# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr. Hans-Georg Stammler' _publ_contact_author_phone '49 521 1066165' _publ_contact_author_fax '49 521 1066146' _publ_contact_author_email georg.stammler@uni-bielefeld.de _publ_section_title ; Silylation products of cyclic tri-aminal carbanions and their lithiation ; loop_ _publ_author_name N.Mitzel C.Sicking G.Stammler A.Mix B.Neumann # Attachment '- COSI19_05_06_08.CIF' #============================================================================== #TrackingRef '- COSI19_05_06_08.CIF' #============================================================================== data_TMTAC _database_code_depnum_ccdc_archive 'CCDC 821375' #TrackingRef '- COSI19_05_06_08.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H15 N3' _chemical_formula_sum 'C6 H15 N3' _chemical_formula_weight 129.21 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 0.0000 0.0000 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5902(2) _cell_length_b 18.9804(3) _cell_length_c 14.0480(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.5696(9) _cell_angle_gamma 90.00 _cell_volume 3075.78(8) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 63369 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description capillary _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9824 _exptl_absorpt_correction_T_max 0.9824 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; crystal has grown on the diffractometer from a small crystal nucleus at 247.6 K and cooling down slowly ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78902 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8927 _reflns_number_gt 6917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0522P)^2^+0.6457P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8927 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 N1 N 0.34217(6) 0.34928(3) 0.62394(5) 0.01935(14) Uani 1 1 d . . . N2 N 0.26177(6) 0.40235(3) 0.75997(5) 0.01914(14) Uani 1 1 d . . . N3 N 0.15679(6) 0.40919(3) 0.60508(5) 0.01905(14) Uani 1 1 d . . . N4 N 0.32731(6) 0.09177(3) 0.62492(5) 0.01961(14) Uani 1 1 d . . . N5 N 0.25291(6) 0.15406(4) 0.75623(5) 0.02014(14) Uani 1 1 d . . . N6 N 0.15049(6) 0.16010(3) 0.59947(5) 0.01837(14) Uani 1 1 d . . . N7 N 0.36730(6) 0.46560(4) 0.19543(5) 0.02139(14) Uani 1 1 d . . . N8 N 0.29206(6) 0.53446(3) 0.32065(5) 0.01776(13) Uani 1 1 d . . . N9 N 0.19009(6) 0.53262(4) 0.16407(5) 0.01877(14) Uani 1 1 d . . . N10 N 0.11851(6) 0.22525(3) 0.31430(5) 0.01785(13) Uani 1 1 d . . . N11 N 0.30616(6) 0.28205(3) 0.33765(5) 0.01740(13) Uani 1 1 d . . . N12 N 0.20233(6) 0.28011(3) 0.18171(5) 0.01837(14) Uani 1 1 d . . . C1 C 0.33113(7) 0.34403(4) 0.72594(6) 0.02016(16) Uani 1 1 d . . . H1A H 0.4099(9) 0.3455(5) 0.7616(8) 0.027(3) Uiso 1 1 d . . . H1B H 0.2941(8) 0.2975(6) 0.7382(7) 0.022(2) Uiso 1 1 d . . . C2 C 0.14722(7) 0.40151(4) 0.70708(6) 0.01947(15) Uani 1 1 d . . . H2A H 0.1049(10) 0.3558(6) 0.7213(8) 0.031(3) Uiso 1 1 d . . . H2B H 0.1016(9) 0.4419(6) 0.7298(7) 0.023(2) Uiso 1 1 d . . . C3 C 0.22719(7) 0.35078(4) 0.57268(6) 0.01993(15) Uani 1 1 d . . . H3A H 0.1899(9) 0.3041(6) 0.5840(7) 0.028(3) Uiso 1 1 d . . . H3B H 0.2339(9) 0.3579(6) 0.5046(8) 0.028(3) Uiso 1 1 d . . . C4 C 0.41335(7) 0.40944(4) 0.60039(6) 0.02253(16) Uani 1 1 d . . . H4A H 0.3800(9) 0.4560(6) 0.6147(8) 0.030(3) Uiso 1 1 d . . . H4B H 0.4225(10) 0.4088(6) 0.5314(8) 0.033(3) Uiso 1 1 d . . . H4C H 0.4906(10) 0.4046(6) 0.6349(8) 0.030(3) Uiso 1 1 d . . . C5 C 0.25157(8) 0.39543(5) 0.86203(6) 0.02771(19) Uani 1 1 d . . . H5A H 0.2037(10) 0.4356(6) 0.8835(8) 0.035(3) Uiso 1 1 d . . . H5B H 0.3293(11) 0.3952(6) 0.8977(9) 0.040(3) Uiso 1 1 d . . . H5C H 0.2138(11) 0.3515(7) 0.8782(9) 0.041(3) Uiso 1 1 d . . . C6 C 0.04195(7) 0.40910(5) 0.55272(7) 0.02541(18) Uani 1 1 d . . . H6A H -0.0007(10) 0.3639(6) 0.5629(8) 0.035(3) Uiso 1 1 d . . . H6B H 0.0482(10) 0.4145(6) 0.4824(8) 0.034(3) Uiso 1 1 d . . . H6C H -0.0028(9) 0.4489(6) 0.5748(8) 0.032(3) Uiso 1 1 d . . . C7 C 0.31292(7) 0.09064(4) 0.72655(6) 0.02141(16) Uani 1 1 d . . . H7A H 0.3911(10) 0.0879(6) 0.7640(8) 0.033(3) Uiso 1 1 d . . . H7B H 0.2664(9) 0.0470(6) 0.7405(8) 0.028(3) Uiso 1 1 d . . . C8 C 0.13902(7) 0.15820(4) 0.70203(6) 0.01974(15) Uani 1 1 d . . . H8A H 0.1000(9) 0.2020(6) 0.7209(7) 0.027(3) Uiso 1 1 d . . . H8B H 0.0894(10) 0.1174(6) 0.7182(8) 0.033(3) Uiso 1 1 d . . . C9 C 0.21349(7) 0.09724(4) 0.57201(6) 0.01947(15) Uani 1 1 d . . . H9A H 0.1694(9) 0.0530(5) 0.5856(7) 0.024(3) Uiso 1 1 d . . . H9B H 0.2214(9) 0.0999(5) 0.5032(8) 0.025(3) Uiso 1 1 d . . . C10 C 0.40576(7) 0.14839(4) 0.60025(6) 0.02170(16) Uani 1 1 d . . . H10A H 0.3792(9) 0.1965(6) 0.6156(7) 0.025(3) Uiso 1 1 d . . . H10B H 0.4140(10) 0.1451(6) 0.5304(8) 0.034(3) Uiso 1 1 d . . . H10C H 0.4819(10) 0.1401(6) 0.6352(8) 0.031(3) Uiso 1 1 d . . . C11 C 0.23983(9) 0.15157(6) 0.85826(6) 0.0301(2) Uani 1 1 d . . . H11A H 0.1979(11) 0.1944(7) 0.8784(9) 0.044(3) Uiso 1 1 d . . . H11B H 0.3178(11) 0.1481(7) 0.8953(9) 0.045(3) Uiso 1 1 d . . . H11C H 0.1922(12) 0.1111(7) 0.8759(9) 0.050(4) Uiso 1 1 d . . . C12 C 0.03567(7) 0.16304(5) 0.54624(6) 0.02314(17) Uani 1 1 d . . . H12A H 0.0433(10) 0.1632(6) 0.4761(9) 0.036(3) Uiso 1 1 d . . . H12B H -0.0024(10) 0.2072(6) 0.5634(8) 0.031(3) Uiso 1 1 d . . . H12C H -0.0150(10) 0.1228(6) 0.5614(8) 0.035(3) Uiso 1 1 d . . . C13 C 0.35366(7) 0.46984(4) 0.29706(6) 0.02130(16) Uani 1 1 d . . . H13A H 0.4314(9) 0.4704(5) 0.3348(7) 0.025(3) Uiso 1 1 d . . . H13B H 0.3091(9) 0.4271(6) 0.3152(7) 0.025(3) Uiso 1 1 d . . . C14 C 0.17846(7) 0.53538(4) 0.26626(5) 0.01873(15) Uani 1 1 d . . . H14A H 0.1281(9) 0.4938(6) 0.2865(7) 0.026(3) Uiso 1 1 d . . . H14B H 0.1368(8) 0.5784(5) 0.2806(7) 0.021(2) Uiso 1 1 d . . . C15 C 0.25321(7) 0.46803(4) 0.14295(6) 0.02244(16) Uani 1 1 d . . . H15A H 0.2084(9) 0.4247(6) 0.1620(7) 0.026(3) Uiso 1 1 d . . . H15B H 0.2605(9) 0.4669(6) 0.0743(8) 0.031(3) Uiso 1 1 d . . . C16 C 0.44491(7) 0.52032(5) 0.16406(6) 0.02300(17) Uani 1 1 d . . . H16A H 0.4534(9) 0.5126(6) 0.0952(8) 0.030(3) Uiso 1 1 d . . . H16B H 0.5202(9) 0.5159(6) 0.2008(8) 0.029(3) Uiso 1 1 d . . . H16C H 0.4172(9) 0.5686(6) 0.1717(7) 0.027(3) Uiso 1 1 d . . . C17 C 0.27975(8) 0.53822(5) 0.42263(6) 0.02503(18) Uani 1 1 d . . . H17A H 0.2388(10) 0.5810(6) 0.4357(8) 0.032(3) Uiso 1 1 d . . . H17B H 0.3575(10) 0.5392(6) 0.4609(8) 0.034(3) Uiso 1 1 d . . . H17C H 0.2343(10) 0.4993(6) 0.4463(8) 0.035(3) Uiso 1 1 d . . . C18 C 0.07587(7) 0.53365(5) 0.11033(6) 0.02589(18) Uani 1 1 d . . . H18A H 0.0255(10) 0.4947(6) 0.1271(8) 0.037(3) Uiso 1 1 d . . . H18B H 0.0839(10) 0.5305(6) 0.0420(9) 0.037(3) Uiso 1 1 d . . . H18C H 0.0356(10) 0.5791(6) 0.1218(8) 0.034(3) Uiso 1 1 d . . . C19 C 0.23337(7) 0.22366(4) 0.36635(6) 0.01816(15) Uani 1 1 d . . . H19A H 0.2681(9) 0.1761(6) 0.3524(7) 0.024(2) Uiso 1 1 d . . . H19B H 0.2252(10) 0.2281(6) 0.4354(8) 0.030(3) Uiso 1 1 d . . . C20 C 0.31657(7) 0.27742(4) 0.23525(6) 0.01840(15) Uani 1 1 d . . . H20A H 0.3640(8) 0.3172(5) 0.2153(7) 0.019(2) Uiso 1 1 d . . . H20B H 0.3589(9) 0.2317(6) 0.2204(8) 0.030(3) Uiso 1 1 d . . . C21 C 0.13081(7) 0.22177(4) 0.21249(6) 0.01900(15) Uani 1 1 d . . . H21A H 0.0528(9) 0.2249(5) 0.1761(8) 0.026(3) Uiso 1 1 d . . . H21B H 0.1681(8) 0.1746(5) 0.2002(7) 0.021(2) Uiso 1 1 d . . . C22 C 0.05034(7) 0.28637(4) 0.33933(6) 0.02062(16) Uani 1 1 d . . . H22A H 0.0395(10) 0.2845(6) 0.4076(8) 0.034(3) Uiso 1 1 d . . . H22B H -0.0269(10) 0.2840(5) 0.3029(8) 0.028(3) Uiso 1 1 d . . . H22C H 0.0848(9) 0.3331(6) 0.3236(7) 0.026(3) Uiso 1 1 d . . . C23 C 0.42070(7) 0.27938(5) 0.39059(6) 0.02316(17) Uani 1 1 d . . . H23A H 0.4640(10) 0.2354(6) 0.3770(8) 0.034(3) Uiso 1 1 d . . . H23B H 0.4131(10) 0.2815(6) 0.4585(9) 0.035(3) Uiso 1 1 d . . . H23C H 0.4670(10) 0.3205(6) 0.3718(8) 0.035(3) Uiso 1 1 d . . . C24 C 0.21342(8) 0.27534(5) 0.07960(6) 0.02622(18) Uani 1 1 d . . . H24A H 0.2622(10) 0.3151(6) 0.0604(8) 0.031(3) Uiso 1 1 d . . . H24B H 0.1360(11) 0.2778(6) 0.0445(9) 0.041(3) Uiso 1 1 d . . . H24C H 0.2517(11) 0.2316(7) 0.0626(9) 0.040(3) Uiso 1 1 d . . . 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 N1 0.0175(3) 0.0185(3) 0.0221(3) 0.0000(2) 0.0022(2) 0.0007(2) N2 0.0195(3) 0.0197(3) 0.0183(3) -0.0005(2) 0.0021(2) 0.0011(2) N3 0.0170(3) 0.0205(3) 0.0196(3) -0.0002(2) 0.0014(2) 0.0018(2) N4 0.0186(3) 0.0186(3) 0.0217(3) -0.0004(2) 0.0023(2) -0.0004(2) N5 0.0208(3) 0.0227(3) 0.0172(3) -0.0006(2) 0.0032(2) -0.0016(3) N6 0.0171(3) 0.0201(3) 0.0181(3) 0.0010(2) 0.0024(2) 0.0001(2) N7 0.0233(3) 0.0178(3) 0.0236(3) -0.0009(2) 0.0051(3) 0.0004(2) N8 0.0185(3) 0.0186(3) 0.0162(3) 0.0001(2) 0.0016(2) 0.0001(2) N9 0.0187(3) 0.0199(3) 0.0175(3) -0.0002(2) 0.0006(2) -0.0020(2) N10 0.0175(3) 0.0174(3) 0.0190(3) 0.0004(2) 0.0031(2) -0.0005(2) N11 0.0166(3) 0.0184(3) 0.0173(3) 0.0001(2) 0.0022(2) -0.0016(2) N12 0.0201(3) 0.0198(3) 0.0153(3) 0.0004(2) 0.0024(2) -0.0018(2) C1 0.0207(4) 0.0178(4) 0.0219(4) 0.0025(3) 0.0017(3) 0.0021(3) C2 0.0179(3) 0.0202(4) 0.0207(4) 0.0001(3) 0.0033(3) 0.0002(3) C3 0.0186(4) 0.0199(4) 0.0211(4) -0.0024(3) 0.0016(3) 0.0008(3) C4 0.0197(4) 0.0232(4) 0.0250(4) 0.0018(3) 0.0036(3) -0.0006(3) C5 0.0302(4) 0.0339(5) 0.0192(4) 0.0009(3) 0.0033(3) -0.0008(4) C6 0.0191(4) 0.0299(4) 0.0266(4) 0.0004(3) -0.0008(3) 0.0028(3) C7 0.0223(4) 0.0193(4) 0.0224(4) 0.0030(3) 0.0011(3) 0.0002(3) C8 0.0190(4) 0.0211(4) 0.0197(4) 0.0005(3) 0.0048(3) -0.0011(3) C9 0.0197(4) 0.0184(4) 0.0204(4) -0.0022(3) 0.0021(3) -0.0008(3) C10 0.0194(4) 0.0220(4) 0.0241(4) -0.0011(3) 0.0048(3) -0.0015(3) C11 0.0290(4) 0.0440(6) 0.0175(4) -0.0001(4) 0.0039(3) -0.0051(4) C12 0.0186(4) 0.0265(4) 0.0241(4) 0.0044(3) 0.0010(3) -0.0005(3) C13 0.0227(4) 0.0175(4) 0.0238(4) 0.0027(3) 0.0029(3) 0.0014(3) C14 0.0177(3) 0.0194(4) 0.0193(4) 0.0006(3) 0.0027(3) -0.0010(3) C15 0.0258(4) 0.0191(4) 0.0225(4) -0.0042(3) 0.0028(3) -0.0032(3) C16 0.0217(4) 0.0220(4) 0.0262(4) 0.0002(3) 0.0068(3) 0.0005(3) C17 0.0261(4) 0.0317(5) 0.0175(4) 0.0012(3) 0.0031(3) -0.0016(3) C18 0.0208(4) 0.0316(5) 0.0243(4) 0.0028(3) -0.0025(3) -0.0062(3) C19 0.0180(3) 0.0174(3) 0.0193(4) 0.0028(3) 0.0024(3) -0.0002(3) C20 0.0184(3) 0.0192(4) 0.0182(3) -0.0005(3) 0.0046(3) -0.0003(3) C21 0.0208(4) 0.0173(4) 0.0189(4) -0.0014(3) 0.0020(3) -0.0022(3) C22 0.0190(4) 0.0215(4) 0.0217(4) -0.0004(3) 0.0036(3) 0.0014(3) C23 0.0176(4) 0.0284(4) 0.0232(4) -0.0011(3) 0.0007(3) 0.0002(3) C24 0.0293(4) 0.0325(5) 0.0173(4) -0.0008(3) 0.0043(3) -0.0003(4) _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 N1 C3 1.4522(10) . ? N1 C1 1.4542(10) . ? N1 C4 1.4651(10) . ? N2 C5 1.4559(10) . ? N2 C2 1.4573(10) . ? N2 C1 1.4747(10) . ? N3 C2 1.4552(10) . ? N3 C6 1.4570(10) . ? N3 C3 1.4746(10) . ? N4 C7 1.4534(10) . ? N4 C9 1.4537(10) . ? N4 C10 1.4707(10) . ? N5 C11 1.4567(10) . ? N5 C8 1.4606(10) . ? N5 C7 1.4706(10) . ? N6 C8 1.4602(10) . ? N6 C12 1.4630(10) . ? N6 C9 1.4698(10) . ? N7 C15 1.4509(11) . ? N7 C13 1.4538(10) . ? N7 C16 1.4694(10) . ? N8 C17 1.4551(10) . ? N8 C14 1.4569(10) . ? N8 C13 1.4729(10) . ? N9 C14 1.4557(10) . ? N9 C18 1.4591(10) . ? N9 C15 1.4724(10) . ? N10 C21 1.4525(10) . ? N10 C19 1.4556(10) . ? N10 C22 1.4656(10) . ? N11 C20 1.4578(10) . ? N11 C23 1.4582(10) . ? N11 C19 1.4726(10) . ? N12 C24 1.4554(10) . ? N12 C20 1.4588(10) . ? N12 C21 1.4729(10) . ? C1 H1A 0.998(11) . ? C1 H1B 1.005(10) . ? C2 H2A 1.026(11) . ? C2 H2B 1.002(10) . ? C3 H3A 1.005(11) . ? C3 H3B 0.977(11) . ? C4 H4A 0.992(11) . ? C4 H4B 0.985(11) . ? C4 H4C 0.980(11) . ? C5 H5A 1.006(12) . ? C5 H5B 0.988(13) . ? C5 H5C 0.979(13) . ? C6 H6A 1.008(12) . ? C6 H6B 1.002(12) . ? C6 H6C 0.983(11) . ? C7 H7A 1.004(12) . ? C7 H7B 1.018(11) . ? C8 H8A 0.995(11) . ? C8 H8B 1.004(12) . ? C9 H9A 1.011(10) . ? C9 H9B 0.982(11) . ? C10 H10A 0.994(11) . ? C10 H10B 0.997(12) . ? C10 H10C 0.980(11) . ? C11 H11A 1.002(13) . ? C11 H11B 1.000(13) . ? C11 H11C 0.991(14) . ? C12 H12A 0.997(12) . ? C12 H12B 0.987(11) . ? C12 H12C 0.999(12) . ? C13 H13A 1.000(11) . ? C13 H13B 1.007(11) . ? C14 H14A 1.037(11) . ? C14 H14B 0.980(10) . ? C15 H15A 1.022(11) . ? C15 H15B 0.976(11) . ? C16 H16A 0.992(11) . ? C16 H16B 0.974(11) . ? C16 H16C 0.981(11) . ? C17 H17A 0.967(11) . ? C17 H17B 1.004(12) . ? C17 H17C 0.984(12) . ? C18 H18A 0.985(12) . ? C18 H18B 0.975(12) . ? C18 H18C 1.000(12) . ? C19 H19A 1.015(10) . ? C19 H19B 0.987(11) . ? C20 H20A 0.991(10) . ? C20 H20B 1.028(11) . ? C21 H21A 0.997(11) . ? C21 H21B 1.016(10) . ? C22 H22A 0.980(12) . ? C22 H22B 0.988(11) . ? C22 H22C 1.006(11) . ? C23 H23A 1.001(12) . ? C23 H23B 0.967(12) . ? C23 H23C 0.997(12) . ? C24 H24A 0.995(11) . ? C24 H24B 0.982(13) . ? C24 H24C 0.982(13) . ? 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 C3 N1 C1 109.01(6) . . ? C3 N1 C4 112.49(6) . . ? C1 N1 C4 112.41(6) . . ? C5 N2 C2 110.13(6) . . ? C5 N2 C1 110.52(7) . . ? C2 N2 C1 108.95(6) . . ? C2 N3 C6 110.11(6) . . ? C2 N3 C3 109.02(6) . . ? C6 N3 C3 110.43(6) . . ? C7 N4 C9 108.56(6) . . ? C7 N4 C10 112.01(6) . . ? C9 N4 C10 112.23(6) . . ? C11 N5 C8 109.85(6) . . ? C11 N5 C7 110.47(7) . . ? C8 N5 C7 108.94(6) . . ? C8 N6 C12 109.86(6) . . ? C8 N6 C9 109.51(6) . . ? C12 N6 C9 110.32(6) . . ? C15 N7 C13 108.46(6) . . ? C15 N7 C16 112.29(7) . . ? C13 N7 C16 112.54(7) . . ? C17 N8 C14 110.23(6) . . ? C17 N8 C13 111.00(6) . . ? C14 N8 C13 108.97(6) . . ? C14 N9 C18 110.09(6) . . ? C14 N9 C15 108.91(6) . . ? C18 N9 C15 110.51(7) . . ? C21 N10 C19 108.74(6) . . ? C21 N10 C22 112.26(6) . . ? C19 N10 C22 112.58(6) . . ? C20 N11 C23 110.04(6) . . ? C20 N11 C19 109.22(6) . . ? C23 N11 C19 110.58(6) . . ? C24 N12 C20 110.08(6) . . ? C24 N12 C21 110.41(6) . . ? C20 N12 C21 109.32(6) . . ? N1 C1 N2 111.77(6) . . ? N1 C1 H1A 109.2(6) . . ? N2 C1 H1A 108.5(6) . . ? N1 C1 H1B 108.0(6) . . ? N2 C1 H1B 110.4(6) . . ? H1A C1 H1B 108.9(8) . . ? N3 C2 N2 110.38(6) . . ? N3 C2 H2A 111.1(6) . . ? N2 C2 H2A 109.8(6) . . ? N3 C2 H2B 109.3(6) . . ? N2 C2 H2B 108.2(6) . . ? H2A C2 H2B 108.0(8) . . ? N1 C3 N3 111.73(6) . . ? N1 C3 H3A 107.0(6) . . ? N3 C3 H3A 110.8(6) . . ? N1 C3 H3B 109.4(6) . . ? N3 C3 H3B 107.3(6) . . ? H3A C3 H3B 110.6(9) . . ? N1 C4 H4A 114.2(6) . . ? N1 C4 H4B 109.2(6) . . ? H4A C4 H4B 106.9(9) . . ? N1 C4 H4C 108.8(6) . . ? H4A C4 H4C 109.7(9) . . ? H4B C4 H4C 107.8(9) . . ? N2 C5 H5A 109.1(7) . . ? N2 C5 H5B 110.1(7) . . ? H5A C5 H5B 110.7(9) . . ? N2 C5 H5C 112.7(7) . . ? H5A C5 H5C 107.7(9) . . ? H5B C5 H5C 106.5(10) . . ? N3 C6 H6A 111.5(7) . . ? N3 C6 H6B 110.3(7) . . ? H6A C6 H6B 108.0(9) . . ? N3 C6 H6C 108.9(6) . . ? H6A C6 H6C 109.1(9) . . ? H6B C6 H6C 108.9(9) . . ? N4 C7 N5 111.65(6) . . ? N4 C7 H7A 109.4(6) . . ? N5 C7 H7A 108.8(6) . . ? N4 C7 H7B 108.3(6) . . ? N5 C7 H7B 109.8(6) . . ? H7A C7 H7B 108.9(9) . . ? N6 C8 N5 110.57(6) . . ? N6 C8 H8A 109.2(6) . . ? N5 C8 H8A 108.5(6) . . ? N6 C8 H8B 110.6(6) . . ? N5 C8 H8B 110.4(6) . . ? H8A C8 H8B 107.5(9) . . ? N4 C9 N6 111.91(6) . . ? N4 C9 H9A 107.1(6) . . ? N6 C9 H9A 110.6(6) . . ? N4 C9 H9B 109.9(6) . . ? N6 C9 H9B 108.3(6) . . ? H9A C9 H9B 109.0(8) . . ? N4 C10 H10A 114.2(6) . . ? N4 C10 H10B 107.8(7) . . ? H10A C10 H10B 109.4(9) . . ? N4 C10 H10C 108.2(6) . . ? H10A C10 H10C 108.7(9) . . ? H10B C10 H10C 108.4(9) . . ? N5 C11 H11A 110.5(7) . . ? N5 C11 H11B 109.8(7) . . ? H11A C11 H11B 110.2(10) . . ? N5 C11 H11C 112.6(8) . . ? H11A C11 H11C 105.1(10) . . ? H11B C11 H11C 108.4(10) . . ? N6 C12 H12A 110.0(7) . . ? N6 C12 H12B 108.3(7) . . ? H12A C12 H12B 108.8(9) . . ? N6 C12 H12C 112.7(7) . . ? H12A C12 H12C 108.9(9) . . ? H12B C12 H12C 108.1(9) . . ? N7 C13 N8 111.62(6) . . ? N7 C13 H13A 110.1(6) . . ? N8 C13 H13A 107.6(6) . . ? N7 C13 H13B 108.1(6) . . ? N8 C13 H13B 110.0(6) . . ? H13A C13 H13B 109.4(8) . . ? N9 C14 N8 110.56(6) . . ? N9 C14 H14A 110.5(6) . . ? N8 C14 H14A 110.6(6) . . ? N9 C14 H14B 109.1(6) . . ? N8 C14 H14B 109.9(6) . . ? H14A C14 H14B 106.0(8) . . ? N7 C15 N9 111.73(6) . . ? N7 C15 H15A 107.6(6) . . ? N9 C15 H15A 110.1(6) . . ? N7 C15 H15B 109.8(6) . . ? N9 C15 H15B 108.0(6) . . ? H15A C15 H15B 109.6(8) . . ? N7 C16 H16A 108.0(6) . . ? N7 C16 H16B 108.9(6) . . ? H16A C16 H16B 109.6(9) . . ? N7 C16 H16C 114.3(6) . . ? H16A C16 H16C 108.0(9) . . ? H16B C16 H16C 108.0(9) . . ? N8 C17 H17A 109.0(7) . . ? N8 C17 H17B 111.1(6) . . ? H17A C17 H17B 108.4(9) . . ? N8 C17 H17C 113.8(7) . . ? H17A C17 H17C 106.1(9) . . ? H17B C17 H17C 108.3(9) . . ? N9 C18 H18A 113.3(7) . . ? N9 C18 H18B 109.9(7) . . ? H18A C18 H18B 107.7(9) . . ? N9 C18 H18C 110.0(7) . . ? H18A C18 H18C 108.2(9) . . ? H18B C18 H18C 107.6(9) . . ? N10 C19 N11 111.54(6) . . ? N10 C19 H19A 106.4(6) . . ? N11 C19 H19A 111.6(6) . . ? N10 C19 H19B 108.7(6) . . ? N11 C19 H19B 108.5(6) . . ? H19A C19 H19B 110.1(8) . . ? N11 C20 N12 110.41(6) . . ? N11 C20 H20A 109.6(6) . . ? N12 C20 H20A 109.2(6) . . ? N11 C20 H20B 109.8(6) . . ? N12 C20 H20B 110.6(6) . . ? H20A C20 H20B 107.2(8) . . ? N10 C21 N12 111.51(6) . . ? N10 C21 H21A 109.4(6) . . ? N12 C21 H21A 108.2(6) . . ? N10 C21 H21B 106.9(5) . . ? N12 C21 H21B 110.6(6) . . ? H21A C21 H21B 110.2(8) . . ? N10 C22 H22A 109.2(7) . . ? N10 C22 H22B 108.8(6) . . ? H22A C22 H22B 108.0(9) . . ? N10 C22 H22C 114.2(6) . . ? H22A C22 H22C 109.8(9) . . ? H22B C22 H22C 106.6(8) . . ? N11 C23 H23A 112.4(7) . . ? N11 C23 H23B 109.7(7) . . ? H23A C23 H23B 108.5(9) . . ? N11 C23 H23C 108.9(7) . . ? H23A C23 H23C 108.0(9) . . ? H23B C23 H23C 109.4(9) . . ? N12 C24 H24A 109.1(6) . . ? N12 C24 H24B 109.2(7) . . ? H24A C24 H24B 110.1(9) . . ? N12 C24 H24C 112.2(7) . . ? H24A C24 H24C 107.1(9) . . ? H24B C24 H24C 109.2(10) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.251 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.036 #============================================================================== data_compound5 _database_code_depnum_ccdc_archive 'CCDC 821376' #TrackingRef '- COSI19_05_06_08.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H34 N6 Si' _chemical_formula_sum 'C14 H34 N6 Si' _chemical_formula_weight 314.56 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 0.0000 0.0000 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.2646(5) _cell_length_b 13.3023(8) _cell_length_c 16.6558(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.950(4) _cell_angle_gamma 90.00 _cell_volume 1817.65(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 27492 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9634 _exptl_absorpt_correction_T_max 0.9920 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17917 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4048 _reflns_number_gt 3211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0563P)^2^+0.8026P] 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_extinction_coef ? _refine_ls_number_reflns 4048 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.56481(5) 0.14715(3) 0.30429(2) 0.01874(12) Uani 1 1 d . . . N1 N 0.86487(16) 0.17974(10) 0.24299(8) 0.0221(3) Uani 1 1 d . . . N2 N 0.63045(16) 0.24123(9) 0.15618(7) 0.0198(3) Uani 1 1 d . . . N3 N 0.89974(16) 0.26733(10) 0.11892(8) 0.0220(3) Uani 1 1 d . . . N4 N 0.51658(15) 0.27781(9) 0.43727(7) 0.0188(3) Uani 1 1 d . . . N5 N 0.27342(16) 0.20773(9) 0.36202(8) 0.0210(3) Uani 1 1 d . . . N6 N 0.25238(16) 0.31811(10) 0.47518(8) 0.0215(3) Uani 1 1 d . . . C1 C 0.70179(18) 0.22292(11) 0.24101(9) 0.0195(3) Uani 1 1 d . . . H1 H 0.7164 0.2905 0.2672 0.023 Uiso 1 1 calc R . . C2 C 0.73745(19) 0.30965(11) 0.11833(9) 0.0213(3) Uani 1 1 d . . . H2A H 0.6903 0.3230 0.0618 0.026 Uiso 1 1 calc R . . H2B H 0.7449 0.3744 0.1478 0.026 Uiso 1 1 calc R . . C3 C 0.9674(2) 0.24696(13) 0.20267(9) 0.0247(3) Uani 1 1 d . . . H3A H 1.0769 0.2166 0.2033 0.030 Uiso 1 1 calc R . . H3B H 0.9800 0.3112 0.2328 0.030 Uiso 1 1 calc R . . C4 C 0.8650(2) 0.07819(12) 0.20786(11) 0.0291(4) Uani 1 1 d . . . H4A H 0.8162 0.0805 0.1513 0.044 Uiso 1 1 calc R . . H4B H 0.8016 0.0328 0.2383 0.044 Uiso 1 1 calc R . . H4C H 0.9773 0.0536 0.2106 0.044 Uiso 1 1 calc R . . C5 C 0.46920(19) 0.28745(11) 0.15005(9) 0.0221(3) Uani 1 1 d . . . H5A H 0.4767 0.3525 0.1779 0.033 Uiso 1 1 calc R . . H5B H 0.3947 0.2433 0.1751 0.033 Uiso 1 1 calc R . . H5C H 0.4279 0.2976 0.0930 0.033 Uiso 1 1 calc R . . C6 C 1.0039(2) 0.33789(13) 0.08192(10) 0.0286(4) Uani 1 1 d . . . H6A H 0.9550 0.3533 0.0267 0.043 Uiso 1 1 calc R . . H6B H 1.1117 0.3078 0.0803 0.043 Uiso 1 1 calc R . . H6C H 1.0150 0.3999 0.1139 0.043 Uiso 1 1 calc R . . C7 C 0.43865(18) 0.24377(11) 0.35673(9) 0.0187(3) Uani 1 1 d . . . H7 H 0.4279 0.3046 0.3212 0.022 Uiso 1 1 calc R . . C8 C 0.17810(19) 0.28617(12) 0.39498(9) 0.0231(3) Uani 1 1 d . . . H8A H 0.0666 0.2609 0.3988 0.028 Uiso 1 1 calc R . . H8B H 0.1694 0.3447 0.3580 0.028 Uiso 1 1 calc R . . C9 C 0.41559(19) 0.35514(11) 0.46878(9) 0.0208(3) Uani 1 1 d . . . H9A H 0.4669 0.3769 0.5228 0.025 Uiso 1 1 calc R . . H9B H 0.4090 0.4143 0.4325 0.025 Uiso 1 1 calc R . . C10 C 0.67861(19) 0.32053(12) 0.43407(10) 0.0230(3) Uani 1 1 d . . . H10A H 0.6701 0.3792 0.3982 0.035 Uiso 1 1 calc R . . H10B H 0.7492 0.2700 0.4133 0.035 Uiso 1 1 calc R . . H10C H 0.7251 0.3411 0.4885 0.035 Uiso 1 1 calc R . . C11 C 0.2664(2) 0.11389(12) 0.40821(10) 0.0272(4) Uani 1 1 d . . . H11A H 0.3155 0.1248 0.4641 0.041 Uiso 1 1 calc R . . H11B H 0.3265 0.0611 0.3834 0.041 Uiso 1 1 calc R . . H11C H 0.1525 0.0933 0.4079 0.041 Uiso 1 1 calc R . . C12 C 0.1538(2) 0.39593(12) 0.50770(10) 0.0271(4) Uani 1 1 d . . . H12A H 0.2072 0.4178 0.5605 0.041 Uiso 1 1 calc R . . H12B H 0.0458 0.3688 0.5138 0.041 Uiso 1 1 calc R . . H12C H 0.1425 0.4533 0.4706 0.041 Uiso 1 1 calc R . . C13 C 0.4269(2) 0.06376(11) 0.23506(10) 0.0239(3) Uani 1 1 d . . . H13A H 0.4651 0.0619 0.1816 0.036 Uiso 1 1 calc R . . H13B H 0.3155 0.0903 0.2300 0.036 Uiso 1 1 calc R . . H13C H 0.4283 -0.0044 0.2575 0.036 Uiso 1 1 calc R . . C14 C 0.6932(2) 0.07139(11) 0.38304(9) 0.0243(3) Uani 1 1 d . . . H14A H 0.6519 0.0795 0.4354 0.036 Uiso 1 1 calc R . . H14B H 0.8064 0.0948 0.3873 0.036 Uiso 1 1 calc R . . H14C H 0.6886 0.0003 0.3676 0.036 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 0.0231(2) 0.0144(2) 0.0186(2) -0.00027(15) 0.00205(16) 0.00043(16) N1 0.0212(7) 0.0224(7) 0.0225(7) 0.0017(5) 0.0024(5) 0.0027(5) N2 0.0222(7) 0.0180(6) 0.0192(7) 0.0008(5) 0.0025(5) 0.0014(5) N3 0.0216(7) 0.0245(7) 0.0203(7) 0.0013(5) 0.0033(5) 0.0005(5) N4 0.0205(6) 0.0176(6) 0.0183(6) -0.0028(5) 0.0021(5) -0.0007(5) N5 0.0215(7) 0.0198(6) 0.0221(7) -0.0025(5) 0.0038(5) -0.0013(5) N6 0.0238(7) 0.0202(6) 0.0206(7) -0.0035(5) 0.0036(5) 0.0013(5) C1 0.0227(8) 0.0172(7) 0.0185(7) -0.0011(5) 0.0018(6) 0.0013(6) C2 0.0252(8) 0.0189(7) 0.0199(8) 0.0004(6) 0.0029(6) 0.0012(6) C3 0.0229(8) 0.0292(8) 0.0220(8) 0.0015(6) 0.0023(6) 0.0002(6) C4 0.0316(9) 0.0232(8) 0.0336(9) 0.0022(7) 0.0076(7) 0.0072(7) C5 0.0237(8) 0.0199(7) 0.0224(8) 0.0007(6) 0.0011(6) 0.0018(6) C6 0.0274(9) 0.0322(9) 0.0269(9) 0.0023(7) 0.0068(7) -0.0016(7) C7 0.0223(8) 0.0168(7) 0.0168(7) 0.0000(5) 0.0017(6) -0.0012(6) C8 0.0222(8) 0.0248(8) 0.0220(8) -0.0031(6) 0.0017(6) 0.0009(6) C9 0.0263(8) 0.0163(7) 0.0198(8) -0.0020(6) 0.0025(6) 0.0002(6) C10 0.0242(8) 0.0207(7) 0.0240(8) -0.0017(6) 0.0022(6) -0.0033(6) C11 0.0300(9) 0.0211(8) 0.0318(9) -0.0030(7) 0.0093(7) -0.0048(7) C12 0.0290(9) 0.0259(8) 0.0269(9) -0.0046(6) 0.0059(7) 0.0034(7) C13 0.0300(9) 0.0179(7) 0.0237(8) -0.0022(6) 0.0023(6) -0.0003(6) C14 0.0298(9) 0.0192(7) 0.0234(8) 0.0016(6) 0.0012(6) 0.0017(6) _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 C14 1.8777(16) . ? Si1 C13 1.8816(16) . ? Si1 C1 1.9228(16) . ? Si1 C7 1.9293(15) . ? N1 C3 1.451(2) . ? N1 C1 1.4618(19) . ? N1 C4 1.472(2) . ? N2 C5 1.4599(19) . ? N2 C2 1.4638(19) . ? N2 C1 1.4838(19) . ? N3 C2 1.454(2) . ? N3 C6 1.460(2) . ? N3 C3 1.4640(19) . ? N4 C9 1.4616(19) . ? N4 C10 1.4616(19) . ? N4 C7 1.4867(18) . ? N5 C8 1.454(2) . ? N5 C7 1.4599(19) . ? N5 C11 1.471(2) . ? N6 C9 1.452(2) . ? N6 C12 1.461(2) . ? N6 C8 1.4640(19) . ? C1 H1 1.0000 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7 1.0000 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Si1 C13 111.16(7) . . ? C14 Si1 C1 110.10(7) . . ? C13 Si1 C1 109.04(7) . . ? C14 Si1 C7 109.40(7) . . ? C13 Si1 C7 110.47(7) . . ? C1 Si1 C7 106.57(6) . . ? C3 N1 C1 109.62(12) . . ? C3 N1 C4 110.66(13) . . ? C1 N1 C4 113.37(13) . . ? C5 N2 C2 107.57(11) . . ? C5 N2 C1 112.95(11) . . ? C2 N2 C1 108.72(12) . . ? C2 N3 C6 109.82(12) . . ? C2 N3 C3 108.89(12) . . ? C6 N3 C3 110.15(12) . . ? C9 N4 C10 107.75(11) . . ? C9 N4 C7 109.55(11) . . ? C10 N4 C7 112.60(11) . . ? C8 N5 C7 109.91(12) . . ? C8 N5 C11 110.72(12) . . ? C7 N5 C11 113.99(12) . . ? C9 N6 C12 110.56(12) . . ? C9 N6 C8 108.79(12) . . ? C12 N6 C8 110.66(12) . . ? N1 C1 N2 110.18(12) . . ? N1 C1 Si1 112.58(10) . . ? N2 C1 Si1 114.55(10) . . ? N1 C1 H1 106.3 . . ? N2 C1 H1 106.3 . . ? Si1 C1 H1 106.3 . . ? N3 C2 N2 111.19(12) . . ? N3 C2 H2A 109.4 . . ? N2 C2 H2A 109.4 . . ? N3 C2 H2B 109.4 . . ? N2 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N1 C3 N3 112.20(13) . . ? N1 C3 H3A 109.2 . . ? N3 C3 H3A 109.2 . . ? N1 C3 H3B 109.2 . . ? N3 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N5 C7 N4 110.60(12) . . ? N5 C7 Si1 111.67(10) . . ? N4 C7 Si1 114.36(10) . . ? N5 C7 H7 106.6 . . ? N4 C7 H7 106.6 . . ? Si1 C7 H7 106.6 . . ? N5 C8 N6 111.48(12) . . ? N5 C8 H8A 109.3 . . ? N6 C8 H8A 109.3 . . ? N5 C8 H8B 109.3 . . ? N6 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N6 C9 N4 111.32(12) . . ? N6 C9 H9A 109.4 . . ? N4 C9 H9A 109.4 . . ? N6 C9 H9B 109.4 . . ? N4 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N4 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 H11A 109.5 . . ? N5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.362 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.050 #============================================================================== data_compound6 _database_code_depnum_ccdc_archive 'CCDC 821377' #TrackingRef '- COSI19_05_06_08.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H15 Cl2 N3 Si' _chemical_formula_sum 'C6 H15 Cl2 N3 Si' _chemical_formula_weight 228.20 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 0.0000 0.0000 '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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' 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 6.7426(2) _cell_length_b 15.1934(3) _cell_length_c 21.4697(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2199.42(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25323 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8275 _exptl_absorpt_correction_T_max 0.8585 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20157 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2505 _reflns_number_gt 2428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^2^+2.8277P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2505 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Cl1 Cl 0.04791(7) 0.17042(3) 0.16123(2) 0.02238(11) Uani 1 1 d . . . Cl2 Cl 0.00923(7) -0.02642(3) 0.10927(2) 0.02557(12) Uani 1 1 d . . . Si3 Si 0.22938(8) 0.07431(3) 0.11984(2) 0.01794(12) Uani 1 1 d . . . N1 N 0.3920(2) 0.01794(10) 0.16574(7) 0.0206(3) Uani 1 1 d . . . N2 N 0.4917(2) 0.14864(10) 0.13235(7) 0.0198(3) Uani 1 1 d . . . N3 N 0.4232(3) 0.16294(11) 0.02617(7) 0.0226(3) Uani 1 1 d . . . C1 C 0.5541(3) 0.07838(13) 0.17578(9) 0.0222(4) Uani 1 1 d . . . H1A H 0.684(3) 0.0521(14) 0.1647(10) 0.024(6) Uiso 1 1 d . . . H1B H 0.559(3) 0.1022(13) 0.2186(9) 0.019(5) Uiso 1 1 d . . . C2 C 0.5809(3) 0.14249(13) 0.06953(9) 0.0223(4) Uani 1 1 d . . . H2A H 0.692(3) 0.1822(14) 0.0638(9) 0.019(5) Uiso 1 1 d . . . H2B H 0.637(3) 0.0815(14) 0.0649(9) 0.020(5) Uiso 1 1 d . . . C3 C 0.2654(3) 0.09802(13) 0.03483(8) 0.0216(4) Uani 1 1 d . . . H3A H 0.300(3) 0.0404(14) 0.0152(9) 0.022(5) Uiso 1 1 d . . . H3B H 0.145(4) 0.1183(14) 0.0196(10) 0.025(6) Uiso 1 1 d . . . C4 C 0.3966(3) -0.06589(14) 0.19790(10) 0.0272(4) Uani 1 1 d . . . H4A H 0.514(4) -0.0991(15) 0.1865(10) 0.028(6) Uiso 1 1 d . . . H4B H 0.279(4) -0.0993(16) 0.1865(11) 0.037(7) Uiso 1 1 d . . . H4C H 0.404(4) -0.0583(15) 0.2431(12) 0.036(6) Uiso 1 1 d . . . C5 C 0.5021(3) 0.23913(13) 0.15716(10) 0.0266(4) Uani 1 1 d . . . H5A H 0.643(4) 0.2550(15) 0.1650(10) 0.031(6) Uiso 1 1 d . . . H5B H 0.425(3) 0.2426(15) 0.1946(11) 0.027(6) Uiso 1 1 d . . . H5C H 0.446(3) 0.2817(14) 0.1268(10) 0.021(5) Uiso 1 1 d . . . C6 C 0.4974(4) 0.16525(15) -0.03788(9) 0.0299(5) Uani 1 1 d . . . H6A H 0.550(3) 0.1083(16) -0.0507(10) 0.028(6) Uiso 1 1 d . . . H6B H 0.604(4) 0.2094(16) -0.0416(11) 0.038(7) Uiso 1 1 d . . . H6C H 0.384(4) 0.1795(15) -0.0664(10) 0.028(6) Uiso 1 1 d . . . 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 Cl1 0.0226(2) 0.0239(2) 0.0207(2) 0.00146(17) 0.00262(17) 0.00595(18) Cl2 0.0216(2) 0.0232(2) 0.0319(2) 0.00089(19) -0.00254(18) -0.00270(18) Si3 0.0180(2) 0.0191(2) 0.0167(2) 0.00071(18) -0.00016(19) 0.0014(2) N1 0.0204(8) 0.0203(7) 0.0211(7) 0.0031(6) -0.0027(6) 0.0005(6) N2 0.0215(8) 0.0182(7) 0.0195(7) -0.0014(6) 0.0005(6) 0.0011(6) N3 0.0263(8) 0.0232(8) 0.0181(7) 0.0028(6) 0.0036(7) 0.0022(7) C1 0.0224(9) 0.0252(9) 0.0190(8) 0.0006(7) -0.0030(7) 0.0014(8) C2 0.0204(9) 0.0230(9) 0.0235(9) 0.0016(7) 0.0035(7) 0.0000(8) C3 0.0247(10) 0.0229(9) 0.0173(8) 0.0000(7) -0.0011(7) 0.0019(8) C4 0.0299(11) 0.0240(10) 0.0278(10) 0.0067(8) -0.0033(9) 0.0037(9) C5 0.0294(11) 0.0197(9) 0.0308(10) -0.0053(8) -0.0002(9) -0.0004(8) C6 0.0388(12) 0.0300(11) 0.0211(9) 0.0057(8) 0.0079(9) 0.0072(10) _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 Cl1 Si3 2.1022(7) . ? Cl2 Si3 2.1441(7) . ? Si3 N1 1.7048(16) . ? Si3 C3 1.8761(18) . ? Si3 N2 2.1154(17) . ? N1 C1 1.444(3) . ? N1 C4 1.449(2) . ? N2 C5 1.476(2) . ? N2 C1 1.479(2) . ? N2 C2 1.480(2) . ? N3 C2 1.447(3) . ? N3 C3 1.463(3) . ? N3 C6 1.464(2) . ? C1 H1A 0.99(2) . ? C1 H1B 0.99(2) . ? C2 H2A 0.97(2) . ? C2 H2B 1.01(2) . ? C3 H3A 1.00(2) . ? C3 H3B 0.93(2) . ? C4 H4A 0.97(2) . ? C4 H4B 0.97(3) . ? C4 H4C 0.98(3) . ? C5 H5A 0.99(2) . ? C5 H5B 0.96(2) . ? C5 H5C 0.99(2) . ? C6 H6A 0.97(2) . ? C6 H6B 0.99(3) . ? C6 H6C 1.00(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 Si3 C3 125.15(9) . . ? N1 Si3 Cl1 118.61(6) . . ? C3 Si3 Cl1 110.68(7) . . ? N1 Si3 N2 69.96(7) . . ? C3 Si3 N2 85.01(8) . . ? Cl1 Si3 N2 93.56(5) . . ? N1 Si3 Cl2 98.50(6) . . ? C3 Si3 Cl2 97.10(7) . . ? Cl1 Si3 Cl2 97.91(3) . . ? N2 Si3 Cl2 166.72(5) . . ? C1 N1 C4 118.12(16) . . ? C1 N1 Si3 104.70(12) . . ? C4 N1 Si3 136.96(14) . . ? C5 N2 C1 115.55(15) . . ? C5 N2 C2 111.61(15) . . ? C1 N2 C2 114.41(15) . . ? C5 N2 Si3 125.65(13) . . ? C1 N2 Si3 86.15(11) . . ? C2 N2 Si3 100.98(11) . . ? C2 N3 C3 107.95(15) . . ? C2 N3 C6 110.99(16) . . ? C3 N3 C6 112.59(16) . . ? N1 C1 N2 98.59(14) . . ? N1 C1 H1A 112.2(13) . . ? N2 C1 H1A 113.0(12) . . ? N1 C1 H1B 113.5(12) . . ? N2 C1 H1B 109.4(12) . . ? H1A C1 H1B 109.8(17) . . ? N3 C2 N2 105.89(15) . . ? N3 C2 H2A 110.7(12) . . ? N2 C2 H2A 113.0(12) . . ? N3 C2 H2B 114.3(12) . . ? N2 C2 H2B 107.6(12) . . ? H2A C2 H2B 105.5(17) . . ? N3 C3 Si3 110.31(12) . . ? N3 C3 H3A 111.5(13) . . ? Si3 C3 H3A 105.8(12) . . ? N3 C3 H3B 111.6(14) . . ? Si3 C3 H3B 107.0(13) . . ? H3A C3 H3B 110.3(18) . . ? N1 C4 H4A 110.8(14) . . ? N1 C4 H4B 108.8(15) . . ? H4A C4 H4B 109.1(19) . . ? N1 C4 H4C 111.7(14) . . ? H4A C4 H4C 105.8(19) . . ? H4B C4 H4C 111(2) . . ? N2 C5 H5A 109.4(14) . . ? N2 C5 H5B 109.1(14) . . ? H5A C5 H5B 111.2(19) . . ? N2 C5 H5C 110.5(12) . . ? H5A C5 H5C 108.6(18) . . ? H5B C5 H5C 108.0(18) . . ? N3 C6 H6A 111.6(13) . . ? N3 C6 H6B 110.0(14) . . ? H6A C6 H6B 109(2) . . ? N3 C6 H6C 108.5(13) . . ? H6A C6 H6C 107.2(19) . . ? H6B C6 H6C 111.0(19) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.314 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.052 #============================================================================== data_compound8 _database_code_depnum_ccdc_archive 'CCDC 821378' #TrackingRef '- COSI19_05_06_08.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H66 Li2 N12 Si2' _chemical_formula_sum 'C28 H66 Li2 N12 Si2' _chemical_formula_weight 640.99 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 0.0000 0.0000 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0976(11) _cell_length_b 12.225(2) _cell_length_c 12.2926(17) _cell_angle_alpha 61.357(6) _cell_angle_beta 77.351(7) _cell_angle_gamma 86.350(6) _cell_volume 912.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4717 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 352 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9609 _exptl_absorpt_correction_T_max 0.9789 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10304 _diffrn_reflns_av_R_equivalents 0.146 _diffrn_reflns_av_sigmaI/netI 0.2327 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3755 _reflns_number_gt 1688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Bruker AXS, 2004' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0512P)^2^+0.0000P] 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_extinction_coef ? _refine_ls_number_reflns 3755 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1894 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.888 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.40039(16) 0.32598(9) 0.75597(10) 0.0220(3) Uani 1 1 d . . . N1 N 0.3258(4) 0.2365(3) 0.5919(3) 0.0226(8) Uani 1 1 d . . . N2 N 0.1548(4) 0.1157(3) 0.8200(3) 0.0236(8) Uani 1 1 d . . . N3 N 0.3642(4) 0.0127(3) 0.7161(3) 0.0244(8) Uani 1 1 d . . . N4 N 0.3647(4) 0.5765(3) 0.7081(3) 0.0199(7) Uani 1 1 d . . . N5 N 0.1029(4) 0.6576(3) 0.8057(3) 0.0217(7) Uani 1 1 d . . . N6 N 0.0960(4) 0.4393(2) 0.8664(3) 0.0197(7) Uani 1 1 d . . . Li1 Li 0.4861(10) 0.4142(6) 0.4714(6) 0.0351(17) Uani 1 1 d . . . C1 C 0.2343(5) 0.2375(3) 0.7129(3) 0.0227(9) Uani 1 1 d . . . H1 H 0.1197 0.2899 0.6940 0.027 Uiso 1 1 calc R . . C2 C 0.2933(6) 0.0215(3) 0.8332(3) 0.0250(9) Uani 1 1 d . . . H2A H 0.2331 -0.0604 0.9015 0.030 Uiso 1 1 calc R . . H2B H 0.4046 0.0400 0.8592 0.030 Uiso 1 1 calc R . . C3 C 0.4577(5) 0.1345(3) 0.6185(3) 0.0263(9) Uani 1 1 d . . . H3A H 0.5667 0.1524 0.6469 0.032 Uiso 1 1 calc R . . H3B H 0.5114 0.1304 0.5392 0.032 Uiso 1 1 calc R . . C4 C 0.1874(6) 0.2295(3) 0.5213(3) 0.0300(10) Uani 1 1 d . . . H4A H 0.2572 0.2435 0.4372 0.045 Uiso 1 1 calc R . . H4B H 0.0925 0.2936 0.5118 0.045 Uiso 1 1 calc R . . H4C H 0.1206 0.1469 0.5679 0.045 Uiso 1 1 calc R . . C5 C -0.0383(5) 0.0756(3) 0.8229(3) 0.0282(10) Uani 1 1 d . . . H5A H -0.0285 0.0490 0.7584 0.042 Uiso 1 1 calc R . . H5B H -0.1243 0.1453 0.8053 0.042 Uiso 1 1 calc R . . H5C H -0.0907 0.0059 0.9070 0.042 Uiso 1 1 calc R . . C6 C 0.5055(6) -0.0834(3) 0.7366(4) 0.0322(10) Uani 1 1 d . . . H6A H 0.6111 -0.0646 0.7657 0.048 Uiso 1 1 calc R . . H6B H 0.5574 -0.0854 0.6569 0.048 Uiso 1 1 calc R . . H6C H 0.4430 -0.1648 0.8010 0.048 Uiso 1 1 calc R . . C7 C 0.2438(5) 0.4627(3) 0.7509(3) 0.0202(9) Uani 1 1 d . . . H7 H 0.1704 0.4837 0.6831 0.024 Uiso 1 1 calc R . . C8 C 0.2426(5) 0.6820(3) 0.6899(3) 0.0255(9) Uani 1 1 d . . . H8A H 0.3248 0.7570 0.6622 0.031 Uiso 1 1 calc R . . H8B H 0.1732 0.6992 0.6221 0.031 Uiso 1 1 calc R . . C9 C -0.0185(5) 0.5487(3) 0.8426(3) 0.0246(9) Uani 1 1 d . . . H9A H -0.0866 0.5659 0.7742 0.029 Uiso 1 1 calc R . . H9B H -0.1171 0.5318 0.9202 0.029 Uiso 1 1 calc R . . C10 C 0.4830(5) 0.5570(3) 0.8004(3) 0.0239(9) Uani 1 1 d . . . H10A H 0.5515 0.6357 0.7745 0.036 Uiso 1 1 calc R . . H10B H 0.5771 0.4939 0.8034 0.036 Uiso 1 1 calc R . . H10C H 0.3990 0.5285 0.8847 0.036 Uiso 1 1 calc R . . C11 C -0.0157(6) 0.7660(3) 0.7840(3) 0.0316(10) Uani 1 1 d . . . H11A H 0.0672 0.8384 0.7606 0.047 Uiso 1 1 calc R . . H11B H -0.1121 0.7478 0.8618 0.047 Uiso 1 1 calc R . . H11C H -0.0813 0.7842 0.7152 0.047 Uiso 1 1 calc R . . C12 C -0.0383(5) 0.3338(3) 0.9060(3) 0.0262(9) Uani 1 1 d . . . H12A H -0.1355 0.3225 0.9812 0.039 Uiso 1 1 calc R . . H12B H 0.0336 0.2577 0.9263 0.039 Uiso 1 1 calc R . . H12C H -0.1026 0.3508 0.8370 0.039 Uiso 1 1 calc R . . C13 C 0.6106(6) 0.3951(4) 0.6291(3) 0.0223(9) Uani 1 1 d . . . H13A H 0.705(5) 0.432(3) 0.644(3) 0.033(10) Uiso 1 1 d . . . H13B H 0.693(6) 0.343(3) 0.611(3) 0.038(12) Uiso 1 1 d . . . C14 C 0.4317(5) 0.2267(3) 0.9242(3) 0.0269(10) Uani 1 1 d . . . H14A H 0.5429 0.1748 0.9249 0.040 Uiso 1 1 calc R . . H14B H 0.3148 0.1732 0.9759 0.040 Uiso 1 1 calc R . . H14C H 0.4537 0.2808 0.9592 0.040 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 0.0235(6) 0.0220(6) 0.0214(6) -0.0111(5) -0.0048(5) 0.0010(5) N1 0.0271(19) 0.0219(18) 0.0189(16) -0.0101(14) -0.0037(15) -0.0017(15) N2 0.0241(19) 0.0179(17) 0.0238(18) -0.0066(14) -0.0028(15) -0.0025(15) N3 0.031(2) 0.0194(18) 0.0239(18) -0.0110(15) -0.0062(16) 0.0029(15) N4 0.0178(18) 0.0206(17) 0.0231(17) -0.0116(14) -0.0049(14) 0.0021(14) N5 0.0214(18) 0.0242(18) 0.0231(17) -0.0150(15) -0.0040(15) 0.0046(15) N6 0.0194(18) 0.0176(17) 0.0222(17) -0.0100(14) -0.0037(14) 0.0018(14) Li1 0.033(4) 0.038(4) 0.036(4) -0.019(3) -0.008(3) -0.001(3) C1 0.026(2) 0.020(2) 0.021(2) -0.0083(17) -0.0062(18) -0.0002(17) C2 0.032(2) 0.018(2) 0.024(2) -0.0092(17) -0.0068(19) -0.0017(19) C3 0.031(2) 0.026(2) 0.023(2) -0.0143(18) 0.0000(19) 0.0001(19) C4 0.035(3) 0.034(2) 0.023(2) -0.0136(19) -0.0093(19) -0.002(2) C5 0.028(2) 0.028(2) 0.029(2) -0.0152(19) -0.0023(19) -0.0054(19) C6 0.037(3) 0.028(2) 0.037(2) -0.019(2) -0.010(2) 0.008(2) C7 0.021(2) 0.022(2) 0.0152(19) -0.0070(16) -0.0043(17) -0.0011(17) C8 0.026(2) 0.019(2) 0.032(2) -0.0128(18) -0.007(2) 0.0031(18) C9 0.017(2) 0.031(2) 0.021(2) -0.0100(18) 0.0002(17) -0.0049(18) C10 0.018(2) 0.028(2) 0.029(2) -0.0157(18) -0.0055(18) 0.0012(17) C11 0.028(2) 0.036(3) 0.033(2) -0.018(2) -0.007(2) 0.005(2) C12 0.020(2) 0.029(2) 0.031(2) -0.0155(19) -0.0040(18) 0.0004(18) C13 0.022(2) 0.026(2) 0.024(2) -0.0167(19) -0.0019(19) 0.000(2) C14 0.026(2) 0.025(2) 0.026(2) -0.0111(18) -0.0018(19) -0.0004(18) _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 C13 1.803(4) . ? Si1 C14 1.887(3) . ? Si1 C7 1.930(4) . ? Si1 C1 1.956(3) . ? Si1 Li1 3.050(7) . ? Si1 Li1 3.063(7) 2_666 ? N1 C3 1.460(5) . ? N1 C4 1.477(4) . ? N1 C1 1.492(4) . ? N1 Li1 2.168(7) . ? N2 C2 1.438(5) . ? N2 C5 1.472(4) . ? N2 C1 1.473(4) . ? N3 C6 1.459(5) . ? N3 C2 1.469(4) . ? N3 C3 1.470(4) . ? N4 C8 1.460(4) . ? N4 C10 1.477(4) . ? N4 C7 1.484(4) . ? N4 Li1 2.181(8) 2_666 ? N5 C8 1.453(4) . ? N5 C9 1.455(4) . ? N5 C11 1.468(4) . ? N6 C9 1.459(4) . ? N6 C12 1.470(4) . ? N6 C7 1.481(4) . ? Li1 N4 2.181(8) 2_666 ? Li1 C13 2.200(8) 2_666 ? Li1 C13 2.210(7) . ? Li1 Li1 2.542(13) 2_666 ? Li1 C7 2.746(8) 2_666 ? Li1 Si1 3.063(7) 2_666 ? Li1 H13B 2.32(4) . ? C1 H1 1.0000 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 Li1 2.746(8) 2_666 ? C7 H7 1.0000 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Li1 2.200(8) 2_666 ? C13 H13A 0.92(3) . ? C13 H13B 0.91(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Si1 C14 119.54(17) . . ? C13 Si1 C7 106.10(18) . . ? C14 Si1 C7 107.70(16) . . ? C13 Si1 C1 109.73(16) . . ? C14 Si1 C1 110.52(15) . . ? C7 Si1 C1 101.62(15) . . ? C13 Si1 Li1 45.79(16) . . ? C14 Si1 Li1 155.34(19) . . ? C7 Si1 Li1 96.43(17) . . ? C1 Si1 Li1 68.17(15) . . ? C13 Si1 Li1 45.13(19) . 2_666 ? C14 Si1 Li1 140.67(16) . 2_666 ? C7 Si1 Li1 61.92(18) . 2_666 ? C1 Si1 Li1 108.77(15) . 2_666 ? Li1 Si1 Li1 49.1(2) . 2_666 ? C3 N1 C4 110.8(3) . . ? C3 N1 C1 109.1(3) . . ? C4 N1 C1 114.5(3) . . ? C3 N1 Li1 110.0(3) . . ? C4 N1 Li1 106.3(3) . . ? C1 N1 Li1 105.8(3) . . ? C2 N2 C5 112.4(3) . . ? C2 N2 C1 110.5(3) . . ? C5 N2 C1 116.4(3) . . ? C6 N3 C2 110.0(3) . . ? C6 N3 C3 109.4(3) . . ? C2 N3 C3 107.2(3) . . ? C8 N4 C10 110.0(3) . . ? C8 N4 C7 110.1(3) . . ? C10 N4 C7 111.1(3) . . ? C8 N4 Li1 112.2(3) . 2_666 ? C10 N4 Li1 117.4(3) . 2_666 ? C7 N4 Li1 95.1(3) . 2_666 ? C8 N5 C9 108.1(3) . . ? C8 N5 C11 110.0(3) . . ? C9 N5 C11 110.1(3) . . ? C9 N6 C12 107.4(3) . . ? C9 N6 C7 110.2(3) . . ? C12 N6 C7 111.9(3) . . ? N1 Li1 N4 109.8(3) . 2_666 ? N1 Li1 C13 131.5(4) . 2_666 ? N4 Li1 C13 90.8(3) 2_666 2_666 ? N1 Li1 C13 91.4(3) . . ? N4 Li1 C13 128.6(3) 2_666 . ? C13 Li1 C13 109.6(3) 2_666 . ? N1 Li1 Li1 126.4(5) . 2_666 ? N4 Li1 Li1 123.7(4) 2_666 2_666 ? C13 Li1 Li1 55.0(3) 2_666 2_666 ? C13 Li1 Li1 54.6(2) . 2_666 ? N1 Li1 C7 141.5(3) . 2_666 ? N4 Li1 C7 32.57(14) 2_666 2_666 ? C13 Li1 C7 73.3(2) 2_666 2_666 ? C13 Li1 C7 108.3(3) . 2_666 ? Li1 Li1 C7 91.4(3) 2_666 2_666 ? N1 Li1 Si1 63.97(18) . . ? N4 Li1 Si1 157.1(3) 2_666 . ? C13 Li1 Si1 109.8(3) 2_666 . ? C13 Li1 Si1 35.78(15) . . ? Li1 Li1 Si1 65.7(3) 2_666 . ? C7 Li1 Si1 143.9(2) 2_666 . ? N1 Li1 Si1 158.4(3) . 2_666 ? N4 Li1 Si1 62.79(18) 2_666 2_666 ? C13 Li1 Si1 35.51(15) 2_666 2_666 ? C13 Li1 Si1 109.1(2) . 2_666 ? Li1 Li1 Si1 65.2(3) 2_666 2_666 ? C7 Li1 Si1 38.33(11) 2_666 2_666 ? Si1 Li1 Si1 130.9(2) . 2_666 ? N1 Li1 H13B 87.0(9) . . ? N4 Li1 H13B 109.3(11) 2_666 . ? C13 Li1 H13B 127.9(10) 2_666 . ? C13 Li1 H13B 23.2(10) . . ? Li1 Li1 H13B 74.5(10) 2_666 . ? C7 Li1 H13B 98.3(10) 2_666 . ? Si1 Li1 H13B 50.2(10) . . ? Si1 Li1 H13B 114.5(9) 2_666 . ? N2 C1 N1 115.4(3) . . ? N2 C1 Si1 113.5(2) . . ? N1 C1 Si1 111.6(2) . . ? N2 C1 H1 105.1 . . ? N1 C1 H1 105.1 . . ? Si1 C1 H1 105.1 . . ? N2 C2 N3 113.3(3) . . ? N2 C2 H2A 108.9 . . ? N3 C2 H2A 108.9 . . ? N2 C2 H2B 108.9 . . ? N3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N1 C3 N3 113.0(3) . . ? N1 C3 H3A 109.0 . . ? N3 C3 H3A 109.0 . . ? N1 C3 H3B 109.0 . . ? N3 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N6 C7 N4 109.9(3) . . ? N6 C7 Si1 117.6(2) . . ? N4 C7 Si1 111.5(2) . . ? N6 C7 Li1 160.5(3) . 2_666 ? N4 C7 Li1 52.3(2) . 2_666 ? Si1 C7 Li1 79.7(2) . 2_666 ? N6 C7 H7 105.7 . . ? N4 C7 H7 105.7 . . ? Si1 C7 H7 105.7 . . ? Li1 C7 H7 75.8 2_666 . ? N5 C8 N4 111.6(3) . . ? N5 C8 H8A 109.3 . . ? N4 C8 H8A 109.3 . . ? N5 C8 H8B 109.3 . . ? N4 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N5 C9 N6 111.1(3) . . ? N5 C9 H9A 109.4 . . ? N6 C9 H9A 109.4 . . ? N5 C9 H9B 109.4 . . ? N6 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N4 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 H11A 109.5 . . ? N5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 Li1 99.4(3) . 2_666 ? Si1 C13 Li1 98.4(2) . . ? Li1 C13 Li1 70.4(3) 2_666 . ? Si1 C13 H13A 117(2) . . ? Li1 C13 H13A 85(2) 2_666 . ? Li1 C13 H13A 140(2) . . ? Si1 C13 H13B 118(2) . . ? Li1 C13 H13B 138(2) 2_666 . ? Li1 C13 H13B 85(2) . . ? H13A C13 H13B 94(3) . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.897 _refine_diff_density_max 0.320 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.068 #===END