0.14801(12) 0.0336(4) Uani 1 1 d . . . H35B H 0.0131 0.9114 -0.0956 0.04 Uiso 1 1 calc R . . H35A H 0.0102 0.993 -0.1592 0.04 Uiso 1 1 calc R . . C36 C -0.01850(15) 0.70395(19) -0.27295(13) 0.0451(6) Uani 1 1 d . . . H36B H -0.0719 0.6731 -0.3094 0.054 Uiso 1 1 calc R . . H36A H 0.0271 0.6646 -0.277 0.054 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 Li1 0.0294(18) 0.0322(17) 0.0362(19) 0.0046(14) 0.0123(15) 0.0049(14) Li2 0.0338(19) 0.0342(18) 0.051(2) -0.0007(16) 0.0233(18) 0.0022(15) Si1 0.0362(3) 0.0381(3) 0.0286(3) 0.0011(2) 0.0176(3) 0.0088(2) Si2 0.0336(3) 0.0313(3) 0.0269(3) 0.0004(2) 0.0116(2) -0.0030(2) Si3 0.0257(3) 0.0315(3) 0.0252(3) -0.0012(2) 0.0117(2) 0.0036(2) Si4 0.0356(3) 0.0315(3) 0.0363(3) -0.0004(2) 0.0182(3) -0.0058(2) N1 0.0329(9) 0.0306(8) 0.0250(8) 0.0037(6) 0.0148(7) 0.0075(7) N2 0.0277(8) 0.0278(8) 0.0229(8) 0.0007(6) 0.0107(7) 0.0044(7) C1 0.0285(10) 0.0242(9) 0.0269(9) 0.0012(7) 0.0132(8) 0.0074(7) C2 0.0306(10) 0.0309(10) 0.0243(10) 0.0008(8) 0.0091(8) 0.0035(8) C3 0.0677(18) 0.0475(14) 0.0663(18) -0.0172(13) 0.0396(16) -0.0005(13) C4 0.0441(13) 0.0619(15) 0.0452(14) 0.0031(12) 0.0281(12) 0.0088(12) C5 0.0589(16) 0.085(2) 0.0334(13) 0.0131(13) 0.0263(12) 0.0266(15) C6 0.0504(15) 0.0590(16) 0.0411(14) 0.0001(12) 0.0085(12) -0.0187(13) C7 0.0454(13) 0.0472(13) 0.0513(14) 0.0014(11) 0.0303(12) -0.0013(11) C8 0.0494(14) 0.0312(11) 0.0388(12) 0.0039(9) 0.0165(11) 0.0009(10) C9 0.0276(10) 0.0249(9) 0.0277(10) 0.0022(7) 0.0126(8) 0.0050(8) C10 0.0331(10) 0.0234(9) 0.0324(10) 0.0035(8) 0.0162(9) 0.0046(8) C11 0.0358(11) 0.0240(9) 0.0345(11) -0.0010(8) 0.0152(9) -0.0023(8) C12 0.0291(10) 0.0333(10) 0.0375(11) -0.0005(9) 0.0116(9) 0.0005(9) C13 0.0302(10) 0.0261(10) 0.0338(11) 0.0023(8) 0.0075(9) 0.0062(8) C14 0.0387(12) 0.0332(11) 0.0287(10) 0.0066(8) 0.0066(9) -0.0009(9) C15 0.0369(11) 0.0362(11) 0.0241(10) -0.0003(8) 0.0127(9) -0.0027(9) C16 0.0314(10) 0.0310(10) 0.0287(10) -0.0002(8) 0.0132(9) -0.0003(8) C17 0.0295(10) 0.0243(9) 0.0318(10) 0.0004(8) 0.0122(8) 0.0031(8) C18 0.0392(12) 0.0312(10) 0.0310(11) -0.0044(8) 0.0129(9) 0.0004(9) C19 0.0281(10) 0.0252(9) 0.0262(9) 0.0006(7) 0.0116(8) 0.0048(8) C20 0.0367(11) 0.0353(11) 0.0286(11) 0.0017(8) 0.0134(9) -0.0035(9) C21 0.0399(12) 0.0335(11) 0.0433(12) -0.0019(9) 0.0210(11) 0.0078(9) C22 0.0356(12) 0.0662(16) 0.0330(12) -0.0132(11) 0.0107(10) 0.0061(11) C23 0.0448(13) 0.0493(14) 0.0487(14) 0.0108(11) 0.0294(12) 0.0073(11) C24 0.0571(17) 0.0409(13) 0.079(2) -0.0157(13) 0.0332(16) -0.0067(12) C25 0.0377(12) 0.0443(13) 0.0474(14) 0.0029(10) 0.0167(11) -0.0059(10) C26 0.0619(17) 0.0640(17) 0.0506(15) 0.0053(13) 0.0317(14) -0.0186(14) C27 0.0287(10) 0.0268(9) 0.0249(9) 0.0033(7) 0.0095(8) 0.0029(8) C28 0.0321(11) 0.0290(10) 0.0299(10) 0.0019(8) 0.0105(9) 0.0010(8) C29 0.0360(12) 0.0318(11) 0.0410(12) -0.0020(9) 0.0089(10) -0.0053(9) C30 0.0297(11) 0.0484(13) 0.0454(13) -0.0005(10) 0.0111(10) -0.0072(10) C31 0.0277(11) 0.0422(12) 0.0433(12) 0.0014(10) 0.0109(10) 0.0047(9) C32 0.0337(12) 0.0496(14) 0.0408(13) 0.0053(11) 0.0009(10) 0.0022(10) C33 0.0381(12) 0.0534(14) 0.0256(11) -0.0002(10) 0.0056(9) -0.0041(10) C34 0.0347(11) 0.0406(11) 0.0267(10) 0.0026(8) 0.0106(9) 0.0005(9) C35 0.0309(11) 0.0312(10) 0.0360(11) 0.0019(8) 0.0122(9) 0.0039(8) C36 0.0374(12) 0.0464(13) 0.0400(13) -0.0116(10) 0.0064(10) -0.0028(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 Li1 N2 2.005(4) . ? Li1 N1 2.012(4) . ? Li1 C1 2.196(4) . ? Li1 C2 2.237(4) . ? Li1 Li2 2.391(5) . ? Li2 N2 1.981(4) . ? Li2 N1 1.990(4) . ? Si1 N1 1.7079(16) . ? Si1 C3 1.868(3) . ? Si1 C5 1.868(2) . ? Si1 C4 1.879(2) . ? Si2 C7 1.868(2) . ? Si2 C2 1.871(2) . ? Si2 C8 1.873(2) . ? Si2 C6 1.873(2) . ? Si3 N2 1.7055(16) . ? Si3 C21 1.875(2) . ? Si3 C23 1.876(2) . ? Si3 C22 1.879(2) . ? Si4 C20 1.855(2) . ? Si4 C24 1.860(3) . ? Si4 C26 1.868(2) . ? Si4 C25 1.883(2) . ? N1 C1 1.403(2) . ? N2 C19 1.396(2) . ? C1 C2 1.372(3) . ? C1 C9 1.544(3) . ? C9 C10 1.538(3) . ? C9 C16 1.538(3) . ? C9 C17 1.555(3) . ? C10 C11 1.532(3) . ? C11 C12 1.529(3) . ? C11 C18 1.534(3) . ? C12 C13 1.534(3) . ? C13 C14 1.531(3) . ? C13 C17 1.533(3) . ? C14 C15 1.536(3) . ? C15 C18 1.531(3) . ? C15 C16 1.536(3) . ? C19 C20 1.360(3) . ? C19 C27 1.560(3) . ? C27 C34 1.542(3) . ? C27 C35 1.545(3) . ? C27 C28 1.549(3) . ? C28 C29 1.532(3) . ? C29 C36 1.524(3) . ? C29 C30 1.530(3) . ? C30 C31 1.530(3) . ? C31 C32 1.534(3) . ? C31 C35 1.536(3) . ? C32 C33 1.530(3) . ? C33 C36 1.525(3) . ? C33 C34 1.531(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Li1 N1 105.52(17) . . ? N2 Li1 C1 125.21(19) . . ? N1 Li1 C1 38.64(9) . . ? N2 Li1 C2 154.6(2) . . ? N1 Li1 C2 68.35(12) . . ? C1 Li1 C2 36.04(9) . . ? N2 Li1 Li2 52.67(13) . . ? N1 Li1 Li2 52.87(13) . . ? C1 Li1 Li2 80.99(15) . . ? C2 Li1 Li2 116.85(18) . . ? N2 Li2 N1 107.31(18) . . ? N2 Li2 C19 36.15(9) . . ? N1 Li2 C19 114.48(18) . . ? N2 Li2 Li1 53.59(13) . . ? N1 Li2 Li1 53.74(13) . . ? C19 Li2 Li1 69.81(14) . . ? N1 Si1 C3 112.89(10) . . ? N1 Si1 C5 109.15(10) . . ? C3 Si1 C5 108.73(14) . . ? N1 Si1 C4 113.16(10) . . ? C3 Si1 C4 107.30(12) . . ? C5 Si1 C4 105.25(12) . . ? C7 Si2 C2 114.74(10) . . ? C7 Si2 C8 109.32(11) . . ? C2 Si2 C8 115.45(10) . . ? C7 Si2 C6 106.86(13) . . ? C2 Si2 C6 103.31(11) . . ? C8 Si2 C6 106.28(12) . . ? N2 Si3 C21 113.28(9) . . ? N2 Si3 C23 110.88(10) . . ? C21 Si3 C23 110.09(10) . . ? N2 Si3 C22 111.69(9) . . ? C21 Si3 C22 106.27(11) . . ? C23 Si3 C22 104.15(12) . . ? C20 Si4 C24 114.56(11) . . ? C20 Si4 C26 106.14(11) . . ? C24 Si4 C26 108.26(14) . . ? C20 Si4 C25 114.23(10) . . ? C24 Si4 C25 106.98(13) . . ? C26 Si4 C25 106.23(12) . . ? C1 N1 Si1 123.06(13) . . ? C1 N1 Li2 122.11(16) . . ? Si1 N1 Li2 112.82(14) . . ? C1 N1 Li1 77.77(14) . . ? Si1 N1 Li1 134.88(14) . . ? Li2 N1 Li1 73.38(15) . . ? C19 N2 Si3 129.23(13) . . ? C19 N2 Li2 87.05(16) . . ? Si3 N2 Li2 130.51(15) . . ? C19 N2 Li1 104.86(16) . . ? Si3 N2 Li1 116.71(13) . . ? Li2 N2 Li1 73.74(15) . . ? C2 C1 N1 119.29(18) . . ? C2 C1 C9 123.13(17) . . ? N1 C1 C9 117.55(16) . . ? C2 C1 Li1 73.64(15) . . ? N1 C1 Li1 63.59(13) . . ? C9 C1 Li1 133.66(15) . . ? C1 C2 Si2 142.33(16) . . ? C1 C2 Li1 70.32(14) . . ? Si2 C2 Li1 132.54(14) . . ? C10 C9 C16 107.70(15) . . ? C10 C9 C1 111.83(15) . . ? C16 C9 C1 113.11(15) . . ? C10 C9 C17 107.64(15) . . ? C16 C9 C17 108.35(15) . . ? C1 C9 C17 108.03(15) . . ? C11 C10 C9 111.76(16) . . ? C12 C11 C10 109.18(16) . . ? C12 C11 C18 110.40(17) . . ? C10 C11 C18 109.15(17) . . ? C11 C12 C13 108.96(17) . . ? C14 C13 C17 109.71(17) . . ? C14 C13 C12 109.28(17) . . ? C17 C13 C12 109.87(16) . . ? C13 C14 C15 109.70(16) . . ? C18 C15 C14 109.03(17) . . ? C18 C15 C16 110.06(17) . . ? C14 C15 C16 109.38(17) . . ? C15 C16 C9 110.95(16) . . ? C13 C17 C9 110.42(16) . . ? C15 C18 C11 108.84(16) . . ? C20 C19 N2 122.42(18) . . ? C20 C19 C27 120.47(17) . . ? N2 C19 C27 116.97(16) . . ? C19 C20 Si4 133.34(17) . . ? C19 C20 Li2 68.33(14) . . ? Si4 C20 Li2 80.96(12) . . ? C34 C27 C35 107.81(16) . . ? C34 C27 C28 107.78(16) . . ? C35 C27 C28 106.61(16) . . ? C34 C27 C19 113.03(16) . . ? C35 C27 C19 109.48(15) . . ? C28 C27 C19 111.85(15) . . ? C29 C28 C27 111.72(17) . . ? C36 C29 C30 110.01(19) . . ? C36 C29 C28 109.61(18) . . ? C30 C29 C28 108.88(18) . . ? C31 C30 C29 109.31(18) . . ? C30 C31 C32 108.8(2) . . ? C30 C31 C35 109.44(18) . . ? C32 C31 C35 110.21(19) . . ? C33 C32 C31 109.34(18) . . ? C36 C33 C32 109.7(2) . . ? C36 C33 C34 109.76(19) . . ? C32 C33 C34 109.07(19) . . ? C33 C34 C27 111.73(17) . . ? C31 C35 C27 111.16(17) . . ? C29 C36 C33 109.25(19) . . ? #===END data_(3)-jul1200 _database_code_depnum_ccdc_archive 'CCDC 668982' _audit_creation_date 2000-07-12T15:10:06-00:00 _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 jul1200 _chemical_formula_moiety 'C52 H82 Li2 N4 Si4, C6 H14' _chemical_formula_sum 'C58 H96 Li2 N4 Si4' _chemical_formula_weight 975.63 _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 10.5486(5) _cell_length_b 11.7160(5) _cell_length_c 13.3180(7) _cell_angle_alpha 70.084(3) _cell_angle_beta 87.413(4) _cell_angle_gamma 74.873(4) _cell_volume 1492.14(12) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7988 _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 colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.137 _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 11231 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_unetI/netI 0.0534 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 23.01 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 4109 _reflns_number_gt 3348 _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 hexane solvate is disordered across an inversion centre and the terminal C atom was not located. The solvate was included with C atoms with a common isotropic displacement parameter, H atoms omitted, and with geomtry restraints. atoms omitted, Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1303P)^2^+2.0918P] 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 4109 _refine_ls_number_parameters 290 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1687 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.671 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.057 #----------------------------------------------------------------------------# # 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 Li Li 0.0947(5) 0.3962(5) 0.0206(4) 0.0322(12) Uani 1 1 d . . . Si1 Si 0.32223(9) 0.12274(8) 0.12430(7) 0.0324(3) Uani 1 1 d . . . Si2 Si 0.20808(9) 0.60569(8) 0.00728(7) 0.0309(3) Uani 1 1 d . . . N1 N 0.2050(2) 0.2532(2) 0.1387(2) 0.0302(6) Uani 1 1 d . . . N2 N 0.0860(2) 0.5413(2) 0.07161(19) 0.0267(6) Uani 1 1 d . . . C1 C 0.1668(3) 0.2675(3) 0.2291(2) 0.0296(7) Uani 1 1 d . . . C2 C 0.0917(3) 0.3817(3) 0.2456(2) 0.0318(7) Uani 1 1 d . . . H2 H 0.0552 0.3695 0.3138 0.038 Uiso 1 1 calc R . . C3 C 0.0645(3) 0.5051(3) 0.1784(2) 0.0255(7) Uani 1 1 d . . . C4 C 0.1970(3) 0.1586(3) 0.3335(2) 0.0308(7) Uani 1 1 d . . . C5 C 0.2831(4) 0.1526(3) 0.4118(3) 0.0393(8) Uani 1 1 d . . . H5 H 0.3238 0.2191 0.4006 0.047 Uiso 1 1 calc R . . C6 C 0.3107(4) 0.0508(3) 0.5062(3) 0.0446(9) Uani 1 1 d . . . H6 H 0.3729 0.0467 0.5576 0.053 Uiso 1 1 calc R . . C7 C 0.2489(4) -0.0447(3) 0.5268(3) 0.0485(10) Uani 1 1 d . . . C8 C 0.1609(4) -0.0378(3) 0.4494(3) 0.0492(10) Uani 1 1 d . . . H8 H 0.117 -0.1023 0.4623 0.059 Uiso 1 1 calc R . . C9 C 0.1361(4) 0.0621(3) 0.3534(3) 0.0413(8) Uani 1 1 d . . . H9 H 0.0767 0.0644 0.3008 0.05 Uiso 1 1 calc R . . C10 C 0.2743(6) -0.1535(4) 0.6321(3) 0.0782(15) Uani 1 1 d . . . H10A H 0.3679 -0.198 0.6411 0.117 Uiso 0.5 1 calc PR . . H10B H 0.2221 -0.2115 0.6322 0.117 Uiso 0.5 1 calc PR . . H10C H 0.2494 -0.1212 0.6911 0.117 Uiso 0.5 1 calc PR . . H10D H 0.1917 -0.1558 0.6685 0.117 Uiso 0.5 1 calc PR . . H10E H 0.3375 -0.1424 0.6774 0.117 Uiso 0.5 1 calc PR . . H10F H 0.3102 -0.2326 0.6185 0.117 Uiso 0.5 1 calc PR . . C11 C 0.0027(3) 0.6079(3) 0.2287(2) 0.0274(7) Uani 1 1 d . . . C12 C -0.0620(3) 0.5588(3) 0.3358(3) 0.0325(7) Uani 1 1 d . . . H12A H -0.1317 0.5211 0.3249 0.039 Uiso 1 1 calc R . . H12B H 0.0048 0.4924 0.3885 0.039 Uiso 1 1 calc R . . C13 C -0.1220(3) 0.6656(3) 0.3799(3) 0.0364(8) Uani 1 1 d . . . H13 H -0.1641 0.6313 0.4485 0.044 Uiso 1 1 calc R . . C14 C -0.2257(4) 0.7685(3) 0.2997(3) 0.0429(9) Uani 1 1 d . . . H14A H -0.2645 0.8369 0.3284 0.051 Uiso 1 1 calc R . . H14B H -0.2969 0.7335 0.287 0.051 Uiso 1 1 calc R . . C15 C -0.1611(3) 0.8203(3) 0.1947(3) 0.0392(8) Uani 1 1 d . . . H15 H -0.2287 0.8876 0.1418 0.047 Uiso 1 1 calc R . . C16 C -0.1028(3) 0.7139(3) 0.1506(3) 0.0334(8) Uani 1 1 d . . . H16A H -0.0633 0.7479 0.0815 0.04 Uiso 1 1 calc R . . H16B H -0.1739 0.6791 0.1372 0.04 Uiso 1 1 calc R . . C17 C 0.1103(3) 0.6654(3) 0.2511(3) 0.0327(8) Uani 1 1 d . . . H17A H 0.1776 0.599 0.3033 0.039 Uiso 1 1 calc R . . H17B H 0.154 0.6985 0.1841 0.039 Uiso 1 1 calc R . . C18 C 0.0518(3) 0.7715(3) 0.2952(3) 0.0365(8) Uani 1 1 d . . . H18 H 0.1231 0.8074 0.3083 0.044 Uiso 1 1 calc R . . C19 C -0.0137(3) 0.7203(3) 0.4008(3) 0.0382(8) Uani 1 1 d . . . H19A H 0.0525 0.6542 0.4542 0.046 Uiso 1 1 calc R . . H19B H -0.0515 0.7889 0.4295 0.046 Uiso 1 1 calc R . . C20 C -0.0522(4) 0.8751(3) 0.2141(3) 0.0426(9) Uani 1 1 d . . . H20A H -0.0896 0.9445 0.242 0.051 Uiso 1 1 calc R . . H20B H -0.0111 0.9095 0.146 0.051 Uiso 1 1 calc R . . C21 C 0.4496(4) 0.0343(4) 0.2352(3) 0.0558(11) Uani 1 1 d . . . H21A H 0.4076 -0.0051 0.3004 0.084 Uiso 1 1 calc R . . H21B H 0.494 0.0922 0.2478 0.084 Uiso 1 1 calc R . . H21C H 0.514 -0.031 0.2158 0.084 Uiso 1 1 calc R . . C22 C 0.4177(3) 0.1856(3) 0.0058(3) 0.0431(9) Uani 1 1 d . . . H22A H 0.4845 0.1158 -0.0056 0.065 Uiso 1 1 calc R . . H22B H 0.4608 0.2444 0.0186 0.065 Uiso 1 1 calc R . . H22C H 0.358 0.2294 -0.0578 0.065 Uiso 1 1 calc R . . C23 C 0.2394(4) 0.0100(3) 0.1027(3) 0.0419(9) Uani 1 1 d . . . H23A H 0.3045 -0.0554 0.0841 0.063 Uiso 1 1 calc R . . H23B H 0.1721 0.055 0.0444 0.063 Uiso 1 1 calc R . . H23C H 0.198 -0.0288 0.1684 0.063 Uiso 1 1 calc R . . C24 C 0.2419(4) 0.5579(3) -0.1140(3) 0.0400(8) Uani 1 1 d . . . H24A H 0.3129 0.5917 -0.1523 0.06 Uiso 1 1 calc R . . H24B H 0.1623 0.5911 -0.1611 0.06 Uiso 1 1 calc R . . H24C H 0.2681 0.4659 -0.0921 0.06 Uiso 1 1 calc R . . C25 C 0.1675(4) 0.7818(3) -0.0477(3) 0.0486(10) Uani 1 1 d . . . H25A H 0.1541 0.815 0.0114 0.073 Uiso 1 1 calc R . . H25B H 0.0871 0.8143 -0.0937 0.073 Uiso 1 1 calc R . . H25C H 0.2402 0.8081 -0.0895 0.073 Uiso 1 1 calc R . . C26 C 0.3622(4) 0.5418(4) 0.0947(3) 0.0495(10) Uani 1 1 d . . . H26A H 0.435 0.5674 0.0527 0.074 Uiso 1 1 calc R . . H26B H 0.3824 0.4497 0.1232 0.074 Uiso 1 1 calc R . . H26C H 0.3499 0.5746 0.154 0.074 Uiso 1 1 calc R . . C1S C 0.5 0.5 0.5 0.270(5) Uiso 1 2 d SD . . C2S C 0.451(3) 0.6477(10) 0.4476(13) 0.270(5) Uiso 0.5 1 d PD . . C3S C 0.4429(17) 0.6666(14) 0.3277(9) 0.270(5) Uiso 1 1 d D . . C4S C 0.486(3) 0.484(2) 0.6204(8) 0.270(5) Uiso 0.5 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li 0.031(3) 0.026(3) 0.033(3) -0.009(2) -0.004(2) 0.001(2) Si1 0.0332(5) 0.0257(5) 0.0325(5) -0.0096(4) -0.0028(4) 0.0023(4) Si2 0.0340(5) 0.0299(5) 0.0280(5) -0.0080(4) 0.0033(4) -0.0096(4) N1 0.0318(15) 0.0241(14) 0.0291(15) -0.0071(11) -0.0019(11) -0.0002(11) N2 0.0296(14) 0.0239(13) 0.0235(14) -0.0053(11) 0.0000(11) -0.0052(11) C1 0.0302(17) 0.0245(17) 0.0294(18) -0.0073(13) -0.0040(13) -0.0012(13) C2 0.0385(18) 0.0250(17) 0.0260(17) -0.0061(14) 0.0022(14) -0.0017(14) C3 0.0233(15) 0.0243(16) 0.0263(17) -0.0070(13) -0.0020(12) -0.0033(12) C4 0.0367(18) 0.0214(16) 0.0292(17) -0.0096(13) -0.0002(14) 0.0025(13) C5 0.050(2) 0.0297(18) 0.0343(19) -0.0132(15) -0.0049(16) -0.0005(15) C6 0.059(2) 0.036(2) 0.0291(19) -0.0129(16) -0.0118(16) 0.0083(17) C7 0.075(3) 0.030(2) 0.0272(19) -0.0057(15) 0.0015(18) 0.0037(18) C8 0.068(3) 0.031(2) 0.040(2) -0.0027(16) 0.0035(19) -0.0114(18) C9 0.052(2) 0.036(2) 0.0317(19) -0.0078(16) -0.0018(16) -0.0086(16) C10 0.129(5) 0.046(3) 0.036(2) 0.003(2) -0.004(3) -0.005(3) C11 0.0325(17) 0.0216(16) 0.0244(16) -0.0060(13) -0.0006(13) -0.0029(13) C12 0.0364(18) 0.0271(17) 0.0308(17) -0.0082(14) 0.0049(14) -0.0056(14) C13 0.042(2) 0.0347(19) 0.0300(18) -0.0117(15) 0.0076(15) -0.0058(15) C14 0.041(2) 0.041(2) 0.044(2) -0.0218(17) 0.0012(16) 0.0037(16) C15 0.046(2) 0.0277(18) 0.0343(19) -0.0104(15) -0.0055(15) 0.0072(15) C16 0.0377(18) 0.0269(17) 0.0295(17) -0.0090(14) -0.0048(14) 0.0022(14) C17 0.0369(18) 0.0288(17) 0.0300(17) -0.0085(14) 0.0022(14) -0.0069(14) C18 0.045(2) 0.0351(19) 0.0334(18) -0.0157(15) 0.0034(15) -0.0128(15) C19 0.050(2) 0.0310(18) 0.0305(18) -0.0114(15) 0.0003(15) -0.0046(15) C20 0.062(2) 0.0269(19) 0.035(2) -0.0106(15) 0.0056(17) -0.0047(16) C21 0.045(2) 0.057(3) 0.049(2) -0.020(2) -0.0103(18) 0.0177(18) C22 0.0318(19) 0.039(2) 0.054(2) -0.0157(17) 0.0053(16) -0.0017(15) C23 0.052(2) 0.0311(19) 0.040(2) -0.0125(16) 0.0070(16) -0.0079(16) C24 0.043(2) 0.043(2) 0.0356(19) -0.0127(16) 0.0087(15) -0.0155(16) C25 0.069(3) 0.034(2) 0.044(2) -0.0111(17) 0.0128(19) -0.0215(18) C26 0.035(2) 0.069(3) 0.045(2) -0.019(2) 0.0025(16) -0.0145(18) #----------------------------------------------------------------------------# # 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 Li N1 1.996(5) . ? Li N2 2.015(6) . ? Li N2 2.132(6) 2_565 ? Li C1 2.702(6) . ? Li C3 2.775(6) . ? Si1 N1 1.759(3) . ? Si1 C21 1.863(4) . ? Si1 C23 1.863(4) . ? Si1 C22 1.871(4) . ? Si2 N2 1.712(3) . ? Si2 C26 1.871(4) . ? Si2 C24 1.874(3) . ? Si2 C25 1.875(4) . ? N1 C1 1.303(4) . ? N2 C3 1.365(4) . ? N2 Li 2.132(6) 2_565 ? C1 C2 1.448(4) . ? C1 C4 1.511(4) . ? C2 C3 1.378(4) . ? C3 C11 1.557(4) . ? C4 C5 1.385(5) . ? C4 C9 1.386(5) . ? C5 C6 1.385(5) . ? C6 C7 1.381(6) . ? C7 C8 1.386(6) . ? C7 C10 1.517(5) . ? C8 C9 1.387(5) . ? C11 C16 1.539(4) . ? C11 C12 1.545(4) . ? C11 C17 1.548(4) . ? C12 C13 1.538(4) . ? C13 C19 1.524(5) . ? C13 C14 1.527(5) . ? C14 C15 1.529(5) . ? C15 C20 1.524(5) . ? C15 C16 1.531(4) . ? C17 C18 1.528(4) . ? C18 C20 1.537(5) . ? C18 C19 1.539(5) . ? C1S C4S 1.554(10) 2_666 ? C1S C4S 1.554(10) . ? C1S C2S 1.578(10) 2_666 ? C1S C2S 1.578(10) . ? C2S C3S 1.539(10) . ? C3S C4S 1.64(2) 2_666 ? 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 Li N2 101.2(2) . . ? N1 Li N2 143.6(3) . 2_565 ? N2 Li N2 101.7(2) . 2_565 ? N1 Si1 C21 116.49(15) . . ? N1 Si1 C23 110.40(15) . . ? C21 Si1 C23 108.37(19) . . ? N1 Si1 C22 106.52(14) . . ? C21 Si1 C22 104.23(18) . . ? C23 Si1 C22 110.61(17) . . ? N2 Si2 C26 110.51(15) . . ? N2 Si2 C24 107.11(14) . . ? C26 Si2 C24 108.28(17) . . ? N2 Si2 C25 116.37(16) . . ? C26 Si2 C25 110.11(19) . . ? C24 Si2 C25 103.95(17) . . ? C1 N1 Si1 125.7(2) . . ? C1 N1 Li 108.1(2) . . ? Si1 N1 Li 125.9(2) . . ? C3 N2 Si2 128.0(2) . . ? C3 N2 Li 108.8(2) . . ? Si2 N2 Li 104.4(2) . . ? C3 N2 Li 110.8(2) . 2_565 ? Si2 N2 Li 114.37(19) . 2_565 ? Li N2 Li 78.3(2) . 2_565 ? N1 C1 C2 127.4(3) . . ? N1 C1 C4 121.5(3) . . ? C2 C1 C4 111.1(3) . . ? C3 C2 C1 130.5(3) . . ? N2 C3 C2 124.1(3) . . ? N2 C3 C11 118.9(2) . . ? C2 C3 C11 117.0(3) . . ? C5 C4 C9 118.3(3) . . ? C5 C4 C1 121.9(3) . . ? C9 C4 C1 119.7(3) . . ? C6 C5 C4 120.8(3) . . ? C7 C6 C5 120.9(3) . . ? C6 C7 C8 118.3(3) . . ? C6 C7 C10 121.1(4) . . ? C8 C7 C10 120.5(4) . . ? C7 C8 C9 120.9(4) . . ? C4 C9 C8 120.7(3) . . ? C16 C11 C12 107.8(3) . . ? C16 C11 C17 108.3(3) . . ? C12 C11 C17 106.9(2) . . ? C16 C11 C3 109.9(2) . . ? C12 C11 C3 114.1(2) . . ? C17 C11 C3 109.8(2) . . ? C13 C12 C11 111.1(3) . . ? C19 C13 C14 109.7(3) . . ? C19 C13 C12 109.4(3) . . ? C14 C13 C12 110.0(3) . . ? C13 C14 C15 109.1(3) . . ? C20 C15 C14 109.8(3) . . ? C20 C15 C16 109.5(3) . . ? C14 C15 C16 109.3(3) . . ? C15 C16 C11 111.5(3) . . ? C18 C17 C11 111.2(3) . . ? C17 C18 C20 109.6(3) . . ? C17 C18 C19 109.8(3) . . ? C20 C18 C19 109.0(3) . . ? C13 C19 C18 109.0(3) . . ? C15 C20 C18 109.4(3) . . ? C4S C1S C2S 100.7(7) 2_666 2_666 ? C4S C1S C2S 100.7(7) . . ? C3S C2S C1S 102.4(8) . . ? C1S C4S C3S 99.2(11) . 2_666 ? #===END data_(4)-sep700 _database_code_depnum_ccdc_archive 'CCDC 668983' _audit_creation_date 2000-09-06T10:30:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 H45 Al1 N2 Si2' _chemical_formula_sum 'C27 H45 Al N2 Si2' _chemical_formula_weight 480.81 _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 6.5294(2) _cell_length_b 12.4764(4) _cell_length_c 17.8535(7) _cell_angle_alpha 97.866(2) _cell_angle_beta 93.585(2) _cell_angle_gamma 98.304(2) _cell_volume 1420.58(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8065 _cell_measurement_theta_min 3.705 _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 0.4 _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION not applied # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.173 _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 12549 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_unetI/netI 0.0475 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.97 _diffrn_measured_fraction_theta_max 0.97 _reflns_number_total 8060 _reflns_number_gt 6885 _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^)+(0.0441P)^2^+0.7313P] 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 8060 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0537 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.43 _refine_diff_density_min -0.422 _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' Al Al 0.0645 0.0514 '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 Si1 Si 0.54820(6) 0.52811(3) 0.34282(2) 0.02217(9) Uani 1 1 d . . . Si2 Si 0.53479(6) 0.72452(3) 0.08727(2) 0.01971(9) Uani 1 1 d . . . Al Al 0.81882(6) 0.64967(3) 0.22012(2) 0.01871(9) Uani 1 1 d . . . N1 N 0.65385(18) 0.64837(9) 0.30687(6) 0.0193(2) Uani 1 1 d . . . N2 N 0.69166(17) 0.75709(9) 0.17405(6) 0.0173(2) Uani 1 1 d . . . C1 C 0.6577(2) 0.75158(10) 0.33955(7) 0.0194(2) Uani 1 1 d . . . C2 C 0.7081(2) 0.84459(10) 0.30332(7) 0.0210(3) Uani 1 1 d . . . H2 H 0.74 0.9127 0.3359 0.025 Uiso 1 1 calc R . . C3 C 0.71719(19) 0.84958(10) 0.22562(7) 0.0167(2) Uani 1 1 d . . . C4 C 0.6277(2) 0.77775(11) 0.42229(7) 0.0233(3) Uani 1 1 d . . . C5 C 0.7700(3) 0.75044(14) 0.47531(9) 0.0317(3) Uani 1 1 d . . . H5 H 0.8813 0.7145 0.4587 0.038 Uiso 1 1 calc R . . C6 C 0.7490(3) 0.77592(16) 0.55266(9) 0.0428(4) Uani 1 1 d . . . H6 H 0.8466 0.7579 0.5888 0.051 Uiso 1 1 calc R . . C7 C 0.5862(4) 0.82733(17) 0.57665(10) 0.0491(5) Uani 1 1 d . . . H7 H 0.5699 0.8429 0.6293 0.059 Uiso 1 1 calc R . . C8 C 0.4466(3) 0.85622(16) 0.52444(10) 0.0446(4) Uani 1 1 d . . . H8 H 0.3356 0.8923 0.5413 0.053 Uiso 1 1 calc R . . C9 C 0.4685(3) 0.83251(13) 0.44699(9) 0.0322(3) Uani 1 1 d . . . H9 H 0.3744 0.8539 0.4112 0.039 Uiso 1 1 calc R . . C10 C 0.7689(3) 0.46308(14) 0.37750(10) 0.0341(3) Uani 1 1 d . . . H10A H 0.8624 0.4527 0.3372 0.051 Uiso 1 1 calc R . . H10B H 0.715 0.3919 0.3918 0.051 Uiso 1 1 calc R . . H10C H 0.8451 0.5105 0.4218 0.051 Uiso 1 1 calc R . . C11 C 0.3929(3) 0.43328(13) 0.26289(10) 0.0385(4) Uani 1 1 d . . . H11A H 0.4809 0.419 0.2213 0.058 Uiso 1 1 calc R . . H11B H 0.2757 0.4668 0.245 0.058 Uiso 1 1 calc R . . H11C H 0.3403 0.3642 0.2804 0.058 Uiso 1 1 calc R . . C12 C 0.3663(2) 0.54924(13) 0.41807(9) 0.0308(3) Uani 1 1 d . . . H12A H 0.4397 0.5988 0.4619 0.046 Uiso 1 1 calc R . . H12B H 0.314 0.4787 0.4336 0.046 Uiso 1 1 calc R . . H12C H 0.2495 0.5813 0.3982 0.046 Uiso 1 1 calc R . . C13 C 0.77359(19) 0.96611(10) 0.20488(7) 0.0170(2) Uani 1 1 d . . . C14 C 0.9793(2) 1.02166(11) 0.25246(8) 0.0224(3) Uani 1 1 d . . . H14A H 0.9602 1.0236 0.3072 0.027 Uiso 1 1 calc R . . H14B H 1.0913 0.9782 0.2402 0.027 Uiso 1 1 calc R . . C15 C 0.6029(2) 1.03673(11) 0.22398(8) 0.0226(3) Uani 1 1 d . . . H15A H 0.4715 1.0034 0.1936 0.027 Uiso 1 1 calc R . . H15B H 0.5787 1.0393 0.2783 0.027 Uiso 1 1 calc R . . C16 C 0.8176(2) 0.96601(10) 0.12117(7) 0.0201(2) Uani 1 1 d . . . H16A H 0.9313 0.9233 0.1097 0.024 Uiso 1 1 calc R . . H16B H 0.6921 0.9301 0.0882 0.024 Uiso 1 1 calc R . . C17 C 1.0422(2) 1.13898(12) 0.23557(9) 0.0266(3) Uani 1 1 d . . . H17 H 1.1728 1.1734 0.2674 0.032 Uiso 1 1 calc R . . C18 C 0.8694(3) 1.20599(12) 0.25492(9) 0.0314(3) Uani 1 1 d . . . H18A H 0.91 1.2819 0.2449 0.038 Uiso 1 1 calc R . . H18B H 0.847 1.2087 0.3094 0.038 Uiso 1 1 calc R . . C19 C 0.6682(2) 1.15365(11) 0.20668(9) 0.0279(3) Uani 1 1 d . . . H19 H 0.556 1.1983 0.219 0.033 Uiso 1 1 calc R . . C20 C 0.7044(2) 1.15004(12) 0.12234(9) 0.0283(3) Uani 1 1 d . . . H20A H 0.5753 1.1159 0.0908 0.034 Uiso 1 1 calc R . . H20B H 0.7428 1.2254 0.1108 0.034 Uiso 1 1 calc R . . C21 C 0.8791(2) 1.08341(11) 0.10400(8) 0.0233(3) Uani 1 1 d . . . H21 H 0.9023 1.0808 0.049 0.028 Uiso 1 1 calc R . . C22 C 1.0791(2) 1.13738(12) 0.15171(9) 0.0269(3) Uani 1 1 d . . . H22A H 1.1187 1.2131 0.141 0.032 Uiso 1 1 calc R . . H22B H 1.1934 1.0957 0.139 0.032 Uiso 1 1 calc R . . C23 C 0.3277(2) 0.81368(14) 0.08014(9) 0.0310(3) Uani 1 1 d . . . H23A H 0.3929 0.8898 0.0815 0.047 Uiso 1 1 calc R . . H23B H 0.2414 0.8085 0.1229 0.047 Uiso 1 1 calc R . . H23C H 0.2409 0.7892 0.0324 0.047 Uiso 1 1 calc R . . C24 C 0.6929(3) 0.72004(13) 0.00349(8) 0.0299(3) Uani 1 1 d . . . H24A H 0.7754 0.7922 0.0035 0.045 Uiso 1 1 calc R . . H24B H 0.6004 0.7001 -0.0433 0.045 Uiso 1 1 calc R . . H24C H 0.7859 0.6654 0.0063 0.045 Uiso 1 1 calc R . . C25 C 0.3822(3) 0.58525(13) 0.08363(9) 0.0320(3) Uani 1 1 d . . . H25A H 0.2971 0.5845 0.1269 0.048 Uiso 1 1 calc R . . H25B H 0.4774 0.5316 0.0858 0.048 Uiso 1 1 calc R . . H25C H 0.292 0.5665 0.0363 0.048 Uiso 1 1 calc R . . C26 C 0.8245(3) 0.50795(12) 0.15625(9) 0.0315(3) Uani 1 1 d . . . H26A H 0.8928 0.4605 0.1858 0.047 Uiso 1 1 calc R . . H26B H 0.9015 0.5203 0.112 0.047 Uiso 1 1 calc R . . H26C H 0.682 0.4728 0.1392 0.047 Uiso 1 1 calc R . . C27 C 1.1041(2) 0.71356(13) 0.26406(9) 0.0268(3) Uani 1 1 d . . . H27A H 1.1678 0.6583 0.2874 0.04 Uiso 1 1 calc R . . H27B H 1.098 0.7766 0.3027 0.04 Uiso 1 1 calc R . . H27C H 1.1876 0.7373 0.2238 0.04 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 Si1 0.02449(19) 0.01725(17) 0.02532(19) 0.00724(14) 0.00358(14) 0.00056(14) Si2 0.02118(18) 0.02122(17) 0.01527(16) 0.00125(13) -0.00013(12) 0.00046(13) Al 0.02121(19) 0.01647(18) 0.01861(19) 0.00260(14) 0.00198(14) 0.00328(14) N1 0.0221(5) 0.0162(5) 0.0193(5) 0.0039(4) 0.0020(4) 0.0002(4) N2 0.0204(5) 0.0156(5) 0.0153(5) 0.0012(4) 0.0004(4) 0.0019(4) C1 0.0226(6) 0.0187(6) 0.0162(5) 0.0028(4) 0.0020(4) 0.0002(5) C2 0.0295(7) 0.0154(5) 0.0169(6) 0.0011(4) 0.0029(5) -0.0001(5) C3 0.0172(5) 0.0156(5) 0.0173(5) 0.0027(4) 0.0015(4) 0.0021(4) C4 0.0333(7) 0.0189(6) 0.0164(6) 0.0027(5) 0.0045(5) -0.0013(5) C5 0.0386(8) 0.0341(8) 0.0216(7) 0.0032(6) 0.0006(6) 0.0045(7) C6 0.0579(12) 0.0490(10) 0.0203(7) 0.0040(7) -0.0023(7) 0.0077(9) C7 0.0768(14) 0.0521(11) 0.0183(7) -0.0002(7) 0.0112(8) 0.0119(10) C8 0.0609(12) 0.0460(10) 0.0303(8) 0.0005(7) 0.0188(8) 0.0184(9) C9 0.0439(9) 0.0301(7) 0.0246(7) 0.0044(6) 0.0088(6) 0.0095(7) C10 0.0358(8) 0.0303(7) 0.0408(9) 0.0135(7) 0.0071(7) 0.0113(6) C11 0.0465(10) 0.0253(7) 0.0387(9) 0.0055(6) -0.0001(7) -0.0102(7) C12 0.0291(7) 0.0304(7) 0.0357(8) 0.0135(6) 0.0104(6) 0.0019(6) C13 0.0189(5) 0.0145(5) 0.0176(5) 0.0033(4) 0.0027(4) 0.0016(4) C14 0.0223(6) 0.0216(6) 0.0225(6) 0.0067(5) -0.0009(5) -0.0009(5) C15 0.0229(6) 0.0193(6) 0.0272(7) 0.0043(5) 0.0071(5) 0.0059(5) C16 0.0241(6) 0.0185(6) 0.0184(6) 0.0043(4) 0.0037(5) 0.0034(5) C17 0.0276(7) 0.0229(6) 0.0267(7) 0.0064(5) -0.0009(5) -0.0060(5) C18 0.0451(9) 0.0160(6) 0.0316(8) 0.0012(5) 0.0069(6) 0.0002(6) C19 0.0326(7) 0.0192(6) 0.0353(8) 0.0075(5) 0.0088(6) 0.0098(5) C20 0.0317(7) 0.0237(6) 0.0325(7) 0.0127(6) 0.0017(6) 0.0067(6) C21 0.0274(7) 0.0218(6) 0.0219(6) 0.0088(5) 0.0031(5) 0.0020(5) C22 0.0257(7) 0.0261(7) 0.0294(7) 0.0109(5) 0.0048(5) -0.0012(5) C23 0.0247(7) 0.0357(8) 0.0320(8) 0.0048(6) -0.0055(6) 0.0058(6) C24 0.0359(8) 0.0328(7) 0.0190(6) 0.0005(5) 0.0062(6) -0.0001(6) C25 0.0323(8) 0.0288(7) 0.0295(7) 0.0005(6) -0.0022(6) -0.0074(6) C26 0.0362(8) 0.0230(7) 0.0344(8) -0.0025(6) 0.0041(6) 0.0075(6) C27 0.0227(6) 0.0296(7) 0.0289(7) 0.0074(6) 0.0000(5) 0.0049(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.7773(11) . ? Si1 C11 1.8641(17) . ? Si1 C12 1.8652(16) . ? Si1 C10 1.8659(17) . ? Si2 N2 1.7674(11) . ? Si2 C25 1.8646(16) . ? Si2 C24 1.8692(15) . ? Si2 C23 1.8798(16) . ? Al N2 1.9235(11) . ? Al N1 1.9417(12) . ? Al C26 1.9749(15) . ? Al C27 1.9846(15) . ? N1 C1 1.3350(16) . ? N2 C3 1.3569(15) . ? C1 C2 1.4124(18) . ? C1 C4 1.5000(18) . ? C2 C3 1.4018(17) . ? C3 C13 1.5479(17) . ? C4 C9 1.386(2) . ? C4 C5 1.395(2) . ? C5 C6 1.394(2) . ? C6 C7 1.380(3) . ? C7 C8 1.382(3) . ? C8 C9 1.395(2) . ? C13 C16 1.5393(17) . ? C13 C15 1.5440(18) . ? C13 C14 1.5598(18) . ? C14 C17 1.5379(19) . ? C15 C19 1.5379(19) . ? C16 C21 1.5393(18) . ? C17 C18 1.528(2) . ? C17 C22 1.529(2) . ? C18 C19 1.533(2) . ? C19 C20 1.534(2) . ? C20 C21 1.532(2) . ? C21 C22 1.528(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 N1 Si1 C11 107.77(7) . . ? N1 Si1 C12 115.24(6) . . ? C11 Si1 C12 105.69(8) . . ? N1 Si1 C10 107.90(7) . . ? C11 Si1 C10 109.27(9) . . ? C12 Si1 C10 110.80(8) . . ? N2 Si2 C25 108.38(6) . . ? N2 Si2 C24 112.12(6) . . ? C25 Si2 C24 107.16(7) . . ? N2 Si2 C23 113.13(6) . . ? C25 Si2 C23 103.04(8) . . ? C24 Si2 C23 112.35(8) . . ? N2 Al N1 97.01(5) . . ? N2 Al C26 117.08(6) . . ? N1 Al C26 117.33(6) . . ? N2 Al C27 110.01(6) . . ? N1 Al C27 104.59(6) . . ? C26 Al C27 109.66(7) . . ? C1 N1 Si1 126.48(9) . . ? C1 N1 Al 108.46(9) . . ? Si1 N1 Al 124.52(6) . . ? C3 N2 Si2 129.16(9) . . ? C3 N2 Al 107.26(8) . . ? Si2 N2 Al 122.66(6) . . ? N1 C1 C2 124.59(12) . . ? N1 C1 C4 120.98(11) . . ? C2 C1 C4 114.17(11) . . ? C3 C2 C1 128.51(12) . . ? N2 C3 C2 121.17(11) . . ? N2 C3 C13 123.52(11) . . ? C2 C3 C13 115.16(10) . . ? C9 C4 C5 119.64(14) . . ? C9 C4 C1 121.64(13) . . ? C5 C4 C1 118.66(14) . . ? C6 C5 C4 120.02(16) . . ? C7 C6 C5 119.91(17) . . ? C6 C7 C8 120.35(16) . . ? C7 C8 C9 120.07(18) . . ? C4 C9 C8 119.97(16) . . ? C16 C13 C15 109.60(11) . . ? C16 C13 C3 113.11(10) . . ? C15 C13 C3 111.47(10) . . ? C16 C13 C14 105.99(10) . . ? C15 C13 C14 108.40(10) . . ? C3 C13 C14 108.01(10) . . ? C17 C14 C13 110.69(11) . . ? C19 C15 C13 110.29(11) . . ? C21 C16 C13 111.12(10) . . ? C18 C17 C22 109.41(13) . . ? C18 C17 C14 109.38(12) . . ? C22 C17 C14 110.24(12) . . ? C17 C18 C19 109.66(12) . . ? C18 C19 C20 109.34(13) . . ? C18 C19 C15 109.53(12) . . ? C20 C19 C15 109.73(12) . . ? C21 C20 C19 109.24(12) . . ? C22 C21 C20 109.73(12) . . ? C22 C21 C16 109.78(11) . . ? C20 C21 C16 109.59(11) . . ? C21 C22 C17 108.59(12) . . ? #===END data_(5)-sep3100 _database_code_depnum_ccdc_archive 'CCDC 668984' _audit_creation_date 2000-09-22T11:00:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36.90 H70.70 Al Cl0.10 N2 Si4' _chemical_formula_sum 'C36.90 H70.70 Al Cl0.10 N2 Si4' _chemical_formula_weight 685.6 _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 11.3363(4) _cell_length_b 12.5576(4) _cell_length_c 17.0946(6) _cell_angle_alpha 70.347(2) _cell_angle_beta 89.000(2) _cell_angle_gamma 65.500(2) _cell_volume 2064.17(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9508 _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 1.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 754 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.198 _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 16679 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_unetI/netI 0.0534 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 27.9 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 9759 _reflns_number_gt 7956 _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 crystal contains 90% of the aluminium methyl compound and 10% of the aluminium chloro compound. The site C37 is unresolved and the C:Cl occupancy was refined. The H atom on C20 was refined. 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^)+(0.0474P)^2^+1.4760P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 9759 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.446 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # 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' Al Al 0.0645 0.0514 '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' Cl Cl 0.1484 0.1585 '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 Al Al 0.11987(5) 0.05309(5) 0.25550(3) 0.01932(12) Uani 1 1 d . A 1 Si1 Si 0.08189(5) 0.18180(5) 0.04131(3) 0.02227(12) Uani 1 1 d . A 1 Si2 Si 0.06774(5) 0.30096(5) 0.29256(3) 0.02421(12) Uani 1 1 d . A 1 Si3 Si 0.19881(6) -0.22609(5) 0.27154(4) 0.02944(13) Uani 1 1 d . A 1 Si4 Si 0.65040(5) -0.23499(5) 0.29314(4) 0.03007(13) Uani 1 1 d . A 1 N1 N 0.14003(14) 0.15786(13) 0.14372(9) 0.0197(3) Uani 1 1 d . A 1 N2 N 0.23803(15) -0.11357(13) 0.28596(9) 0.0212(3) Uani 1 1 d . A 1 C1 C 0.21946(16) 0.18373(15) 0.18225(11) 0.0182(3) Uani 1 1 d . A 1 C2 C 0.19824(17) 0.16638(16) 0.26972(11) 0.0194(3) Uani 1 1 d . A 1 H2 H 0.277(2) 0.140(2) 0.3081(14) 0.027(5) Uiso 1 1 d . B 1 C3 C 0.1872(2) 0.04513(19) 0.01217(13) 0.0319(4) Uani 1 1 d . A 1 H3C H 0.1915 -0.0323 0.0546 0.048 Uiso 1 1 calc R A 1 H3B H 0.2756 0.0404 0.0093 0.048 Uiso 1 1 calc R A 1 H3A H 0.1499 0.0554 -0.0426 0.048 Uiso 1 1 calc R A 1 C4 C -0.08720(19) 0.1944(2) 0.04752(13) 0.0330(4) Uani 1 1 d . A 1 H4C H -0.1257 0.2052 -0.0071 0.049 Uiso 1 1 calc R A 1 H4B H -0.1407 0.2667 0.0628 0.049 Uiso 1 1 calc R A 1 H4A H -0.0842 0.1177 0.0901 0.049 Uiso 1 1 calc R A 1 C5 C 0.0593(2) 0.33337(19) -0.04154(13) 0.0328(4) Uani 1 1 d . A 1 H5C H 0.0181 0.3418 -0.0946 0.049 Uiso 1 1 calc R A 1 H5B H 0.1447 0.3346 -0.0489 0.049 Uiso 1 1 calc R A 1 H5A H 0.0032 0.4033 -0.0246 0.049 Uiso 1 1 calc R A 1 C6 C 0.32576(17) 0.22155(16) 0.14305(11) 0.0208(3) Uani 1 1 d . A 1 C7 C 0.2649(2) 0.36604(17) 0.09837(13) 0.0293(4) Uani 1 1 d . A 1 H7B H 0.1927 0.393 0.0539 0.035 Uiso 1 1 calc R A 1 H7A H 0.2282 0.4069 0.1393 0.035 Uiso 1 1 calc R A 1 C8 C 0.3705(2) 0.4064(2) 0.05917(15) 0.0395(5) Uani 1 1 d . A 1 H8 H 0.3303 0.4996 0.0302 0.047 Uiso 1 1 calc R A 1 C9 C 0.4258(2) 0.3440(2) -0.00462(14) 0.0385(5) Uani 1 1 d . A 1 H9B H 0.3545 0.3694 -0.0493 0.046 Uiso 1 1 calc R A 1 H9A H 0.4919 0.3713 -0.031 0.046 Uiso 1 1 calc R A 1 C10 C 0.4889(2) 0.2012(2) 0.03964(13) 0.0326(4) Uani 1 1 d . A 1 H10 H 0.5254 0.1604 -0.002 0.039 Uiso 1 1 calc R A 1 C11 C 0.38533(18) 0.15926(18) 0.07937(12) 0.0253(4) Uani 1 1 d . A 1 H11B H 0.4262 0.0669 0.1079 0.03 Uiso 1 1 calc R A 1 H11A H 0.3151 0.1821 0.0348 0.03 Uiso 1 1 calc R A 1 C12 C 0.43751(18) 0.18419(19) 0.21129(12) 0.0282(4) Uani 1 1 d . A 1 H12B H 0.4017 0.2249 0.2524 0.034 Uiso 1 1 calc R A 1 H12A H 0.4776 0.0922 0.2415 0.034 Uiso 1 1 calc R A 1 C13 C 0.5428(2) 0.2242(2) 0.17193(15) 0.0383(5) Uani 1 1 d . A 1 H13 H 0.6148 0.1984 0.2171 0.046 Uiso 1 1 calc R A 1 C14 C 0.4807(3) 0.3669(2) 0.12808(16) 0.0459(6) Uani 1 1 d . A 1 H14B H 0.5477 0.394 0.1033 0.055 Uiso 1 1 calc R A 1 H14A H 0.4452 0.4074 0.1693 0.055 Uiso 1 1 calc R A 1 C15 C 0.5990(2) 0.1621(2) 0.10841(15) 0.0403(5) Uani 1 1 d . A 1 H15B H 0.6404 0.0697 0.1368 0.048 Uiso 1 1 calc R A 1 H15A H 0.6667 0.188 0.0834 0.048 Uiso 1 1 calc R A 1 C16 C 0.1198(2) 0.4259(2) 0.28978(16) 0.0390(5) Uani 1 1 d . A 1 H16C H 0.1368 0.4636 0.2331 0.058 Uiso 1 1 calc R A 1 H16B H 0.1997 0.3886 0.3297 0.058 Uiso 1 1 calc R A 1 H16A H 0.05 0.4909 0.3051 0.058 Uiso 1 1 calc R A 1 C17 C 0.0388(2) 0.2374(2) 0.40322(14) 0.0376(5) Uani 1 1 d . A 1 H17C H -0.0246 0.3063 0.4184 0.056 Uiso 1 1 calc R A 1 H17B H 0.1215 0.1966 0.4411 0.056 Uiso 1 1 calc R A 1 H17A H 0.0042 0.176 0.4081 0.056 Uiso 1 1 calc R A 1 C18 C -0.0845(2) 0.3814(2) 0.21513(15) 0.0371(5) Uani 1 1 d . A 1 H18C H -0.1207 0.3218 0.2179 0.056 Uiso 1 1 calc R A 1 H18B H -0.0638 0.4128 0.1585 0.056 Uiso 1 1 calc R A 1 H18A H -0.149 0.4519 0.2283 0.056 Uiso 1 1 calc R A 1 C19 C 0.36793(17) -0.15240(15) 0.32524(11) 0.0200(3) Uani 1 1 d . A 1 C20 C 0.46723(19) -0.16574(17) 0.27865(12) 0.0246(4) Uani 1 1 d . A 1 H20 H 0.438(2) -0.144(2) 0.2222(14) 0.027(5) Uiso 1 1 d . C 1 C21 C 0.0584(2) -0.1526(2) 0.18525(14) 0.0373(5) Uani 1 1 d . A 1 H21C H 0.0831 -0.1113 0.1324 0.056 Uiso 1 1 calc R A 1 H21B H -0.0177 -0.0903 0.1985 0.056 Uiso 1 1 calc R A 1 H21A H 0.0364 -0.2176 0.1797 0.056 Uiso 1 1 calc R A 1 C22 C 0.3388(3) -0.3429(2) 0.2409(2) 0.0537(7) Uani 1 1 d . A 1 H22C H 0.3141 -0.4061 0.2349 0.081 Uiso 1 1 calc R A 1 H22B H 0.4151 -0.384 0.2844 0.081 Uiso 1 1 calc R A 1 H22A H 0.3607 -0.2998 0.1874 0.081 Uiso 1 1 calc R A 1 C23 C 0.1418(3) -0.3135(2) 0.36488(16) 0.0518(7) Uani 1 1 d . A 1 H23C H 0.0619 -0.2543 0.3774 0.078 Uiso 1 1 calc R A 1 H23B H 0.2103 -0.3555 0.4135 0.078 Uiso 1 1 calc R A 1 H23A H 0.1236 -0.3763 0.3523 0.078 Uiso 1 1 calc R A 1 C24 C 0.38366(17) -0.18044(16) 0.42048(11) 0.0198(3) Uani 1 1 d . A 1 C25 C 0.25415(18) -0.10962(18) 0.44928(11) 0.0251(4) Uani 1 1 d . A 1 H25B H 0.223 -0.0182 0.4194 0.03 Uiso 1 1 calc R A 1 H25A H 0.1869 -0.1334 0.4346 0.03 Uiso 1 1 calc R A 1 C26 C 0.2713(2) -0.13961(19) 0.54434(12) 0.0301(4) Uani 1 1 d . A 1 H26 H 0.1859 -0.0917 0.5608 0.036 Uiso 1 1 calc R A 1 C27 C 0.3150(2) -0.2806(2) 0.59030(13) 0.0340(5) Uani 1 1 d . A 1 H27B H 0.3257 -0.3011 0.6517 0.041 Uiso 1 1 calc R A 1 H27A H 0.2478 -0.3047 0.5759 0.041 Uiso 1 1 calc R A 1 C28 C 0.4451(2) -0.35327(18) 0.56421(12) 0.0296(4) Uani 1 1 d . A 1 H28 H 0.4741 -0.4454 0.5941 0.036 Uiso 1 1 calc R A 1 C29 C 0.42882(19) -0.32273(17) 0.46919(11) 0.0252(4) Uani 1 1 d . A 1 H29B H 0.3634 -0.3482 0.454 0.03 Uiso 1 1 calc R A 1 H29A H 0.5132 -0.3709 0.4531 0.03 Uiso 1 1 calc R A 1 C30 C 0.48738(19) -0.14493(18) 0.44691(12) 0.0255(4) Uani 1 1 d . A 1 H30B H 0.5723 -0.1917 0.4306 0.031 Uiso 1 1 calc R A 1 H30A H 0.4607 -0.0541 0.417 0.031 Uiso 1 1 calc R A 1 C31 C 0.5041(2) -0.1751(2) 0.54214(12) 0.0314(4) Uani 1 1 d . A 1 H31 H 0.5718 -0.1512 0.5574 0.038 Uiso 1 1 calc R A 1 C32 C 0.5483(2) -0.3165(2) 0.58814(13) 0.0341(5) Uani 1 1 d . A 1 H32B H 0.6334 -0.3643 0.5725 0.041 Uiso 1 1 calc R A 1 H32A H 0.5598 -0.3371 0.6495 0.041 Uiso 1 1 calc R A 1 C33 C 0.3743(2) -0.1020(2) 0.56764(13) 0.0340(5) Uani 1 1 d . A 1 H33B H 0.3456 -0.0107 0.5383 0.041 Uiso 1 1 calc R A 1 H33A H 0.385 -0.1207 0.6289 0.041 Uiso 1 1 calc R A 1 C34 C 0.7323(2) -0.1455(2) 0.31863(16) 0.0399(5) Uani 1 1 d . A 1 H34C H 0.7042 -0.0635 0.2733 0.06 Uiso 1 1 calc R A 1 H34B H 0.8275 -0.1928 0.3245 0.06 Uiso 1 1 calc R A 1 H34A H 0.7079 -0.1333 0.3713 0.06 Uiso 1 1 calc R A 1 C35 C 0.6893(3) -0.2406(3) 0.18723(17) 0.0538(7) Uani 1 1 d . A 1 H35C H 0.6552 -0.2932 0.1734 0.081 Uiso 1 1 calc R A 1 H35B H 0.7844 -0.2761 0.1878 0.081 Uiso 1 1 calc R A 1 H35A H 0.6485 -0.1555 0.145 0.081 Uiso 1 1 calc R A 1 C36 C 0.7337(2) -0.4004(2) 0.37018(19) 0.0515(7) Uani 1 1 d . A 1 H36C H 0.7066 -0.4034 0.4253 0.077 Uiso 1 1 calc R A 1 H36B H 0.8288 -0.4296 0.3743 0.077 Uiso 1 1 calc R A 1 H36A H 0.7091 -0.4548 0.3511 0.077 Uiso 1 1 calc R A 1 C37 C -0.06114(15) 0.07434(16) 0.27943(11) 0.0326(6) Uani 0.900(4) 1 d P A 1 H37A H -0.1202 0.1639 0.2622 0.049 Uiso 0.900(4) 1 calc PR A 1 H37B H -0.0587 0.0329 0.3397 0.049 Uiso 0.900(4) 1 calc PR A 1 H37C H -0.0927 0.0365 0.2481 0.049 Uiso 0.900(4) 1 calc PR A 1 Cl Cl -0.06114(15) 0.07434(16) 0.27943(11) 0.0326(6) Uani 0.100(4) 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 Al 0.0187(3) 0.0193(2) 0.0216(3) -0.0078(2) 0.0048(2) -0.0095(2) Si1 0.0198(2) 0.0236(2) 0.0213(2) -0.00702(19) 0.00162(18) -0.0084(2) Si2 0.0218(2) 0.0226(2) 0.0303(3) -0.0134(2) 0.0058(2) -0.0085(2) Si3 0.0369(3) 0.0220(3) 0.0312(3) -0.0087(2) -0.0045(2) -0.0149(2) Si4 0.0255(3) 0.0273(3) 0.0371(3) -0.0135(2) 0.0130(2) -0.0101(2) N1 0.0177(7) 0.0196(7) 0.0216(7) -0.0072(6) 0.0035(6) -0.0079(6) N2 0.0231(7) 0.0185(7) 0.0230(7) -0.0073(6) 0.0012(6) -0.0100(6) C1 0.0149(7) 0.0127(7) 0.0231(8) -0.0051(6) 0.0020(6) -0.0034(6) C2 0.0185(8) 0.0192(8) 0.0222(8) -0.0082(7) 0.0045(7) -0.0093(7) C3 0.0326(10) 0.0336(10) 0.0348(11) -0.0185(9) 0.0066(9) -0.0146(9) C4 0.0234(9) 0.0405(11) 0.0338(11) -0.0120(9) -0.0002(8) -0.0136(9) C5 0.0317(10) 0.0298(10) 0.0261(10) -0.0020(8) -0.0008(8) -0.0095(9) C6 0.0182(8) 0.0178(8) 0.0256(9) -0.0059(7) 0.0049(7) -0.0087(7) C7 0.0304(10) 0.0194(9) 0.0351(10) -0.0073(8) 0.0092(8) -0.0102(8) C8 0.0476(13) 0.0274(10) 0.0463(13) -0.0068(9) 0.0142(10) -0.0242(10) C9 0.0413(12) 0.0380(11) 0.0362(12) -0.0046(9) 0.0141(9) -0.0246(10) C10 0.0268(10) 0.0365(11) 0.0355(11) -0.0119(9) 0.0152(8) -0.0159(9) C11 0.0211(9) 0.0248(9) 0.0307(10) -0.0100(7) 0.0087(7) -0.0107(7) C12 0.0229(9) 0.0354(10) 0.0298(10) -0.0090(8) 0.0046(7) -0.0180(8) C13 0.0290(11) 0.0524(13) 0.0405(12) -0.0120(10) 0.0059(9) -0.0279(10) C14 0.0561(15) 0.0534(14) 0.0535(15) -0.0224(12) 0.0215(12) -0.0452(13) C15 0.0232(10) 0.0501(13) 0.0474(13) -0.0121(11) 0.0130(9) -0.0205(10) C16 0.0383(12) 0.0350(11) 0.0572(14) -0.0290(11) 0.0130(11) -0.0190(10) C17 0.0375(12) 0.0383(11) 0.0352(11) -0.0191(9) 0.0139(9) -0.0105(10) C18 0.0280(10) 0.0271(10) 0.0483(13) -0.0134(9) -0.0007(9) -0.0047(8) C19 0.0226(8) 0.0148(7) 0.0228(8) -0.0071(6) 0.0035(7) -0.0082(7) C20 0.0281(9) 0.0235(9) 0.0227(9) -0.0090(7) 0.0062(7) -0.0112(8) C21 0.0420(12) 0.0376(11) 0.0362(11) -0.0128(9) -0.0045(9) -0.0210(10) C22 0.0525(15) 0.0347(12) 0.0774(19) -0.0324(13) -0.0033(14) -0.0122(11) C23 0.0728(18) 0.0499(14) 0.0431(13) 0.0000(11) -0.0094(12) -0.0487(14) C24 0.0219(8) 0.0188(8) 0.0206(8) -0.0074(6) 0.0046(7) -0.0104(7) C25 0.0254(9) 0.0249(9) 0.0223(9) -0.0072(7) 0.0050(7) -0.0096(7) C26 0.0350(11) 0.0312(10) 0.0236(9) -0.0114(8) 0.0103(8) -0.0130(9) C27 0.0437(12) 0.0364(11) 0.0232(10) -0.0051(8) 0.0088(9) -0.0232(10) C28 0.0380(11) 0.0225(9) 0.0248(9) -0.0027(7) 0.0006(8) -0.0143(8) C29 0.0297(9) 0.0212(8) 0.0247(9) -0.0068(7) 0.0024(7) -0.0122(8) C30 0.0274(9) 0.0282(9) 0.0261(9) -0.0100(7) 0.0047(7) -0.0166(8) C31 0.0396(11) 0.0360(11) 0.0273(10) -0.0118(8) 0.0010(8) -0.0240(9) C32 0.0353(11) 0.0363(11) 0.0259(10) -0.0071(8) -0.0040(8) -0.0142(9) C33 0.0524(13) 0.0319(10) 0.0230(9) -0.0130(8) 0.0066(9) -0.0208(10) C34 0.0272(10) 0.0414(12) 0.0524(14) -0.0171(11) 0.0112(10) -0.0161(10) C35 0.0486(15) 0.0687(18) 0.0553(16) -0.0362(14) 0.0318(13) -0.0259(14) C36 0.0346(12) 0.0290(11) 0.0750(18) -0.0106(12) 0.0179(12) -0.0059(10) C37 0.0272(9) 0.0381(10) 0.0391(10) -0.0166(7) 0.0117(6) -0.0185(7) Cl 0.0272(9) 0.0381(10) 0.0391(10) -0.0166(7) 0.0117(6) -0.0185(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 Al N2 1.8471(16) . ? Al N1 1.9945(15) . ? Al C37 2.0097(15) . ? Al C2 2.0399(17) . ? Al C1 2.3748(17) . ? Si1 N1 1.7639(16) . ? Si1 C4 1.861(2) . ? Si1 C3 1.864(2) . ? Si1 C5 1.868(2) . ? Si2 C18 1.867(2) . ? Si2 C17 1.872(2) . ? Si2 C16 1.879(2) . ? Si2 C2 1.8834(18) . ? Si3 N2 1.7361(15) . ? Si3 C22 1.872(3) . ? Si3 C21 1.873(2) . ? Si3 C23 1.882(2) . ? Si4 C20 1.872(2) . ? Si4 C35 1.873(3) . ? Si4 C36 1.876(2) . ? Si4 C34 1.877(2) . ? N1 C1 1.326(2) . ? N2 C19 1.441(2) . ? C1 C2 1.467(2) . ? C1 C6 1.536(2) . ? C6 C11 1.537(3) . ? C6 C12 1.541(3) . ? C6 C7 1.549(2) . ? C7 C8 1.545(3) . ? C8 C9 1.530(3) . ? C8 C14 1.529(4) . ? C9 C10 1.530(3) . ? C10 C15 1.528(3) . ? C10 C11 1.536(2) . ? C12 C13 1.541(3) . ? C13 C15 1.525(3) . ? C13 C14 1.528(3) . ? C19 C20 1.353(2) . ? C19 C24 1.542(2) . ? C24 C30 1.541(2) . ? C24 C25 1.541(2) . ? C24 C29 1.550(2) . ? C25 C26 1.536(3) . ? C26 C33 1.531(3) . ? C26 C27 1.533(3) . ? C27 C28 1.530(3) . ? C28 C32 1.529(3) . ? C28 C29 1.534(3) . ? C30 C31 1.538(3) . ? C31 C33 1.525(3) . ? C31 C32 1.536(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al N1 111.95(7) . . ? N2 Al C37 112.41(7) . . ? N1 Al C37 118.53(7) . . ? N2 Al C2 114.29(7) . . ? N1 Al C2 69.95(7) . . ? C37 Al C2 123.14(7) . . ? N1 Si1 C4 104.43(8) . . ? N1 Si1 C3 109.85(8) . . ? C4 Si1 C3 110.92(10) . . ? N1 Si1 C5 115.70(9) . . ? C4 Si1 C5 104.13(10) . . ? C3 Si1 C5 111.42(10) . . ? C18 Si2 C17 112.91(11) . . ? C18 Si2 C16 106.10(11) . . ? C17 Si2 C16 105.07(11) . . ? C18 Si2 C2 112.01(9) . . ? C17 Si2 C2 107.40(9) . . ? C16 Si2 C2 113.24(9) . . ? N2 Si3 C22 111.76(10) . . ? N2 Si3 C21 111.12(9) . . ? C22 Si3 C21 106.46(12) . . ? N2 Si3 C23 114.39(10) . . ? C22 Si3 C23 108.60(14) . . ? C21 Si3 C23 103.95(11) . . ? C20 Si4 C35 102.66(11) . . ? C20 Si4 C36 114.51(10) . . ? C35 Si4 C36 106.79(13) . . ? C20 Si4 C34 118.50(9) . . ? C35 Si4 C34 106.55(12) . . ? C36 Si4 C34 106.90(12) . . ? C1 N1 Si1 139.77(12) . . ? C1 N1 Al 88.96(10) . . ? Si1 N1 Al 130.96(8) . . ? C19 N2 Si3 118.52(11) . . ? C19 N2 Al 118.38(11) . . ? Si3 N2 Al 123.08(9) . . ? N1 C1 C2 111.71(14) . . ? N1 C1 C6 125.17(15) . . ? C2 C1 C6 123.06(15) . . ? C1 C2 Si2 118.47(12) . . ? C1 C2 Al 83.53(10) . . ? Si2 C2 Al 109.13(8) . . ? C1 C6 C11 112.03(14) . . ? C1 C6 C12 110.75(14) . . ? C11 C6 C12 108.07(15) . . ? C1 C6 C7 108.97(14) . . ? C11 C6 C7 109.15(15) . . ? C12 C6 C7 107.75(15) . . ? C8 C7 C6 109.87(16) . . ? C9 C8 C14 109.7(2) . . ? C9 C8 C7 109.46(18) . . ? C14 C8 C7 109.64(18) . . ? C10 C9 C8 109.53(17) . . ? C15 C10 C9 109.66(19) . . ? C15 C10 C11 109.17(17) . . ? C9 C10 C11 109.49(16) . . ? C10 C11 C6 110.91(16) . . ? C13 C12 C6 110.63(16) . . ? C15 C13 C14 109.64(19) . . ? C15 C13 C12 110.09(18) . . ? C14 C13 C12 108.95(18) . . ? C13 C14 C8 109.36(18) . . ? C13 C15 C10 109.35(18) . . ? C20 C19 N2 119.50(16) . . ? C20 C19 C24 124.47(16) . . ? N2 C19 C24 115.99(14) . . ? C19 C20 Si4 139.64(15) . . ? C30 C24 C25 108.10(15) . . ? C30 C24 C19 111.60(14) . . ? C25 C24 C19 112.12(14) . . ? C30 C24 C29 107.56(15) . . ? C25 C24 C29 107.48(14) . . ? C19 C24 C29 109.78(14) . . ? C26 C25 C24 111.41(15) . . ? C33 C26 C27 109.90(17) . . ? C33 C26 C25 109.75(16) . . ? C27 C26 C25 109.08(16) . . ? C28 C27 C26 109.06(16) . . ? C32 C28 C27 109.16(17) . . ? C32 C28 C29 109.60(16) . . ? C27 C28 C29 110.10(16) . . ? C28 C29 C24 110.88(15) . . ? C31 C30 C24 111.27(15) . . ? C33 C31 C32 109.60(17) . . ? C33 C31 C30 109.78(17) . . ? C32 C31 C30 109.15(17) . . ? C28 C32 C31 109.37(16) . . ? C31 C33 C26 109.03(16) . . ? #===END data_(6)-jul3700 _database_code_depnum_ccdc_archive 'CCDC 668985' _audit_creation_date 2000-07-27T13:46:47-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C44 H76 Al N3 Si4' _chemical_formula_sum 'C44 H76 Al N3 Si4' _chemical_formula_weight 786.42 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9220(2) _cell_length_b 19.0977(3) _cell_length_c 41.4159(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 9429.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 44074 _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 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _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 50445 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_unetI/netI 0.0637 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 8303 _reflns_number_gt 5601 _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^)+(0.0598P)^2^+4.1700P] 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 8303 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.384 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.052 #----------------------------------------------------------------------------# # 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' Al Al 0.0645 0.0514 '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 Al Al 0.00105(6) 0.19727(4) 0.144513(18) 0.0247(2) Uani 1 1 d . . . Si1 Si -0.27576(7) 0.17432(4) 0.12865(2) 0.0365(2) Uani 1 1 d . . . Si2 Si -0.00650(6) 0.20822(4) 0.221871(18) 0.0296(2) Uani 1 1 d . . . Si3 Si 0.24111(7) 0.22028(5) 0.11597(2) 0.0384(2) Uani 1 1 d . . . Si4 Si 0.03338(11) 0.40703(5) 0.05239(2) 0.0621(3) Uani 1 1 d . . . N1 N -0.15250(17) 0.22710(11) 0.13485(5) 0.0258(5) Uani 1 1 d . . . N2 N 0.01211(16) 0.24907(11) 0.18422(5) 0.0235(5) Uani 1 1 d . . . N3 N 0.09692(18) 0.23015(11) 0.11262(5) 0.0279(5) Uani 1 1 d . . . C1 C -0.1605(2) 0.29659(14) 0.13886(6) 0.0274(6) Uani 1 1 d . . . C2 C -0.0788(2) 0.33906(14) 0.15406(6) 0.0275(6) Uani 1 1 d . . . H2 H -0.0757 0.3867 0.1476 0.033 Uiso 1 1 calc R . . C3 C -0.0032(2) 0.31804(13) 0.17745(6) 0.0253(6) Uani 1 1 d . . . C4 C -0.2621(2) 0.33739(14) 0.12836(7) 0.0316(7) Uani 1 1 d . . . C5 C -0.3315(3) 0.36740(15) 0.15123(8) 0.0433(8) Uani 1 1 d . . . H5 H -0.3176 0.3598 0.1735 0.052 Uiso 1 1 calc R . . C6 C -0.4219(3) 0.40879(17) 0.14170(10) 0.0570(10) Uani 1 1 d . . . H6 H -0.4708 0.4281 0.1575 0.068 Uiso 1 1 calc R . . C7 C -0.4403(3) 0.42167(17) 0.10960(10) 0.0561(10) Uani 1 1 d . . . H7 H -0.5025 0.4494 0.1031 0.067 Uiso 1 1 calc R . . C8 C -0.3695(3) 0.39480(18) 0.08695(9) 0.0615(11) Uani 1 1 d . . . H8 H -0.3808 0.4054 0.0648 0.074 Uiso 1 1 calc R . . C9 C -0.2813(3) 0.35211(16) 0.09613(8) 0.0486(9) Uani 1 1 d . . . H9 H -0.2334 0.3327 0.0801 0.058 Uiso 1 1 calc R . . C10 C -0.3514(3) 0.18701(18) 0.08995(8) 0.0545(9) Uani 1 1 d . . . H10C H -0.3014 0.1754 0.0719 0.082 Uiso 1 1 calc R . . H10B H -0.3753 0.2359 0.0881 0.082 Uiso 1 1 calc R . . H10A H -0.4173 0.1564 0.0894 0.082 Uiso 1 1 calc R . . C11 C -0.2353(3) 0.08076(16) 0.13038(10) 0.0639(11) Uani 1 1 d . . . H11C H -0.3028 0.0516 0.1295 0.096 Uiso 1 1 calc R . . H11B H -0.1949 0.0716 0.1506 0.096 Uiso 1 1 calc R . . H11A H -0.1867 0.0696 0.112 0.096 Uiso 1 1 calc R . . C12 C -0.3772(3) 0.19129(19) 0.16209(8) 0.0570(9) Uani 1 1 d . . . H12C H -0.4432 0.1613 0.1593 0.086 Uiso 1 1 calc R . . H12B H -0.4002 0.2406 0.1616 0.086 Uiso 1 1 calc R . . H12A H -0.3414 0.1809 0.1828 0.086 Uiso 1 1 calc R . . C16 C 0.0655(2) 0.37750(13) 0.19375(6) 0.0269(6) Uani 1 1 d . . . C17 C 0.1507(2) 0.35088(14) 0.21855(7) 0.0351(7) Uani 1 1 d . . . H17B H 0.2013 0.3165 0.2081 0.042 Uiso 1 1 calc R . . H17A H 0.1106 0.3268 0.2363 0.042 Uiso 1 1 calc R . . C18 C 0.2204(3) 0.41128(15) 0.23244(8) 0.0427(8) Uani 1 1 d . . . H18 H 0.2743 0.3924 0.2488 0.051 Uiso 1 1 calc R . . C19 C 0.2851(3) 0.44649(18) 0.20555(9) 0.0582(10) Uani 1 1 d . . . H19B H 0.3363 0.4124 0.1952 0.07 Uiso 1 1 calc R . . H19A H 0.3308 0.4853 0.2144 0.07 Uiso 1 1 calc R . . C20 C 0.2030(3) 0.47478(17) 0.18076(8) 0.0548(9) Uani 1 1 d . . . H20 H 0.2453 0.4983 0.163 0.066 Uiso 1 1 calc R . . C21 C 0.1322(3) 0.41484(16) 0.16671(7) 0.0415(8) Uani 1 1 d . . . H21B H 0.1819 0.3807 0.1558 0.05 Uiso 1 1 calc R . . H21A H 0.0794 0.4338 0.1505 0.05 Uiso 1 1 calc R . . C22 C -0.0106(2) 0.43229(14) 0.21030(7) 0.0363(7) Uani 1 1 d . . . H22B H -0.065 0.451 0.1944 0.044 Uiso 1 1 calc R . . H22A H -0.0533 0.4097 0.2279 0.044 Uiso 1 1 calc R . . C23 C 0.0596(3) 0.49218(16) 0.22398(8) 0.0461(8) Uani 1 1 d . . . H23 H 0.009 0.5269 0.2347 0.055 Uiso 1 1 calc R . . C24 C 0.1422(3) 0.46338(16) 0.24874(8) 0.0496(9) Uani 1 1 d . . . H24B H 0.1864 0.5022 0.2581 0.06 Uiso 1 1 calc R . . H24A H 0.1007 0.44 0.2664 0.06 Uiso 1 1 calc R . . C25 C 0.1231(3) 0.52783(16) 0.19678(9) 0.0588(10) Uani 1 1 d . . . H25B H 0.1666 0.5678 0.2054 0.071 Uiso 1 1 calc R . . H25A H 0.0695 0.5461 0.1806 0.071 Uiso 1 1 calc R . . C26 C -0.1116(3) 0.13694(16) 0.21728(7) 0.0432(8) Uani 1 1 d . . . H26C H -0.0829 0.1016 0.2022 0.065 Uiso 1 1 calc R . . H26B H -0.1818 0.1565 0.2089 0.065 Uiso 1 1 calc R . . H26A H -0.1255 0.1152 0.2383 0.065 Uiso 1 1 calc R . . C27 C -0.0741(3) 0.26566(16) 0.25280(8) 0.0553(9) Uani 1 1 d . . . H27C H -0.093 0.2378 0.2719 0.083 Uiso 1 1 calc R . . H27B H -0.1426 0.2862 0.2438 0.083 Uiso 1 1 calc R . . H27A H -0.0221 0.3031 0.2589 0.083 Uiso 1 1 calc R . . C28 C 0.1236(3) 0.16813(17) 0.23800(7) 0.0461(8) Uani 1 1 d . . . H28C H 0.1078 0.1462 0.2589 0.069 Uiso 1 1 calc R . . H28B H 0.1809 0.2044 0.2408 0.069 Uiso 1 1 calc R . . H28A H 0.1509 0.1326 0.2229 0.069 Uiso 1 1 calc R . . C29 C 0.0570(2) 0.26219(14) 0.08304(6) 0.0304(7) Uani 1 1 d . . . C30 C 0.0514(3) 0.33261(15) 0.08102(7) 0.0412(8) Uani 1 1 d . . . H30 H 0.0599 0.3513 0.1021 0.068(11) Uiso 1 1 calc R . . C31 C 0.0287(2) 0.21253(14) 0.05480(6) 0.0320(7) Uani 1 1 d . . . C32 C 0.0234(3) 0.13552(15) 0.06512(7) 0.0396(8) Uani 1 1 d . . . H32B H -0.0363 0.1296 0.0815 0.047 Uiso 1 1 calc R . . H32A H 0.0956 0.1221 0.0752 0.047 Uiso 1 1 calc R . . C33 C -0.0005(3) 0.08697(17) 0.03630(7) 0.0476(8) Uani 1 1 d . . . H33 H -0.0018 0.0372 0.0438 0.056(10) Uiso 1 1 calc R . . C34 C -0.1139(3) 0.10597(18) 0.02194(9) 0.0581(10) Uani 1 1 d . . . H34B H -0.1735 0.0995 0.0383 0.07 Uiso 1 1 calc R . . H34A H -0.1306 0.0751 0.0034 0.07 Uiso 1 1 calc R . . C35 C -0.1111(3) 0.18221(18) 0.01091(8) 0.0545(10) Uani 1 1 d . . . H35 H -0.1856 0.1952 0.0016 0.065 Uiso 1 1 calc R . . C36 C -0.0202(3) 0.19115(19) -0.01475(8) 0.0632(11) Uani 1 1 d . . . H36B H -0.0366 0.1606 -0.0335 0.076 Uiso 1 1 calc R . . H36A H -0.0187 0.2403 -0.0223 0.076 Uiso 1 1 calc R . . C37 C 0.0934(3) 0.17169(17) -0.00030(7) 0.0492(9) Uani 1 1 d . . . H37 H 0.1531 0.1774 -0.0171 0.059 Uiso 1 1 calc R . . C38 C 0.1190(3) 0.21929(16) 0.02827(7) 0.0433(8) Uani 1 1 d . . . H38B H 0.1225 0.2685 0.0208 0.052 Uiso 1 1 calc R . . H38A H 0.1931 0.2069 0.0374 0.052 Uiso 1 1 calc R . . C39 C -0.0853(3) 0.22981(16) 0.03989(7) 0.0457(8) Uani 1 1 d . . . H39B H -0.0857 0.2793 0.0328 0.055 Uiso 1 1 calc R . . H39A H -0.1445 0.224 0.0564 0.055 Uiso 1 1 calc R . . C40 C 0.0908(3) 0.09611(17) 0.01101(7) 0.0520(9) Uani 1 1 d . . . H40B H 0.1644 0.0833 0.0203 0.062 Uiso 1 1 calc R . . H40A H 0.0758 0.0648 -0.0076 0.062 Uiso 1 1 calc R . . C41 C -0.0401(4) 0.4763(2) 0.07437(12) 0.1058(18) Uani 1 1 d . . . H41C H -0.0341 0.5204 0.0624 0.159 Uiso 1 1 calc R . . H41B H -0.0063 0.482 0.0958 0.159 Uiso 1 1 calc R . . H41A H -0.1193 0.4636 0.0768 0.159 Uiso 1 1 calc R . . C42 C -0.0252(9) 0.3971(3) 0.01227(13) 0.263(6) Uani 1 1 d . . . H42C H -0.1048 0.3847 0.0139 0.395 Uiso 1 1 calc R . . H42B H 0.015 0.3599 0.0008 0.395 Uiso 1 1 calc R . . H42A H -0.0176 0.4412 0.0004 0.395 Uiso 1 1 calc R . . C43 C 0.1787(5) 0.4419(3) 0.04674(18) 0.172(3) Uani 1 1 d . . . H43C H 0.2225 0.409 0.0337 0.258 Uiso 1 1 calc R . . H43B H 0.2146 0.4479 0.0679 0.258 Uiso 1 1 calc R . . H43A H 0.1752 0.4873 0.0357 0.258 Uiso 1 1 calc R . . C44 C 0.3024(3) 0.1388(2) 0.09743(9) 0.0667(11) Uani 1 1 d . . . H44C H 0.384 0.139 0.1002 0.1 Uiso 1 1 calc R . . H44B H 0.2843 0.1374 0.0744 0.1 Uiso 1 1 calc R . . H44A H 0.2707 0.0974 0.1081 0.1 Uiso 1 1 calc R . . C45 C 0.2833(2) 0.21417(18) 0.15916(8) 0.0481(8) Uani 1 1 d . . . H45C H 0.3645 0.2068 0.1606 0.072 Uiso 1 1 calc R . . H45B H 0.2442 0.1748 0.1693 0.072 Uiso 1 1 calc R . . H45A H 0.2634 0.2577 0.1703 0.072 Uiso 1 1 calc R . . C46 C 0.3191(3) 0.2953(2) 0.09787(9) 0.0654(11) Uani 1 1 d . . . H46C H 0.2993 0.3385 0.1093 0.098 Uiso 1 1 calc R . . H46B H 0.2989 0.2998 0.075 0.098 Uiso 1 1 calc R . . H46A H 0.3999 0.287 0.0998 0.098 Uiso 1 1 calc R . . C47 C 0.0385(2) 0.09664(12) 0.15202(6) 0.0217(6) Uani 1 1 d . . . H47C H -0.026 0.073 0.1618 0.033 Uiso 1 1 calc R . . H47B H 0.1032 0.0933 0.1665 0.033 Uiso 1 1 calc R . . H47A H 0.0566 0.0742 0.1314 0.102(14) 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 Al 0.0230(4) 0.0224(4) 0.0287(4) -0.0014(3) -0.0003(3) 0.0001(3) Si1 0.0250(4) 0.0300(5) 0.0545(5) -0.0026(4) -0.0054(4) -0.0036(4) Si2 0.0314(4) 0.0283(4) 0.0291(4) 0.0031(3) 0.0013(3) 0.0029(3) Si3 0.0252(4) 0.0497(5) 0.0401(5) -0.0095(4) 0.0050(4) -0.0015(4) Si4 0.1094(9) 0.0299(5) 0.0468(6) 0.0058(4) 0.0168(6) 0.0031(5) N1 0.0239(12) 0.0235(12) 0.0300(12) -0.0001(10) 0.0002(10) -0.0003(9) N2 0.0216(12) 0.0211(11) 0.0276(12) -0.0005(10) -0.0001(9) 0.0012(9) N3 0.0279(13) 0.0288(13) 0.0270(12) -0.0018(10) 0.0018(10) -0.0006(10) C1 0.0269(15) 0.0255(15) 0.0299(15) 0.0005(12) -0.0006(12) 0.0004(12) C2 0.0273(16) 0.0209(14) 0.0343(15) 0.0015(12) -0.0006(12) -0.0017(11) C3 0.0200(14) 0.0285(15) 0.0272(14) -0.0030(12) 0.0070(12) -0.0017(12) C4 0.0274(16) 0.0236(15) 0.0436(17) -0.0034(13) -0.0085(13) 0.0011(12) C5 0.0404(19) 0.0385(18) 0.051(2) 0.0030(15) 0.0036(16) 0.0081(15) C6 0.042(2) 0.041(2) 0.088(3) -0.0030(19) 0.007(2) 0.0109(16) C7 0.041(2) 0.038(2) 0.089(3) -0.007(2) -0.029(2) 0.0097(16) C8 0.074(3) 0.048(2) 0.063(2) -0.0102(19) -0.035(2) 0.024(2) C9 0.057(2) 0.0443(19) 0.0445(19) -0.0110(16) -0.0147(16) 0.0166(17) C10 0.0357(19) 0.063(2) 0.065(2) -0.0115(19) -0.0110(17) -0.0117(16) C11 0.043(2) 0.0311(19) 0.117(3) -0.006(2) -0.019(2) -0.0088(16) C12 0.037(2) 0.063(2) 0.071(2) 0.0088(19) 0.0069(17) -0.0103(17) C16 0.0245(15) 0.0230(14) 0.0334(15) -0.0049(12) -0.0027(12) -0.0016(11) C17 0.0329(17) 0.0266(15) 0.0456(18) -0.0087(14) -0.0075(14) 0.0032(13) C18 0.0396(19) 0.0313(17) 0.057(2) -0.0130(16) -0.0160(16) 0.0028(14) C19 0.037(2) 0.049(2) 0.089(3) -0.021(2) -0.0099(19) -0.0119(16) C20 0.054(2) 0.049(2) 0.061(2) 0.0011(18) 0.0031(18) -0.0273(18) C21 0.0402(19) 0.0382(18) 0.0461(18) -0.0024(15) 0.0028(15) -0.0132(14) C22 0.0328(17) 0.0289(16) 0.0472(18) -0.0073(14) -0.0066(14) 0.0035(13) C23 0.050(2) 0.0296(17) 0.058(2) -0.0138(16) -0.0136(17) 0.0081(15) C24 0.058(2) 0.0354(18) 0.055(2) -0.0159(16) -0.0193(17) 0.0015(15) C25 0.070(3) 0.0281(18) 0.079(3) 0.0001(18) -0.033(2) -0.0114(17) C26 0.046(2) 0.0429(19) 0.0410(18) 0.0096(15) 0.0069(15) -0.0056(15) C27 0.074(3) 0.0416(19) 0.051(2) 0.0032(17) 0.0241(18) 0.0016(17) C28 0.047(2) 0.0459(19) 0.0459(19) 0.0142(16) -0.0052(16) 0.0008(15) C29 0.0306(16) 0.0314(16) 0.0293(16) -0.0020(13) 0.0080(12) -0.0027(13) C30 0.060(2) 0.0316(17) 0.0317(17) -0.0015(15) 0.0119(15) -0.0033(15) C31 0.0390(17) 0.0289(16) 0.0282(15) -0.0023(13) 0.0021(12) 0.0008(13) C32 0.054(2) 0.0317(17) 0.0331(16) -0.0031(14) -0.0040(14) -0.0002(14) C33 0.069(2) 0.0324(18) 0.0410(18) -0.0056(15) -0.0104(17) 0.0020(16) C34 0.062(2) 0.052(2) 0.061(2) -0.0231(19) -0.0127(19) -0.0029(18) C35 0.055(2) 0.058(2) 0.051(2) -0.0191(18) -0.0236(18) 0.0176(18) C36 0.102(3) 0.051(2) 0.0364(19) -0.0030(17) -0.017(2) 0.015(2) C37 0.062(2) 0.053(2) 0.0326(17) -0.0091(16) 0.0066(16) 0.0033(18) C38 0.054(2) 0.0421(19) 0.0335(17) -0.0038(15) 0.0078(15) -0.0007(15) C39 0.046(2) 0.0434(19) 0.0481(19) -0.0071(16) -0.0104(16) 0.0105(15) C40 0.067(2) 0.048(2) 0.0409(19) -0.0185(16) -0.0071(17) 0.0176(17) C41 0.146(4) 0.052(3) 0.120(4) 0.025(3) 0.047(3) 0.033(3) C42 0.655(19) 0.050(3) 0.085(4) 0.035(3) -0.144(7) -0.033(6) C43 0.156(5) 0.075(4) 0.285(9) 0.086(5) 0.132(6) 0.020(4) C44 0.039(2) 0.089(3) 0.072(2) -0.031(2) -0.0037(18) 0.0234(19) C45 0.0271(17) 0.063(2) 0.054(2) -0.0100(17) -0.0044(15) 0.0065(16) C46 0.040(2) 0.089(3) 0.068(2) 0.004(2) 0.0134(18) -0.0178(19) C47 0.0197(14) 0.0165(13) 0.0289(14) -0.0003(12) -0.0003(11) 0.0018(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 Al N3 1.856(2) . ? Al N2 1.924(2) . ? Al N1 1.959(2) . ? Al C47 1.997(2) . ? Si1 N1 1.800(2) . ? Si1 C11 1.852(3) . ? Si1 C10 1.855(3) . ? Si1 C12 1.867(3) . ? Si2 N2 1.758(2) . ? Si2 C28 1.854(3) . ? Si2 C26 1.860(3) . ? Si2 C27 1.869(3) . ? Si3 N3 1.735(2) . ? Si3 C45 1.862(3) . ? Si3 C46 1.865(3) . ? Si3 C44 1.883(3) . ? Si4 C42 1.813(5) . ? Si4 C41 1.829(4) . ? Si4 C30 1.863(3) . ? Si4 C43 1.871(5) . ? N1 C1 1.341(3) . ? N2 C3 1.359(3) . ? N3 C29 1.450(3) . ? C1 C2 1.415(4) . ? C1 C4 1.504(4) . ? C2 C3 1.383(3) . ? C3 C16 1.554(3) . ? C4 C5 1.382(4) . ? C4 C9 1.383(4) . ? C5 C6 1.393(4) . ? C6 C7 1.370(5) . ? C7 C8 1.362(5) . ? C8 C9 1.384(4) . ? C16 C17 1.531(4) . ? C16 C22 1.545(4) . ? C16 C21 1.547(4) . ? C17 C18 1.534(4) . ? C18 C19 1.512(5) . ? C18 C24 1.522(4) . ? C19 C20 1.518(5) . ? C20 C21 1.537(4) . ? C20 C25 1.541(5) . ? C22 C23 1.526(4) . ? C23 C25 1.519(5) . ? C23 C24 1.524(4) . ? C29 C30 1.349(4) . ? C29 C31 1.543(4) . ? C31 C39 1.528(4) . ? C31 C32 1.533(4) . ? C31 C38 1.543(4) . ? C32 C33 1.538(4) . ? C33 C40 1.520(4) . ? C33 C34 1.521(4) . ? C34 C35 1.526(5) . ? C35 C36 1.527(5) . ? C35 C39 1.537(4) . ? C36 C37 1.527(5) . ? C37 C40 1.518(4) . ? C37 C38 1.523(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 N3 Al N2 113.09(10) . . ? N3 Al N1 109.37(10) . . ? N2 Al N1 95.12(9) . . ? N3 Al C47 107.38(10) . . ? N2 Al C47 110.27(10) . . ? N1 Al C47 121.36(10) . . ? N1 Si1 C11 108.77(12) . . ? N1 Si1 C10 116.53(13) . . ? C11 Si1 C10 106.62(17) . . ? N1 Si1 C12 109.02(13) . . ? C11 Si1 C12 107.92(17) . . ? C10 Si1 C12 107.67(15) . . ? N2 Si2 C28 113.41(12) . . ? N2 Si2 C26 108.62(12) . . ? C28 Si2 C26 107.35(15) . . ? N2 Si2 C27 113.69(13) . . ? C28 Si2 C27 110.87(16) . . ? C26 Si2 C27 102.06(15) . . ? N3 Si3 C45 110.56(12) . . ? N3 Si3 C46 112.22(14) . . ? C45 Si3 C46 107.45(16) . . ? N3 Si3 C44 116.20(14) . . ? C45 Si3 C44 103.59(16) . . ? C46 Si3 C44 106.14(18) . . ? C42 Si4 C41 110.3(3) . . ? C42 Si4 C30 123.20(19) . . ? C41 Si4 C30 106.88(17) . . ? C42 Si4 C43 106.2(4) . . ? C41 Si4 C43 104.4(3) . . ? C30 Si4 C43 104.1(2) . . ? C1 N1 Si1 120.92(18) . . ? C1 N1 Al 109.20(17) . . ? Si1 N1 Al 128.99(12) . . ? C3 N2 Si2 126.61(17) . . ? C3 N2 Al 108.24(16) . . ? Si2 N2 Al 121.43(11) . . ? C29 N3 Si3 116.00(17) . . ? C29 N3 Al 122.84(17) . . ? Si3 N3 Al 121.10(12) . . ? N1 C1 C2 125.0(2) . . ? N1 C1 C4 122.3(2) . . ? C2 C1 C4 112.7(2) . . ? C3 C2 C1 126.4(2) . . ? N2 C3 C2 120.9(2) . . ? N2 C3 C16 123.2(2) . . ? C2 C3 C16 115.8(2) . . ? C5 C4 C9 118.6(3) . . ? C5 C4 C1 119.9(3) . . ? C9 C4 C1 121.2(3) . . ? C4 C5 C6 120.3(3) . . ? C7 C6 C5 120.0(3) . . ? C8 C7 C6 120.1(3) . . ? C7 C8 C9 120.2(3) . . ? C4 C9 C8 120.7(3) . . ? C17 C16 C22 108.5(2) . . ? C17 C16 C21 107.3(2) . . ? C22 C16 C21 108.1(2) . . ? C17 C16 C3 113.5(2) . . ? C22 C16 C3 112.2(2) . . ? C21 C16 C3 107.0(2) . . ? C16 C17 C18 111.2(2) . . ? C19 C18 C24 110.4(3) . . ? C19 C18 C17 109.5(3) . . ? C24 C18 C17 109.0(2) . . ? C18 C19 C20 109.1(3) . . ? C19 C20 C21 110.2(3) . . ? C19 C20 C25 110.0(3) . . ? C21 C20 C25 108.3(3) . . ? C20 C21 C16 110.6(2) . . ? C23 C22 C16 110.5(2) . . ? C25 C23 C24 109.8(3) . . ? C25 C23 C22 109.5(3) . . ? C24 C23 C22 109.5(2) . . ? C18 C24 C23 109.5(3) . . ? C23 C25 C20 109.4(3) . . ? C30 C29 N3 119.3(2) . . ? C30 C29 C31 123.7(3) . . ? N3 C29 C31 116.9(2) . . ? C29 C30 Si4 143.7(2) . . ? C39 C31 C32 106.4(2) . . ? C39 C31 C29 111.6(2) . . ? C32 C31 C29 112.8(2) . . ? C39 C31 C38 108.3(2) . . ? C32 C31 C38 107.9(2) . . ? C29 C31 C38 109.6(2) . . ? C31 C32 C33 111.7(2) . . ? C40 C33 C34 109.8(3) . . ? C40 C33 C32 109.5(3) . . ? C34 C33 C32 108.9(3) . . ? C33 C34 C35 109.0(3) . . ? C34 C35 C36 109.3(3) . . ? C34 C35 C39 109.6(3) . . ? C36 C35 C39 109.6(3) . . ? C37 C36 C35 109.2(3) . . ? C40 C37 C38 109.4(3) . . ? C40 C37 C36 109.5(3) . . ? C38 C37 C36 109.7(3) . . ? C37 C38 C31 111.3(3) . . ? C31 C39 C35 111.5(2) . . ? C37 C40 C33 109.7(3) . . ? #===END data_(7)-jul2900 _database_code_depnum_ccdc_archive 'CCDC 668986' _audit_creation_date 2000-07-28T16:44:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H68 N2 Si4 Sn' _chemical_formula_sum 'C36 H68 N2 Si4 Sn' _chemical_formula_weight 759.97 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.1969(3) _cell_length_b 23.3707(5) _cell_length_c 22.0743(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8355.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25849 _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 0.2 _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.751 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.834 #----------------------------------------------------------------------------# # 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 38603 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 27.86 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 9857 _reflns_number_gt 7747 _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^)+(0.0272P)^2^+5.5835P] 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 9857 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.073 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.35 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.062 #----------------------------------------------------------------------------# # 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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 Sn Sn 0.587394(9) 0.245434(6) 0.175231(6) 0.02478(5) Uani 1 1 d . . . Si1 Si 0.41332(4) 0.17424(3) 0.14213(3) 0.02746(13) Uani 1 1 d . . . Si2 Si 0.67416(4) 0.09241(3) 0.18419(3) 0.02988(14) Uani 1 1 d . . . Si3 Si 0.76014(4) 0.31912(3) 0.14193(3) 0.02959(14) Uani 1 1 d . . . Si4 Si 0.49867(4) 0.39654(2) 0.17862(2) 0.02321(12) Uani 1 1 d . . . N1 N 0.61577(11) 0.14188(7) 0.14600(7) 0.0245(4) Uani 1 1 d . . . N2 N 0.55618(10) 0.34583(7) 0.14112(7) 0.0224(3) Uani 1 1 d . . . C1 C 0.51054(13) 0.19698(8) 0.10338(9) 0.0236(4) Uani 1 1 d . . . H1 H 0.5003 0.22 0.066 0.028 Uiso 1 1 calc R . . C2 C 0.57653(12) 0.15535(8) 0.09615(9) 0.0206(4) Uani 1 1 d . . . C3 C 0.60137(13) 0.13130(8) 0.03370(9) 0.0254(4) Uani 1 1 d . . . C4 C 0.59407(15) 0.06533(9) 0.03552(10) 0.0326(5) Uani 1 1 d . . . H4A H 0.6297 0.05 0.0682 0.039 Uiso 1 1 calc R . . H4B H 0.5363 0.0544 0.0445 0.039 Uiso 1 1 calc R . . C5 C 0.62030(17) 0.03929(10) -0.02556(11) 0.0438(6) Uani 1 1 d . . . H5 H 0.6155 -0.0033 -0.0234 0.053 Uiso 1 1 calc R . . C6 C 0.56446(19) 0.06178(12) -0.07567(11) 0.0493(7) Uani 1 1 d . . . H6A H 0.5064 0.0511 -0.0672 0.059 Uiso 1 1 calc R . . H6B H 0.5806 0.0446 -0.1149 0.059 Uiso 1 1 calc R . . C7 C 0.57236(18) 0.12673(12) -0.07889(10) 0.0450(6) Uani 1 1 d . . . H7 H 0.5359 0.1416 -0.1119 0.054 Uiso 1 1 calc R . . C8 C 0.54583(15) 0.15301(10) -0.01812(9) 0.0333(5) Uani 1 1 d . . . H8A H 0.4877 0.1427 -0.0096 0.04 Uiso 1 1 calc R . . H8B H 0.5495 0.1952 -0.0206 0.04 Uiso 1 1 calc R . . C9 C 0.69120(14) 0.14726(9) 0.01864(10) 0.0312(5) Uani 1 1 d . . . H9A H 0.6965 0.1894 0.0164 0.037 Uiso 1 1 calc R . . H9B H 0.7281 0.1334 0.0513 0.037 Uiso 1 1 calc R . . C10 C 0.71765(16) 0.12082(11) -0.04199(11) 0.0434(6) Uani 1 1 d . . . H10 H 0.7762 0.1315 -0.0507 0.052 Uiso 1 1 calc R . . C11 C 0.71026(18) 0.05562(12) -0.03844(12) 0.0503(7) Uani 1 1 d . . . H11A H 0.7463 0.0408 -0.0058 0.06 Uiso 1 1 calc R . . H11B H 0.7283 0.0383 -0.0772 0.06 Uiso 1 1 calc R . . C12 C 0.66215(18) 0.14325(12) -0.09240(11) 0.0515(7) Uani 1 1 d . . . H12A H 0.6794 0.1267 -0.1317 0.062 Uiso 1 1 calc R . . H12B H 0.6671 0.1854 -0.0951 0.062 Uiso 1 1 calc R . . C13 C 0.43102(17) 0.14928(14) 0.22127(12) 0.0544(8) Uani 1 1 d . . . H13A H 0.4681 0.1161 0.2209 0.082 Uiso 1 1 calc R . . H13B H 0.3782 0.1384 0.2396 0.082 Uiso 1 1 calc R . . H13C H 0.4561 0.1802 0.245 0.082 Uiso 1 1 calc R . . C14 C 0.34252(17) 0.23694(12) 0.14145(17) 0.0591(8) Uani 1 1 d . . . H14A H 0.3338 0.2496 0.0996 0.089 Uiso 1 1 calc R . . H14B H 0.367 0.2682 0.165 0.089 Uiso 1 1 calc R . . H14C H 0.2894 0.2261 0.1594 0.089 Uiso 1 1 calc R . . C15 C 0.36324(18) 0.11403(13) 0.10045(13) 0.0590(8) Uani 1 1 d . . . H15A H 0.3999 0.0807 0.1007 0.088 Uiso 1 1 calc R . . H15B H 0.3525 0.1257 0.0585 0.088 Uiso 1 1 calc R . . H15C H 0.311 0.1041 0.1202 0.088 Uiso 1 1 calc R . . C16 C 0.77726(16) 0.07431(12) 0.15186(12) 0.0483(7) Uani 1 1 d . . . H16A H 0.7701 0.0573 0.1116 0.072 Uiso 1 1 calc R . . H16B H 0.8053 0.047 0.1785 0.072 Uiso 1 1 calc R . . H16C H 0.8105 0.1092 0.1484 0.072 Uiso 1 1 calc R . . C17 C 0.6133(2) 0.02502(12) 0.19573(14) 0.0553(7) Uani 1 1 d . . . H17A H 0.6025 0.007 0.1564 0.083 Uiso 1 1 calc R . . H17B H 0.5607 0.0342 0.2155 0.083 Uiso 1 1 calc R . . H17C H 0.6448 -0.0014 0.2213 0.083 Uiso 1 1 calc R . . C18 C 0.69253(17) 0.12445(12) 0.26015(11) 0.0472(7) Uani 1 1 d . . . H18A H 0.6395 0.1345 0.2787 0.071 Uiso 1 1 calc R . . H18B H 0.7264 0.159 0.2558 0.071 Uiso 1 1 calc R . . H18C H 0.7214 0.0968 0.2859 0.071 Uiso 1 1 calc R . . C19 C 0.66555(12) 0.29192(8) 0.10262(9) 0.0238(4) Uani 1 1 d . . . H19 H 0.6781 0.2675 0.0666 0.029 Uiso 1 1 calc R . . C20 C 0.59778(12) 0.33138(8) 0.09263(9) 0.0208(4) Uani 1 1 d . . . C21 C 0.57359(12) 0.35172(8) 0.02828(9) 0.0222(4) Uani 1 1 d . . . C22 C 0.48447(13) 0.33295(9) 0.01313(9) 0.0267(4) Uani 1 1 d . . . H22A H 0.4808 0.2907 0.0139 0.032 Uiso 1 1 calc R . . H22B H 0.4461 0.3483 0.044 0.032 Uiso 1 1 calc R . . C23 C 0.45932(15) 0.35500(9) -0.04984(10) 0.0333(5) Uani 1 1 d . . . H23 H 0.4016 0.3424 -0.059 0.04 Uiso 1 1 calc R . . C24 C 0.46334(15) 0.42020(9) -0.05077(10) 0.0339(5) Uani 1 1 d . . . H24A H 0.4251 0.4361 -0.0201 0.041 Uiso 1 1 calc R . . H24B H 0.4462 0.4345 -0.0911 0.041 Uiso 1 1 calc R . . C25 C 0.55150(14) 0.43957(9) -0.03716(9) 0.0302(5) Uani 1 1 d . . . H25 H 0.5539 0.4823 -0.0378 0.036 Uiso 1 1 calc R . . C26 C 0.57722(13) 0.41799(8) 0.02589(9) 0.0252(4) Uani 1 1 d . . . H26A H 0.5398 0.4342 0.0569 0.03 Uiso 1 1 calc R . . H26B H 0.634 0.431 0.035 0.03 Uiso 1 1 calc R . . C27 C 0.63163(14) 0.32847(9) -0.02109(9) 0.0291(5) Uani 1 1 d . . . H27A H 0.6889 0.3407 -0.0124 0.035 Uiso 1 1 calc R . . H27B H 0.6302 0.2861 -0.0207 0.035 Uiso 1 1 calc R . . C28 C 0.60584(17) 0.35034(10) -0.08400(10) 0.0370(6) Uani 1 1 d . . . H28 H 0.6443 0.3346 -0.1152 0.044 Uiso 1 1 calc R . . C29 C 0.61043(17) 0.41596(10) -0.08476(10) 0.0380(6) Uani 1 1 d . . . H29A H 0.6675 0.4286 -0.0759 0.046 Uiso 1 1 calc R . . H29B H 0.5949 0.4305 -0.1253 0.046 Uiso 1 1 calc R . . C30 C 0.51803(17) 0.33071(10) -0.09793(10) 0.0424(6) Uani 1 1 d . . . H30A H 0.5154 0.2884 -0.0977 0.051 Uiso 1 1 calc R . . H30B H 0.5014 0.3443 -0.1386 0.051 Uiso 1 1 calc R . . C31 C 0.8075(2) 0.37919(17) 0.09814(15) 0.0877(13) Uani 1 1 d . . . H31A H 0.7687 0.4113 0.0963 0.132 Uiso 1 1 calc R . . H31B H 0.8203 0.3662 0.057 0.132 Uiso 1 1 calc R . . H31C H 0.8584 0.3916 0.1182 0.132 Uiso 1 1 calc R . . C32 C 0.8336(2) 0.25870(14) 0.1454(2) 0.0838(13) Uani 1 1 d . . . H32A H 0.8439 0.2444 0.1043 0.126 Uiso 1 1 calc R . . H32B H 0.8101 0.228 0.1702 0.126 Uiso 1 1 calc R . . H32C H 0.8856 0.2717 0.1634 0.126 Uiso 1 1 calc R . . C33 C 0.74025(16) 0.34680(14) 0.21957(12) 0.0555(8) Uani 1 1 d . . . H33A H 0.7017 0.379 0.2174 0.083 Uiso 1 1 calc R . . H33B H 0.7923 0.3596 0.2377 0.083 Uiso 1 1 calc R . . H33C H 0.7163 0.3163 0.2445 0.083 Uiso 1 1 calc R . . C34 C 0.39620(14) 0.41585(10) 0.14546(10) 0.0348(5) Uani 1 1 d . . . H34A H 0.4042 0.4319 0.1049 0.052 Uiso 1 1 calc R . . H34B H 0.3691 0.4443 0.1714 0.052 Uiso 1 1 calc R . . H34C H 0.3616 0.3815 0.1428 0.052 Uiso 1 1 calc R . . C35 C 0.47899(15) 0.36657(10) 0.25541(10) 0.0366(5) Uani 1 1 d . . . H35A H 0.4455 0.3318 0.2518 0.055 Uiso 1 1 calc R . . H35B H 0.4494 0.3949 0.28 0.055 Uiso 1 1 calc R . . H35C H 0.5317 0.3573 0.2749 0.055 Uiso 1 1 calc R . . C36 C 0.56204(15) 0.46266(10) 0.18760(11) 0.0365(5) Uani 1 1 d . . . H36A H 0.5731 0.4793 0.1477 0.055 Uiso 1 1 calc R . . H36B H 0.6144 0.453 0.2074 0.055 Uiso 1 1 calc R . . H36C H 0.5319 0.4904 0.2125 0.055 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 Sn 0.02740(8) 0.02698(8) 0.01997(8) -0.00074(5) -0.00117(6) -0.00013(6) Si1 0.0227(3) 0.0304(3) 0.0293(3) -0.0032(2) 0.0028(2) -0.0004(2) Si2 0.0299(3) 0.0323(3) 0.0275(3) 0.0057(2) 0.0014(3) 0.0065(2) Si3 0.0217(3) 0.0360(3) 0.0310(3) -0.0050(3) -0.0042(2) -0.0002(2) Si4 0.0234(3) 0.0248(3) 0.0215(3) -0.0015(2) 0.0008(2) 0.0007(2) N1 0.0255(9) 0.0271(9) 0.0210(9) -0.0018(7) 0.0008(7) 0.0016(7) N2 0.0218(9) 0.0256(8) 0.0199(8) 0.0010(7) 0.0003(7) -0.0003(7) C1 0.0267(11) 0.0249(10) 0.0190(10) 0.0016(8) 0.0001(8) 0.0014(8) C2 0.0212(10) 0.0197(9) 0.0209(10) 0.0006(7) 0.0039(8) -0.0052(7) C3 0.0295(11) 0.0231(9) 0.0237(10) -0.0025(8) 0.0020(8) -0.0028(8) C4 0.0398(13) 0.0269(11) 0.0312(12) -0.0049(9) 0.0050(10) -0.0052(10) C5 0.0592(17) 0.0300(12) 0.0421(14) -0.0143(11) 0.0100(13) -0.0068(11) C6 0.0638(18) 0.0527(16) 0.0316(14) -0.0183(12) 0.0041(12) -0.0165(14) C7 0.0619(18) 0.0512(16) 0.0220(12) -0.0059(11) -0.0016(11) -0.0046(13) C8 0.0387(13) 0.0395(12) 0.0217(11) -0.0011(9) -0.0008(9) -0.0025(10) C9 0.0317(12) 0.0326(11) 0.0293(11) -0.0076(9) 0.0100(9) -0.0063(9) C10 0.0437(15) 0.0508(15) 0.0357(14) -0.0148(11) 0.0193(11) -0.0093(12) C11 0.0566(18) 0.0514(16) 0.0428(15) -0.0220(12) 0.0155(13) 0.0049(13) C12 0.071(2) 0.0567(17) 0.0262(13) -0.0093(12) 0.0200(13) -0.0125(15) C13 0.0377(15) 0.086(2) 0.0391(15) 0.0161(14) 0.0086(12) -0.0093(14) C14 0.0324(15) 0.0514(17) 0.094(2) 0.0082(16) 0.0166(15) 0.0123(12) C15 0.0495(18) 0.0667(19) 0.0607(18) -0.0250(15) 0.0166(14) -0.0286(15) C16 0.0379(15) 0.0604(17) 0.0466(15) 0.0035(13) 0.0014(12) 0.0219(12) C17 0.071(2) 0.0419(15) 0.0532(17) 0.0183(13) 0.0023(15) -0.0034(14) C18 0.0457(16) 0.0664(18) 0.0294(13) 0.0043(12) -0.0084(11) 0.0128(13) C19 0.0249(11) 0.0249(10) 0.0216(10) -0.0027(8) -0.0022(8) 0.0021(8) C20 0.0220(10) 0.0197(9) 0.0207(10) -0.0011(7) -0.0027(8) -0.0049(7) C21 0.0257(11) 0.0211(9) 0.0197(10) 0.0004(8) 0.0002(8) 0.0001(8) C22 0.0316(12) 0.0241(10) 0.0245(11) 0.0028(8) -0.0069(9) -0.0024(8) C23 0.0392(13) 0.0322(11) 0.0285(12) 0.0011(9) -0.0127(10) -0.0006(10) C24 0.0413(14) 0.0321(12) 0.0283(12) 0.0025(9) -0.0091(10) 0.0043(10) C25 0.0401(13) 0.0235(10) 0.0271(11) 0.0048(8) -0.0006(10) 0.0014(9) C26 0.0262(11) 0.0238(10) 0.0256(11) -0.0010(8) 0.0002(8) -0.0010(8) C27 0.0363(13) 0.0289(11) 0.0222(10) 0.0002(8) 0.0031(9) 0.0070(9) C28 0.0564(16) 0.0352(12) 0.0194(11) 0.0011(9) 0.0063(10) 0.0104(11) C29 0.0513(15) 0.0370(13) 0.0258(12) 0.0084(10) 0.0052(11) 0.0032(11) C30 0.0695(19) 0.0347(13) 0.0229(12) -0.0010(10) -0.0126(12) 0.0028(12) C31 0.079(3) 0.118(3) 0.066(2) 0.027(2) -0.0257(19) -0.066(2) C32 0.0469(18) 0.079(2) 0.125(3) -0.052(2) -0.046(2) 0.0318(17) C33 0.0326(14) 0.086(2) 0.0476(16) -0.0264(15) -0.0090(12) -0.0038(14) C34 0.0299(12) 0.0413(13) 0.0331(12) -0.0023(10) -0.0022(10) 0.0073(10) C35 0.0396(14) 0.0446(13) 0.0256(11) 0.0013(10) 0.0073(10) 0.0061(11) C36 0.0397(13) 0.0300(11) 0.0397(13) -0.0065(10) 0.0017(11) -0.0036(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 Sn C1 2.312(2) . ? Sn C19 2.313(2) . ? Sn N2 2.5156(16) . ? Sn N1 2.5466(16) . ? Si1 C14 1.861(3) . ? Si1 C13 1.864(3) . ? Si1 C15 1.867(3) . ? Si1 C1 1.869(2) . ? Si2 N1 1.7152(18) . ? Si2 C18 1.860(2) . ? Si2 C16 1.865(3) . ? Si2 C17 1.876(3) . ? Si3 C32 1.848(3) . ? Si3 C33 1.860(3) . ? Si3 C31 1.869(3) . ? Si3 C19 1.872(2) . ? Si4 N2 1.7196(17) . ? Si4 C35 1.862(2) . ? Si4 C36 1.866(2) . ? Si4 C34 1.869(2) . ? N1 C2 1.309(2) . ? N2 C20 1.309(2) . ? C1 C2 1.454(3) . ? C2 C3 1.542(3) . ? C3 C9 1.538(3) . ? C3 C8 1.541(3) . ? C3 C4 1.547(3) . ? C4 C5 1.539(3) . ? C5 C6 1.522(4) . ? C5 C11 1.533(4) . ? C6 C7 1.525(4) . ? C7 C12 1.534(4) . ? C7 C8 1.537(3) . ? C9 C10 1.535(3) . ? C10 C12 1.524(4) . ? C10 C11 1.531(4) . ? C19 C20 1.451(3) . ? C20 C21 1.548(3) . ? C21 C27 1.538(3) . ? C21 C22 1.545(3) . ? C21 C26 1.551(3) . ? C22 C23 1.538(3) . ? C23 C24 1.525(3) . ? C23 C30 1.534(3) . ? C24 C25 1.528(3) . ? C25 C29 1.523(3) . ? C25 C26 1.538(3) . ? C27 C28 1.538(3) . ? C28 C30 1.526(4) . ? C28 C29 1.535(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn C19 92.83(7) . . ? C1 Sn N2 98.24(6) . . ? C19 Sn N2 57.63(6) . . ? C1 Sn N1 57.18(6) . . ? C19 Sn N1 99.90(6) . . ? N2 Sn N1 147.88(5) . . ? C14 Si1 C13 110.42(15) . . ? C14 Si1 C15 108.77(15) . . ? C13 Si1 C15 107.04(15) . . ? C14 Si1 C1 106.95(11) . . ? C13 Si1 C1 112.85(11) . . ? C15 Si1 C1 110.79(11) . . ? N1 Si2 C18 105.06(10) . . ? N1 Si2 C16 117.29(10) . . ? C18 Si2 C16 107.04(13) . . ? N1 Si2 C17 110.05(12) . . ? C18 Si2 C17 107.44(13) . . ? C16 Si2 C17 109.41(14) . . ? C32 Si3 C33 109.85(17) . . ? C32 Si3 C31 109.3(2) . . ? C33 Si3 C31 106.64(16) . . ? C32 Si3 C19 106.63(12) . . ? C33 Si3 C19 113.80(11) . . ? C31 Si3 C19 110.57(12) . . ? N2 Si4 C35 105.77(9) . . ? N2 Si4 C36 108.90(10) . . ? C35 Si4 C36 108.00(11) . . ? N2 Si4 C34 117.32(9) . . ? C35 Si4 C34 107.18(11) . . ? C36 Si4 C34 109.28(11) . . ? C2 N1 Si2 147.45(15) . . ? C2 N1 Sn 84.08(11) . . ? Si2 N1 Sn 127.99(9) . . ? C20 N2 Si4 148.23(15) . . ? C20 N2 Sn 84.30(11) . . ? Si4 N2 Sn 127.42(8) . . ? C2 C1 Si1 118.63(14) . . ? C2 C1 Sn 90.41(12) . . ? Si1 C1 Sn 106.19(9) . . ? N1 C2 C1 115.18(17) . . ? N1 C2 C3 122.49(17) . . ? C1 C2 C3 122.25(17) . . ? C9 C3 C8 108.17(17) . . ? C9 C3 C2 110.58(16) . . ? C8 C3 C2 113.04(17) . . ? C9 C3 C4 108.63(17) . . ? C8 C3 C4 107.62(17) . . ? C2 C3 C4 108.67(16) . . ? C5 C4 C3 110.51(18) . . ? C6 C5 C11 110.1(2) . . ? C6 C5 C4 109.6(2) . . ? C11 C5 C4 109.1(2) . . ? C5 C6 C7 109.1(2) . . ? C6 C7 C12 109.8(2) . . ? C6 C7 C8 109.5(2) . . ? C12 C7 C8 109.5(2) . . ? C7 C8 C3 110.68(19) . . ? C10 C9 C3 110.78(18) . . ? C12 C10 C11 109.5(2) . . ? C12 C10 C9 109.5(2) . . ? C11 C10 C9 109.53(19) . . ? C10 C11 C5 109.4(2) . . ? C10 C12 C7 109.3(2) . . ? C20 C19 Si3 118.28(14) . . ? C20 C19 Sn 89.42(12) . . ? Si3 C19 Sn 106.63(9) . . ? N2 C20 C19 115.42(17) . . ? N2 C20 C21 122.74(17) . . ? C19 C20 C21 121.74(17) . . ? C27 C21 C22 108.50(16) . . ? C27 C21 C20 112.76(16) . . ? C22 C21 C20 110.34(16) . . ? C27 C21 C26 107.79(16) . . ? C22 C21 C26 108.15(16) . . ? C20 C21 C26 109.16(15) . . ? C23 C22 C21 110.36(17) . . ? C24 C23 C30 109.51(19) . . ? C24 C23 C22 109.62(17) . . ? C30 C23 C22 109.71(18) . . ? C23 C24 C25 109.47(18) . . ? C29 C25 C24 110.04(19) . . ? C29 C25 C26 109.62(18) . . ? C24 C25 C26 109.50(17) . . ? C25 C26 C21 110.38(16) . . ? C28 C27 C21 110.88(17) . . ? C30 C28 C29 110.1(2) . . ? C30 C28 C27 109.58(19) . . ? C29 C28 C27 109.19(18) . . ? C25 C29 C28 108.91(19) . . ? C28 C30 C23 109.10(18) . . ? #===END data_(8)-jul100 _database_code_depnum_ccdc_archive 'CCDC 668987' _audit_creation_date 2000-07-06T17:06:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H76 Li N3 O2 Si3' _chemical_formula_sum 'C42 H76 Li N3 O2 Si3' _chemical_formula_weight 746.27 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.3106(7) _cell_length_b 18.0975(4) _cell_length_c 13.1943(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4611.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22541 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.138 _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 18684 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_unetI/netI 0.047 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.97 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 7935 _reflns_number_gt 7322 _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^)+(0.0404P)^2^+1.3615P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7935 _refine_ls_number_parameters 464 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.07(8) _refine_diff_density_max 0.221 _refine_diff_density_min -0.179 _refine_diff_density_rms 0.033 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li Li 0.2117(2) 1.0322(2) 0.5839(3) 0.0395(9) Uani 1 1 d . . . Si1 Si 0.20069(3) 0.97859(3) 0.36752(4) 0.02280(12) Uani 1 1 d . . . Si2 Si 0.45326(3) 0.90807(3) 0.46442(6) 0.03768(16) Uani 1 1 d . . . Si3 Si 0.25379(3) 0.93159(3) 0.21813(5) 0.02951(13) Uani 1 1 d . . . N1 N 0.13569(9) 0.91365(9) 0.40284(14) 0.0270(4) Uani 1 1 d . . . N2 N 0.13462(8) 1.04601(9) 0.34889(13) 0.0250(4) Uani 1 1 d . . . N3 N 0.25536(8) 1.01160(9) 0.45433(14) 0.0258(4) Uani 1 1 d . . . O1 O 0.12924(8) 1.08393(9) 0.61562(13) 0.0403(4) Uani 1 1 d . . . O2 O 0.24783(10) 1.00387(11) 0.71450(16) 0.0530(5) Uani 1 1 d . . . C1 C 0.06947(11) 0.94505(11) 0.40831(16) 0.0257(4) Uani 1 1 d . . . C2 C 0.06922(10) 1.02125(11) 0.37970(16) 0.0245(4) Uani 1 1 d . . . C3 C 0.00844(11) 1.06183(12) 0.38803(16) 0.0297(5) Uani 1 1 d . . . H3 H 0.0084 1.113 0.3717 0.036 Uiso 1 1 calc R . . C4 C -0.05234(12) 1.02794(14) 0.42022(17) 0.0344(5) Uani 1 1 d . . . H4 H -0.0936 1.0561 0.4265 0.041 Uiso 1 1 calc R . . C5 C -0.05294(11) 0.95345(13) 0.44312(18) 0.0350(5) Uani 1 1 d . . . H5 H -0.0949 0.9302 0.4629 0.042 Uiso 1 1 calc R . . C6 C 0.00815(11) 0.91219(12) 0.43733(16) 0.0302(5) Uani 1 1 d . . . H6 H 0.0074 0.861 0.4535 0.036 Uiso 1 1 calc R . . C7 C 0.14183(12) 0.83284(12) 0.4040(2) 0.0372(6) Uani 1 1 d . . . H7B H 0.1775 0.8188 0.3537 0.045 Uiso 1 1 calc R . . H7A H 0.0973 0.8121 0.3801 0.045 Uiso 1 1 calc R . . C8 C 0.16008(13) 0.79488(14) 0.5045(2) 0.0473(7) Uani 1 1 d . . . C9 C 0.10924(18) 0.8114(2) 0.5872(3) 0.0689(9) Uani 1 1 d . . . H9C H 0.0631 0.7946 0.5667 0.103 Uiso 1 1 calc R . . H9B H 0.1082 0.8647 0.5999 0.103 Uiso 1 1 calc R . . H9A H 0.1232 0.7856 0.6493 0.103 Uiso 1 1 calc R . . C10 C 0.23289(15) 0.81698(16) 0.5365(3) 0.0671(10) Uani 1 1 d . . . H10C H 0.2461 0.7892 0.5973 0.101 Uiso 1 1 calc R . . H10B H 0.234 0.87 0.5513 0.101 Uiso 1 1 calc R . . H10A H 0.2654 0.8059 0.4816 0.101 Uiso 1 1 calc R . . C11 C 0.16023(17) 0.71095(15) 0.4822(3) 0.0748(12) Uani 1 1 d . . . H11C H 0.1138 0.6955 0.4609 0.112 Uiso 1 1 calc R . . H11B H 0.1735 0.6839 0.5435 0.112 Uiso 1 1 calc R . . H11A H 0.1935 0.7003 0.428 0.112 Uiso 1 1 calc R . . C12 C 0.14668(11) 1.12583(11) 0.34416(16) 0.0284(5) Uani 1 1 d . . . H12B H 0.1942 1.1353 0.3693 0.034 Uiso 1 1 calc R . . H12A H 0.1143 1.1498 0.3922 0.034 Uiso 1 1 calc R . . C13 C 0.13909(12) 1.16507(12) 0.24101(17) 0.0330(5) Uani 1 1 d . . . C14 C 0.19502(14) 1.13789(14) 0.1694(2) 0.0445(6) Uani 1 1 d . . . H14C H 0.1922 1.1652 0.1054 0.067 Uiso 1 1 calc R . . H14B H 0.1884 1.0851 0.1563 0.067 Uiso 1 1 calc R . . H14A H 0.2406 1.1458 0.2002 0.067 Uiso 1 1 calc R . . C15 C 0.06873(13) 1.15321(16) 0.19198(19) 0.0469(7) Uani 1 1 d . . . H15C H 0.0666 1.1804 0.1278 0.07 Uiso 1 1 calc R . . H15B H 0.0323 1.1711 0.2375 0.07 Uiso 1 1 calc R . . H15A H 0.0619 1.1004 0.179 0.07 Uiso 1 1 calc R . . C16 C 0.14926(16) 1.24790(13) 0.2608(2) 0.0490(7) Uani 1 1 d . . . H16C H 0.1126 1.2658 0.3059 0.073 Uiso 1 1 calc R . . H16B H 0.1472 1.2748 0.1964 0.073 Uiso 1 1 calc R . . H16A H 0.1945 1.256 0.2927 0.073 Uiso 1 1 calc R . . C17 C 0.32701(10) 1.00843(11) 0.46407(17) 0.0252(4) Uani 1 1 d . . . C18 C 0.36401(11) 0.94454(11) 0.45517(18) 0.0304(5) Uani 1 1 d . . . H18 H 0.3323(14) 0.9009(15) 0.441(2) 0.043(7) Uiso 1 1 d . . . C19 C 0.18364(13) 0.92037(14) 0.12133(19) 0.0409(6) Uani 1 1 d . . . H19C H 0.2026 0.8964 0.0608 0.061 Uiso 1 1 calc R . . H19B H 0.1652 0.969 0.1031 0.061 Uiso 1 1 calc R . . H19A H 0.1464 0.8898 0.1495 0.061 Uiso 1 1 calc R . . C20 C 0.32591(13) 0.98981(15) 0.1670(2) 0.0443(6) Uani 1 1 d . . . H20C H 0.308 1.0387 0.1488 0.066 Uiso 1 1 calc R . . H20B H 0.3455 0.9661 0.1067 0.066 Uiso 1 1 calc R . . H20A H 0.362 0.9951 0.2187 0.066 Uiso 1 1 calc R . . C21 C 0.29426(15) 0.83670(15) 0.2297(2) 0.0497(7) Uani 1 1 d . . . H21C H 0.313 0.8216 0.1638 0.075 Uiso 1 1 calc R . . H21B H 0.259 0.8011 0.2515 0.075 Uiso 1 1 calc R . . H21A H 0.3317 0.8382 0.2797 0.075 Uiso 1 1 calc R . . C22 C 0.51745(16) 0.9496(2) 0.3741(4) 0.0792(11) Uani 1 1 d . . . H22C H 0.5206 1.0029 0.3861 0.119 Uiso 1 1 calc R . . H22B H 0.5023 0.9406 0.3043 0.119 Uiso 1 1 calc R . . H22A H 0.5629 0.9268 0.3847 0.119 Uiso 1 1 calc R . . C23 C 0.44486(17) 0.80793(17) 0.4295(3) 0.0708(11) Uani 1 1 d . . . H23C H 0.4264 0.8038 0.3605 0.106 Uiso 1 1 calc R . . H23B H 0.4134 0.7834 0.477 0.106 Uiso 1 1 calc R . . H23A H 0.4905 0.7843 0.4326 0.106 Uiso 1 1 calc R . . C24 C 0.49213(16) 0.90669(17) 0.5944(2) 0.0588(8) Uani 1 1 d . . . H24C H 0.4638 0.8757 0.639 0.088 Uiso 1 1 calc R . . H24B H 0.4938 0.9571 0.6214 0.088 Uiso 1 1 calc R . . H24A H 0.5392 0.8866 0.5909 0.088 Uiso 1 1 calc R . . C25 C 0.36086(10) 1.08461(11) 0.48388(17) 0.0294(5) Uani 1 1 d . . . C26 C 0.37829(13) 1.11974(13) 0.3809(2) 0.0431(6) Uani 1 1 d . . . H26B H 0.3355 1.1243 0.34 0.052 Uiso 1 1 calc R . . H26A H 0.4109 1.0874 0.3437 0.052 Uiso 1 1 calc R . . C27 C 0.41097(16) 1.19661(15) 0.3950(3) 0.0607(8) Uani 1 1 d . . . H27 H 0.422 1.2185 0.3273 0.073 Uiso 1 1 calc R . . C28 C 0.47766(15) 1.18918(16) 0.4575(3) 0.0719(10) Uani 1 1 d . . . H28B H 0.5107 1.1563 0.422 0.086 Uiso 1 1 calc R . . H28A H 0.4997 1.2382 0.4656 0.086 Uiso 1 1 calc R . . C29 C 0.45999(14) 1.15706(15) 0.5615(3) 0.0616(9) Uani 1 1 d . . . H29 H 0.5034 1.1523 0.6023 0.074 Uiso 1 1 calc R . . C30 C 0.42791(13) 1.08024(13) 0.5463(2) 0.0450(6) Uani 1 1 d . . . H30B H 0.4177 1.058 0.6132 0.054 Uiso 1 1 calc R . . H30A H 0.4615 1.0479 0.5111 0.054 Uiso 1 1 calc R . . C31 C 0.31154(12) 1.13758(12) 0.5406(2) 0.0386(6) Uani 1 1 d . . . H31B H 0.2678 1.1422 0.5021 0.046 Uiso 1 1 calc R . . H31A H 0.3004 1.1166 0.608 0.046 Uiso 1 1 calc R . . C32 C 0.34381(14) 1.21418(14) 0.5541(3) 0.0519(7) Uani 1 1 d . . . H32 H 0.3103 1.247 0.5902 0.062 Uiso 1 1 calc R . . C33 C 0.40948(16) 1.20710(16) 0.6169(3) 0.0641(9) Uani 1 1 d . . . H33B H 0.4305 1.2564 0.6272 0.077 Uiso 1 1 calc R . . H33A H 0.3984 1.186 0.6842 0.077 Uiso 1 1 calc R . . C34 C 0.36025(16) 1.24687(14) 0.4515(3) 0.0615(8) Uani 1 1 d . . . H34B H 0.3809 1.2965 0.4602 0.074 Uiso 1 1 calc R . . H34A H 0.3171 1.2522 0.4117 0.074 Uiso 1 1 calc R . . C35 C 0.12611(15) 1.16210(14) 0.6348(2) 0.0477(6) Uani 1 1 d . . . H35B H 0.1208 1.1898 0.5705 0.057 Uiso 1 1 calc R . . H35A H 0.1688 1.1791 0.6692 0.057 Uiso 1 1 calc R . . C36 C 0.06390(14) 1.17337(15) 0.7019(2) 0.0473(6) Uani 1 1 d . . . H36B H 0.0431 1.2228 0.6916 0.057 Uiso 1 1 calc R . . H36A H 0.076 1.1672 0.7743 0.057 Uiso 1 1 calc R . . C37 C 0.01575(13) 1.11269(15) 0.6662(2) 0.0450(6) Uani 1 1 d . . . H37B H -0.0189 1.1001 0.7187 0.054 Uiso 1 1 calc R . . H37A H -0.0086 1.127 0.6031 0.054 Uiso 1 1 calc R . . C38 C 0.06509(12) 1.04925(13) 0.64789(18) 0.0369(5) Uani 1 1 d . . . H38B H 0.0722 1.0204 0.7108 0.044 Uiso 1 1 calc R . . H38A H 0.0471 1.0159 0.5946 0.044 Uiso 1 1 calc R . . C39 C 0.2336(2) 1.0460(2) 0.8041(2) 0.0718(10) Uani 1 1 d . . . H39B H 0.1832 1.0456 0.8182 0.086 Uiso 1 1 calc R . . H39A H 0.2484 1.0978 0.7943 0.086 Uiso 1 1 calc R . . C40 C 0.2713(2) 1.0131(2) 0.8891(3) 0.0723(10) Uani 1 1 d . . . H40B H 0.2399 1.0037 0.9469 0.087 Uiso 1 1 calc R . . H40A H 0.3092 1.046 0.9118 0.087 Uiso 1 1 calc R . . C41 C 0.2997(3) 0.9420(2) 0.8482(3) 0.0986(15) Uani 1 1 d . . . H41B H 0.3471 0.9331 0.8742 0.118 Uiso 1 1 calc R . . H41A H 0.2699 0.8999 0.868 0.118 Uiso 1 1 calc R . . C42 C 0.3005(3) 0.9508(3) 0.7393(3) 0.0980(16) Uani 1 1 d . . . H42B H 0.3464 0.9686 0.7165 0.118 Uiso 1 1 calc R . . H42A H 0.2907 0.903 0.7056 0.118 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 Li 0.036(2) 0.046(2) 0.037(2) -0.0054(18) 0.0031(17) 0.0071(18) Si1 0.0205(2) 0.0201(2) 0.0277(3) -0.0003(2) -0.0016(2) -0.0010(2) Si2 0.0265(3) 0.0335(3) 0.0530(4) -0.0074(3) -0.0046(3) 0.0075(3) Si3 0.0280(3) 0.0304(3) 0.0301(3) -0.0067(3) -0.0014(2) 0.0025(2) N1 0.0221(9) 0.0202(8) 0.0389(10) 0.0035(7) -0.0016(7) -0.0017(7) N2 0.0226(8) 0.0217(8) 0.0307(10) 0.0030(7) -0.0002(7) -0.0023(7) N3 0.0217(8) 0.0257(9) 0.0298(10) -0.0024(8) -0.0010(7) -0.0010(7) O1 0.0323(9) 0.0371(9) 0.0515(11) -0.0086(7) 0.0062(8) 0.0023(7) O2 0.0599(11) 0.0658(11) 0.0332(9) -0.0012(9) 0.0014(8) 0.0204(10) C1 0.0237(10) 0.0261(11) 0.0274(11) -0.0005(8) -0.0032(8) -0.0014(8) C2 0.0250(9) 0.0257(10) 0.0228(10) 0.0007(8) -0.0022(9) -0.0020(8) C3 0.0301(11) 0.0311(11) 0.0278(12) 0.0026(9) 0.0000(9) 0.0044(9) C4 0.0249(11) 0.0465(14) 0.0319(12) 0.0017(10) 0.0037(9) 0.0084(10) C5 0.0229(11) 0.0463(13) 0.0359(13) 0.0053(10) 0.0025(9) -0.0041(10) C6 0.0256(11) 0.0320(11) 0.0331(12) 0.0050(9) -0.0018(9) -0.0054(9) C7 0.0310(12) 0.0204(11) 0.0602(16) 0.0025(10) 0.0003(11) -0.0024(9) C8 0.0316(12) 0.0297(12) 0.081(2) 0.0214(12) -0.0076(13) -0.0039(10) C9 0.068(2) 0.078(2) 0.060(2) 0.0350(17) -0.0058(16) 0.0077(18) C10 0.0474(16) 0.0438(16) 0.110(3) 0.0342(17) -0.0298(17) -0.0118(14) C11 0.0573(18) 0.0271(13) 0.140(4) 0.0253(17) -0.020(2) -0.0046(13) C12 0.0298(10) 0.0193(10) 0.0359(13) -0.0007(8) -0.0033(9) -0.0010(8) C13 0.0366(12) 0.0245(11) 0.0380(14) 0.0056(9) 0.0023(10) -0.0007(9) C14 0.0514(15) 0.0347(13) 0.0475(15) 0.0069(11) 0.0117(12) 0.0026(11) C15 0.0417(14) 0.0614(17) 0.0377(15) 0.0198(12) -0.0077(11) -0.0033(12) C16 0.0637(17) 0.0257(12) 0.0576(17) 0.0082(11) 0.0119(14) 0.0032(12) C17 0.0212(9) 0.0244(10) 0.0300(11) -0.0030(9) -0.0018(9) -0.0019(8) C18 0.0257(10) 0.0249(10) 0.0406(13) -0.0069(10) -0.0047(10) -0.0024(8) C19 0.0414(13) 0.0427(13) 0.0387(14) -0.0062(10) -0.0085(11) 0.0008(11) C20 0.0365(13) 0.0539(16) 0.0426(14) -0.0092(12) 0.0081(11) -0.0057(12) C21 0.0587(16) 0.0456(14) 0.0449(15) -0.0129(12) -0.0062(13) 0.0198(13) C22 0.0482(18) 0.083(2) 0.106(3) 0.015(2) 0.030(2) 0.0222(17) C23 0.0573(18) 0.0465(16) 0.109(3) -0.0306(17) -0.0339(18) 0.0258(14) C24 0.0510(17) 0.0551(17) 0.070(2) -0.0106(15) -0.0215(15) 0.0178(14) C25 0.0232(10) 0.0230(10) 0.0419(13) -0.0055(9) -0.0015(9) -0.0019(8) C26 0.0459(14) 0.0316(12) 0.0518(16) 0.0007(11) 0.0083(12) -0.0082(11) C27 0.0637(19) 0.0353(14) 0.083(2) 0.0055(14) 0.0142(16) -0.0199(14) C28 0.0439(16) 0.0410(15) 0.131(3) -0.0191(19) 0.018(2) -0.0219(13) C29 0.0364(14) 0.0377(14) 0.111(3) -0.0170(16) -0.0204(16) -0.0096(12) C30 0.0294(12) 0.0330(13) 0.0726(19) -0.0101(12) -0.0131(12) -0.0027(10) C31 0.0351(12) 0.0284(12) 0.0521(15) -0.0138(11) 0.0009(11) -0.0017(10) C32 0.0433(14) 0.0286(13) 0.084(2) -0.0204(13) 0.0005(14) -0.0024(11) C33 0.0600(18) 0.0431(15) 0.089(2) -0.0277(15) -0.0183(17) -0.0134(14) C34 0.0602(17) 0.0243(11) 0.100(2) -0.0047(15) -0.0068(18) -0.0087(12) C35 0.0531(15) 0.0338(13) 0.0563(17) -0.0009(11) 0.0061(13) -0.0027(12) C36 0.0519(15) 0.0449(14) 0.0451(16) -0.0118(12) -0.0053(12) 0.0151(12) C37 0.0328(12) 0.0611(16) 0.0410(14) -0.0082(12) 0.0022(11) 0.0067(12) C38 0.0395(13) 0.0382(13) 0.0329(13) 0.0006(10) -0.0008(10) -0.0031(10) C39 0.079(2) 0.096(3) 0.0398(17) -0.0157(17) -0.0056(15) 0.023(2) C40 0.092(3) 0.074(2) 0.051(2) 0.0021(16) -0.0139(18) 0.005(2) C41 0.148(4) 0.071(2) 0.076(3) -0.0075(19) -0.054(3) 0.014(3) C42 0.130(4) 0.104(3) 0.059(2) 0.012(2) 0.010(2) 0.075(3) #----------------------------------------------------------------------------# # 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 Li O1 1.894(4) . ? Li O2 1.928(5) . ? Li N3 1.942(4) . ? Si1 N3 1.6683(17) . ? Si1 N1 1.7814(18) . ? Si1 N2 1.7824(17) . ? Si1 Si3 2.3791(8) . ? Si2 C18 1.850(2) . ? Si2 C24 1.873(3) . ? Si2 C22 1.876(4) . ? Si2 C23 1.877(3) . ? Si3 C20 1.872(3) . ? Si3 C19 1.873(2) . ? Si3 C21 1.893(3) . ? N1 C1 1.401(3) . ? N1 C7 1.467(3) . ? N2 C2 1.400(3) . ? N2 C12 1.464(3) . ? N3 C17 1.391(3) . ? O1 C35 1.438(3) . ? O1 C38 1.453(3) . ? O2 C39 1.433(4) . ? O2 C42 1.436(4) . ? C1 C6 1.379(3) . ? C1 C2 1.430(3) . ? C2 C3 1.389(3) . ? C3 C4 1.391(3) . ? C4 C5 1.382(3) . ? C5 C6 1.398(3) . ? C7 C8 1.534(4) . ? C8 C9 1.498(4) . ? C8 C10 1.522(4) . ? C8 C11 1.547(4) . ? C12 C13 1.542(3) . ? C13 C14 1.517(3) . ? C13 C15 1.520(3) . ? C13 C16 1.534(3) . ? C17 C18 1.364(3) . ? C17 C25 1.548(3) . ? C25 C30 1.537(3) . ? C25 C26 1.538(3) . ? C25 C31 1.545(3) . ? C26 C27 1.539(3) . ? C27 C34 1.531(4) . ? C27 C28 1.535(5) . ? C28 C29 1.529(6) . ? C29 C33 1.519(4) . ? C29 C30 1.535(3) . ? C31 C32 1.530(3) . ? C32 C34 1.511(5) . ? C32 C33 1.520(4) . ? C35 C36 1.506(4) . ? C36 C37 1.514(4) . ? C37 C38 1.511(3) . ? C39 C40 1.464(5) . ? C40 C41 1.498(5) . ? C41 C42 1.446(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li O2 103.8(2) . . ? O1 Li N3 130.9(2) . . ? O2 Li N3 125.4(2) . . ? N3 Si1 N1 120.16(9) . . ? N3 Si1 N2 107.61(8) . . ? N1 Si1 N2 89.05(8) . . ? N3 Si1 Si3 115.09(6) . . ? N1 Si1 Si3 106.53(7) . . ? N2 Si1 Si3 116.04(6) . . ? C18 Si2 C24 116.02(13) . . ? C18 Si2 C22 115.52(13) . . ? C24 Si2 C22 108.82(19) . . ? C18 Si2 C23 104.34(12) . . ? C24 Si2 C23 104.29(15) . . ? C22 Si2 C23 106.70(19) . . ? C20 Si3 C19 110.69(12) . . ? C20 Si3 C21 103.44(13) . . ? C19 Si3 C21 104.78(12) . . ? C20 Si3 Si1 114.71(9) . . ? C19 Si3 Si1 106.98(9) . . ? C21 Si3 Si1 115.83(9) . . ? C1 N1 C7 118.51(17) . . ? C1 N1 Si1 112.89(13) . . ? C7 N1 Si1 127.10(15) . . ? C2 N2 C12 118.13(17) . . ? C2 N2 Si1 112.73(13) . . ? C12 N2 Si1 124.56(13) . . ? C17 N3 Si1 132.71(15) . . ? C17 N3 Li 111.00(18) . . ? Si1 N3 Li 113.48(15) . . ? C35 O1 C38 109.74(18) . . ? C35 O1 Li 124.1(2) . . ? C38 O1 Li 124.61(19) . . ? C39 O2 C42 107.7(3) . . ? C39 O2 Li 121.8(2) . . ? C42 O2 Li 129.6(2) . . ? C6 C1 N1 128.54(19) . . ? C6 C1 C2 119.09(19) . . ? N1 C1 C2 112.37(17) . . ? C3 C2 N2 128.02(18) . . ? C3 C2 C1 119.47(18) . . ? N2 C2 C1 112.47(17) . . ? C2 C3 C4 120.3(2) . . ? C5 C4 C3 120.3(2) . . ? C4 C5 C6 120.1(2) . . ? C1 C6 C5 120.6(2) . . ? N1 C7 C8 118.3(2) . . ? C9 C8 C10 110.5(3) . . ? C9 C8 C7 113.0(2) . . ? C10 C8 C7 109.5(2) . . ? C9 C8 C11 109.6(3) . . ? C10 C8 C11 108.0(2) . . ? C7 C8 C11 106.0(3) . . ? N2 C12 C13 118.47(17) . . ? C14 C13 C15 109.0(2) . . ? C14 C13 C16 109.36(19) . . ? C15 C13 C16 109.0(2) . . ? C14 C13 C12 109.44(19) . . ? C15 C13 C12 113.30(18) . . ? C16 C13 C12 106.71(19) . . ? C18 C17 N3 123.22(18) . . ? C18 C17 C25 123.25(18) . . ? N3 C17 C25 113.52(16) . . ? C17 C18 Si2 141.69(17) . . ? C30 C25 C26 108.1(2) . . ? C30 C25 C31 106.97(19) . . ? C26 C25 C31 107.85(19) . . ? C30 C25 C17 113.60(18) . . ? C26 C25 C17 108.14(18) . . ? C31 C25 C17 111.98(17) . . ? C25 C26 C27 110.8(2) . . ? C34 C27 C28 109.1(3) . . ? C34 C27 C26 109.5(2) . . ? C28 C27 C26 109.3(2) . . ? C29 C28 C27 109.1(2) . . ? C33 C29 C28 110.4(3) . . ? C33 C29 C30 110.1(2) . . ? C28 C29 C30 108.5(3) . . ? C29 C30 C25 111.3(2) . . ? C32 C31 C25 111.6(2) . . ? C34 C32 C33 110.2(3) . . ? C34 C32 C31 109.6(2) . . ? C33 C32 C31 109.1(2) . . ? C29 C33 C32 108.9(2) . . ? C32 C34 C27 109.8(2) . . ? O1 C35 C36 105.7(2) . . ? C35 C36 C37 102.0(2) . . ? C38 C37 C36 102.32(19) . . ? O1 C38 C37 104.84(19) . . ? O2 C39 C40 108.7(3) . . ? C39 C40 C41 104.8(3) . . ? C42 C41 C40 105.5(3) . . ? O2 C42 C41 107.0(3) . . ? #===END