Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Forbes, Glenn C.' 'Kennedy, Alan R.' 'Mulvey, R. E.' 'Rodger, Philip J. A.' _publ_contact_author_name 'Prof R E Mulvey' _publ_contact_author_address ; Prof R E Mulvey Department of Pure & Applied Chemistry University of Strathclyde Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email 'R.E.MULVEY@STRATH.AC.UK' _publ_contact_letter ; Dear Sir, This file contains the supplementary X-ray data for paper b102184m which was recently resubmitted to you by Forbes, Kennedy, Mulvey & Rodger, after changes were made following the refereeing process. If there are any problems with it please contact me. Yours Sincerely Alan Kennedy a.r.kennedy@strath.ac.uk 0141 548 2016 P & A Chemistry University of Strathclyde 295 Cathedral St Glasgow G1 1XL Scotland ; #------------------------------------------------------------------------- #-----------------------------COMPOUND 1------------------------------------ #--------------------------------------------------------------------------- data_gr14 _database_code_CSD 160882 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H72 Mg2 N4 O2 Si4' _chemical_formula_weight 681.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 16.6987(6) _cell_length_b 11.3018(3) _cell_length_c 22.5795(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.7610(10) _cell_angle_gamma 90.00 _cell_volume 4260.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4902 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 30.51 _exptl_crystal_description 'cut needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.197 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi + omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5424 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 23.00 _reflns_number_total 5424 _reflns_number_gt 3664 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Denzo & Collect (Otwinowski & Minor, 1997; Hooft & Nonius 1988) ; _computing_cell_refinement 'Denzo & Collect' _computing_data_reduction 'Denzo & Collect' _computing_structure_solution 'SIR-97 ' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+5.0807P] 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 5424 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.13618(7) 0.14124(9) 0.05855(5) 0.0295(3) Uani 1 d . . . Si2 Si 0.29007(7) 0.16692(10) 0.13079(5) 0.0301(3) Uani 1 d . . . Si3 Si 0.22560(7) -0.23810(10) 0.38126(5) 0.0298(3) Uani 1 d . . . Si4 Si 0.05431(7) -0.18967(10) 0.41790(5) 0.0337(3) Uani 1 d . . . Mg1 Mg 0.14841(8) 0.02931(10) 0.18574(5) 0.0263(3) Uani 1 d . . . Mg2 Mg 0.11928(7) -0.07273(11) 0.30239(5) 0.0264(3) Uani 1 d . . . O1 O 0.11062(14) -0.1192(2) 0.21861(10) 0.0263(6) Uani 1 d . . . O2 O 0.15769(15) 0.0779(2) 0.26821(10) 0.0288(7) Uani 1 d . . . N1 N 0.19422(17) 0.1182(2) 0.12025(12) 0.0251(8) Uani 1 d . . . N2 N 0.08519(18) -0.1965(2) 0.17001(12) 0.0252(8) Uani 1 d . . . N3 N 0.13336(17) -0.1772(2) 0.37134(12) 0.0246(8) Uani 1 d . . . N4 N 0.11046(18) 0.1375(3) 0.31391(12) 0.0277(8) Uani 1 d . . . C1 C 0.0316(2) 0.0957(4) 0.07629(18) 0.0508(13) Uani 1 d . . . H1A H 0.0312 0.0124 0.0882 0.076 Uiso 1 calc R . . H1B H -0.0029 0.1063 0.0412 0.076 Uiso 1 calc R . . H1C H 0.0116 0.1447 0.1087 0.076 Uiso 1 calc R . . C2 C 0.1665(3) 0.0498(4) -0.00646(17) 0.0463(12) Uani 1 d . . . H2A H 0.2226 0.0658 -0.0156 0.070 Uiso 1 calc R . . H2B H 0.1326 0.0699 -0.0408 0.070 Uiso 1 calc R . . H2C H 0.1600 -0.0343 0.0030 0.070 Uiso 1 calc R . . C3 C 0.1348(3) 0.2989(4) 0.0342(2) 0.0617(15) Uani 1 d . . . H3A H 0.1180 0.3492 0.0671 0.092 Uiso 1 calc R . . H3B H 0.0972 0.3081 0.0009 0.092 Uiso 1 calc R . . H3C H 0.1886 0.3222 0.0219 0.092 Uiso 1 calc R . . C4 C 0.3565(3) 0.1387(4) 0.06634(18) 0.0547(13) Uani 1 d . . . H4A H 0.3550 0.0544 0.0563 0.082 Uiso 1 calc R . . H4B H 0.4115 0.1616 0.0767 0.082 Uiso 1 calc R . . H4C H 0.3377 0.1853 0.0323 0.082 Uiso 1 calc R . . C5 C 0.2962(3) 0.3293(3) 0.14681(18) 0.0423(12) Uani 1 d . . . H5A H 0.2708 0.3735 0.1143 0.063 Uiso 1 calc R . . H5B H 0.3525 0.3528 0.1507 0.063 Uiso 1 calc R . . H5C H 0.2685 0.3465 0.1838 0.063 Uiso 1 calc R . . C6 C 0.3364(2) 0.0865(3) 0.19544(17) 0.0341(11) Uani 1 d . . . H6A H 0.3038 0.0989 0.2306 0.051 Uiso 1 calc R . . H6B H 0.3906 0.1169 0.2029 0.051 Uiso 1 calc R . . H6C H 0.3391 0.0017 0.1866 0.051 Uiso 1 calc R . . C7 C 0.1519(2) -0.2784(3) 0.15518(16) 0.0282(10) Uani 1 d . . . C8 C 0.1237(2) -0.3490(4) 0.10066(17) 0.0398(11) Uani 1 d . . . H8A H 0.1192 -0.2947 0.0664 0.048 Uiso 1 calc R . . H8B H 0.1646 -0.4093 0.0912 0.048 Uiso 1 calc R . . C9 C 0.0434(3) -0.4105(4) 0.10927(18) 0.0437(12) Uani 1 d . . . H9A H 0.0259 -0.4486 0.0718 0.052 Uiso 1 calc R . . H9B H 0.0489 -0.4726 0.1399 0.052 Uiso 1 calc R . . C10 C -0.0182(2) -0.3207(4) 0.12801(17) 0.0379(11) Uani 1 d . . . H10A H -0.0694 -0.3621 0.1354 0.046 Uiso 1 calc R . . H10B H -0.0275 -0.2644 0.0950 0.046 Uiso 1 calc R . . C11 C 0.0057(2) -0.2506(3) 0.18381(17) 0.0310(10) Uani 1 d . . . C12 C 0.2233(2) -0.2032(3) 0.13666(18) 0.0376(11) Uani 1 d . . . H12A H 0.2050 -0.1412 0.1093 0.056 Uiso 1 calc R . . H12B H 0.2627 -0.2534 0.1170 0.056 Uiso 1 calc R . . H12C H 0.2479 -0.1668 0.1718 0.056 Uiso 1 calc R . . C13 C 0.1799(2) -0.3619(3) 0.20492(18) 0.0402(11) Uani 1 d . . . H13A H 0.1793 -0.3196 0.2428 0.060 Uiso 1 calc R . . H13B H 0.2345 -0.3891 0.1969 0.060 Uiso 1 calc R . . H13C H 0.1439 -0.4302 0.2068 0.060 Uiso 1 calc R . . C14 C -0.0553(2) -0.1509(4) 0.19085(19) 0.0437(12) Uani 1 d . . . H14A H -0.0461 -0.1111 0.2289 0.066 Uiso 1 calc R . . H14B H -0.1095 -0.1840 0.1896 0.066 Uiso 1 calc R . . H14C H -0.0493 -0.0938 0.1586 0.066 Uiso 1 calc R . . C15 C 0.0029(2) -0.3287(3) 0.23948(17) 0.0394(11) Uani 1 d . . . H15A H 0.0252 -0.4068 0.2306 0.059 Uiso 1 calc R . . H15B H -0.0528 -0.3374 0.2520 0.059 Uiso 1 calc R . . H15C H 0.0344 -0.2917 0.2714 0.059 Uiso 1 calc R . . C16 C 0.0457(2) 0.2114(3) 0.28490(16) 0.0292(10) Uani 1 d . . . C17 C 0.0001(2) 0.2725(3) 0.33487(17) 0.0380(11) Uani 1 d . . . H17A H -0.0409 0.3255 0.3172 0.046 Uiso 1 calc R . . H17B H -0.0281 0.2117 0.3583 0.046 Uiso 1 calc R . . C18 C 0.0535(3) 0.3441(4) 0.37607(18) 0.0435(12) Uani 1 d . . . H18A H 0.0216 0.3771 0.4088 0.052 Uiso 1 calc R . . H18B H 0.0777 0.4108 0.3542 0.052 Uiso 1 calc R . . C19 C 0.1189(3) 0.2646(4) 0.40089(17) 0.0429(12) Uani 1 d . . . H19A H 0.0941 0.2041 0.4265 0.051 Uiso 1 calc R . . H19B H 0.1554 0.3127 0.4260 0.051 Uiso 1 calc R . . C20 C 0.1683(2) 0.2019(3) 0.35376(17) 0.0334(11) Uani 1 d . . . C21 C -0.0131(2) 0.1267(3) 0.25423(17) 0.0386(11) Uani 1 d . . . H21A H 0.0124 0.0914 0.2196 0.058 Uiso 1 calc R . . H21B H -0.0610 0.1705 0.2415 0.058 Uiso 1 calc R . . H21C H -0.0283 0.0641 0.2819 0.058 Uiso 1 calc R . . C22 C 0.0744(3) 0.3011(3) 0.23882(17) 0.0388(11) Uani 1 d . . . H22A H 0.0954 0.3715 0.2591 0.058 Uiso 1 calc R . . H22B H 0.0294 0.3238 0.2129 0.058 Uiso 1 calc R . . H22C H 0.1167 0.2654 0.2150 0.058 Uiso 1 calc R . . C23 C 0.2244(2) 0.2883(3) 0.32209(19) 0.0438(12) Uani 1 d . . . H23A H 0.2451 0.2508 0.2863 0.066 Uiso 1 calc R . . H23B H 0.2692 0.3091 0.3486 0.066 Uiso 1 calc R . . H23C H 0.1947 0.3600 0.3112 0.066 Uiso 1 calc R . . C24 C 0.2209(3) 0.1086(3) 0.38424(18) 0.0441(12) Uani 1 d . . . H24A H 0.1869 0.0469 0.4011 0.066 Uiso 1 calc R . . H24B H 0.2527 0.1459 0.4159 0.066 Uiso 1 calc R . . H24C H 0.2568 0.0732 0.3552 0.066 Uiso 1 calc R . . C25 C 0.2242(3) -0.4031(4) 0.3772(2) 0.0564(14) Uani 1 d . . . H25A H 0.1972 -0.4350 0.4120 0.085 Uiso 1 calc R . . H25B H 0.2793 -0.4329 0.3762 0.085 Uiso 1 calc R . . H25C H 0.1955 -0.4280 0.3412 0.085 Uiso 1 calc R . . C26 C 0.2946(2) -0.1849(3) 0.32179(16) 0.0359(11) Uani 1 d . . . H26A H 0.2740 -0.2104 0.2830 0.054 Uiso 0.50 calc PR . . H26B H 0.3481 -0.2182 0.3285 0.054 Uiso 0.50 calc PR . . H26C H 0.2976 -0.0983 0.3229 0.054 Uiso 0.50 calc PR . . H26D H 0.3391 -0.1409 0.3399 0.054 Uiso 0.50 calc PR . . H26E H 0.2650 -0.1330 0.2944 0.054 Uiso 0.50 calc PR . . H26F H 0.3155 -0.2529 0.3000 0.054 Uiso 0.50 calc PR . . C27 C 0.2745(3) -0.1986(4) 0.45334(18) 0.0530(13) Uani 1 d . . . H27A H 0.2770 -0.1123 0.4572 0.080 Uiso 1 calc R . . H27B H 0.3289 -0.2312 0.4548 0.080 Uiso 1 calc R . . H27C H 0.2433 -0.2315 0.4859 0.080 Uiso 1 calc R . . C28 C -0.0300(2) -0.0999(4) 0.38620(18) 0.0396(11) Uani 1 d . . . H28A H -0.0143 -0.0164 0.3849 0.059 Uiso 1 calc R . . H28B H -0.0772 -0.1088 0.4111 0.059 Uiso 1 calc R . . H28C H -0.0426 -0.1276 0.3460 0.059 Uiso 1 calc R . . C29 C 0.0744(3) -0.1302(5) 0.49415(18) 0.0630(15) Uani 1 d . . . H29A H 0.1113 -0.1832 0.5153 0.094 Uiso 1 calc R . . H29B H 0.0240 -0.1250 0.5157 0.094 Uiso 1 calc R . . H29C H 0.0984 -0.0513 0.4913 0.094 Uiso 1 calc R . . C30 C 0.0176(3) -0.3449(4) 0.4270(2) 0.0666(16) Uani 1 d . . . H30A H 0.0048 -0.3786 0.3880 0.100 Uiso 1 calc R . . H30B H -0.0306 -0.3448 0.4513 0.100 Uiso 1 calc R . . H30C H 0.0593 -0.3926 0.4464 0.100 Uiso 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 0.0322(7) 0.0332(7) 0.0229(6) 0.0008(5) -0.0033(5) -0.0020(5) Si2 0.0274(7) 0.0366(7) 0.0263(7) 0.0011(5) 0.0008(5) -0.0053(5) Si3 0.0299(7) 0.0303(7) 0.0293(7) 0.0044(5) 0.0001(5) 0.0023(5) Si4 0.0353(8) 0.0338(7) 0.0322(7) 0.0047(5) 0.0118(6) 0.0040(6) Mg1 0.0298(9) 0.0280(8) 0.0210(7) -0.0009(6) 0.0001(6) -0.0021(6) Mg2 0.0291(8) 0.0296(8) 0.0207(7) -0.0011(6) 0.0013(6) 0.0011(6) O1 0.0329(17) 0.0250(15) 0.0210(15) -0.0087(11) 0.0051(12) -0.0072(12) O2 0.0435(18) 0.0233(15) 0.0197(15) -0.0054(11) -0.0016(13) 0.0037(12) N1 0.024(2) 0.0298(19) 0.0211(18) 0.0019(14) 0.0008(15) -0.0031(15) N2 0.028(2) 0.0269(19) 0.0206(18) -0.0094(14) 0.0030(15) -0.0021(15) N3 0.028(2) 0.0270(18) 0.0192(17) -0.0002(14) 0.0030(15) 0.0027(15) N4 0.038(2) 0.0255(19) 0.0196(18) -0.0059(14) -0.0017(16) 0.0010(16) C1 0.032(3) 0.081(3) 0.040(3) -0.008(2) -0.004(2) -0.004(2) C2 0.043(3) 0.068(3) 0.027(3) -0.010(2) 0.003(2) -0.008(2) C3 0.090(4) 0.042(3) 0.052(3) 0.009(2) -0.037(3) -0.007(3) C4 0.036(3) 0.086(4) 0.042(3) -0.004(3) 0.007(2) -0.013(3) C5 0.044(3) 0.043(3) 0.040(3) 0.013(2) -0.014(2) -0.013(2) C6 0.024(3) 0.037(3) 0.042(3) -0.003(2) -0.004(2) -0.0015(19) C7 0.028(3) 0.028(2) 0.028(2) -0.0031(18) 0.0033(19) 0.0000(19) C8 0.046(3) 0.036(3) 0.037(3) -0.011(2) 0.015(2) -0.002(2) C9 0.056(3) 0.042(3) 0.034(3) -0.015(2) 0.002(2) -0.009(2) C10 0.034(3) 0.040(3) 0.039(3) -0.009(2) -0.010(2) -0.011(2) C11 0.028(3) 0.032(2) 0.032(3) -0.007(2) 0.006(2) -0.007(2) C12 0.031(3) 0.037(3) 0.045(3) -0.005(2) 0.012(2) -0.001(2) C13 0.039(3) 0.032(3) 0.049(3) 0.003(2) -0.006(2) 0.002(2) C14 0.030(3) 0.045(3) 0.057(3) -0.009(2) 0.009(2) -0.004(2) C15 0.042(3) 0.035(3) 0.041(3) -0.003(2) 0.011(2) -0.013(2) C16 0.035(3) 0.023(2) 0.029(2) -0.0011(18) 0.000(2) 0.0014(19) C17 0.040(3) 0.036(3) 0.039(3) -0.006(2) 0.008(2) 0.007(2) C18 0.052(3) 0.042(3) 0.037(3) -0.015(2) 0.009(2) 0.005(2) C19 0.057(3) 0.039(3) 0.033(3) -0.011(2) 0.000(2) -0.005(2) C20 0.039(3) 0.031(3) 0.030(2) -0.0084(19) -0.004(2) -0.002(2) C21 0.041(3) 0.039(3) 0.035(3) 0.002(2) -0.006(2) 0.005(2) C22 0.050(3) 0.029(3) 0.037(3) 0.003(2) 0.000(2) 0.005(2) C23 0.043(3) 0.036(3) 0.052(3) -0.013(2) -0.005(2) -0.003(2) C24 0.056(3) 0.039(3) 0.037(3) -0.010(2) -0.020(2) -0.002(2) C25 0.042(3) 0.036(3) 0.091(4) 0.009(3) 0.009(3) 0.003(2) C26 0.031(3) 0.042(3) 0.035(3) -0.003(2) 0.003(2) 0.005(2) C27 0.034(3) 0.087(4) 0.038(3) 0.006(3) -0.006(2) 0.009(3) C28 0.030(3) 0.045(3) 0.044(3) -0.004(2) 0.006(2) -0.001(2) C29 0.060(4) 0.097(4) 0.032(3) 0.001(3) 0.011(3) 0.025(3) C30 0.064(4) 0.042(3) 0.096(4) 0.018(3) 0.048(3) 0.007(3) _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 1.706(3) . ? Si1 C3 1.864(4) . ? Si1 C1 1.869(4) . ? Si1 C2 1.871(4) . ? Si1 Mg1 3.1422(16) . ? Si2 N1 1.707(3) . ? Si2 C4 1.868(4) . ? Si2 C5 1.873(4) . ? Si2 C6 1.878(4) . ? Si2 Mg1 3.1036(17) . ? Si3 N3 1.699(3) . ? Si3 C27 1.865(4) . ? Si3 C25 1.867(4) . ? Si3 C26 1.879(4) . ? Si3 Mg2 3.1197(16) . ? Si4 N3 1.704(3) . ? Si4 C28 1.869(4) . ? Si4 C30 1.871(4) . ? Si4 C29 1.874(4) . ? Si4 Mg2 3.1307(16) . ? Mg1 O1 1.944(3) . ? Mg1 O2 1.946(3) . ? Mg1 N1 1.952(3) . ? Mg1 N2 2.782(3) . ? Mg1 Mg2 2.9221(17) . ? Mg2 N3 1.965(3) . ? Mg2 O1 1.967(3) . ? Mg2 O2 1.979(3) . ? Mg2 N4 2.395(3) . ? O1 N2 1.461(3) . ? O2 N4 1.471(3) . ? N2 C7 1.490(4) . ? N2 C11 1.498(5) . ? N4 C20 1.500(5) . ? N4 C16 1.509(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? 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 C12 1.527(5) . ? C7 C13 1.535(5) . ? C7 C8 1.536(5) . ? C8 C9 1.525(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.509(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.537(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C14 1.529(5) . ? C11 C15 1.537(5) . ? 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 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.529(5) . ? C16 C17 1.534(5) . ? C16 C22 1.535(5) . ? C17 C18 1.515(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.516(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.529(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C24 1.530(5) . ? C20 C23 1.536(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 N1 Si1 C3 113.04(17) . . ? N1 Si1 C1 107.77(17) . . ? C3 Si1 C1 108.5(2) . . ? N1 Si1 C2 113.55(18) . . ? C3 Si1 C2 107.4(2) . . ? C1 Si1 C2 106.2(2) . . ? N1 Si1 Mg1 33.18(10) . . ? C3 Si1 Mg1 130.88(15) . . ? C1 Si1 Mg1 75.11(14) . . ? C2 Si1 Mg1 118.67(14) . . ? N1 Si2 C4 113.66(17) . . ? N1 Si2 C5 113.09(17) . . ? C4 Si2 C5 106.6(2) . . ? N1 Si2 C6 109.15(16) . . ? C4 Si2 C6 106.3(2) . . ? C5 Si2 C6 107.65(17) . . ? N1 Si2 Mg1 34.45(10) . . ? C4 Si2 Mg1 133.55(15) . . ? C5 Si2 Mg1 116.99(14) . . ? C6 Si2 Mg1 75.82(12) . . ? N3 Si3 C27 113.80(17) . . ? N3 Si3 C25 112.81(18) . . ? C27 Si3 C25 106.7(2) . . ? N3 Si3 C26 109.82(16) . . ? C27 Si3 C26 106.36(19) . . ? C25 Si3 C26 107.0(2) . . ? N3 Si3 Mg2 34.31(10) . . ? C27 Si3 Mg2 126.44(15) . . ? C25 Si3 Mg2 124.31(16) . . ? C26 Si3 Mg2 75.51(13) . . ? N3 Si4 C28 107.72(17) . . ? N3 Si4 C30 113.78(18) . . ? C28 Si4 C30 107.7(2) . . ? N3 Si4 C29 113.97(19) . . ? C28 Si4 C29 106.4(2) . . ? C30 Si4 C29 106.9(2) . . ? N3 Si4 Mg2 34.04(10) . . ? C28 Si4 Mg2 73.71(13) . . ? C30 Si4 Mg2 127.25(16) . . ? C29 Si4 Mg2 123.64(17) . . ? O1 Mg1 O2 84.28(10) . . ? O1 Mg1 N1 149.99(12) . . ? O2 Mg1 N1 123.56(12) . . ? O1 Mg1 N2 29.81(9) . . ? O2 Mg1 N2 113.97(10) . . ? N1 Mg1 N2 121.80(11) . . ? O1 Mg1 Mg2 41.95(7) . . ? O2 Mg1 Mg2 42.33(8) . . ? N1 Mg1 Mg2 163.24(11) . . ? N2 Mg1 Mg2 71.68(7) . . ? O1 Mg1 Si2 146.97(9) . . ? O2 Mg1 Si2 100.94(9) . . ? N1 Mg1 Si2 29.65(9) . . ? N2 Mg1 Si2 134.30(8) . . ? Mg2 Mg1 Si2 134.03(5) . . ? O1 Mg1 Si1 132.77(9) . . ? O2 Mg1 Si1 139.86(9) . . ? N1 Mg1 Si1 28.59(9) . . ? N2 Mg1 Si1 103.45(7) . . ? Mg2 Mg1 Si1 166.69(6) . . ? Si2 Mg1 Si1 58.23(4) . . ? N3 Mg2 O1 127.44(12) . . ? N3 Mg2 O2 142.13(12) . . ? O1 Mg2 O2 82.80(10) . . ? N3 Mg2 N4 121.12(12) . . ? O1 Mg2 N4 111.44(11) . . ? O2 Mg2 N4 37.80(9) . . ? N3 Mg2 Mg1 158.66(10) . . ? O1 Mg2 Mg1 41.35(7) . . ? O2 Mg2 Mg1 41.45(7) . . ? N4 Mg2 Mg1 73.59(8) . . ? N3 Mg2 Si3 29.17(9) . . ? O1 Mg2 Si3 115.03(9) . . ? O2 Mg2 Si3 123.56(9) . . ? N4 Mg2 Si3 124.59(9) . . ? Mg1 Mg2 Si3 130.59(5) . . ? N3 Mg2 Si4 29.04(9) . . ? O1 Mg2 Si4 131.81(9) . . ? O2 Mg2 Si4 143.66(9) . . ? N4 Mg2 Si4 107.81(8) . . ? Mg1 Mg2 Si4 168.88(6) . . ? Si3 Mg2 Si4 58.16(4) . . ? N2 O1 Mg1 108.78(17) . . ? N2 O1 Mg2 154.02(19) . . ? Mg1 O1 Mg2 96.69(11) . . ? N4 O2 Mg1 139.8(2) . . ? N4 O2 Mg2 86.61(16) . . ? Mg1 O2 Mg2 96.22(11) . . ? Si2 N1 Si1 125.87(17) . . ? Si2 N1 Mg1 115.90(16) . . ? Si1 N1 Mg1 118.23(16) . . ? O1 N2 C7 109.2(3) . . ? O1 N2 C11 109.7(2) . . ? C7 N2 C11 117.4(3) . . ? O1 N2 Mg1 41.41(12) . . ? C7 N2 Mg1 108.4(2) . . ? C11 N2 Mg1 133.2(2) . . ? Si3 N3 Si4 126.39(17) . . ? Si3 N3 Mg2 116.52(16) . . ? Si4 N3 Mg2 116.92(16) . . ? O2 N4 C20 107.2(3) . . ? O2 N4 C16 109.7(2) . . ? C20 N4 C16 116.4(3) . . ? O2 N4 Mg2 55.59(13) . . ? C20 N4 Mg2 120.4(2) . . ? C16 N4 Mg2 123.1(2) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C12 107.7(3) . . ? N2 C7 C13 116.1(3) . . ? C12 C7 C13 108.1(3) . . ? N2 C7 C8 106.3(3) . . ? C12 C7 C8 107.6(3) . . ? C13 C7 C8 110.8(3) . . ? C9 C8 C7 113.3(3) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 109.5(3) . . ? C10 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? C10 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C9 C10 C11 113.9(3) . . ? C9 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? N2 C11 C14 108.3(3) . . ? N2 C11 C10 105.2(3) . . ? C14 C11 C10 107.4(3) . . ? N2 C11 C15 116.2(3) . . ? C14 C11 C15 108.1(3) . . ? C10 C11 C15 111.4(3) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C13 H13A 109.5 . . ? C7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C21 107.6(3) . . ? N4 C16 C17 106.9(3) . . ? C21 C16 C17 107.1(3) . . ? N4 C16 C22 115.5(3) . . ? C21 C16 C22 108.1(3) . . ? C17 C16 C22 111.3(3) . . ? C18 C17 C16 113.5(3) . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C17 C18 C19 109.0(3) . . ? C17 C18 H18A 109.9 . . ? C19 C18 H18A 109.9 . . ? C17 C18 H18B 109.9 . . ? C19 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? C18 C19 C20 114.2(3) . . ? C18 C19 H19A 108.7 . . ? C20 C19 H19A 108.7 . . ? C18 C19 H19B 108.7 . . ? C20 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? N4 C20 C19 107.0(3) . . ? N4 C20 C24 107.3(3) . . ? C19 C20 C24 108.5(3) . . ? N4 C20 C23 114.9(3) . . ? C19 C20 C23 111.6(3) . . ? C24 C20 C23 107.3(3) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si3 C26 H26A 109.5 . . ? Si3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si3 C26 H26D 109.5 . . ? H26A C26 H26D 141.1 . . ? H26B C26 H26D 56.3 . . ? H26C C26 H26D 56.3 . . ? Si3 C26 H26E 109.5 . . ? H26A C26 H26E 56.3 . . ? H26B C26 H26E 141.1 . . ? H26C C26 H26E 56.3 . . ? H26D C26 H26E 109.5 . . ? Si3 C26 H26F 109.5 . . ? H26A C26 H26F 56.3 . . ? H26B C26 H26F 56.3 . . ? H26C C26 H26F 141.1 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? Si3 C27 H27A 109.5 . . ? Si3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si4 C30 H30A 109.5 . . ? Si4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Si2 Mg1 O1 120.6(2) . . . . ? C4 Si2 Mg1 O1 54.6(3) . . . . ? C5 Si2 Mg1 O1 -147.3(2) . . . . ? C6 Si2 Mg1 O1 -44.5(2) . . . . ? N1 Si2 Mg1 O2 -143.0(2) . . . . ? C4 Si2 Mg1 O2 151.0(2) . . . . ? C5 Si2 Mg1 O2 -50.97(17) . . . . ? C6 Si2 Mg1 O2 51.87(15) . . . . ? C4 Si2 Mg1 N1 -66.0(3) . . . . ? C5 Si2 Mg1 N1 92.0(2) . . . . ? C6 Si2 Mg1 N1 -165.1(2) . . . . ? N1 Si2 Mg1 N2 76.9(2) . . . . ? C4 Si2 Mg1 N2 10.9(2) . . . . ? C5 Si2 Mg1 N2 168.96(17) . . . . ? C6 Si2 Mg1 N2 -88.20(16) . . . . ? N1 Si2 Mg1 Mg2 -173.65(19) . . . . ? C4 Si2 Mg1 Mg2 120.4(2) . . . . ? C5 Si2 Mg1 Mg2 -81.61(16) . . . . ? C6 Si2 Mg1 Mg2 21.24(14) . . . . ? N1 Si2 Mg1 Si1 -0.24(17) . . . . ? C4 Si2 Mg1 Si1 -66.2(2) . . . . ? C5 Si2 Mg1 Si1 91.80(14) . . . . ? C6 Si2 Mg1 Si1 -165.36(13) . . . . ? N1 Si1 Mg1 O1 -140.1(2) . . . . ? C3 Si1 Mg1 O1 152.1(2) . . . . ? C1 Si1 Mg1 O1 50.23(19) . . . . ? C2 Si1 Mg1 O1 -50.4(2) . . . . ? N1 Si1 Mg1 O2 67.4(2) . . . . ? C3 Si1 Mg1 O2 -0.4(3) . . . . ? C1 Si1 Mg1 O2 -102.2(2) . . . . ? C2 Si1 Mg1 O2 157.2(2) . . . . ? C3 Si1 Mg1 N1 -67.8(3) . . . . ? C1 Si1 Mg1 N1 -169.6(2) . . . . ? C2 Si1 Mg1 N1 89.8(2) . . . . ? N1 Si1 Mg1 N2 -133.9(2) . . . . ? C3 Si1 Mg1 N2 158.3(2) . . . . ? C1 Si1 Mg1 N2 56.47(16) . . . . ? C2 Si1 Mg1 N2 -44.13(18) . . . . ? N1 Si1 Mg1 Mg2 159.2(3) . . . . ? C3 Si1 Mg1 Mg2 91.4(3) . . . . ? C1 Si1 Mg1 Mg2 -10.4(3) . . . . ? C2 Si1 Mg1 Mg2 -111.0(3) . . . . ? N1 Si1 Mg1 Si2 0.25(18) . . . . ? C3 Si1 Mg1 Si2 -67.5(2) . . . . ? C1 Si1 Mg1 Si2 -169.38(15) . . . . ? C2 Si1 Mg1 Si2 90.03(16) . . . . ? O1 Mg1 Mg2 N3 67.7(3) . . . . ? O2 Mg1 Mg2 N3 -112.3(3) . . . . ? N1 Mg1 Mg2 N3 -75.2(5) . . . . ? N2 Mg1 Mg2 N3 70.4(3) . . . . ? Si2 Mg1 Mg2 N3 -64.3(3) . . . . ? Si1 Mg1 Mg2 N3 140.8(3) . . . . ? O2 Mg1 Mg2 O1 -179.96(17) . . . . ? N1 Mg1 Mg2 O1 -142.9(4) . . . . ? N2 Mg1 Mg2 O1 2.72(13) . . . . ? Si2 Mg1 Mg2 O1 -131.98(14) . . . . ? Si1 Mg1 Mg2 O1 73.1(3) . . . . ? O1 Mg1 Mg2 O2 179.96(17) . . . . ? N1 Mg1 Mg2 O2 37.0(4) . . . . ? N2 Mg1 Mg2 O2 -177.32(14) . . . . ? Si2 Mg1 Mg2 O2 47.99(13) . . . . ? Si1 Mg1 Mg2 O2 -106.9(3) . . . . ? O1 Mg1 Mg2 N4 -155.67(15) . . . . ? O2 Mg1 Mg2 N4 24.36(13) . . . . ? N1 Mg1 Mg2 N4 61.4(4) . . . . ? N2 Mg1 Mg2 N4 -152.96(11) . . . . ? Si2 Mg1 Mg2 N4 72.35(10) . . . . ? Si1 Mg1 Mg2 N4 -82.5(2) . . . . ? O1 Mg1 Mg2 Si3 82.52(13) . . . . ? O2 Mg1 Mg2 Si3 -97.45(13) . . . . ? N1 Mg1 Mg2 Si3 -60.4(4) . . . . ? N2 Mg1 Mg2 Si3 85.23(9) . . . . ? Si2 Mg1 Mg2 Si3 -49.46(10) . . . . ? Si1 Mg1 Mg2 Si3 155.6(2) . . . . ? O1 Mg1 Mg2 Si4 -56.7(3) . . . . ? O2 Mg1 Mg2 Si4 123.3(3) . . . . ? N1 Mg1 Mg2 Si4 160.3(4) . . . . ? N2 Mg1 Mg2 Si4 -54.0(3) . . . . ? Si2 Mg1 Mg2 Si4 171.3(2) . . . . ? Si1 Mg1 Mg2 Si4 16.4(5) . . . . ? C27 Si3 Mg2 N3 -78.9(2) . . . . ? C25 Si3 Mg2 N3 80.4(3) . . . . ? C26 Si3 Mg2 N3 -178.8(2) . . . . ? N3 Si3 Mg2 O1 -122.7(2) . . . . ? C27 Si3 Mg2 O1 158.37(19) . . . . ? C25 Si3 Mg2 O1 -42.3(2) . . . . ? C26 Si3 Mg2 O1 58.53(16) . . . . ? N3 Si3 Mg2 O2 139.0(2) . . . . ? C27 Si3 Mg2 O2 60.1(2) . . . . ? C25 Si3 Mg2 O2 -140.6(2) . . . . ? C26 Si3 Mg2 O2 -39.74(16) . . . . ? N3 Si3 Mg2 N4 93.0(2) . . . . ? C27 Si3 Mg2 N4 14.1(2) . . . . ? C25 Si3 Mg2 N4 173.4(2) . . . . ? C26 Si3 Mg2 N4 -85.77(16) . . . . ? N3 Si3 Mg2 Mg1 -169.00(19) . . . . ? C27 Si3 Mg2 Mg1 112.07(19) . . . . ? C25 Si3 Mg2 Mg1 -88.6(2) . . . . ? C26 Si3 Mg2 Mg1 12.23(14) . . . . ? N3 Si3 Mg2 Si4 2.49(17) . . . . ? C27 Si3 Mg2 Si4 -76.45(18) . . . . ? C25 Si3 Mg2 Si4 82.85(19) . . . . ? C26 Si3 Mg2 Si4 -176.29(13) . . . . ? C28 Si4 Mg2 N3 -177.4(2) . . . . ? C30 Si4 Mg2 N3 -77.3(3) . . . . ? C29 Si4 Mg2 N3 83.5(3) . . . . ? N3 Si4 Mg2 O1 94.0(2) . . . . ? C28 Si4 Mg2 O1 -83.44(18) . . . . ? C30 Si4 Mg2 O1 16.7(2) . . . . ? C29 Si4 Mg2 O1 177.5(2) . . . . ? N3 Si4 Mg2 O2 -107.2(2) . . . . ? C28 Si4 Mg2 O2 75.4(2) . . . . ? C30 Si4 Mg2 O2 175.5(2) . . . . ? C29 Si4 Mg2 O2 -23.7(3) . . . . ? N3 Si4 Mg2 N4 -122.7(2) . . . . ? C28 Si4 Mg2 N4 59.93(16) . . . . ? C30 Si4 Mg2 N4 160.1(2) . . . . ? C29 Si4 Mg2 N4 -39.2(2) . . . . ? N3 Si4 Mg2 Mg1 141.8(3) . . . . ? C28 Si4 Mg2 Mg1 -35.6(3) . . . . ? C30 Si4 Mg2 Mg1 64.6(4) . . . . ? C29 Si4 Mg2 Mg1 -134.7(3) . . . . ? N3 Si4 Mg2 Si3 -2.50(17) . . . . ? C28 Si4 Mg2 Si3 -179.91(14) . . . . ? C30 Si4 Mg2 Si3 -79.8(2) . . . . ? C29 Si4 Mg2 Si3 80.99(18) . . . . ? O2 Mg1 O1 N2 174.8(2) . . . . ? N1 Mg1 O1 N2 -25.5(4) . . . . ? Mg2 Mg1 O1 N2 174.8(2) . . . . ? Si2 Mg1 O1 N2 -83.9(2) . . . . ? Si1 Mg1 O1 N2 12.3(2) . . . . ? O2 Mg1 O1 Mg2 0.03(12) . . . . ? N1 Mg1 O1 Mg2 159.7(2) . . . . ? N2 Mg1 O1 Mg2 -174.8(2) . . . . ? Si2 Mg1 O1 Mg2 101.32(15) . . . . ? Si1 Mg1 O1 Mg2 -162.54(8) . . . . ? N3 Mg2 O1 N2 36.4(5) . . . . ? O2 Mg2 O1 N2 -168.7(5) . . . . ? N4 Mg2 O1 N2 -143.6(4) . . . . ? Mg1 Mg2 O1 N2 -168.7(5) . . . . ? Si3 Mg2 O1 N2 67.5(5) . . . . ? Si4 Mg2 O1 N2 -1.2(5) . . . . ? N3 Mg2 O1 Mg1 -154.91(14) . . . . ? O2 Mg2 O1 Mg1 -0.02(11) . . . . ? N4 Mg2 O1 Mg1 25.12(15) . . . . ? Si3 Mg2 O1 Mg1 -123.81(9) . . . . ? Si4 Mg2 O1 Mg1 167.51(8) . . . . ? O1 Mg1 O2 N4 -92.1(3) . . . . ? N1 Mg1 O2 N4 99.9(3) . . . . ? N2 Mg1 O2 N4 -89.3(3) . . . . ? Mg2 Mg1 O2 N4 -92.1(3) . . . . ? Si2 Mg1 O2 N4 120.8(3) . . . . ? Si1 Mg1 O2 N4 67.9(3) . . . . ? O1 Mg1 O2 Mg2 -0.03(12) . . . . ? N1 Mg1 O2 Mg2 -167.96(13) . . . . ? N2 Mg1 O2 Mg2 2.78(14) . . . . ? Si2 Mg1 O2 Mg2 -147.04(8) . . . . ? Si1 Mg1 O2 Mg2 160.02(9) . . . . ? N3 Mg2 O2 N4 -73.5(3) . . . . ? O1 Mg2 O2 N4 139.81(17) . . . . ? Mg1 Mg2 O2 N4 139.8(2) . . . . ? Si3 Mg2 O2 N4 -104.85(16) . . . . ? Si4 Mg2 O2 N4 -24.4(2) . . . . ? N3 Mg2 O2 Mg1 146.73(17) . . . . ? O1 Mg2 O2 Mg1 0.02(11) . . . . ? N4 Mg2 O2 Mg1 -139.8(2) . . . . ? Si3 Mg2 O2 Mg1 115.36(10) . . . . ? Si4 Mg2 O2 Mg1 -164.22(10) . . . . ? C4 Si2 N1 Si1 -46.8(3) . . . . ? C5 Si2 N1 Si1 75.0(3) . . . . ? C6 Si2 N1 Si1 -165.2(2) . . . . ? Mg1 Si2 N1 Si1 179.5(3) . . . . ? C4 Si2 N1 Mg1 133.7(2) . . . . ? C5 Si2 N1 Mg1 -104.5(2) . . . . ? C6 Si2 N1 Mg1 15.3(2) . . . . ? C3 Si1 N1 Si2 -49.0(3) . . . . ? C1 Si1 N1 Si2 -169.0(2) . . . . ? C2 Si1 N1 Si2 73.7(3) . . . . ? Mg1 Si1 N1 Si2 -179.5(3) . . . . ? C3 Si1 N1 Mg1 130.5(2) . . . . ? C1 Si1 N1 Mg1 10.5(2) . . . . ? C2 Si1 N1 Mg1 -106.8(2) . . . . ? O1 Mg1 N1 Si2 -110.3(3) . . . . ? O2 Mg1 N1 Si2 45.1(2) . . . . ? N2 Mg1 N1 Si2 -124.90(15) . . . . ? Mg2 Mg1 N1 Si2 16.0(5) . . . . ? Si1 Mg1 N1 Si2 179.6(3) . . . . ? O1 Mg1 N1 Si1 70.1(3) . . . . ? O2 Mg1 N1 Si1 -134.42(16) . . . . ? N2 Mg1 N1 Si1 55.5(2) . . . . ? Mg2 Mg1 N1 Si1 -163.6(2) . . . . ? Si2 Mg1 N1 Si1 -179.6(3) . . . . ? Mg1 O1 N2 C7 96.3(2) . . . . ? Mg2 O1 N2 C7 -95.6(5) . . . . ? Mg1 O1 N2 C11 -133.8(2) . . . . ? Mg2 O1 N2 C11 34.4(6) . . . . ? Mg2 O1 N2 Mg1 168.2(5) . . . . ? O2 Mg1 N2 O1 -5.6(2) . . . . ? N1 Mg1 N2 O1 165.3(2) . . . . ? Mg2 Mg1 N2 O1 -3.65(17) . . . . ? Si2 Mg1 N2 O1 130.77(18) . . . . ? Si1 Mg1 N2 O1 -170.77(18) . . . . ? O1 Mg1 N2 C7 -98.5(3) . . . . ? O2 Mg1 N2 C7 -104.2(2) . . . . ? N1 Mg1 N2 C7 66.8(2) . . . . ? Mg2 Mg1 N2 C7 -102.2(2) . . . . ? Si2 Mg1 N2 C7 32.2(3) . . . . ? Si1 Mg1 N2 C7 90.7(2) . . . . ? O1 Mg1 N2 C11 68.7(3) . . . . ? O2 Mg1 N2 C11 63.0(3) . . . . ? N1 Mg1 N2 C11 -126.0(3) . . . . ? Mg2 Mg1 N2 C11 65.0(3) . . . . ? Si2 Mg1 N2 C11 -160.6(3) . . . . ? Si1 Mg1 N2 C11 -102.1(3) . . . . ? C27 Si3 N3 Si4 -54.8(3) . . . . ? C25 Si3 N3 Si4 66.9(3) . . . . ? C26 Si3 N3 Si4 -173.9(2) . . . . ? Mg2 Si3 N3 Si4 -175.2(3) . . . . ? C27 Si3 N3 Mg2 120.4(2) . . . . ? C25 Si3 N3 Mg2 -117.9(2) . . . . ? C26 Si3 N3 Mg2 1.3(2) . . . . ? C28 Si4 N3 Si3 177.8(2) . . . . ? C30 Si4 N3 Si3 -62.9(3) . . . . ? C29 Si4 N3 Si3 60.0(3) . . . . ? Mg2 Si4 N3 Si3 175.2(3) . . . . ? C28 Si4 N3 Mg2 2.6(2) . . . . ? C30 Si4 N3 Mg2 122.0(2) . . . . ? C29 Si4 N3 Mg2 -115.2(2) . . . . ? O1 Mg2 N3 Si3 73.8(2) . . . . ? O2 Mg2 N3 Si3 -62.9(3) . . . . ? N4 Mg2 N3 Si3 -106.21(18) . . . . ? Mg1 Mg2 N3 Si3 23.5(4) . . . . ? Si4 Mg2 N3 Si3 -175.6(3) . . . . ? O1 Mg2 N3 Si4 -110.53(18) . . . . ? O2 Mg2 N3 Si4 112.8(2) . . . . ? N4 Mg2 N3 Si4 69.4(2) . . . . ? Mg1 Mg2 N3 Si4 -160.88(18) . . . . ? Si3 Mg2 N3 Si4 175.6(3) . . . . ? Mg1 O2 N4 C20 -148.9(3) . . . . ? Mg2 O2 N4 C20 115.5(2) . . . . ? Mg1 O2 N4 C16 -21.6(4) . . . . ? Mg2 O2 N4 C16 -117.3(2) . . . . ? Mg1 O2 N4 Mg2 95.6(3) . . . . ? N3 Mg2 N4 O2 136.57(18) . . . . ? O1 Mg2 N4 O2 -43.46(18) . . . . ? Mg1 Mg2 N4 O2 -26.46(14) . . . . ? Si3 Mg2 N4 O2 101.93(16) . . . . ? Si4 Mg2 N4 O2 165.08(15) . . . . ? N3 Mg2 N4 C20 45.8(3) . . . . ? O1 Mg2 N4 C20 -134.2(2) . . . . ? O2 Mg2 N4 C20 -90.8(3) . . . . ? Mg1 Mg2 N4 C20 -117.2(3) . . . . ? Si3 Mg2 N4 C20 11.1(3) . . . . ? Si4 Mg2 N4 C20 74.3(3) . . . . ? N3 Mg2 N4 C16 -131.1(3) . . . . ? O1 Mg2 N4 C16 48.9(3) . . . . ? O2 Mg2 N4 C16 92.3(3) . . . . ? Mg1 Mg2 N4 C16 65.9(2) . . . . ? Si3 Mg2 N4 C16 -165.7(2) . . . . ? Si4 Mg2 N4 C16 -102.6(3) . . . . ? O1 N2 C7 C12 -60.2(3) . . . . ? C11 N2 C7 C12 174.2(3) . . . . ? Mg1 N2 C7 C12 -16.3(3) . . . . ? O1 N2 C7 C13 61.1(4) . . . . ? C11 N2 C7 C13 -64.6(4) . . . . ? Mg1 N2 C7 C13 105.0(3) . . . . ? O1 N2 C7 C8 -175.2(3) . . . . ? C11 N2 C7 C8 59.1(4) . . . . ? Mg1 N2 C7 C8 -131.4(2) . . . . ? N2 C7 C8 C9 -54.1(4) . . . . ? C12 C7 C8 C9 -169.2(3) . . . . ? C13 C7 C8 C9 72.8(4) . . . . ? C7 C8 C9 C10 54.5(5) . . . . ? C8 C9 C10 C11 -55.8(5) . . . . ? O1 N2 C11 C14 60.7(4) . . . . ? C7 N2 C11 C14 -173.9(3) . . . . ? Mg1 N2 C11 C14 19.8(4) . . . . ? O1 N2 C11 C10 175.3(3) . . . . ? C7 N2 C11 C10 -59.3(4) . . . . ? Mg1 N2 C11 C10 134.4(3) . . . . ? O1 N2 C11 C15 -61.1(4) . . . . ? C7 N2 C11 C15 64.3(4) . . . . ? Mg1 N2 C11 C15 -102.0(4) . . . . ? C9 C10 C11 N2 55.6(4) . . . . ? C9 C10 C11 C14 170.8(3) . . . . ? C9 C10 C11 C15 -71.1(4) . . . . ? O2 N4 C16 C21 66.4(3) . . . . ? C20 N4 C16 C21 -171.7(3) . . . . ? Mg2 N4 C16 C21 5.3(4) . . . . ? O2 N4 C16 C17 -178.9(3) . . . . ? C20 N4 C16 C17 -57.0(4) . . . . ? Mg2 N4 C16 C17 120.0(3) . . . . ? O2 N4 C16 C22 -54.5(4) . . . . ? C20 N4 C16 C22 67.4(4) . . . . ? Mg2 N4 C16 C22 -115.6(3) . . . . ? N4 C16 C17 C18 55.3(4) . . . . ? C21 C16 C17 C18 170.4(3) . . . . ? C22 C16 C17 C18 -71.7(4) . . . . ? C16 C17 C18 C19 -55.8(5) . . . . ? C17 C18 C19 C20 55.4(5) . . . . ? O2 N4 C20 C19 179.5(3) . . . . ? C16 N4 C20 C19 56.3(4) . . . . ? Mg2 N4 C20 C19 -120.7(3) . . . . ? O2 N4 C20 C24 -64.1(3) . . . . ? C16 N4 C20 C24 172.7(3) . . . . ? Mg2 N4 C20 C24 -4.4(4) . . . . ? O2 N4 C20 C23 55.1(4) . . . . ? C16 N4 C20 C23 -68.1(4) . . . . ? Mg2 N4 C20 C23 114.8(3) . . . . ? C18 C19 C20 N4 -54.3(4) . . . . ? C18 C19 C20 C24 -169.7(3) . . . . ? C18 C19 C20 C23 72.2(4) . . . . ? _refine_diff_density_max 0.227 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.053 #------------------------------------------------------------------------- #-----------------------------COMPOUND 2----------------------------------- #--------------------------------------------------------------------------- data_grem4 _database_code_CSD 160883 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H72 Li2 N4 O2 Si4' _chemical_formula_weight 647.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9309(2) _cell_length_b 14.8370(3) _cell_length_c 21.8416(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.3837(11) _cell_angle_gamma 90.00 _cell_volume 4183.13(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54220 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18189 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9522 _reflns_number_gt 6578 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Denzo & Collect (Otwinowski & Minor, 1997; Hooft & Nonius 1988) ; _computing_cell_refinement 'Denzo & Collect' _computing_data_reduction 'Denzo & Collect' _computing_structure_solution 'SIR-97 ' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+3.4903P] 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 9522 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.29486(5) 0.47997(5) 0.18537(3) 0.03631(17) Uani 1 d . . . Si2 Si 0.32817(5) 0.27999(5) 0.19458(3) 0.03346(16) Uani 1 d . . . Si3 Si 0.12825(5) 0.45970(4) 0.38343(3) 0.03109(16) Uani 1 d . . . Si4 Si 0.07238(5) 0.27070(4) 0.35063(3) 0.03236(16) Uani 1 d . . . O1 O 0.40958(15) 0.35464(13) 0.36919(9) 0.0567(5) Uani 1 d . . . O2 O -0.00299(13) 0.38366(13) 0.18860(8) 0.0487(5) Uani 1 d . . . N1 N 0.49158(15) 0.34927(14) 0.40422(9) 0.0385(5) Uani 1 d . . . N2 N -0.08138(14) 0.39508(13) 0.15055(8) 0.0318(4) Uani 1 d . . . N3 N 0.27737(13) 0.37851(12) 0.21895(8) 0.0284(4) Uani 1 d . . . N4 N 0.13706(14) 0.36768(12) 0.33735(8) 0.0273(4) Uani 1 d . . . C1 C 0.4847(2) 0.2951(2) 0.46100(11) 0.0464(7) Uani 1 d . A 1 C2 C 0.5735(3) 0.3106(3) 0.50744(19) 0.0522(10) Uiso 0.728(4) d P A 1 H2A H 0.5619 0.3680 0.5292 0.063 Uiso 0.728(4) calc PR A 1 H2B H 0.5747 0.2615 0.5381 0.063 Uiso 0.728(4) calc PR A 1 C3 C 0.6754(3) 0.3146(3) 0.47990(19) 0.0466(10) Uiso 0.728(4) d P A 1 H3A H 0.6876 0.2582 0.4572 0.056 Uiso 0.728(4) calc PR A 1 H3B H 0.7313 0.3214 0.5125 0.056 Uiso 0.728(4) calc PR A 1 C4 C 0.6752(3) 0.3950(3) 0.43626(18) 0.0466(10) Uiso 0.728(4) d P A 1 H4A H 0.7445 0.4011 0.4197 0.056 Uiso 0.728(4) calc PR A 1 H4B H 0.6609 0.4508 0.4592 0.056 Uiso 0.728(4) calc PR A 1 C5 C 0.5892(2) 0.3835(2) 0.38021(13) 0.0539(7) Uani 1 d . A 1 C6 C 0.4807(3) 0.1945(3) 0.4388(2) 0.0599(12) Uiso 0.728(4) d P A 1 H6A H 0.4251 0.1873 0.4067 0.090 Uiso 0.728(4) calc PR A 1 H6B H 0.4674 0.1550 0.4735 0.090 Uiso 0.728(4) calc PR A 1 H6C H 0.5471 0.1782 0.4224 0.090 Uiso 0.728(4) calc PR A 1 C7 C 0.3817(3) 0.3165(3) 0.4875(2) 0.0626(12) Uiso 0.728(4) d P A 1 H7A H 0.3777 0.3813 0.4958 0.094 Uiso 0.728(4) calc PR A 1 H7B H 0.3758 0.2829 0.5257 0.094 Uiso 0.728(4) calc PR A 1 H7C H 0.3251 0.2992 0.4580 0.094 Uiso 0.728(4) calc PR A 1 C8 C 0.5786(4) 0.4710(4) 0.3503(3) 0.0795(15) Uiso 0.728(4) d P A 1 H8A H 0.5416 0.4639 0.3101 0.119 Uiso 0.728(4) calc PR A 1 H8B H 0.6475 0.4963 0.3449 0.119 Uiso 0.728(4) calc PR A 1 H8C H 0.5397 0.5118 0.3757 0.119 Uiso 0.728(4) calc PR A 1 C9 C 0.6307(3) 0.3116(3) 0.33755(19) 0.0552(11) Uiso 0.728(4) d P A 1 H9A H 0.5765 0.2954 0.3062 0.083 Uiso 0.728(4) calc PR A 1 H9B H 0.6511 0.2580 0.3615 0.083 Uiso 0.728(4) calc PR A 1 H9C H 0.6909 0.3354 0.3177 0.083 Uiso 0.728(4) calc PR A 1 C10 C -0.18511(19) 0.39880(17) 0.17721(12) 0.0410(6) Uani 1 d . . . C11 C -0.2638(2) 0.4390(2) 0.12992(15) 0.0573(8) Uani 1 d . . . H11A H -0.3343 0.4307 0.1444 0.069 Uiso 1 calc R . . H11B H -0.2511 0.5046 0.1268 0.069 Uiso 1 calc R . . C12 C -0.2597(2) 0.3977(2) 0.06725(15) 0.0612(8) Uani 1 d . . . H12A H -0.3131 0.4255 0.0389 0.073 Uiso 1 calc R . . H12B H -0.2738 0.3323 0.0694 0.073 Uiso 1 calc R . . C13 C -0.1533(2) 0.41333(19) 0.04389(12) 0.0484(7) Uani 1 d . . . H13A H -0.1417 0.4790 0.0402 0.058 Uiso 1 calc R . . H13B H -0.1512 0.3869 0.0024 0.058 Uiso 1 calc R . . C14 C -0.06567(19) 0.37302(16) 0.08486(11) 0.0364(5) Uani 1 d . . . C15 C -0.1748(3) 0.4587(2) 0.23387(15) 0.0710(10) Uani 1 d . . . H15A H -0.1265 0.4309 0.2646 0.107 Uiso 1 calc R . . H15B H -0.2427 0.4656 0.2510 0.107 Uiso 1 calc R . . H15C H -0.1485 0.5180 0.2225 0.107 Uiso 1 calc R . . C16 C -0.2161(2) 0.30295(18) 0.19553(13) 0.0493(7) Uani 1 d . . . H16A H -0.2257 0.2655 0.1587 0.074 Uiso 1 calc R . . H16B H -0.2810 0.3052 0.2165 0.074 Uiso 1 calc R . . H16C H -0.1614 0.2770 0.2231 0.074 Uiso 1 calc R . . C17 C -0.0589(2) 0.27019(17) 0.07819(13) 0.0522(7) Uani 1 d . . . H17A H -0.0118 0.2459 0.1109 0.078 Uiso 1 calc R . . H17B H -0.0329 0.2553 0.0382 0.078 Uiso 1 calc R . . H17C H -0.1279 0.2438 0.0813 0.078 Uiso 1 calc R . . C18 C 0.0370(2) 0.4149(2) 0.06891(12) 0.0497(7) Uani 1 d . . . H18A H 0.0350 0.4800 0.0760 0.075 Uiso 1 calc R . . H18B H 0.0486 0.4033 0.0257 0.075 Uiso 1 calc R . . H18C H 0.0935 0.3882 0.0948 0.075 Uiso 1 calc R . . C19 C 0.1805(2) 0.55479(18) 0.19696(13) 0.0488(7) Uani 1 d . . . H19A H 0.1184 0.5285 0.1762 0.073 Uiso 1 calc R . . H19B H 0.1932 0.6146 0.1798 0.073 Uiso 1 calc R . . H19C H 0.1704 0.5603 0.2409 0.073 Uiso 1 calc R . . C20 C 0.3116(2) 0.4782(2) 0.09982(12) 0.0568(8) Uani 1 d . . . H20A H 0.3829 0.4612 0.0923 0.085 Uiso 1 calc R . . H20B H 0.2968 0.5382 0.0827 0.085 Uiso 1 calc R . . H20C H 0.2636 0.4343 0.0803 0.085 Uiso 1 calc R . . C21 C 0.4107(2) 0.5451(2) 0.21688(15) 0.0609(9) Uani 1 d . . . H21A H 0.4051 0.5550 0.2609 0.091 Uiso 1 calc R . . H21B H 0.4135 0.6033 0.1959 0.091 Uiso 1 calc R . . H21C H 0.4739 0.5109 0.2103 0.091 Uiso 1 calc R . . C22 C 0.4600(2) 0.2904(2) 0.16233(13) 0.0551(8) Uani 1 d . . . H22A H 0.4531 0.3202 0.1222 0.083 Uiso 1 calc R . . H22B H 0.4899 0.2303 0.1577 0.083 Uiso 1 calc R . . H22C H 0.5055 0.3263 0.1903 0.083 Uiso 1 calc R . . C23 C 0.3483(2) 0.19816(17) 0.26004(12) 0.0418(6) Uani 1 d . . . H23A H 0.4050 0.2194 0.2881 0.063 Uiso 1 calc R . . H23B H 0.3658 0.1387 0.2440 0.063 Uiso 1 calc R . . H23C H 0.2846 0.1937 0.2821 0.063 Uiso 1 calc R . . C24 C 0.2425(2) 0.22112(19) 0.13440(12) 0.0498(7) Uani 1 d . . . H24A H 0.1744 0.2101 0.1503 0.075 Uiso 1 calc R . . H24B H 0.2740 0.1635 0.1238 0.075 Uiso 1 calc R . . H24C H 0.2346 0.2591 0.0977 0.075 Uiso 1 calc R . . C25 C 0.2449(2) 0.53430(17) 0.37608(12) 0.0450(6) Uani 1 d . . . H25A H 0.3068 0.5037 0.3937 0.067 Uiso 1 calc R . . H25B H 0.2350 0.5910 0.3980 0.067 Uiso 1 calc R . . H25C H 0.2536 0.5471 0.3327 0.067 Uiso 1 calc R . . C26 C 0.1257(2) 0.4358(2) 0.46803(11) 0.0464(6) Uani 1 d . . . H26A H 0.0621 0.4031 0.4761 0.070 Uiso 1 calc R . . H26B H 0.1277 0.4928 0.4908 0.070 Uiso 1 calc R . . H26C H 0.1860 0.3991 0.4812 0.070 Uiso 1 calc R . . C27 C 0.0106(2) 0.53062(17) 0.36468(13) 0.0481(7) Uani 1 d . . . H27A H 0.0122 0.5529 0.3225 0.072 Uiso 1 calc R . . H27B H 0.0100 0.5818 0.3930 0.072 Uiso 1 calc R . . H27C H -0.0519 0.4942 0.3687 0.072 Uiso 1 calc R . . C28 C 0.0524(2) 0.20364(16) 0.27772(12) 0.0418(6) Uani 1 d . . . H28A H 0.0110 0.2389 0.2473 0.063 Uiso 1 calc R . . H28B H 0.0161 0.1475 0.2862 0.063 Uiso 1 calc R . . H28C H 0.1198 0.1896 0.2617 0.063 Uiso 1 calc R . . C29 C -0.0612(2) 0.28598(19) 0.37984(13) 0.0468(6) Uani 1 d . . . H29A H -0.0559 0.3193 0.4186 0.070 Uiso 1 calc R . . H29B H -0.0923 0.2268 0.3864 0.070 Uiso 1 calc R . . H29C H -0.1047 0.3198 0.3496 0.070 Uiso 1 calc R . . C30 C 0.1409(2) 0.19299(19) 0.40756(13) 0.0528(7) Uani 1 d . . . H30A H 0.2104 0.1797 0.3943 0.079 Uiso 1 calc R . . H30B H 0.1016 0.1368 0.4101 0.079 Uiso 1 calc R . . H30C H 0.1466 0.2220 0.4479 0.079 Uiso 1 calc R . . Li1 Li 0.2877(3) 0.3661(3) 0.31334(16) 0.0319(8) Uani 1 d . . . Li2 Li 0.1245(3) 0.3804(3) 0.24269(17) 0.0319(8) Uani 1 d . . . C2A C 0.6019(12) 0.2697(11) 0.4834(7) 0.083(4) Uiso 0.272(4) d P A 2 C3A C 0.6876(8) 0.3505(8) 0.4662(5) 0.041(2) Uiso 0.272(4) d P A 2 C4A C 0.6756(10) 0.3515(9) 0.3940(6) 0.070(4) Uiso 0.272(4) d P A 2 C6A C 0.4504(10) 0.3801(8) 0.5067(6) 0.064(3) Uiso 0.272(4) d P A 2 C7A C 0.4093(13) 0.2246(11) 0.4664(7) 0.091(5) Uiso 0.272(4) d P A 2 C8A C 0.5568(8) 0.3684(7) 0.3008(5) 0.053(3) Uiso 0.272(4) d P A 2 C9A C 0.5565(7) 0.4940(6) 0.3797(4) 0.037(2) Uiso 0.272(4) d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0310(4) 0.0421(4) 0.0351(3) 0.0127(3) -0.0043(3) -0.0068(3) Si2 0.0284(3) 0.0418(4) 0.0307(3) -0.0047(3) 0.0052(2) 0.0052(3) Si3 0.0347(4) 0.0293(3) 0.0293(3) -0.0039(3) 0.0021(3) 0.0044(3) Si4 0.0340(4) 0.0271(3) 0.0371(3) 0.0015(3) 0.0116(3) -0.0008(3) O1 0.0575(12) 0.0575(12) 0.0516(11) -0.0084(10) -0.0267(9) 0.0152(10) O2 0.0396(10) 0.0616(12) 0.0432(10) 0.0158(9) -0.0137(8) -0.0168(9) N1 0.0330(11) 0.0494(12) 0.0327(10) 0.0056(9) -0.0010(8) 0.0134(9) N2 0.0298(10) 0.0339(10) 0.0313(10) 0.0041(8) -0.0016(8) -0.0090(8) N3 0.0266(10) 0.0321(10) 0.0270(9) 0.0031(8) 0.0048(7) 0.0004(8) N4 0.0301(10) 0.0246(9) 0.0279(9) 0.0000(7) 0.0075(7) 0.0006(7) C1 0.0444(15) 0.0597(17) 0.0358(13) 0.0070(12) 0.0083(11) 0.0119(13) C5 0.0601(19) 0.0536(17) 0.0495(16) 0.0037(14) 0.0168(14) -0.0066(14) C10 0.0384(14) 0.0380(13) 0.0478(14) -0.0020(11) 0.0130(11) -0.0103(11) C11 0.0308(14) 0.0463(16) 0.095(2) 0.0115(16) 0.0087(14) 0.0003(12) C12 0.0466(17) 0.0598(18) 0.074(2) 0.0129(16) -0.0243(15) -0.0084(14) C13 0.0574(17) 0.0480(16) 0.0379(14) 0.0058(12) -0.0117(12) -0.0079(13) C14 0.0423(14) 0.0346(13) 0.0322(12) -0.0005(10) 0.0016(10) -0.0047(11) C15 0.092(3) 0.0587(19) 0.066(2) -0.0194(16) 0.0385(18) -0.0267(18) C16 0.0447(15) 0.0467(15) 0.0579(17) 0.0047(13) 0.0137(13) -0.0133(12) C17 0.0651(19) 0.0369(14) 0.0554(17) -0.0065(13) 0.0094(14) 0.0019(13) C18 0.0489(16) 0.0553(17) 0.0465(15) 0.0075(13) 0.0168(12) -0.0051(13) C19 0.0539(17) 0.0358(14) 0.0549(16) 0.0081(12) -0.0116(13) 0.0045(12) C20 0.0425(16) 0.088(2) 0.0398(14) 0.0234(15) 0.0022(12) -0.0065(15) C21 0.0513(18) 0.0595(18) 0.069(2) 0.0248(16) -0.0190(15) -0.0238(15) C22 0.0382(15) 0.082(2) 0.0469(15) -0.0051(15) 0.0156(12) 0.0101(14) C23 0.0386(14) 0.0379(13) 0.0493(15) 0.0005(12) 0.0048(11) 0.0096(11) C24 0.0499(16) 0.0532(16) 0.0457(15) -0.0130(13) -0.0020(12) 0.0068(13) C25 0.0532(16) 0.0339(13) 0.0476(15) -0.0079(12) 0.0008(12) -0.0082(12) C26 0.0468(16) 0.0597(17) 0.0329(13) -0.0064(12) 0.0041(11) 0.0075(13) C27 0.0508(16) 0.0365(14) 0.0556(16) -0.0104(12) -0.0095(13) 0.0142(12) C28 0.0428(15) 0.0316(12) 0.0521(15) -0.0071(11) 0.0136(12) -0.0066(11) C29 0.0410(15) 0.0468(15) 0.0542(16) -0.0047(13) 0.0176(12) -0.0044(12) C30 0.0619(18) 0.0404(15) 0.0571(17) 0.0172(13) 0.0109(14) 0.0004(13) Li1 0.0281(19) 0.039(2) 0.0287(18) 0.0041(16) 0.0030(15) 0.0043(16) Li2 0.029(2) 0.038(2) 0.0296(18) -0.0011(16) 0.0047(15) 0.0012(16) _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 N3 1.6954(19) . ? Si1 C19 1.878(3) . ? Si1 C21 1.879(3) . ? Si1 C20 1.894(3) . ? Si1 Li2 2.988(4) . ? Si2 N3 1.7009(19) . ? Si2 C23 1.882(3) . ? Si2 C24 1.883(3) . ? Si2 C22 1.889(3) . ? Si2 Li1 2.965(4) . ? Si3 N4 1.7040(18) . ? Si3 C27 1.875(2) . ? Si3 C26 1.884(2) . ? Si3 C25 1.886(3) . ? Si3 Li1 2.983(4) . ? Si4 N4 1.6977(18) . ? Si4 C30 1.879(3) . ? Si4 C28 1.883(2) . ? Si4 C29 1.890(2) . ? Si4 Li2 2.974(4) . ? O1 N1 1.273(2) . ? O1 Li1 1.943(4) . ? O2 N2 1.284(2) . ? O2 Li2 1.971(4) . ? N1 C1 1.485(3) . ? N1 C5 1.485(3) . ? N2 C10 1.495(3) . ? N2 C14 1.497(3) . ? N3 Li1 2.066(4) . ? N3 Li2 2.073(4) . ? N4 Li1 2.047(4) . ? N4 Li2 2.073(4) . ? C1 C2 1.505(5) . ? C1 C7 1.516(5) . ? C1 C6 1.570(5) . ? C2 C3 1.481(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.527(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.614(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C8 1.456(6) . ? C5 C9 1.534(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.523(4) . ? C10 C11 1.528(4) . ? C10 C16 1.537(3) . ? C11 C12 1.503(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.513(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.524(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C18 1.525(3) . ? C14 C17 1.536(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? Li1 Li2 2.549(5) . ? C2A C3A 1.690(19) . ? C3A C4A 1.574(16) . ? 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 Si1 C19 109.90(11) . . ? N3 Si1 C21 114.96(11) . . ? C19 Si1 C21 105.27(14) . . ? N3 Si1 C20 116.13(13) . . ? C19 Si1 C20 106.13(13) . . ? C21 Si1 C20 103.52(14) . . ? N3 Si1 Li2 42.20(9) . . ? C19 Si1 Li2 68.30(11) . . ? C21 Si1 Li2 133.82(12) . . ? C20 Si1 Li2 122.44(12) . . ? N3 Si2 C23 110.82(10) . . ? N3 Si2 C24 113.26(11) . . ? C23 Si2 C24 106.29(13) . . ? N3 Si2 C22 114.82(12) . . ? C23 Si2 C22 104.40(13) . . ? C24 Si2 C22 106.52(13) . . ? N3 Si2 Li1 42.67(9) . . ? C23 Si2 Li1 68.72(11) . . ? C24 Si2 Li1 133.12(12) . . ? C22 Si2 Li1 120.03(12) . . ? N4 Si3 C27 113.72(11) . . ? N4 Si3 C26 115.73(11) . . ? C27 Si3 C26 105.01(13) . . ? N4 Si3 C25 109.78(10) . . ? C27 Si3 C25 107.15(13) . . ? C26 Si3 C25 104.74(12) . . ? N4 Si3 Li1 41.53(10) . . ? C27 Si3 Li1 136.53(11) . . ? C26 Si3 Li1 117.93(11) . . ? C25 Si3 Li1 69.44(11) . . ? N4 Si4 C30 114.52(11) . . ? N4 Si4 C28 110.34(10) . . ? C30 Si4 C28 105.73(13) . . ? N4 Si4 C29 115.17(11) . . ? C30 Si4 C29 104.79(13) . . ? C28 Si4 C29 105.46(12) . . ? N4 Si4 Li2 42.62(9) . . ? C30 Si4 Li2 137.72(12) . . ? C28 Si4 Li2 69.19(11) . . ? C29 Si4 Li2 117.15(12) . . ? N1 O1 Li1 177.5(2) . . ? N2 O2 Li2 172.69(19) . . ? O1 N1 C1 116.5(2) . . ? O1 N1 C5 117.5(2) . . ? C1 N1 C5 125.1(2) . . ? O2 N2 C10 116.44(18) . . ? O2 N2 C14 116.43(19) . . ? C10 N2 C14 123.86(18) . . ? Si1 N3 Si2 124.32(10) . . ? Si1 N3 Li1 120.56(15) . . ? Si2 N3 Li1 103.42(14) . . ? Si1 N3 Li2 104.48(14) . . ? Si2 N3 Li2 118.76(15) . . ? Li1 N3 Li2 76.00(15) . . ? Si4 N4 Si3 121.83(10) . . ? Si4 N4 Li1 121.32(14) . . ? Si3 N4 Li1 104.97(14) . . ? Si4 N4 Li2 103.71(14) . . ? Si3 N4 Li2 120.82(14) . . ? Li1 N4 Li2 76.42(15) . . ? N1 C1 C2 113.5(3) . . ? N1 C1 C7 107.6(2) . . ? C2 C1 C7 111.3(3) . . ? N1 C1 C6 105.0(2) . . ? C2 C1 C6 111.3(3) . . ? C7 C1 C6 107.7(3) . . ? C3 C2 C1 113.2(3) . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 108.4(3) . . ? C2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? C2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C3 C4 C5 111.5(3) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C8 C5 N1 113.9(3) . . ? C8 C5 C9 112.0(3) . . ? N1 C5 C9 108.1(3) . . ? C8 C5 C4 106.8(3) . . ? N1 C5 C4 109.3(2) . . ? C9 C5 C4 106.5(3) . . ? N2 C10 C15 107.5(2) . . ? N2 C10 C11 109.2(2) . . ? C15 C10 C11 110.2(3) . . ? N2 C10 C16 108.7(2) . . ? C15 C10 C16 109.9(2) . . ? C11 C10 C16 111.3(2) . . ? C12 C11 C10 113.5(2) . . ? C12 C11 H11A 108.9 . . ? C10 C11 H11A 108.9 . . ? C12 C11 H11B 108.9 . . ? C10 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 C12 C13 109.0(2) . . ? C11 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? C11 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C12 C13 C14 113.7(2) . . ? C12 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? C12 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? N2 C14 C13 109.8(2) . . ? N2 C14 C18 107.41(19) . . ? C13 C14 C18 109.5(2) . . ? N2 C14 C17 108.7(2) . . ? C13 C14 C17 112.2(2) . . ? C18 C14 C17 109.1(2) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si2 C24 H24A 109.5 . . ? Si2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si3 C26 H26A 109.5 . . ? Si3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si3 C27 H27A 109.5 . . ? Si3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si4 C28 H28A 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si4 C30 H30A 109.5 . . ? Si4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 Li1 N4 126.1(2) . . ? O1 Li1 N3 129.5(2) . . ? N4 Li1 N3 104.36(17) . . ? O1 Li1 Li2 178.3(2) . . ? N4 Li1 Li2 52.24(13) . . ? N3 Li1 Li2 52.12(12) . . ? O1 Li1 Si2 109.46(16) . . ? N4 Li1 Si2 116.66(16) . . ? N3 Li1 Si2 33.91(8) . . ? Li2 Li1 Si2 71.86(12) . . ? O1 Li1 Si3 106.15(16) . . ? N4 Li1 Si3 33.50(8) . . ? N3 Li1 Si3 117.68(15) . . ? Li2 Li1 Si3 72.50(12) . . ? Si2 Li1 Si3 144.34(13) . . ? O2 Li2 N4 127.8(2) . . ? O2 Li2 N3 128.8(2) . . ? N4 Li2 N3 103.22(17) . . ? O2 Li2 Li1 176.6(2) . . ? N4 Li2 Li1 51.34(12) . . ? N3 Li2 Li1 51.88(13) . . ? O2 Li2 Si4 105.55(15) . . ? N4 Li2 Si4 33.68(8) . . ? N3 Li2 Si4 117.07(16) . . ? Li1 Li2 Si4 72.12(12) . . ? O2 Li2 Si1 110.35(16) . . ? N4 Li2 Si1 116.52(16) . . ? N3 Li2 Si1 33.32(8) . . ? Li1 Li2 Si1 71.95(12) . . ? Si4 Li2 Si1 144.07(14) . . ? C4A C3A C2A 101.7(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Li2 O2 N2 C10 -124.2(15) . . . . ? Li2 O2 N2 C14 75.5(16) . . . . ? C19 Si1 N3 Si2 151.13(13) . . . . ? C21 Si1 N3 Si2 -90.34(18) . . . . ? C20 Si1 N3 Si2 30.69(17) . . . . ? Li2 Si1 N3 Si2 141.1(2) . . . . ? C19 Si1 N3 Li1 -72.03(18) . . . . ? C21 Si1 N3 Li1 46.5(2) . . . . ? C20 Si1 N3 Li1 167.52(16) . . . . ? Li2 Si1 N3 Li1 -82.09(19) . . . . ? C19 Si1 N3 Li2 10.06(17) . . . . ? C21 Si1 N3 Li2 128.58(17) . . . . ? C20 Si1 N3 Li2 -110.39(16) . . . . ? C23 Si2 N3 Si1 152.54(13) . . . . ? C24 Si2 N3 Si1 -88.12(16) . . . . ? C22 Si2 N3 Si1 34.56(17) . . . . ? Li1 Si2 N3 Si1 142.7(2) . . . . ? C23 Si2 N3 Li1 9.81(16) . . . . ? C24 Si2 N3 Li1 129.15(16) . . . . ? C22 Si2 N3 Li1 -108.17(16) . . . . ? C23 Si2 N3 Li2 -71.41(18) . . . . ? C24 Si2 N3 Li2 47.94(19) . . . . ? C22 Si2 N3 Li2 170.62(16) . . . . ? Li1 Si2 N3 Li2 -81.21(19) . . . . ? C30 Si4 N4 Si3 -84.61(16) . . . . ? C28 Si4 N4 Si3 156.25(13) . . . . ? C29 Si4 N4 Si3 37.02(17) . . . . ? Li2 Si4 N4 Si3 140.54(19) . . . . ? C30 Si4 N4 Li1 52.58(19) . . . . ? C28 Si4 N4 Li1 -66.56(18) . . . . ? C29 Si4 N4 Li1 174.21(17) . . . . ? Li2 Si4 N4 Li1 -82.27(19) . . . . ? C30 Si4 N4 Li2 134.85(16) . . . . ? C28 Si4 N4 Li2 15.71(16) . . . . ? C29 Si4 N4 Li2 -103.52(16) . . . . ? C27 Si3 N4 Si4 -82.55(16) . . . . ? C26 Si3 N4 Si4 39.17(17) . . . . ? C25 Si3 N4 Si4 157.43(13) . . . . ? Li1 Si3 N4 Si4 143.1(2) . . . . ? C27 Si3 N4 Li1 134.39(16) . . . . ? C26 Si3 N4 Li1 -103.89(16) . . . . ? C25 Si3 N4 Li1 14.36(17) . . . . ? C27 Si3 N4 Li2 51.48(19) . . . . ? C26 Si3 N4 Li2 173.20(16) . . . . ? C25 Si3 N4 Li2 -68.54(18) . . . . ? Li1 Si3 N4 Li2 -82.91(19) . . . . ? O1 N1 C1 C2 -165.2(3) . . . . ? C5 N1 C1 C2 26.0(4) . . . . ? O1 N1 C1 C7 -41.5(3) . . . . ? C5 N1 C1 C7 149.6(3) . . . . ? O1 N1 C1 C6 73.0(3) . . . . ? C5 N1 C1 C6 -95.9(3) . . . . ? N1 C1 C2 C3 -43.0(4) . . . . ? C7 C1 C2 C3 -164.6(4) . . . . ? C6 C1 C2 C3 75.3(4) . . . . ? C1 C2 C3 C4 62.8(5) . . . . ? C2 C3 C4 C5 -63.0(4) . . . . ? O1 N1 C5 C8 45.9(4) . . . . ? C1 N1 C5 C8 -145.4(3) . . . . ? O1 N1 C5 C9 -79.3(3) . . . . ? C1 N1 C5 C9 89.4(3) . . . . ? O1 N1 C5 C4 165.1(2) . . . . ? C1 N1 C5 C4 -26.1(4) . . . . ? C3 C4 C5 C8 166.9(4) . . . . ? C3 C4 C5 N1 43.3(4) . . . . ? C3 C4 C5 C9 -73.3(4) . . . . ? O2 N2 C10 C15 44.3(3) . . . . ? C14 N2 C10 C15 -156.9(2) . . . . ? O2 N2 C10 C11 163.8(2) . . . . ? C14 N2 C10 C11 -37.4(3) . . . . ? O2 N2 C10 C16 -74.6(3) . . . . ? C14 N2 C10 C16 84.2(3) . . . . ? N2 C10 C11 C12 47.9(3) . . . . ? C15 C10 C11 C12 165.7(2) . . . . ? C16 C10 C11 C12 -72.2(3) . . . . ? C10 C11 C12 C13 -60.7(3) . . . . ? C11 C12 C13 C14 59.4(3) . . . . ? O2 N2 C14 C13 -164.68(19) . . . . ? C10 N2 C14 C13 36.5(3) . . . . ? O2 N2 C14 C18 -45.7(3) . . . . ? C10 N2 C14 C18 155.5(2) . . . . ? O2 N2 C14 C17 72.2(3) . . . . ? C10 N2 C14 C17 -86.5(3) . . . . ? C12 C13 C14 N2 -45.6(3) . . . . ? C12 C13 C14 C18 -163.3(2) . . . . ? C12 C13 C14 C17 75.4(3) . . . . ? Si4 N4 Li1 O1 -81.8(3) . . . . ? Si3 N4 Li1 O1 61.5(3) . . . . ? Li2 N4 Li1 O1 -179.8(3) . . . . ? Si4 N4 Li1 N3 97.89(18) . . . . ? Si3 N4 Li1 N3 -118.81(15) . . . . ? Li2 N4 Li1 N3 -0.06(17) . . . . ? Si4 N4 Li1 Li2 97.95(17) . . . . ? Si3 N4 Li1 Li2 -118.75(15) . . . . ? Si4 N4 Li1 Si2 64.0(2) . . . . ? Si3 N4 Li1 Si2 -152.71(12) . . . . ? Li2 N4 Li1 Si2 -33.96(17) . . . . ? Si4 N4 Li1 Si3 -143.30(18) . . . . ? Li2 N4 Li1 Si3 118.75(15) . . . . ? Si1 N3 Li1 O1 -81.5(3) . . . . ? Si2 N3 Li1 O1 63.0(3) . . . . ? Li2 N3 Li1 O1 179.8(3) . . . . ? Si1 N3 Li1 N4 98.81(18) . . . . ? Si2 N3 Li1 N4 -116.70(16) . . . . ? Li2 N3 Li1 N4 0.06(17) . . . . ? Si1 N3 Li1 Li2 98.74(17) . . . . ? Si2 N3 Li1 Li2 -116.76(15) . . . . ? Si1 N3 Li1 Si2 -144.49(18) . . . . ? Li2 N3 Li1 Si2 116.76(15) . . . . ? Si1 N3 Li1 Si3 65.7(2) . . . . ? Si2 N3 Li1 Si3 -149.80(13) . . . . ? Li2 N3 Li1 Si3 -33.03(17) . . . . ? N3 Si2 Li1 O1 -133.2(2) . . . . ? C23 Si2 Li1 O1 56.62(17) . . . . ? C24 Si2 Li1 O1 149.35(17) . . . . ? C22 Si2 Li1 O1 -38.1(2) . . . . ? N3 Si2 Li1 N4 75.56(18) . . . . ? C23 Si2 Li1 N4 -94.60(19) . . . . ? C24 Si2 Li1 N4 -1.9(3) . . . . ? C22 Si2 Li1 N4 170.63(17) . . . . ? C23 Si2 Li1 N3 -170.16(16) . . . . ? C24 Si2 Li1 N3 -77.43(19) . . . . ? C22 Si2 Li1 N3 95.07(17) . . . . ? N3 Si2 Li1 Li2 47.87(14) . . . . ? C23 Si2 Li1 Li2 -122.30(15) . . . . ? C24 Si2 Li1 Li2 -29.6(2) . . . . ? C22 Si2 Li1 Li2 142.93(15) . . . . ? N3 Si2 Li1 Si3 49.8(2) . . . . ? C23 Si2 Li1 Si3 -120.3(3) . . . . ? C24 Si2 Li1 Si3 -27.6(3) . . . . ? C22 Si2 Li1 Si3 144.9(2) . . . . ? N4 Si3 Li1 O1 -132.3(2) . . . . ? C27 Si3 Li1 O1 155.66(16) . . . . ? C26 Si3 Li1 O1 -34.2(2) . . . . ? C25 Si3 Li1 O1 62.09(17) . . . . ? C27 Si3 Li1 N4 -72.0(2) . . . . ? C26 Si3 Li1 N4 98.19(16) . . . . ? C25 Si3 Li1 N4 -165.56(17) . . . . ? N4 Si3 Li1 N3 73.44(19) . . . . ? C27 Si3 Li1 N3 1.4(3) . . . . ? C26 Si3 Li1 N3 171.63(17) . . . . ? C25 Si3 Li1 N3 -92.13(19) . . . . ? N4 Si3 Li1 Li2 46.62(14) . . . . ? C27 Si3 Li1 Li2 -25.4(2) . . . . ? C26 Si3 Li1 Li2 144.81(14) . . . . ? C25 Si3 Li1 Li2 -118.95(15) . . . . ? N4 Si3 Li1 Si2 44.7(2) . . . . ? C27 Si3 Li1 Si2 -27.3(3) . . . . ? C26 Si3 Li1 Si2 142.9(2) . . . . ? C25 Si3 Li1 Si2 -120.9(3) . . . . ? N2 O2 Li2 N4 127.9(15) . . . . ? N2 O2 Li2 N3 -57.4(17) . . . . ? N2 O2 Li2 Si4 156.6(15) . . . . ? N2 O2 Li2 Si1 -25.1(17) . . . . ? Si4 N4 Li2 O2 56.4(3) . . . . ? Si3 N4 Li2 O2 -84.7(3) . . . . ? Li1 N4 Li2 O2 175.8(3) . . . . ? Si4 N4 Li2 N3 -119.38(15) . . . . ? Si3 N4 Li2 N3 99.58(18) . . . . ? Li1 N4 Li2 N3 0.06(17) . . . . ? Si4 N4 Li2 Li1 -119.44(15) . . . . ? Si3 N4 Li2 Li1 99.52(17) . . . . ? Si3 N4 Li2 Si4 -141.04(18) . . . . ? Li1 N4 Li2 Si4 119.44(15) . . . . ? Si4 N4 Li2 Si1 -152.02(13) . . . . ? Si3 N4 Li2 Si1 66.9(2) . . . . ? Li1 N4 Li2 Si1 -32.58(17) . . . . ? Si1 N3 Li2 O2 65.8(3) . . . . ? Si2 N3 Li2 O2 -77.9(3) . . . . ? Li1 N3 Li2 O2 -175.8(3) . . . . ? Si1 N3 Li2 N4 -118.54(15) . . . . ? Si2 N3 Li2 N4 97.75(17) . . . . ? Li1 N3 Li2 N4 -0.06(17) . . . . ? Si1 N3 Li2 Li1 -118.48(15) . . . . ? Si2 N3 Li2 Li1 97.81(16) . . . . ? Si1 N3 Li2 Si4 -151.40(13) . . . . ? Si2 N3 Li2 Si4 64.9(2) . . . . ? Li1 N3 Li2 Si4 -32.93(17) . . . . ? Si2 N3 Li2 Si1 -143.71(18) . . . . ? Li1 N3 Li2 Si1 118.48(15) . . . . ? N3 Li1 Li2 N4 179.9(2) . . . . ? Si2 Li1 Li2 N4 148.31(16) . . . . ? Si3 Li1 Li2 N4 -30.49(8) . . . . ? N4 Li1 Li2 N3 -179.9(2) . . . . ? Si2 Li1 Li2 N3 -31.61(9) . . . . ? Si3 Li1 Li2 N3 149.59(16) . . . . ? N4 Li1 Li2 Si4 -30.49(9) . . . . ? N3 Li1 Li2 Si4 149.43(16) . . . . ? Si2 Li1 Li2 Si4 117.82(10) . . . . ? Si3 Li1 Li2 Si4 -60.98(6) . . . . ? N4 Li1 Li2 Si1 149.55(16) . . . . ? N3 Li1 Li2 Si1 -30.52(9) . . . . ? Si2 Li1 Li2 Si1 -62.14(6) . . . . ? Si3 Li1 Li2 Si1 119.07(10) . . . . ? N4 Si4 Li2 O2 -137.0(2) . . . . ? C30 Si4 Li2 O2 149.56(17) . . . . ? C28 Si4 Li2 O2 58.80(16) . . . . ? C29 Si4 Li2 O2 -38.4(2) . . . . ? C30 Si4 Li2 N4 -73.5(2) . . . . ? C28 Si4 Li2 N4 -164.24(16) . . . . ? C29 Si4 Li2 N4 98.54(15) . . . . ? N4 Si4 Li2 N3 72.30(18) . . . . ? C30 Si4 Li2 N3 -1.2(3) . . . . ? C28 Si4 Li2 N3 -91.94(19) . . . . ? C29 Si4 Li2 N3 170.85(16) . . . . ? N4 Si4 Li2 Li1 45.61(14) . . . . ? C30 Si4 Li2 Li1 -27.9(2) . . . . ? C28 Si4 Li2 Li1 -118.63(15) . . . . ? C29 Si4 Li2 Li1 144.15(14) . . . . ? N4 Si4 Li2 Si1 45.7(2) . . . . ? C30 Si4 Li2 Si1 -27.8(3) . . . . ? C28 Si4 Li2 Si1 -118.6(3) . . . . ? C29 Si4 Li2 Si1 144.2(2) . . . . ? N3 Si1 Li2 O2 -130.7(2) . . . . ? C19 Si1 Li2 O2 59.47(17) . . . . ? C21 Si1 Li2 O2 150.11(18) . . . . ? C20 Si1 Li2 O2 -36.4(2) . . . . ? N3 Si1 Li2 N4 72.91(18) . . . . ? C19 Si1 Li2 N4 -96.92(19) . . . . ? C21 Si1 Li2 N4 -6.3(3) . . . . ? C20 Si1 Li2 N4 167.26(17) . . . . ? C19 Si1 Li2 N3 -169.82(17) . . . . ? C21 Si1 Li2 N3 -79.2(2) . . . . ? C20 Si1 Li2 N3 94.36(17) . . . . ? N3 Si1 Li2 Li1 46.66(14) . . . . ? C19 Si1 Li2 Li1 -123.16(15) . . . . ? C21 Si1 Li2 Li1 -32.5(2) . . . . ? C20 Si1 Li2 Li1 141.01(16) . . . . ? N3 Si1 Li2 Si4 46.6(2) . . . . ? C19 Si1 Li2 Si4 -123.2(3) . . . . ? C21 Si1 Li2 Si4 -32.6(3) . . . . ? C20 Si1 Li2 Si4 140.9(2) . . . . ? _refine_diff_density_max 0.519 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.054 #------------------------------------------------------------------------- #-----------------------------COMPOUND 3------------------------------------ #--------------------------------------------------------------------------- data_g16 _database_code_CSD 160884 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H126 Li2 Mg1 N7 O3 Si8' _chemical_formula_weight 1148.5 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 '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 8.4559(2) _cell_length_b 21.3384(5) _cell_length_c 21.3655(6) _cell_angle_alpha 103.0160(10) _cell_angle_beta 94.8590(10) _cell_angle_gamma 92.6790(10) _cell_volume 3733.93(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12462 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.022 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1270 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi + omega scans to fill ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24487 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.1186 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 24.99 _reflns_number_total 13018 _reflns_number_gt 7206 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Denzo & Collect (Otwinowski & Minor, 1997; Hooft & Nonius 1988) ; _computing_cell_refinement 'Denzo & Collect' _computing_data_reduction 'Denzo & Collect' _computing_structure_solution 'SIR-97 ' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The H atoms of the minor disorder component were not included. 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 w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+1.5001P] 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 13018 _refine_ls_number_parameters 725 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1379 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1382 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.38066(12) 0.41075(5) 0.85832(5) 0.0382(3) Uani 1 d . . . Si2 Si 0.66513(12) 0.47378(4) 0.81920(5) 0.0381(3) Uani 1 d . . . Si3 Si 0.35998(11) 0.42583(5) 0.61925(5) 0.0379(3) Uani 1 d . . . Si4 Si 0.61822(12) 0.33890(5) 0.58198(5) 0.0400(3) Uani 1 d . . . Si5 Si 0.32592(12) 0.20247(4) 0.67611(5) 0.0435(3) Uani 1 d . . . Si6 Si 0.61131(14) 0.22263(5) 0.77190(6) 0.0562(3) Uani 1 d . . . Si7 Si 0.01327(12) -0.04205(5) 0.83155(5) 0.0412(3) Uani 1 d . . . Si8 Si 0.34340(11) -0.07826(5) 0.86822(5) 0.0389(3) Uani 1 d . . . Mg1 Mg 0.49414(12) 0.34564(5) 0.72116(5) 0.0319(3) Uani 1 d . . . O1 O 0.0716(2) -0.22616(9) 0.74739(10) 0.0333(5) Uani 1 d . . . O2 O 0.1445(3) -0.13170(11) 0.65331(12) 0.0588(7) Uani 1 d . . . O3 O 0.0466(3) -0.21453(11) 0.90681(12) 0.0526(7) Uani 1 d . . . N1 N 0.5152(3) 0.41509(11) 0.80405(12) 0.0320(7) Uani 1 d . . . N2 N 0.4884(3) 0.37104(12) 0.63468(12) 0.0324(7) Uani 1 d . . . N3 N 0.4764(3) 0.25085(12) 0.72295(13) 0.0386(7) Uani 1 d . . . N4 N 0.1604(3) -0.09451(11) 0.82560(12) 0.0310(7) Uani 1 d . . . N5 N 0.0204(3) -0.28393(11) 0.71560(12) 0.0302(6) Uani 1 d . . . N6 N 0.2005(4) -0.11424(13) 0.60529(14) 0.0448(8) Uani 1 d . . . N7 N 0.0297(3) -0.25434(14) 0.94299(14) 0.0445(8) Uani 1 d . . . C1 C 0.2145(4) 0.34901(17) 0.82176(17) 0.0474(10) Uani 1 d . . . H1A H 0.1577 0.3616 0.7851 0.071 Uiso 1 calc R . . H1B H 0.1408 0.3461 0.8542 0.071 Uiso 1 calc R . . H1C H 0.2579 0.3070 0.8069 0.071 Uiso 1 calc R . . C2 C 0.4674(5) 0.3898(2) 0.93439(19) 0.0749(14) Uani 1 d . . . H2A H 0.5214 0.3497 0.9233 0.112 Uiso 1 calc R . . H2B H 0.3819 0.3841 0.9613 0.112 Uiso 1 calc R . . H2C H 0.5439 0.4247 0.9582 0.112 Uiso 1 calc R . . C3 C 0.2820(5) 0.48740(18) 0.8869(2) 0.0646(12) Uani 1 d . . . H3A H 0.3614 0.5207 0.9115 0.097 Uiso 1 calc R . . H3B H 0.1996 0.4800 0.9145 0.097 Uiso 1 calc R . . H3C H 0.2334 0.5016 0.8496 0.097 Uiso 1 calc R . . C4 C 0.7889(5) 0.4806(2) 0.89797(18) 0.0675(13) Uani 1 d . . . H4A H 0.7289 0.5007 0.9336 0.101 Uiso 1 calc R . . H4B H 0.8872 0.5070 0.8988 0.101 Uiso 1 calc R . . H4C H 0.8151 0.4375 0.9026 0.101 Uiso 1 calc R . . C5 C 0.5954(5) 0.55703(16) 0.8219(2) 0.0663(13) Uani 1 d . . . H5A H 0.5228 0.5560 0.7834 0.099 Uiso 1 calc R . . H5B H 0.6874 0.5872 0.8232 0.099 Uiso 1 calc R . . H5C H 0.5399 0.5712 0.8606 0.099 Uiso 1 calc R . . C6 C 0.8063(4) 0.45929(17) 0.75584(17) 0.0484(10) Uani 1 d . . . H6A H 0.8559 0.4187 0.7558 0.073 Uiso 1 calc R . . H6B H 0.8887 0.4948 0.7649 0.073 Uiso 1 calc R . . H6C H 0.7484 0.4567 0.7135 0.073 Uiso 1 calc R . . C7 C 0.2064(4) 0.43835(16) 0.67771(17) 0.0459(10) Uani 1 d . . . H7A H 0.1458 0.3974 0.6749 0.069 Uiso 1 calc R . . H7B H 0.1342 0.4700 0.6673 0.069 Uiso 1 calc R . . H7C H 0.2585 0.4543 0.7216 0.069 Uiso 1 calc R . . C8 C 0.4610(5) 0.50801(17) 0.6244(2) 0.0603(12) Uani 1 d . . . H8A H 0.5030 0.5271 0.6692 0.090 Uiso 1 calc R . . H8B H 0.3839 0.5359 0.6100 0.090 Uiso 1 calc R . . H8C H 0.5486 0.5036 0.5968 0.090 Uiso 1 calc R . . C9 C 0.2484(5) 0.4023(2) 0.53669(19) 0.0658(12) Uani 1 d . . . H9A H 0.3229 0.4022 0.5039 0.099 Uiso 1 calc R . . H9B H 0.1685 0.4334 0.5327 0.099 Uiso 1 calc R . . H9C H 0.1955 0.3592 0.5303 0.099 Uiso 1 calc R . . C10 C 0.7420(5) 0.40025(18) 0.55257(19) 0.0605(12) Uani 1 d . . . H10A H 0.6731 0.4221 0.5263 0.091 Uiso 1 calc R . . H10B H 0.8219 0.3785 0.5264 0.091 Uiso 1 calc R . . H10C H 0.7955 0.4320 0.5897 0.091 Uiso 1 calc R . . C11 C 0.5222(5) 0.28217(17) 0.50588(17) 0.0542(11) Uani 1 d . . . H11A H 0.4427 0.2527 0.5170 0.081 Uiso 1 calc R . . H11B H 0.6037 0.2573 0.4835 0.081 Uiso 1 calc R . . H11C H 0.4704 0.3071 0.4776 0.081 Uiso 1 calc R . . C12 C 0.7633(4) 0.29090(19) 0.61897(19) 0.0616(12) Uani 1 d . . . H12A H 0.8237 0.3189 0.6570 0.092 Uiso 1 calc R . . H12B H 0.8365 0.2730 0.5874 0.092 Uiso 1 calc R . . H12C H 0.7056 0.2557 0.6319 0.092 Uiso 1 calc R . . C13 C 0.1749(4) 0.25005(17) 0.6421(2) 0.0620(12) Uani 1 d . . . H13A H 0.1292 0.2789 0.6774 0.093 Uiso 1 calc R . . H13B H 0.0903 0.2206 0.6153 0.093 Uiso 1 calc R . . H13C H 0.2259 0.2756 0.6157 0.093 Uiso 1 calc R . . C14 C 0.3938(5) 0.14495(16) 0.60441(18) 0.0547(11) Uani 1 d . . . H14A H 0.4484 0.1694 0.5779 0.082 Uiso 1 calc R . . H14B H 0.3014 0.1196 0.5786 0.082 Uiso 1 calc R . . H14C H 0.4669 0.1159 0.6194 0.082 Uiso 1 calc R . . C15 C 0.2136(5) 0.15037(18) 0.7194(2) 0.0675(13) Uani 1 d . . . H15A H 0.2859 0.1215 0.7352 0.101 Uiso 1 calc R . . H15B H 0.1275 0.1247 0.6897 0.101 Uiso 1 calc R . . H15C H 0.1685 0.1776 0.7560 0.101 Uiso 1 calc R . . C16 C 0.7000(6) 0.14690(19) 0.7303(3) 0.101(2) Uani 1 d . . . H16A H 0.6189 0.1108 0.7211 0.151 Uiso 1 calc R . . H16B H 0.7893 0.1376 0.7583 0.151 Uiso 1 calc R . . H16C H 0.7379 0.1528 0.6898 0.151 Uiso 1 calc R . . C17 C 0.5290(6) 0.2037(2) 0.8453(2) 0.0970(18) Uani 1 d . . . H17A H 0.4862 0.2423 0.8704 0.145 Uiso 1 calc R . . H17B H 0.6139 0.1896 0.8719 0.145 Uiso 1 calc R . . H17C H 0.4439 0.1693 0.8316 0.145 Uiso 1 calc R . . C18 C 0.7831(4) 0.28307(18) 0.8022(2) 0.0618(12) Uani 1 d . . . H18A H 0.8305 0.2942 0.7655 0.093 Uiso 1 calc R . . H18B H 0.8629 0.2648 0.8276 0.093 Uiso 1 calc R . . H18C H 0.7461 0.3219 0.8293 0.093 Uiso 1 calc R . . C19 C -0.140(3) -0.0706(14) 0.7619(15) 0.071(7) Uani 0.613(7) d P A 1 H19A H -0.0960 -0.0656 0.7222 0.107 Uiso 0.613(7) calc PR A 1 H19B H -0.2331 -0.0452 0.7685 0.107 Uiso 0.613(7) calc PR A 1 H19C H -0.1713 -0.1162 0.7583 0.107 Uiso 0.613(7) calc PR A 1 C20 C -0.0969(10) -0.0495(5) 0.9057(4) 0.070(3) Uani 0.613(7) d P A 1 H20A H -0.1437 -0.0936 0.8994 0.105 Uiso 0.613(7) calc PR A 1 H20B H -0.1813 -0.0193 0.9107 0.105 Uiso 0.613(7) calc PR A 1 H20C H -0.0214 -0.0393 0.9446 0.105 Uiso 0.613(7) calc PR A 1 C21 C 0.0734(9) 0.0389(3) 0.8108(5) 0.071(3) Uani 0.613(7) d P A 1 H21A H 0.1543 0.0632 0.8440 0.106 Uiso 0.613(7) calc PR A 1 H21B H -0.0202 0.0640 0.8090 0.106 Uiso 0.613(7) calc PR A 1 H21C H 0.1167 0.0304 0.7688 0.106 Uiso 0.613(7) calc PR A 1 C19A C -0.157(5) -0.073(2) 0.767(2) 0.047(8) Uiso 0.387(7) d P A 2 H19D H -0.1148 -0.0910 0.7262 0.071 Uiso 0.387(7) calc PR A 2 H19E H -0.2217 -0.0368 0.7623 0.071 Uiso 0.387(7) calc PR A 2 H19F H -0.2226 -0.1059 0.7799 0.071 Uiso 0.387(7) calc PR A 2 C20A C -0.0625(18) -0.0141(6) 0.9086(7) 0.056(4) Uiso 0.387(7) d P A 2 H20D H -0.1128 -0.0506 0.9219 0.084 Uiso 0.387(7) calc PR A 2 H20E H -0.1411 0.0176 0.9050 0.084 Uiso 0.387(7) calc PR A 2 H20F H 0.0253 0.0061 0.9408 0.084 Uiso 0.387(7) calc PR A 2 C21A C 0.0689(17) 0.0417(6) 0.8518(7) 0.062(4) Uiso 0.387(7) d P A 2 H21D H 0.1199 0.0540 0.8961 0.093 Uiso 0.387(7) calc PR A 2 H21E H -0.0260 0.0659 0.8484 0.093 Uiso 0.387(7) calc PR A 2 H21F H 0.1435 0.0516 0.8221 0.093 Uiso 0.387(7) calc PR A 2 C22 C 0.4669(4) -0.14812(17) 0.84116(19) 0.0571(11) Uani 1 d . . . H22A H 0.4125 -0.1877 0.8470 0.086 Uiso 1 calc R . . H22B H 0.5706 -0.1406 0.8668 0.086 Uiso 1 calc R . . H22C H 0.4823 -0.1527 0.7954 0.086 Uiso 1 calc R . . C23 C 0.4588(5) -0.00553(18) 0.8566(2) 0.0672(13) Uani 1 d . . . H23A H 0.4670 -0.0093 0.8104 0.101 Uiso 1 calc R . . H23B H 0.5657 -0.0024 0.8792 0.101 Uiso 1 calc R . . H23C H 0.4043 0.0332 0.8740 0.101 Uiso 1 calc R . . C24 C 0.3364(5) -0.0700(2) 0.95669(18) 0.0674(13) Uani 1 d . . . H24A H 0.2814 -0.0316 0.9745 0.101 Uiso 1 calc R . . H24B H 0.4450 -0.0660 0.9779 0.101 Uiso 1 calc R . . H24C H 0.2791 -0.1083 0.9642 0.101 Uiso 1 calc R . . C25 C 0.1350(4) -0.32272(15) 0.67573(17) 0.0411(9) Uani 1 d . . . C26 C 0.0792(4) -0.39380(15) 0.66327(19) 0.0502(10) Uani 1 d . . . H26A H 0.1417 -0.4188 0.6303 0.060 Uiso 1 calc R . . H26B H 0.1018 -0.4087 0.7036 0.060 Uiso 1 calc R . . C27 C -0.0955(4) -0.40824(16) 0.64065(19) 0.0487(10) Uani 1 d . . . H27A H -0.1234 -0.4551 0.6330 0.058 Uiso 1 calc R . . H27B H -0.1202 -0.3947 0.5997 0.058 Uiso 1 calc R . . C28 C -0.1903(4) -0.37160(16) 0.69241(19) 0.0515(10) Uani 1 d . . . H28A H -0.1672 -0.3871 0.7323 0.062 Uiso 1 calc R . . H28B H -0.3051 -0.3816 0.6783 0.062 Uiso 1 calc R . . C29 C -0.1563(4) -0.29888(15) 0.70800(16) 0.0363(9) Uani 1 d . . . C30 C 0.2978(4) -0.3104(2) 0.7127(2) 0.0791(15) Uani 1 d . . . H30A H 0.3335 -0.2649 0.7189 0.119 Uiso 1 calc R . . H30B H 0.3729 -0.3374 0.6884 0.119 Uiso 1 calc R . . H30C H 0.2927 -0.3209 0.7549 0.119 Uiso 1 calc R . . C31 C 0.1397(6) -0.30026(18) 0.6127(2) 0.0745(14) Uani 1 d . . . H31A H 0.0398 -0.3147 0.5854 0.112 Uiso 1 calc R . . H31B H 0.2288 -0.3186 0.5900 0.112 Uiso 1 calc R . . H31C H 0.1535 -0.2531 0.6224 0.112 Uiso 1 calc R . . C32 C -0.2210(4) -0.26887(18) 0.77106(18) 0.0527(11) Uani 1 d . . . H32A H -0.1618 -0.2826 0.8065 0.079 Uiso 1 calc R . . H32B H -0.3338 -0.2828 0.7689 0.079 Uiso 1 calc R . . H32C H -0.2093 -0.2218 0.7785 0.079 Uiso 1 calc R . . C33 C -0.2293(5) -0.26852(18) 0.65490(19) 0.0612(12) Uani 1 d . . . H33A H -0.1897 -0.2232 0.6632 0.092 Uiso 1 calc R . . H33B H -0.3454 -0.2712 0.6545 0.092 Uiso 1 calc R . . H33C H -0.1995 -0.2917 0.6130 0.092 Uiso 1 calc R . . C34 C 0.3686(5) -0.08584(16) 0.61622(18) 0.0500(10) Uani 1 d . . . C35 C 0.4267(5) -0.08249(19) 0.5516(2) 0.0644(12) Uani 1 d . . . H35A H 0.5260 -0.0542 0.5595 0.077 Uiso 1 calc R . . H35B H 0.4528 -0.1262 0.5293 0.077 Uiso 1 calc R . . C36 C 0.3083(6) -0.05745(19) 0.5073(2) 0.0636(12) Uani 1 d . . . H36A H 0.2825 -0.0133 0.5283 0.076 Uiso 1 calc R . . H36B H 0.3543 -0.0558 0.4666 0.076 Uiso 1 calc R . . C37 C 0.1604(5) -0.10196(19) 0.49340(19) 0.0614(12) Uani 1 d . . . H37A H 0.1881 -0.1457 0.4722 0.074 Uiso 1 calc R . . H37B H 0.0844 -0.0871 0.4628 0.074 Uiso 1 calc R . . C38 C 0.0797(5) -0.10552(19) 0.55368(19) 0.0556(11) Uani 1 d . . . C39 C 0.4694(5) -0.13006(19) 0.6477(2) 0.0669(12) Uani 1 d . . . H39A H 0.4383 -0.1286 0.6911 0.100 Uiso 1 calc R . . H39B H 0.5820 -0.1156 0.6506 0.100 Uiso 1 calc R . . H39C H 0.4525 -0.1743 0.6216 0.100 Uiso 1 calc R . . C40 C 0.3730(6) -0.01897(18) 0.6622(2) 0.0855(16) Uani 1 d . . . H40A H 0.3174 0.0105 0.6403 0.128 Uiso 1 calc R . . H40B H 0.4838 -0.0024 0.6751 0.128 Uiso 1 calc R . . H40C H 0.3206 -0.0224 0.7006 0.128 Uiso 1 calc R . . C41 C -0.0045(6) -0.0439(2) 0.5791(2) 0.0922(17) Uani 1 d . . . H41A H -0.0410 -0.0449 0.6212 0.138 Uiso 1 calc R . . H41B H -0.0961 -0.0413 0.5486 0.138 Uiso 1 calc R . . H41C H 0.0699 -0.0061 0.5836 0.138 Uiso 1 calc R . . C42 C -0.0394(6) -0.1645(2) 0.5384(2) 0.0924(17) Uani 1 d . . . H42A H 0.0175 -0.2038 0.5267 0.139 Uiso 1 calc R . . H42B H -0.1163 -0.1618 0.5023 0.139 Uiso 1 calc R . . H42C H -0.0956 -0.1657 0.5764 0.139 Uiso 1 calc R . . C43 C 0.1374(4) -0.30863(17) 0.93533(17) 0.0455(10) Uani 1 d . A 1 C44 C 0.1223(10) -0.3452(5) 0.9883(5) 0.083(3) Uani 0.613(7) d P A 1 H44A H 0.1422 -0.3907 0.9701 0.099 Uiso 0.613(7) calc PR A 1 H44B H 0.2088 -0.3278 1.0229 0.099 Uiso 0.613(7) calc PR A 1 C45 C -0.0234(6) -0.3447(2) 1.0177(2) 0.0725(14) Uani 1 d . A 1 H45A H -0.0080 -0.3643 1.0555 0.087 Uiso 1 calc R A 1 H45B H -0.1059 -0.3721 0.9865 0.087 Uiso 1 calc R A 1 C46 C -0.0842(10) -0.2777(4) 1.0399(4) 0.071(3) Uani 0.613(7) d P A 1 H46A H -0.1910 -0.2823 1.0548 0.086 Uiso 0.613(7) calc PR A 1 H46B H -0.0123 -0.2529 1.0771 0.086 Uiso 0.613(7) calc PR A 1 C47 C -0.0944(5) -0.24115(18) 0.98877(18) 0.0502(10) Uani 1 d . A 1 C48 C 0.0659(11) -0.3538(3) 0.8702(3) 0.078(3) Uani 0.613(7) d P A 1 H48A H 0.0607 -0.3294 0.8364 0.117 Uiso 0.613(7) calc PR A 1 H48B H -0.0414 -0.3704 0.8749 0.117 Uiso 0.613(7) calc PR A 1 H48C H 0.1334 -0.3898 0.8584 0.117 Uiso 0.613(7) calc PR A 1 C49 C 0.3024(9) -0.2876(4) 0.9344(6) 0.102(4) Uani 0.613(7) d P A 1 H49A H 0.3161 -0.2748 0.8939 0.153 Uiso 0.613(7) calc PR A 1 H49B H 0.3698 -0.3231 0.9379 0.153 Uiso 0.613(7) calc PR A 1 H49C H 0.3329 -0.2508 0.9708 0.153 Uiso 0.613(7) calc PR A 1 C50 C -0.2531(8) -0.2515(5) 0.9480(4) 0.073(3) Uani 0.613(7) d P A 1 H50A H -0.2460 -0.2311 0.9114 0.109 Uiso 0.613(7) calc PR A 1 H50B H -0.3356 -0.2323 0.9743 0.109 Uiso 0.613(7) calc PR A 1 H50C H -0.2802 -0.2978 0.9318 0.109 Uiso 0.613(7) calc PR A 1 C51 C -0.0744(16) -0.1673(4) 1.0236(5) 0.141(5) Uani 0.613(7) d P A 1 H51A H 0.0379 -0.1552 1.0386 0.212 Uiso 0.613(7) calc PR A 1 H51B H -0.1380 -0.1594 1.0605 0.212 Uiso 0.613(7) calc PR A 1 H51C H -0.1107 -0.1416 0.9932 0.212 Uiso 0.613(7) calc PR A 1 C44A C 0.0674(15) -0.3671(5) 0.9533(6) 0.051(4) Uiso 0.387(7) d P A 2 C46A C -0.1526(13) -0.3105(5) 1.0027(6) 0.049(3) Uiso 0.387(7) d P A 2 C48A C 0.1918(13) -0.3257(5) 0.8650(5) 0.045(3) Uiso 0.387(7) d P A 2 C49A C 0.2920(16) -0.2746(6) 0.9837(6) 0.062(4) Uiso 0.387(7) d P A 2 C50A C -0.2300(18) -0.2084(7) 0.9646(7) 0.071(5) Uiso 0.387(7) d P A 2 C51A C -0.0074(14) -0.1982(6) 1.0505(6) 0.057(4) Uiso 0.387(7) d P A 2 Li1 Li 0.0790(7) -0.1792(3) 0.8390(3) 0.0409(15) Uani 1 d . . . Li2 Li 0.1486(7) -0.1420(3) 0.7357(3) 0.0426(15) Uani 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 Si1 0.0331(6) 0.0471(6) 0.0336(6) 0.0083(5) 0.0066(5) -0.0062(5) Si2 0.0377(6) 0.0359(5) 0.0379(6) 0.0028(4) 0.0090(5) -0.0094(4) Si3 0.0312(6) 0.0428(6) 0.0408(6) 0.0113(5) 0.0049(5) 0.0044(5) Si4 0.0356(6) 0.0413(6) 0.0380(6) -0.0026(5) 0.0073(5) 0.0009(5) Si5 0.0345(6) 0.0304(5) 0.0602(7) 0.0020(5) -0.0009(5) -0.0025(4) Si6 0.0496(7) 0.0401(6) 0.0771(9) 0.0193(6) -0.0167(6) -0.0016(5) Si7 0.0349(6) 0.0375(6) 0.0459(6) -0.0021(5) 0.0049(5) 0.0032(5) Si8 0.0327(6) 0.0416(6) 0.0381(6) 0.0022(5) 0.0015(5) -0.0045(5) Mg1 0.0280(6) 0.0292(6) 0.0365(7) 0.0042(5) 0.0017(5) -0.0006(5) O1 0.0396(14) 0.0221(12) 0.0354(13) 0.0016(10) 0.0070(11) -0.0067(10) O2 0.091(2) 0.0527(16) 0.0396(16) 0.0216(13) 0.0138(15) 0.0063(15) O3 0.0672(19) 0.0497(15) 0.0467(16) 0.0233(13) 0.0112(14) -0.0060(13) N1 0.0290(16) 0.0327(15) 0.0328(16) 0.0047(12) 0.0056(13) -0.0035(12) N2 0.0285(16) 0.0341(15) 0.0315(16) 0.0011(12) 0.0021(13) 0.0010(12) N3 0.0316(17) 0.0319(15) 0.0502(19) 0.0084(13) -0.0031(14) -0.0020(13) N4 0.0305(16) 0.0287(15) 0.0318(16) 0.0040(12) 0.0037(13) -0.0039(12) N5 0.0348(17) 0.0257(15) 0.0306(16) 0.0072(12) 0.0051(13) -0.0013(13) N6 0.069(2) 0.0375(17) 0.0323(19) 0.0144(14) 0.0110(17) 0.0077(16) N7 0.046(2) 0.0501(19) 0.0424(19) 0.0231(16) 0.0073(16) -0.0055(16) C1 0.036(2) 0.058(2) 0.049(2) 0.0130(19) 0.0126(19) -0.0110(18) C2 0.055(3) 0.124(4) 0.051(3) 0.038(3) 0.003(2) -0.020(3) C3 0.058(3) 0.065(3) 0.068(3) -0.001(2) 0.036(2) 0.000(2) C4 0.058(3) 0.082(3) 0.052(3) 0.007(2) -0.008(2) -0.039(2) C5 0.078(3) 0.039(2) 0.082(3) 0.006(2) 0.037(3) -0.009(2) C6 0.035(2) 0.053(2) 0.053(3) 0.0047(19) 0.0141(19) -0.0143(18) C7 0.041(2) 0.043(2) 0.058(3) 0.0171(19) 0.014(2) 0.0124(17) C8 0.046(3) 0.052(2) 0.089(3) 0.024(2) 0.019(2) 0.0092(19) C9 0.059(3) 0.086(3) 0.053(3) 0.018(2) -0.003(2) 0.018(2) C10 0.058(3) 0.063(3) 0.055(3) -0.005(2) 0.030(2) -0.009(2) C11 0.060(3) 0.053(2) 0.045(2) 0.0008(19) 0.011(2) 0.000(2) C12 0.044(3) 0.074(3) 0.062(3) 0.001(2) 0.007(2) 0.025(2) C13 0.047(3) 0.046(2) 0.079(3) -0.006(2) -0.021(2) 0.0031(19) C14 0.059(3) 0.038(2) 0.062(3) 0.0027(19) 0.001(2) 0.0021(19) C15 0.056(3) 0.052(3) 0.089(3) 0.005(2) 0.013(2) -0.013(2) C16 0.081(4) 0.051(3) 0.151(5) 0.002(3) -0.047(4) 0.022(2) C17 0.097(4) 0.102(4) 0.107(4) 0.073(3) -0.022(3) -0.025(3) C18 0.045(3) 0.066(3) 0.072(3) 0.021(2) -0.023(2) -0.003(2) C19 0.048(9) 0.097(12) 0.057(10) -0.011(5) -0.004(6) 0.041(8) C20 0.040(5) 0.116(8) 0.056(5) 0.011(5) 0.022(4) 0.028(5) C21 0.065(6) 0.040(4) 0.114(8) 0.030(5) 0.003(6) 0.008(3) C22 0.043(2) 0.058(2) 0.065(3) 0.008(2) 0.000(2) 0.006(2) C23 0.045(3) 0.057(3) 0.096(4) 0.018(2) -0.004(2) -0.018(2) C24 0.053(3) 0.099(3) 0.040(2) 0.001(2) -0.004(2) -0.004(2) C25 0.034(2) 0.0318(19) 0.052(2) -0.0062(17) 0.0181(19) -0.0020(16) C26 0.054(3) 0.031(2) 0.060(3) -0.0020(18) 0.008(2) 0.0024(18) C27 0.055(3) 0.030(2) 0.057(3) 0.0037(18) 0.003(2) -0.0078(18) C28 0.042(2) 0.044(2) 0.064(3) 0.006(2) 0.003(2) -0.0133(18) C29 0.024(2) 0.040(2) 0.042(2) 0.0054(17) 0.0010(17) -0.0021(16) C30 0.031(2) 0.065(3) 0.121(4) -0.024(3) 0.011(3) 0.004(2) C31 0.109(4) 0.051(3) 0.063(3) -0.001(2) 0.055(3) -0.012(2) C32 0.032(2) 0.062(3) 0.059(3) 0.002(2) 0.012(2) -0.0015(19) C33 0.058(3) 0.061(3) 0.059(3) 0.011(2) -0.020(2) 0.013(2) C34 0.069(3) 0.031(2) 0.048(3) 0.0083(18) 0.001(2) -0.003(2) C35 0.076(3) 0.052(3) 0.072(3) 0.020(2) 0.023(3) 0.009(2) C36 0.096(4) 0.054(3) 0.052(3) 0.025(2) 0.030(3) 0.012(3) C37 0.092(4) 0.056(3) 0.043(3) 0.024(2) 0.009(2) 0.012(3) C38 0.062(3) 0.065(3) 0.050(3) 0.033(2) 0.005(2) 0.009(2) C39 0.070(3) 0.059(3) 0.069(3) 0.020(2) -0.015(2) -0.005(2) C40 0.137(5) 0.040(2) 0.070(3) 0.001(2) -0.005(3) -0.007(3) C41 0.100(4) 0.119(4) 0.087(4) 0.062(3) 0.041(3) 0.061(3) C42 0.088(4) 0.122(4) 0.078(4) 0.063(3) -0.022(3) -0.023(3) C43 0.043(2) 0.054(2) 0.043(2) 0.0197(19) 0.0045(19) 0.0022(19) C44 0.068(6) 0.112(7) 0.093(8) 0.076(7) 0.008(6) 0.016(5) C45 0.105(4) 0.074(3) 0.050(3) 0.035(2) 0.023(3) -0.001(3) C46 0.069(6) 0.087(6) 0.076(6) 0.044(5) 0.033(5) 0.018(5) C47 0.054(3) 0.061(3) 0.040(2) 0.017(2) 0.014(2) 0.002(2) C48 0.101(7) 0.052(4) 0.069(5) -0.004(4) -0.017(5) 0.019(5) C49 0.045(5) 0.107(7) 0.165(12) 0.047(7) 0.034(6) -0.003(5) C50 0.037(5) 0.134(9) 0.057(5) 0.034(6) 0.015(4) 0.015(5) C51 0.238(14) 0.067(6) 0.111(9) -0.027(6) 0.108(9) -0.007(8) Li1 0.046(4) 0.041(3) 0.036(3) 0.009(3) 0.007(3) -0.002(3) Li2 0.061(4) 0.033(3) 0.031(3) 0.002(3) 0.007(3) -0.004(3) _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 1.705(3) . ? Si1 C1 1.870(3) . ? Si1 C3 1.873(4) . ? Si1 C2 1.880(4) . ? Si1 Mg1 3.1947(14) . ? Si2 N1 1.697(3) . ? Si2 C6 1.863(3) . ? Si2 C4 1.878(4) . ? Si2 C5 1.888(4) . ? Si2 Mg1 3.2391(13) . ? Si3 N2 1.699(3) . ? Si3 C7 1.864(3) . ? Si3 C9 1.878(4) . ? Si3 C8 1.890(4) . ? Si3 Mg1 3.2246(15) . ? Si4 N2 1.695(3) . ? Si4 C12 1.870(4) . ? Si4 C10 1.887(4) . ? Si4 C11 1.888(4) . ? Si4 Mg1 3.2117(15) . ? Si5 N3 1.698(3) . ? Si5 C13 1.867(4) . ? Si5 C15 1.873(4) . ? Si5 C14 1.884(4) . ? Si5 Mg1 3.2125(13) . ? Si6 N3 1.704(3) . ? Si6 C18 1.866(4) . ? Si6 C16 1.882(4) . ? Si6 C17 1.884(5) . ? Si6 Mg1 3.2232(15) . ? Si7 N4 1.706(3) . ? Si7 C21A 1.773(13) . ? Si7 C20A 1.803(14) . ? Si7 C19 1.86(3) . ? Si7 C19A 1.89(5) . ? Si7 C21 1.934(7) . ? Si7 C20 1.937(8) . ? Si7 Li2 2.951(6) . ? Si7 Li1 3.042(6) . ? Si8 N4 1.707(3) . ? Si8 C24 1.865(4) . ? Si8 C23 1.870(4) . ? Si8 C22 1.873(4) . ? Si8 Li1 2.956(6) . ? Si8 Li2 3.137(6) . ? Mg1 N1 2.026(3) . ? Mg1 N3 2.030(3) . ? Mg1 N2 2.037(3) . ? O1 N5 1.301(3) . ? O1 Li2 1.957(6) . ? O1 Li1 1.982(6) . ? O2 N6 1.286(3) . ? O2 Li2 1.821(6) . ? O3 N7 1.282(3) . ? O3 Li1 1.812(6) . ? N4 Li2 1.951(6) . ? N4 Li1 1.993(6) . ? N5 C25 1.499(4) . ? N5 C29 1.501(4) . ? N6 C38 1.488(5) . ? N6 C34 1.497(5) . ? N7 C47 1.488(4) . ? N7 C43 1.496(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? 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 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? 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 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C30 1.509(5) . ? C25 C26 1.524(4) . ? C25 C31 1.530(5) . ? C26 C27 1.510(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.515(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.520(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C32 1.514(5) . ? C29 C33 1.529(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.520(5) . ? C34 C39 1.527(5) . ? C34 C40 1.537(5) . ? C35 C36 1.517(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.501(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.523(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C42 1.532(6) . ? C38 C41 1.537(6) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C49 1.448(8) . ? C43 C44 1.523(8) . ? C43 C48 1.558(7) . ? C44 C45 1.429(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.530(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.477(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C50 1.515(8) . ? C47 C51 1.577(9) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? Li1 Li2 2.610(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C1 110.72(14) . . ? N1 Si1 C3 114.29(16) . . ? C1 Si1 C3 105.18(18) . . ? N1 Si1 C2 114.05(17) . . ? C1 Si1 C2 107.35(18) . . ? C3 Si1 C2 104.6(2) . . ? N1 Si1 Mg1 34.22(8) . . ? C1 Si1 Mg1 77.04(11) . . ? C3 Si1 Mg1 131.63(14) . . ? C2 Si1 Mg1 121.14(15) . . ? N1 Si2 C6 111.39(14) . . ? N1 Si2 C4 113.85(16) . . ? C6 Si2 C4 105.86(18) . . ? N1 Si2 C5 113.73(16) . . ? C6 Si2 C5 105.94(18) . . ? C4 Si2 C5 105.4(2) . . ? N1 Si2 Mg1 32.54(9) . . ? C6 Si2 Mg1 78.98(11) . . ? C4 Si2 Mg1 128.59(14) . . ? C5 Si2 Mg1 122.72(15) . . ? N2 Si3 C7 111.58(15) . . ? N2 Si3 C9 113.75(16) . . ? C7 Si3 C9 106.21(18) . . ? N2 Si3 C8 113.15(15) . . ? C7 Si3 C8 106.23(17) . . ? C9 Si3 C8 105.3(2) . . ? N2 Si3 Mg1 33.52(9) . . ? C7 Si3 Mg1 79.05(11) . . ? C9 Si3 Mg1 133.81(14) . . ? C8 Si3 Mg1 117.34(14) . . ? N2 Si4 C12 111.39(16) . . ? N2 Si4 C10 114.35(15) . . ? C12 Si4 C10 105.81(19) . . ? N2 Si4 C11 114.38(16) . . ? C12 Si4 C11 105.55(18) . . ? C10 Si4 C11 104.55(18) . . ? N2 Si4 Mg1 33.89(9) . . ? C12 Si4 Mg1 77.70(13) . . ? C10 Si4 Mg1 130.04(12) . . ? C11 Si4 Mg1 122.83(13) . . ? N3 Si5 C13 111.78(15) . . ? N3 Si5 C15 114.18(17) . . ? C13 Si5 C15 106.0(2) . . ? N3 Si5 C14 113.50(16) . . ? C13 Si5 C14 105.61(18) . . ? C15 Si5 C14 105.09(18) . . ? N3 Si5 Mg1 33.65(9) . . ? C13 Si5 Mg1 78.74(12) . . ? C15 Si5 Mg1 132.66(13) . . ? C14 Si5 Mg1 119.17(13) . . ? N3 Si6 C18 110.66(16) . . ? N3 Si6 C16 113.63(19) . . ? C18 Si6 C16 105.6(2) . . ? N3 Si6 C17 114.04(19) . . ? C18 Si6 C17 106.6(2) . . ? C16 Si6 C17 105.8(2) . . ? N3 Si6 Mg1 33.41(9) . . ? C18 Si6 Mg1 78.03(12) . . ? C16 Si6 Mg1 132.03(18) . . ? C17 Si6 Mg1 119.20(17) . . ? N4 Si7 C21A 118.2(5) . . ? N4 Si7 C20A 119.0(5) . . ? C21A Si7 C20A 76.3(6) . . ? N4 Si7 C19 108.8(9) . . ? C21A Si7 C19 116.2(10) . . ? C20A Si7 C19 115.5(9) . . ? N4 Si7 C19A 111.1(13) . . ? C21A Si7 C19A 118.2(13) . . ? C20A Si7 C19A 109.9(14) . . ? C19 Si7 C19A 6(2) . . ? N4 Si7 C21 113.7(3) . . ? C21A Si7 C21 26.7(4) . . ? C20A Si7 C21 101.0(5) . . ? C19 Si7 C21 96.4(9) . . ? C19A Si7 C21 100.2(12) . . ? N4 Si7 C20 107.7(3) . . ? C21A Si7 C20 100.2(6) . . ? C20A Si7 C20 23.9(4) . . ? C19 Si7 C20 104.0(9) . . ? C19A Si7 C20 97.9(13) . . ? C21 Si7 C20 124.2(5) . . ? N4 Si7 Li2 39.10(14) . . ? C21A Si7 Li2 126.9(5) . . ? C20A Si7 Li2 151.6(4) . . ? C19 Si7 Li2 72.0(8) . . ? C19A Si7 Li2 75.7(13) . . ? C21 Si7 Li2 105.4(3) . . ? C20 Si7 Li2 130.1(3) . . ? N4 Si7 Li1 37.91(14) . . ? C21A Si7 Li1 150.4(5) . . ? C20A Si7 Li1 100.0(4) . . ? C19 Si7 Li1 92.1(9) . . ? C19A Si7 Li1 90.9(12) . . ? C21 Si7 Li1 151.3(3) . . ? C20 Si7 Li1 79.6(3) . . ? Li2 Si7 Li1 51.60(15) . . ? N4 Si8 C24 113.15(16) . . ? N4 Si8 C23 115.08(16) . . ? C24 Si8 C23 107.8(2) . . ? N4 Si8 C22 108.41(15) . . ? C24 Si8 C22 105.64(19) . . ? C23 Si8 C22 106.07(19) . . ? N4 Si8 Li1 40.46(14) . . ? C24 Si8 Li1 91.21(17) . . ? C23 Si8 Li1 154.97(18) . . ? C22 Si8 Li1 83.32(17) . . ? N4 Si8 Li2 33.31(14) . . ? C24 Si8 Li2 140.91(18) . . ? C23 Si8 Li2 107.05(18) . . ? C22 Si8 Li2 80.81(16) . . ? Li1 Si8 Li2 50.61(15) . . ? N1 Mg1 N3 120.92(12) . . ? N1 Mg1 N2 119.68(11) . . ? N3 Mg1 N2 119.40(11) . . ? N1 Mg1 Si1 28.26(7) . . ? N3 Mg1 Si1 101.30(9) . . ? N2 Mg1 Si1 133.82(8) . . ? N1 Mg1 Si4 132.88(9) . . ? N3 Mg1 Si4 101.30(9) . . ? N2 Mg1 Si4 27.65(7) . . ? Si1 Mg1 Si4 157.40(4) . . ? N1 Mg1 Si5 134.90(9) . . ? N3 Mg1 Si5 27.60(8) . . ? N2 Mg1 Si5 100.21(8) . . ? Si1 Mg1 Si5 107.89(4) . . ? Si4 Mg1 Si5 92.23(4) . . ? N1 Mg1 Si6 101.67(9) . . ? N3 Mg1 Si6 27.52(8) . . ? N2 Mg1 Si6 134.11(8) . . ? Si1 Mg1 Si6 92.04(4) . . ? Si4 Mg1 Si6 108.25(4) . . ? Si5 Mg1 Si6 55.12(3) . . ? N1 Mg1 Si3 100.67(8) . . ? N3 Mg1 Si3 133.42(9) . . ? N2 Mg1 Si3 27.43(7) . . ? Si1 Mg1 Si3 107.56(4) . . ? Si4 Mg1 Si3 55.06(3) . . ? Si5 Mg1 Si3 107.11(4) . . ? Si6 Mg1 Si3 157.65(4) . . ? N1 Mg1 Si2 26.79(7) . . ? N3 Mg1 Si2 133.89(9) . . ? N2 Mg1 Si2 102.00(8) . . ? Si1 Mg1 Si2 55.04(3) . . ? Si4 Mg1 Si2 107.64(4) . . ? Si5 Mg1 Si2 157.79(5) . . ? Si6 Mg1 Si2 107.62(4) . . ? Si3 Mg1 Si2 92.70(4) . . ? N5 O1 Li2 142.5(2) . . ? N5 O1 Li1 134.1(2) . . ? Li2 O1 Li1 83.0(2) . . ? N6 O2 Li2 155.7(3) . . ? N7 O3 Li1 163.6(3) . . ? Si2 N1 Si1 121.78(15) . . ? Si2 N1 Mg1 120.67(14) . . ? Si1 N1 Mg1 117.52(13) . . ? Si4 N2 Si3 122.42(16) . . ? Si4 N2 Mg1 118.47(14) . . ? Si3 N2 Mg1 119.06(14) . . ? Si5 N3 Si6 122.17(16) . . ? Si5 N3 Mg1 118.75(15) . . ? Si6 N3 Mg1 119.07(14) . . ? Si7 N4 Si8 124.33(14) . . ? Si7 N4 Li2 107.4(2) . . ? Si8 N4 Li2 118.0(2) . . ? Si7 N4 Li1 110.4(2) . . ? Si8 N4 Li1 105.8(2) . . ? Li2 N4 Li1 82.8(2) . . ? O1 N5 C25 116.8(2) . . ? O1 N5 C29 116.5(2) . . ? C25 N5 C29 124.5(2) . . ? O2 N6 C38 115.4(3) . . ? O2 N6 C34 116.4(3) . . ? C38 N6 C34 125.3(3) . . ? O3 N7 C47 116.3(3) . . ? O3 N7 C43 116.8(3) . . ? C47 N7 C43 126.9(3) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si4 C10 H10A 109.5 . . ? Si4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si4 C11 H11A 109.5 . . ? Si4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si4 C12 H12A 109.5 . . ? Si4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si5 C13 H13A 109.5 . . ? Si5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si5 C14 H14A 109.5 . . ? Si5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si5 C15 H15A 109.5 . . ? Si5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si6 C16 H16A 109.5 . . ? Si6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si6 C17 H17A 109.5 . . ? Si6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si6 C18 H18A 109.5 . . ? Si6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si7 C19 H19A 109.5 . . ? Si7 C19 H19B 109.5 . . ? Si7 C19 H19C 109.5 . . ? Si7 C20 H20A 109.5 . . ? Si7 C20 H20B 109.5 . . ? Si7 C20 H20C 109.5 . . ? Si7 C21 H21A 109.5 . . ? Si7 C21 H21B 109.5 . . ? Si7 C21 H21C 109.5 . . ? Si7 C19A H19D 109.5 . . ? Si7 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? Si7 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? Si7 C20A H20D 109.5 . . ? Si7 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? Si7 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? Si7 C21A H21D 109.5 . . ? Si7 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? Si7 C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? Si8 C22 H22A 109.5 . . ? Si8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si8 C23 H23A 109.5 . . ? Si8 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si8 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si8 C24 H24A 109.5 . . ? Si8 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si8 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 C30 108.5(3) . . ? N5 C25 C26 108.4(3) . . ? C30 C25 C26 110.5(3) . . ? N5 C25 C31 108.3(3) . . ? C30 C25 C31 109.4(3) . . ? C26 C25 C31 111.6(3) . . ? C27 C26 C25 114.3(3) . . ? C27 C26 H26A 108.7 . . ? C25 C26 H26A 108.7 . . ? C27 C26 H26B 108.7 . . ? C25 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C26 C27 C28 108.3(3) . . ? C26 C27 H27A 110.0 . . ? C28 C27 H27A 110.0 . . ? C26 C27 H27B 110.0 . . ? C28 C27 H27B 110.0 . . ? H27A C27 H27B 108.4 . . ? C27 C28 C29 114.3(3) . . ? C27 C28 H28A 108.7 . . ? C29 C28 H28A 108.7 . . ? C27 C28 H28B 108.7 . . ? C29 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? N5 C29 C32 108.3(3) . . ? N5 C29 C28 108.9(3) . . ? C32 C29 C28 109.8(3) . . ? N5 C29 C33 108.4(3) . . ? C32 C29 C33 109.1(3) . . ? C28 C29 C33 112.2(3) . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 C31 H31A 109.5 . . ? C25 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C25 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N6 C34 C35 109.0(3) . . ? N6 C34 C39 107.7(3) . . ? C35 C34 C39 109.9(3) . . ? N6 C34 C40 108.3(3) . . ? C35 C34 C40 112.1(3) . . ? C39 C34 C40 109.7(3) . . ? C36 C35 C34 114.2(4) . . ? C36 C35 H35A 108.7 . . ? C34 C35 H35A 108.7 . . ? C36 C35 H35B 108.7 . . ? C34 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C37 C36 C35 108.5(3) . . ? C37 C36 H36A 110.0 . . ? C35 C36 H36A 110.0 . . ? C37 C36 H36B 110.0 . . ? C35 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? C36 C37 C38 113.1(3) . . ? C36 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? C36 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? N6 C38 C37 109.6(3) . . ? N6 C38 C42 107.4(3) . . ? C37 C38 C42 109.3(4) . . ? N6 C38 C41 108.5(3) . . ? C37 C38 C41 111.6(3) . . ? C42 C38 C41 110.4(4) . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C40 H40A 109.5 . . ? C34 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C34 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C49 C43 N7 112.9(4) . . ? C49 C43 C44 109.8(6) . . ? N7 C43 C44 110.7(4) . . ? C49 C43 C48 112.8(6) . . ? N7 C43 C48 102.4(4) . . ? C44 C43 C48 107.9(6) . . ? C45 C44 C43 118.8(6) . . ? C45 C44 H44A 107.6 . . ? C43 C44 H44A 107.6 . . ? C45 C44 H44B 107.6 . . ? C43 C44 H44B 107.6 . . ? H44A C44 H44B 107.0 . . ? C44 C45 C46 114.3(6) . . ? C44 C45 H45A 108.7 . . ? C46 C45 H45A 108.7 . . ? C44 C45 H45B 108.7 . . ? C46 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? C47 C46 C45 113.2(6) . . ? C47 C46 H46A 108.9 . . ? C45 C46 H46A 108.9 . . ? C47 C46 H46B 108.9 . . ? C45 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? C46 C47 N7 114.5(4) . . ? C46 C47 C50 114.1(5) . . ? N7 C47 C50 106.4(4) . . ? C46 C47 C51 107.0(6) . . ? N7 C47 C51 108.0(4) . . ? C50 C47 C51 106.5(7) . . ? O3 Li1 O1 126.3(3) . . ? O3 Li1 N4 137.1(3) . . ? O1 Li1 N4 96.0(3) . . ? O3 Li1 Li2 172.1(3) . . ? O1 Li1 Li2 48.10(18) . . ? N4 Li1 Li2 47.88(18) . . ? O3 Li1 Si8 112.9(3) . . ? O1 Li1 Si8 109.4(2) . . ? N4 Li1 Si8 33.76(12) . . ? Li2 Li1 Si8 68.30(18) . . ? O3 Li1 Si7 125.3(3) . . ? O1 Li1 Si7 103.8(2) . . ? N4 Li1 Si7 31.72(12) . . ? Li2 Li1 Si7 62.41(17) . . ? Si8 Li1 Si7 60.40(11) . . ? O2 Li2 N4 142.9(3) . . ? O2 Li2 O1 117.2(3) . . ? N4 Li2 O1 98.2(3) . . ? O2 Li2 Li1 162.8(3) . . ? N4 Li2 Li1 49.28(19) . . ? O1 Li2 Li1 48.92(18) . . ? O2 Li2 Si7 117.7(3) . . ? N4 Li2 Si7 33.46(12) . . ? O1 Li2 Si7 107.8(2) . . ? Li1 Li2 Si7 65.99(18) . . ? O2 Li2 Si8 135.9(3) . . ? N4 Li2 Si8 28.72(12) . . ? O1 Li2 Si8 103.6(2) . . ? Li1 Li2 Si8 61.10(17) . . ? Si7 Li2 Si8 59.33(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Si2 N1 Si1 172.59(18) . . . . ? C4 Si2 N1 Si1 53.0(2) . . . . ? C5 Si2 N1 Si1 -67.8(2) . . . . ? C6 Si2 N1 Mg1 -5.5(2) . . . . ? C4 Si2 N1 Mg1 -125.1(2) . . . . ? C5 Si2 N1 Mg1 114.14(19) . . . . ? C1 Si1 N1 Si2 171.19(18) . . . . ? C3 Si1 N1 Si2 52.6(2) . . . . ? C2 Si1 N1 Si2 -67.6(2) . . . . ? C1 Si1 N1 Mg1 -10.7(2) . . . . ? C3 Si1 N1 Mg1 -129.22(19) . . . . ? C2 Si1 N1 Mg1 110.5(2) . . . . ? N3 Mg1 N1 Si2 127.35(16) . . . . ? N2 Mg1 N1 Si2 -53.3(2) . . . . ? Si1 Mg1 N1 Si2 178.2(3) . . . . ? Si4 Mg1 N1 Si2 -22.8(2) . . . . ? Si5 Mg1 N1 Si2 157.86(10) . . . . ? Si6 Mg1 N1 Si2 106.07(15) . . . . ? Si3 Mg1 N1 Si2 -74.51(16) . . . . ? N3 Mg1 N1 Si1 -50.8(2) . . . . ? N2 Mg1 N1 Si1 128.55(15) . . . . ? C12 Si4 N2 Si3 170.86(18) . . . . ? C10 Si4 N2 Si3 51.0(2) . . . . ? C11 Si4 N2 Si3 -69.6(2) . . . . ? C12 Si4 N2 Mg1 -6.5(2) . . . . ? C10 Si4 N2 Mg1 -126.35(19) . . . . ? C11 Si4 N2 Mg1 113.12(18) . . . . ? C7 Si3 N2 Si4 167.96(17) . . . . ? C9 Si3 N2 Si4 47.8(2) . . . . ? C8 Si3 N2 Si4 -72.3(2) . . . . ? Mg1 Si3 N2 Si4 -177.3(3) . . . . ? C7 Si3 N2 Mg1 -14.7(2) . . . . ? C9 Si3 N2 Mg1 -134.86(19) . . . . ? C8 Si3 N2 Mg1 105.0(2) . . . . ? N1 Mg1 N2 Si4 126.86(15) . . . . ? N3 Mg1 N2 Si4 -53.77(19) . . . . ? N1 Mg1 N2 Si3 -50.6(2) . . . . ? N3 Mg1 N2 Si3 128.82(15) . . . . ? C13 Si5 N3 Si6 167.8(2) . . . . ? C15 Si5 N3 Si6 47.5(3) . . . . ? C14 Si5 N3 Si6 -72.9(2) . . . . ? Mg1 Si5 N3 Si6 179.3(3) . . . . ? C13 Si5 N3 Mg1 -11.5(2) . . . . ? C15 Si5 N3 Mg1 -131.77(19) . . . . ? C14 Si5 N3 Mg1 107.81(19) . . . . ? C18 Si6 N3 Si5 167.6(2) . . . . ? C16 Si6 N3 Si5 49.1(3) . . . . ? C17 Si6 N3 Si5 -72.2(3) . . . . ? Mg1 Si6 N3 Si5 -179.3(3) . . . . ? C18 Si6 N3 Mg1 -13.0(3) . . . . ? C16 Si6 N3 Mg1 -131.6(2) . . . . ? C17 Si6 N3 Mg1 107.1(2) . . . . ? N1 Mg1 N3 Si5 129.06(16) . . . . ? N2 Mg1 N3 Si5 -50.3(2) . . . . ? Si1 Mg1 N3 Si5 107.09(16) . . . . ? Si4 Mg1 N3 Si5 -72.75(17) . . . . ? Si6 Mg1 N3 Si5 179.3(3) . . . . ? Si3 Mg1 N3 Si5 -20.7(2) . . . . ? Si2 Mg1 N3 Si5 158.87(11) . . . . ? N1 Mg1 N3 Si6 -50.3(2) . . . . ? N2 Mg1 N3 Si6 130.36(17) . . . . ? Si1 Mg1 N3 Si6 -72.25(17) . . . . ? Si4 Mg1 N3 Si6 107.92(16) . . . . ? Si5 Mg1 N3 Si6 -179.3(3) . . . . ? Si3 Mg1 N3 Si6 159.97(11) . . . . ? Si2 Mg1 N3 Si6 -20.5(2) . . . . ? C21A Si7 N4 Si8 29.3(6) . . . . ? C20A Si7 N4 Si8 -60.1(5) . . . . ? C19 Si7 N4 Si8 164.8(9) . . . . ? C19A Si7 N4 Si8 170.8(13) . . . . ? C21 Si7 N4 Si8 58.7(4) . . . . ? C20 Si7 N4 Si8 -83.1(4) . . . . ? Li2 Si7 N4 Si8 144.1(3) . . . . ? Li1 Si7 N4 Si8 -127.2(3) . . . . ? C21A Si7 N4 Li2 -114.8(5) . . . . ? C20A Si7 N4 Li2 155.8(5) . . . . ? C19 Si7 N4 Li2 20.7(9) . . . . ? C19A Si7 N4 Li2 26.7(13) . . . . ? C21 Si7 N4 Li2 -85.4(4) . . . . ? C20 Si7 N4 Li2 132.8(4) . . . . ? Li1 Si7 N4 Li2 88.7(3) . . . . ? C21A Si7 N4 Li1 156.5(5) . . . . ? C20A Si7 N4 Li1 67.1(5) . . . . ? C19 Si7 N4 Li1 -68.0(9) . . . . ? C19A Si7 N4 Li1 -62.0(13) . . . . ? C21 Si7 N4 Li1 -174.1(4) . . . . ? C20 Si7 N4 Li1 44.1(4) . . . . ? Li2 Si7 N4 Li1 -88.7(3) . . . . ? C24 Si8 N4 Si7 66.9(2) . . . . ? C23 Si8 N4 Si7 -57.7(3) . . . . ? C22 Si8 N4 Si7 -176.3(2) . . . . ? Li1 Si8 N4 Si7 129.1(3) . . . . ? Li2 Si8 N4 Si7 -140.7(3) . . . . ? C24 Si8 N4 Li2 -152.4(3) . . . . ? C23 Si8 N4 Li2 83.0(3) . . . . ? C22 Si8 N4 Li2 -35.6(3) . . . . ? Li1 Si8 N4 Li2 -90.2(3) . . . . ? C24 Si8 N4 Li1 -62.2(3) . . . . ? C23 Si8 N4 Li1 173.2(2) . . . . ? C22 Si8 N4 Li1 54.6(3) . . . . ? Li2 Si8 N4 Li1 90.2(3) . . . . ? Li2 O1 N5 C25 63.3(5) . . . . ? Li1 O1 N5 C25 -127.0(4) . . . . ? Li2 O1 N5 C29 -101.0(4) . . . . ? Li1 O1 N5 C29 68.8(4) . . . . ? Li2 O2 N6 C38 -159.3(6) . . . . ? Li2 O2 N6 C34 2.4(8) . . . . ? Li1 O3 N7 C47 -142.0(10) . . . . ? Li1 O3 N7 C43 38.6(12) . . . . ? O1 N5 C25 C30 39.3(4) . . . . ? C29 N5 C25 C30 -157.8(3) . . . . ? O1 N5 C25 C26 159.4(3) . . . . ? C29 N5 C25 C26 -37.7(4) . . . . ? O1 N5 C25 C31 -79.3(3) . . . . ? C29 N5 C25 C31 83.6(4) . . . . ? N5 C25 C26 C27 47.7(4) . . . . ? C30 C25 C26 C27 166.5(3) . . . . ? C31 C25 C26 C27 -71.6(4) . . . . ? C25 C26 C27 C28 -60.4(4) . . . . ? C26 C27 C28 C29 59.6(4) . . . . ? O1 N5 C29 C32 -40.5(4) . . . . ? C25 N5 C29 C32 156.6(3) . . . . ? O1 N5 C29 C28 -159.8(3) . . . . ? C25 N5 C29 C28 37.2(4) . . . . ? O1 N5 C29 C33 77.8(3) . . . . ? C25 N5 C29 C33 -85.1(4) . . . . ? C27 C28 C29 N5 -46.4(4) . . . . ? C27 C28 C29 C32 -164.8(3) . . . . ? C27 C28 C29 C33 73.7(4) . . . . ? O2 N6 C34 C35 167.1(3) . . . . ? C38 N6 C34 C35 -33.1(4) . . . . ? O2 N6 C34 C39 47.9(4) . . . . ? C38 N6 C34 C39 -152.4(3) . . . . ? O2 N6 C34 C40 -70.7(4) . . . . ? C38 N6 C34 C40 89.1(4) . . . . ? N6 C34 C35 C36 44.4(4) . . . . ? C39 C34 C35 C36 162.3(3) . . . . ? C40 C34 C35 C36 -75.5(5) . . . . ? C34 C35 C36 C37 -60.6(4) . . . . ? C35 C36 C37 C38 61.4(4) . . . . ? O2 N6 C38 C37 -165.6(3) . . . . ? C34 N6 C38 C37 34.4(5) . . . . ? O2 N6 C38 C42 -47.1(4) . . . . ? C34 N6 C38 C42 153.0(3) . . . . ? O2 N6 C38 C41 72.3(4) . . . . ? C34 N6 C38 C41 -87.7(4) . . . . ? C36 C37 C38 N6 -46.9(4) . . . . ? C36 C37 C38 C42 -164.3(3) . . . . ? C36 C37 C38 C41 73.4(5) . . . . ? O3 N7 C43 C49 47.2(7) . . . . ? C47 N7 C43 C49 -132.1(6) . . . . ? O3 N7 C43 C44 170.8(5) . . . . ? C47 N7 C43 C44 -8.5(7) . . . . ? O3 N7 C43 C48 -74.3(5) . . . . ? C47 N7 C43 C48 106.4(5) . . . . ? C49 C43 C44 C45 151.8(9) . . . . ? N7 C43 C44 C45 26.4(10) . . . . ? C48 C43 C44 C45 -84.9(10) . . . . ? C43 C44 C45 C46 -49.3(12) . . . . ? C44 C45 C46 C47 52.0(10) . . . . ? C45 C46 C47 N7 -33.1(8) . . . . ? C45 C46 C47 C50 89.8(8) . . . . ? C45 C46 C47 C51 -152.7(8) . . . . ? O3 N7 C47 C46 -165.7(5) . . . . ? C43 N7 C47 C46 13.6(6) . . . . ? O3 N7 C47 C50 67.3(5) . . . . ? C43 N7 C47 C50 -113.4(5) . . . . ? O3 N7 C47 C51 -46.7(7) . . . . ? C43 N7 C47 C51 132.6(7) . . . . ? N7 O3 Li1 O1 15.5(13) . . . . ? N7 O3 Li1 N4 -152.9(8) . . . . ? N7 O3 Li1 Li2 -27(3) . . . . ? N7 O3 Li1 Si8 -123.6(10) . . . . ? N7 O3 Li1 Si7 167.4(9) . . . . ? N5 O1 Li1 O3 13.4(6) . . . . ? Li2 O1 Li1 O3 -172.9(4) . . . . ? N5 O1 Li1 N4 -174.5(2) . . . . ? Li2 O1 Li1 N4 -0.7(3) . . . . ? N5 O1 Li1 Li2 -173.7(4) . . . . ? N5 O1 Li1 Si8 153.7(2) . . . . ? Li2 O1 Li1 Si8 -32.6(3) . . . . ? N5 O1 Li1 Si7 -143.2(3) . . . . ? Li2 O1 Li1 Si7 30.5(2) . . . . ? Si7 N4 Li1 O3 -82.6(5) . . . . ? Si8 N4 Li1 O3 54.3(5) . . . . ? Li2 N4 Li1 O3 171.4(5) . . . . ? Si7 N4 Li1 O1 106.7(2) . . . . ? Si8 N4 Li1 O1 -116.4(2) . . . . ? Li2 N4 Li1 O1 0.7(3) . . . . ? Si7 N4 Li1 Li2 106.0(2) . . . . ? Si8 N4 Li1 Li2 -117.1(2) . . . . ? Si7 N4 Li1 Si8 -136.9(2) . . . . ? Li2 N4 Li1 Si8 117.1(2) . . . . ? Si8 N4 Li1 Si7 136.9(2) . . . . ? Li2 N4 Li1 Si7 -106.0(2) . . . . ? N4 Si8 Li1 O3 -143.2(4) . . . . ? C24 Si8 Li1 O3 -17.6(3) . . . . ? C23 Si8 Li1 O3 -157.9(4) . . . . ? C22 Si8 Li1 O3 88.0(3) . . . . ? Li2 Si8 Li1 O3 171.5(4) . . . . ? N4 Si8 Li1 O1 70.9(3) . . . . ? C24 Si8 Li1 O1 -163.6(3) . . . . ? C23 Si8 Li1 O1 56.1(5) . . . . ? C22 Si8 Li1 O1 -58.0(3) . . . . ? Li2 Si8 Li1 O1 25.6(2) . . . . ? C24 Si8 Li1 N4 125.5(2) . . . . ? C23 Si8 Li1 N4 -14.8(5) . . . . ? C22 Si8 Li1 N4 -128.9(2) . . . . ? Li2 Si8 Li1 N4 -45.3(2) . . . . ? N4 Si8 Li1 Li2 45.3(2) . . . . ? C24 Si8 Li1 Li2 170.8(2) . . . . ? C23 Si8 Li1 Li2 30.5(5) . . . . ? C22 Si8 Li1 Li2 -83.6(2) . . . . ? N4 Si8 Li1 Si7 -24.40(15) . . . . ? C24 Si8 Li1 Si7 101.14(15) . . . . ? C23 Si8 Li1 Si7 -39.2(4) . . . . ? C22 Si8 Li1 Si7 -153.25(15) . . . . ? Li2 Si8 Li1 Si7 -69.69(17) . . . . ? N4 Si7 Li1 O3 124.3(4) . . . . ? C21A Si7 Li1 O3 79.0(10) . . . . ? C20A Si7 Li1 O3 -0.8(6) . . . . ? C19 Si7 Li1 O3 -117.2(9) . . . . ? C19A Si7 Li1 O3 -111.2(13) . . . . ? C21 Si7 Li1 O3 135.5(7) . . . . ? C20 Si7 Li1 O3 -13.3(4) . . . . ? Li2 Si7 Li1 O3 177.8(4) . . . . ? N4 Si7 Li1 O1 -78.8(3) . . . . ? C21A Si7 Li1 O1 -124.1(9) . . . . ? C20A Si7 Li1 O1 156.1(5) . . . . ? C19 Si7 Li1 O1 39.8(8) . . . . ? C19A Si7 Li1 O1 45.7(13) . . . . ? C21 Si7 Li1 O1 -67.5(7) . . . . ? C20 Si7 Li1 O1 143.6(4) . . . . ? Li2 Si7 Li1 O1 -25.2(2) . . . . ? C21A Si7 Li1 N4 -45.3(10) . . . . ? C20A Si7 Li1 N4 -125.1(5) . . . . ? C19 Si7 Li1 N4 118.6(8) . . . . ? C19A Si7 Li1 N4 124.5(13) . . . . ? C21 Si7 Li1 N4 11.3(7) . . . . ? C20 Si7 Li1 N4 -137.6(3) . . . . ? Li2 Si7 Li1 N4 53.6(2) . . . . ? N6 O2 Li2 N4 65.4(10) . . . . ? N6 O2 Li2 O1 -133.7(6) . . . . ? N6 O2 Li2 Li1 -166.5(9) . . . . ? N6 O2 Li2 Si7 95.2(7) . . . . ? N6 O2 Li2 Si8 21.8(9) . . . . ? Si7 N4 Li2 O2 53.0(7) . . . . ? Si8 N4 Li2 O2 -93.7(6) . . . . ? Li1 N4 Li2 O2 162.2(6) . . . . ? Si7 N4 Li2 O1 -109.9(2) . . . . ? Si8 N4 Li2 O1 103.3(3) . . . . ? Li1 N4 Li2 O1 -0.8(3) . . . . ? Si7 N4 Li2 Li1 -109.2(2) . . . . ? Si8 N4 Li2 Li1 104.1(3) . . . . ? Si8 N4 Li2 Si7 -146.7(3) . . . . ? Li1 N4 Li2 Si7 109.2(2) . . . . ? Si7 N4 Li2 Si8 146.7(3) . . . . ? Li1 N4 Li2 Si8 -104.1(3) . . . . ? N5 O1 Li2 O2 4.8(6) . . . . ? Li1 O1 Li2 O2 -167.8(4) . . . . ? N5 O1 Li2 N4 173.4(3) . . . . ? Li1 O1 Li2 N4 0.8(3) . . . . ? N5 O1 Li2 Li1 172.6(4) . . . . ? N5 O1 Li2 Si7 140.4(3) . . . . ? Li1 O1 Li2 Si7 -32.2(2) . . . . ? N5 O1 Li2 Si8 -157.9(3) . . . . ? Li1 O1 Li2 Si8 29.5(2) . . . . ? _refine_diff_density_max 0.321 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.051 #--------------------------------------------------------------------------- #------------------------------COMPOUND 4--------------------------------- #----------------------------------------------------------------------- data_temp _database_code_CSD 160885 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H72 N4 Na2 O2 Si4' _chemical_formula_weight 679.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 13.152(3) _cell_length_b 14.690(3) _cell_length_c 22.634(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.432(17) _cell_angle_gamma 90.00 _cell_volume 4371.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 13.64 _cell_measurement_theta_max 16.91 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.183 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method '\w/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.50 _diffrn_reflns_number 8969 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0934 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 26.04 _reflns_number_total 8584 _reflns_number_gt 5956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/Rigaku Diff control' _computing_cell_refinement ' " ' _computing_data_reduction 'texsan' _computing_structure_solution 'SIR' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+1.3990P] 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 8584 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1061 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1692 _refine_ls_wR_factor_gt 0.1529 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.33290(6) 0.22307(6) 0.18844(4) 0.0273(2) Uani 1 d . . . Si2 Si 0.30486(7) 0.01952(7) 0.17744(4) 0.0332(2) Uani 1 d . . . Si3 Si 0.11783(6) 0.04104(6) 0.38387(4) 0.0264(2) Uani 1 d . . . Si4 Si 0.07006(6) 0.23580(6) 0.35456(4) 0.0255(2) Uani 1 d . . . Na1 Na 0.30105(8) 0.13251(8) 0.31468(5) 0.0262(3) Uani 1 d . A 1 Na2 Na 0.11103(8) 0.11810(9) 0.23679(5) 0.0280(3) Uani 1 d . A 1 O1 O 0.43578(17) 0.1409(2) 0.37373(10) 0.0481(7) Uani 1 d . . . O2 O -0.02821(17) 0.11005(18) 0.18076(10) 0.0422(6) Uani 1 d . . . N1 N 0.51266(18) 0.13831(18) 0.40893(10) 0.0274(6) Uani 1 d . . . N2 N -0.10026(18) 0.10196(18) 0.14225(10) 0.0248(5) Uani 1 d . . . N3 N 0.28602(17) 0.12141(17) 0.20917(10) 0.0245(5) Uani 1 d . . . N4 N 0.12750(18) 0.13561(17) 0.34236(10) 0.0233(5) Uani 1 d . . . C1 C 0.5030(2) 0.1917(2) 0.46470(13) 0.0316(7) Uani 1 d . . . C2 C 0.5894(3) 0.1659(3) 0.50800(13) 0.0413(9) Uani 1 d . . . H2A H 0.5923 0.2107 0.5406 0.050 Uiso 1 calc R . . H2B H 0.5747 0.1055 0.5253 0.050 Uiso 1 calc R . . C3 C 0.6921(2) 0.1624(3) 0.47915(14) 0.0416(9) Uani 1 d . . . H3A H 0.7082 0.2227 0.4622 0.050 Uiso 1 calc R . . H3B H 0.7456 0.1471 0.5091 0.050 Uiso 1 calc R . . C4 C 0.6897(2) 0.0916(2) 0.43115(14) 0.0356(8) Uani 1 d . . . H4A H 0.6755 0.0315 0.4489 0.043 Uiso 1 calc R . . H4B H 0.7577 0.0884 0.4134 0.043 Uiso 1 calc R . . C5 C 0.6108(2) 0.1103(2) 0.38260(13) 0.0296(7) Uani 1 d . . . C6 C 0.4009(3) 0.1665(3) 0.49111(17) 0.0522(11) Uani 1 d . . . H6A H 0.3455 0.1842 0.4636 0.078 Uiso 1 calc R . . H6B H 0.3932 0.1985 0.5287 0.078 Uiso 1 calc R . . H6C H 0.3984 0.1006 0.4979 0.078 Uiso 1 calc R . . C7 C 0.5045(3) 0.2934(3) 0.45005(19) 0.0503(10) Uani 1 d . . . H7A H 0.5730 0.3111 0.4386 0.075 Uiso 1 calc R . . H7B H 0.4850 0.3284 0.4848 0.075 Uiso 1 calc R . . H7C H 0.4563 0.3057 0.4173 0.075 Uiso 1 calc R . . C8 C 0.5912(3) 0.0233(3) 0.34717(18) 0.0566(11) Uani 1 d . . . H8A H 0.5602 -0.0225 0.3726 0.085 Uiso 1 calc R . . H8B H 0.6557 -0.0001 0.3326 0.085 Uiso 1 calc R . . H8C H 0.5450 0.0366 0.3136 0.085 Uiso 1 calc R . . C9 C 0.6455(3) 0.1870(3) 0.34146(14) 0.0401(9) Uani 1 d . . . H9A H 0.5903 0.2019 0.3132 0.060 Uiso 1 calc R . . H9B H 0.7052 0.1669 0.3199 0.060 Uiso 1 calc R . . H9C H 0.6630 0.2410 0.3650 0.060 Uiso 1 calc R . . C10 C -0.2054(2) 0.1007(2) 0.16565(13) 0.0292(7) Uani 1 d . . . C11 C -0.2795(2) 0.0683(3) 0.11757(15) 0.0378(8) Uani 1 d . . . H11A H -0.2719 0.0017 0.1128 0.045 Uiso 1 calc R . . H11B H -0.3497 0.0803 0.1302 0.045 Uiso 1 calc R . . C12 C -0.2641(3) 0.1137(3) 0.05827(14) 0.0417(9) Uani 1 d . . . H12A H -0.3149 0.0906 0.0290 0.050 Uiso 1 calc R . . H12B H -0.2734 0.1803 0.0620 0.050 Uiso 1 calc R . . C13 C -0.1580(3) 0.0932(2) 0.03786(13) 0.0358(8) Uani 1 d . . . H13A H -0.1490 0.1214 -0.0014 0.043 Uiso 1 calc R . . H13B H -0.1506 0.0265 0.0332 0.043 Uiso 1 calc R . . C14 C -0.0744(2) 0.1276(2) 0.08001(12) 0.0291(7) Uani 1 d . . . C15 C -0.2052(3) 0.0351(3) 0.21759(16) 0.0495(10) Uani 1 d . . . H15A H -0.1799 -0.0244 0.2049 0.074 Uiso 1 calc R . . H15B H -0.2746 0.0284 0.2318 0.074 Uiso 1 calc R . . H15C H -0.1610 0.0588 0.2495 0.074 Uiso 1 calc R . . C16 C -0.2314(2) 0.1975(2) 0.18692(14) 0.0355(8) Uani 1 d . . . H16A H -0.1781 0.2188 0.2147 0.053 Uiso 1 calc R . . H16B H -0.2968 0.1966 0.2067 0.053 Uiso 1 calc R . . H16C H -0.2357 0.2388 0.1529 0.053 Uiso 1 calc R . . C17 C 0.0263(3) 0.0814(3) 0.06624(15) 0.0421(9) Uani 1 d . . . H17A H 0.0804 0.1066 0.0919 0.063 Uiso 1 calc R . . H17B H 0.0425 0.0923 0.0248 0.063 Uiso 1 calc R . . H17C H 0.0205 0.0158 0.0732 0.063 Uiso 1 calc R . . C18 C -0.0605(3) 0.2310(2) 0.07662(17) 0.0474(9) Uani 1 d . . . H18A H -0.1268 0.2609 0.0793 0.071 Uiso 1 calc R . . H18B H -0.0297 0.2470 0.0390 0.071 Uiso 1 calc R . . H18C H -0.0160 0.2513 0.1094 0.071 Uiso 1 calc R . . C19 C 0.3506(3) 0.3000(2) 0.25445(15) 0.0362(8) Uani 1 d . A 2 H19A H 0.2866 0.3043 0.2755 0.054 Uiso 1 calc R A 2 H19B H 0.3709 0.3608 0.2412 0.054 Uiso 1 calc R A 2 H19C H 0.4037 0.2751 0.2810 0.054 Uiso 1 calc R A 2 C20 C 0.4631(3) 0.2196(3) 0.15545(16) 0.0480(10) Uani 1 d . A 2 H20A H 0.5095 0.1853 0.1816 0.072 Uiso 1 calc R A 2 H20B H 0.4886 0.2818 0.1509 0.072 Uiso 1 calc R A 2 H20C H 0.4587 0.1898 0.1167 0.072 Uiso 1 calc R A 2 C21 C 0.2464(3) 0.2851(3) 0.13443(15) 0.0401(8) Uani 1 d . A 2 H21A H 0.2338 0.2468 0.0996 0.060 Uiso 1 calc R A 2 H21B H 0.2788 0.3421 0.1225 0.060 Uiso 1 calc R A 2 H21C H 0.1818 0.2987 0.1532 0.060 Uiso 1 calc R A 2 C22 C 0.4194(3) -0.0428(3) 0.20857(18) 0.0537(11) Uani 1 d . A 2 H22A H 0.4808 -0.0069 0.2017 0.081 Uiso 1 calc R A 2 H22B H 0.4251 -0.1021 0.1891 0.081 Uiso 1 calc R A 2 H22C H 0.4119 -0.0518 0.2511 0.081 Uiso 1 calc R A 2 C23 C 0.1925(3) -0.0580(3) 0.19038(17) 0.0478(10) Uani 1 d . A 2 H23A H 0.1771 -0.0582 0.2325 0.072 Uiso 1 calc R A 2 H23B H 0.2091 -0.1200 0.1778 0.072 Uiso 1 calc R A 2 H23C H 0.1332 -0.0360 0.1675 0.072 Uiso 1 calc R A 2 C24 C 0.3197(3) 0.0206(3) 0.09487(15) 0.0573(12) Uani 1 d . A 2 H24A H 0.2688 0.0613 0.0768 0.086 Uiso 1 calc R A 2 H24B H 0.3099 -0.0412 0.0793 0.086 Uiso 1 calc R A 2 H24C H 0.3880 0.0420 0.0856 0.086 Uiso 1 calc R A 2 C25 C 0.1178(3) 0.0599(3) 0.46631(14) 0.0400(8) Uani 1 d . A 2 H25A H 0.1780 0.0951 0.4784 0.060 Uiso 1 calc R A 2 H25B H 0.1190 0.0009 0.4866 0.060 Uiso 1 calc R A 2 H25C H 0.0563 0.0933 0.4768 0.060 Uiso 1 calc R A 2 C26 C 0.0012(3) -0.0280(2) 0.36494(16) 0.0428(9) Uani 1 d . A 2 H26A H -0.0592 0.0108 0.3670 0.064 Uiso 1 calc R A 2 H26B H -0.0044 -0.0783 0.3931 0.064 Uiso 1 calc R A 2 H26C H 0.0064 -0.0524 0.3249 0.064 Uiso 1 calc R A 2 C27 C 0.2320(3) -0.0345(2) 0.37235(15) 0.0383(8) Uani 1 d . A 2 H27A H 0.2415 -0.0432 0.3299 0.058 Uiso 1 calc R A 2 H27B H 0.2209 -0.0936 0.3911 0.058 Uiso 1 calc R A 2 H27C H 0.2927 -0.0058 0.3900 0.058 Uiso 1 calc R A 2 C28 C 0.1461(3) 0.3137(2) 0.40415(16) 0.0426(9) Uani 1 d . A 2 H28A H 0.1524 0.2868 0.4437 0.064 Uiso 1 calc R A 2 H28B H 0.1116 0.3727 0.4066 0.064 Uiso 1 calc R A 2 H28C H 0.2139 0.3222 0.3881 0.064 Uiso 1 calc R A 2 C29 C -0.0604(3) 0.2277(3) 0.38801(16) 0.0429(9) Uani 1 d . A 2 H29A H -0.1064 0.1944 0.3610 0.064 Uiso 1 calc R A 2 H29B H -0.0871 0.2891 0.3945 0.064 Uiso 1 calc R A 2 H29C H -0.0550 0.1954 0.4259 0.064 Uiso 1 calc R A 2 C30 C 0.0472(3) 0.2996(2) 0.28300(14) 0.0346(7) Uani 1 d . A 2 H30A H 0.1112 0.3048 0.2620 0.052 Uiso 1 calc R A 2 H30B H 0.0211 0.3605 0.2915 0.052 Uiso 1 calc R A 2 H30C H -0.0027 0.2665 0.2583 0.052 Uiso 1 calc R A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0220(4) 0.0377(5) 0.0225(4) 0.0044(4) 0.0050(3) -0.0002(4) Si2 0.0308(5) 0.0389(6) 0.0297(5) -0.0144(4) -0.0061(4) 0.0076(4) Si3 0.0279(4) 0.0292(5) 0.0221(4) 0.0039(3) 0.0008(3) -0.0033(4) Si4 0.0258(4) 0.0286(5) 0.0225(4) -0.0001(3) 0.0056(3) 0.0022(3) Na1 0.0222(6) 0.0370(7) 0.0192(6) -0.0009(5) -0.0008(4) -0.0004(5) Na2 0.0231(6) 0.0410(7) 0.0198(6) -0.0026(5) -0.0009(4) 0.0011(5) O1 0.0293(12) 0.080(2) 0.0346(13) -0.0001(13) -0.0124(10) -0.0089(13) O2 0.0307(12) 0.0669(18) 0.0284(12) -0.0129(12) -0.0093(10) 0.0090(12) N1 0.0259(13) 0.0377(16) 0.0183(12) 0.0001(11) -0.0049(10) -0.0059(11) N2 0.0230(12) 0.0329(15) 0.0183(12) -0.0013(10) -0.0017(10) 0.0058(11) N3 0.0270(13) 0.0305(15) 0.0159(11) -0.0026(10) 0.0023(10) 0.0007(11) N4 0.0260(12) 0.0246(14) 0.0195(12) 0.0006(10) 0.0049(10) -0.0009(10) C1 0.0312(16) 0.040(2) 0.0243(16) -0.0059(14) 0.0073(13) -0.0039(14) C2 0.0412(19) 0.064(3) 0.0181(15) -0.0053(16) -0.0012(14) -0.0136(18) C3 0.0325(18) 0.063(3) 0.0286(17) 0.0018(17) -0.0097(14) -0.0064(17) C4 0.0324(17) 0.042(2) 0.0324(17) 0.0080(15) 0.0009(14) 0.0000(15) C5 0.0327(17) 0.0373(18) 0.0188(14) -0.0051(13) 0.0022(12) -0.0016(14) C6 0.038(2) 0.077(3) 0.043(2) -0.003(2) 0.0176(17) -0.009(2) C7 0.050(2) 0.038(2) 0.064(3) -0.0074(19) 0.0177(19) -0.0023(18) C8 0.066(3) 0.056(3) 0.048(2) -0.022(2) 0.005(2) -0.009(2) C9 0.0386(19) 0.058(2) 0.0239(16) 0.0095(16) 0.0032(14) -0.0022(17) C10 0.0282(16) 0.0348(18) 0.0247(15) -0.0013(13) 0.0062(12) 0.0066(14) C11 0.0224(15) 0.046(2) 0.046(2) -0.0081(17) 0.0058(14) 0.0004(15) C12 0.0364(19) 0.054(2) 0.0336(18) -0.0108(16) -0.0162(15) 0.0154(17) C13 0.0467(19) 0.042(2) 0.0183(15) -0.0007(14) -0.0006(13) 0.0111(16) C14 0.0357(17) 0.0335(18) 0.0185(14) -0.0014(13) 0.0069(12) 0.0011(14) C15 0.057(2) 0.052(2) 0.040(2) 0.0127(18) 0.0190(18) 0.0131(19) C16 0.0334(17) 0.043(2) 0.0302(17) -0.0102(15) 0.0070(14) 0.0065(15) C17 0.0406(19) 0.051(2) 0.0352(18) -0.0070(17) 0.0142(15) 0.0046(17) C18 0.059(2) 0.035(2) 0.049(2) 0.0086(17) 0.0146(18) -0.0052(18) C19 0.0363(18) 0.0325(19) 0.0397(19) 0.0024(15) 0.0000(15) -0.0093(15) C20 0.0335(19) 0.069(3) 0.042(2) 0.014(2) 0.0128(16) 0.0021(18) C21 0.0363(18) 0.049(2) 0.0351(18) 0.0154(16) 0.0009(15) 0.0034(16) C22 0.049(2) 0.049(2) 0.062(3) -0.027(2) -0.0176(19) 0.0199(19) C23 0.052(2) 0.036(2) 0.055(2) -0.0182(18) -0.0171(18) -0.0005(17) C24 0.054(2) 0.083(3) 0.035(2) -0.026(2) -0.0004(17) 0.018(2) C25 0.0416(19) 0.052(2) 0.0269(17) 0.0106(16) 0.0027(14) -0.0043(17) C26 0.045(2) 0.038(2) 0.046(2) 0.0073(17) -0.0030(16) -0.0113(17) C27 0.0440(19) 0.033(2) 0.0378(19) 0.0065(15) 0.0015(15) 0.0037(16) C28 0.053(2) 0.032(2) 0.042(2) -0.0106(16) -0.0019(17) 0.0018(17) C29 0.0344(18) 0.056(2) 0.0394(19) 0.0082(17) 0.0137(15) 0.0132(17) C30 0.0374(18) 0.0321(18) 0.0342(17) 0.0061(14) 0.0032(14) 0.0035(15) _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 N3 1.687(3) . ? Si1 C19 1.884(3) . ? Si1 C21 1.884(3) . ? Si1 C20 1.885(3) . ? Si1 Na1 3.1890(14) . ? Si1 Na2 3.5001(15) . ? Si2 N3 1.681(3) . ? Si2 C24 1.884(4) . ? Si2 C22 1.884(4) . ? Si2 C23 1.894(4) . ? Si2 Na2 3.2514(15) . ? Si2 Na1 3.5233(15) . ? Si3 N4 1.684(3) . ? Si3 C26 1.879(3) . ? Si3 C25 1.886(3) . ? Si3 C27 1.890(3) . ? Si3 Na1 3.2021(15) . ? Si3 Na2 3.5151(15) . ? Si4 N4 1.680(3) . ? Si4 C28 1.874(4) . ? Si4 C30 1.889(3) . ? Si4 C29 1.896(3) . ? Si4 Na2 3.2338(15) . ? Na1 O1 2.196(2) . ? Na1 N4 2.382(3) . ? Na1 N3 2.397(2) . ? Na1 Na2 3.0296(17) . ? Na2 O2 2.205(2) . ? Na2 N3 2.400(3) . ? Na2 N4 2.408(3) . ? O1 N1 1.272(3) . ? O2 N2 1.277(3) . ? N1 C5 1.493(4) . ? N1 C1 1.494(4) . ? N2 C10 1.493(4) . ? N2 C14 1.505(4) . ? C1 C7 1.529(5) . ? C1 C2 1.530(5) . ? C1 C6 1.530(4) . ? C2 C3 1.515(5) . ? C3 C4 1.503(5) . ? C4 C5 1.517(4) . ? C5 C8 1.528(5) . ? C5 C9 1.537(4) . ? C10 C11 1.519(4) . ? C10 C15 1.521(4) . ? C10 C16 1.542(4) . ? C11 C12 1.517(5) . ? C12 C13 1.512(5) . ? C13 C14 1.524(4) . ? C14 C17 1.526(4) . ? C14 C18 1.533(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 N3 Si1 C19 110.47(13) . . ? N3 Si1 C21 112.95(14) . . ? C19 Si1 C21 106.57(17) . . ? N3 Si1 C20 115.35(16) . . ? C19 Si1 C20 103.57(17) . . ? C21 Si1 C20 107.19(16) . . ? N3 Si1 Na1 47.49(8) . . ? C19 Si1 Na1 63.65(11) . . ? C21 Si1 Na1 133.83(11) . . ? C20 Si1 Na1 118.98(12) . . ? N3 Si1 Na2 37.77(8) . . ? C19 Si1 Na2 95.98(11) . . ? C21 Si1 Na2 85.50(11) . . ? C20 Si1 Na2 152.16(14) . . ? Na1 Si1 Na2 53.62(3) . . ? N3 Si2 C24 115.88(17) . . ? N3 Si2 C22 113.44(14) . . ? C24 Si2 C22 105.86(18) . . ? N3 Si2 C23 110.20(15) . . ? C24 Si2 C23 105.00(19) . . ? C22 Si2 C23 105.65(19) . . ? N3 Si2 Na2 45.70(8) . . ? C24 Si2 Na2 120.52(13) . . ? C22 Si2 Na2 133.60(14) . . ? C23 Si2 Na2 65.24(12) . . ? N3 Si2 Na1 36.73(8) . . ? C24 Si2 Na1 151.03(16) . . ? C22 Si2 Na1 85.87(12) . . ? C23 Si2 Na1 96.81(12) . . ? Na2 Si2 Na1 52.94(3) . . ? N4 Si3 C26 112.99(14) . . ? N4 Si3 C25 115.65(15) . . ? C26 Si3 C25 106.50(16) . . ? N4 Si3 C27 109.64(14) . . ? C26 Si3 C27 107.37(17) . . ? C25 Si3 C27 104.02(16) . . ? N4 Si3 Na1 46.58(8) . . ? C26 Si3 Na1 137.30(12) . . ? C25 Si3 Na1 116.17(11) . . ? C27 Si3 Na1 64.46(11) . . ? N4 Si3 Na2 37.47(8) . . ? C26 Si3 Na2 87.52(12) . . ? C25 Si3 Na2 152.75(12) . . ? C27 Si3 Na2 93.44(11) . . ? Na1 Si3 Na2 53.37(3) . . ? N4 Si4 C28 113.44(15) . . ? N4 Si4 C30 110.86(14) . . ? C28 Si4 C30 106.39(16) . . ? N4 Si4 C29 115.19(15) . . ? C28 Si4 C29 105.88(17) . . ? C30 Si4 C29 104.32(15) . . ? N4 Si4 Na2 46.48(8) . . ? C28 Si4 Na2 136.28(12) . . ? C30 Si4 Na2 65.45(11) . . ? C29 Si4 Na2 117.81(13) . . ? O1 Na1 N4 127.06(10) . . ? O1 Na1 N3 130.94(10) . . ? N4 Na1 N3 101.98(9) . . ? O1 Na1 Na2 177.97(8) . . ? N4 Na1 Na2 51.14(6) . . ? N3 Na1 Na2 50.89(6) . . ? O1 Na1 Si1 113.57(8) . . ? N4 Na1 Si1 112.08(7) . . ? N3 Na1 Si1 31.25(6) . . ? Na2 Na1 Si1 68.45(4) . . ? O1 Na1 Si3 109.36(8) . . ? N4 Na1 Si3 30.88(6) . . ? N3 Na1 Si3 114.48(7) . . ? Na2 Na1 Si3 68.61(4) . . ? Si1 Na1 Si3 136.93(4) . . ? O1 Na1 Si2 122.26(8) . . ? N4 Na1 Si2 106.00(7) . . ? N3 Na1 Si2 24.80(6) . . ? Na2 Na1 Si2 58.92(3) . . ? Si1 Na1 Si2 53.24(3) . . ? Si3 Na1 Si2 105.12(4) . . ? O2 Na2 N3 129.74(9) . . ? O2 Na2 N4 129.01(10) . . ? N3 Na2 N4 101.14(9) . . ? O2 Na2 Na1 178.94(9) . . ? N3 Na2 Na1 50.79(6) . . ? N4 Na2 Na1 50.40(6) . . ? O2 Na2 Si4 110.47(7) . . ? N3 Na2 Si4 112.61(7) . . ? N4 Na2 Si4 30.40(6) . . ? Na1 Na2 Si4 68.59(4) . . ? O2 Na2 Si2 112.77(7) . . ? N3 Na2 Si2 30.08(6) . . ? N4 Na2 Si2 113.93(7) . . ? Na1 Na2 Si2 68.14(4) . . ? Si4 Na2 Si2 136.65(4) . . ? O2 Na2 Si1 122.06(8) . . ? N3 Na2 Si1 25.49(6) . . ? N4 Na2 Si1 102.02(7) . . ? Na1 Na2 Si1 57.93(3) . . ? Si4 Na2 Si1 100.35(4) . . ? Si2 Na2 Si1 53.03(3) . . ? O2 Na2 Si3 121.91(8) . . ? N3 Na2 Si3 104.56(7) . . ? N4 Na2 Si3 25.18(6) . . ? Na1 Na2 Si3 58.02(3) . . ? Si4 Na2 Si3 52.58(3) . . ? Si2 Na2 Si3 104.25(4) . . ? Si1 Na2 Si3 115.87(4) . . ? N1 O1 Na1 175.0(2) . . ? N2 O2 Na2 171.61(19) . . ? O1 N1 C5 116.1(2) . . ? O1 N1 C1 115.5(3) . . ? C5 N1 C1 125.0(2) . . ? O2 N2 C10 115.9(2) . . ? O2 N2 C14 115.7(2) . . ? C10 N2 C14 124.6(2) . . ? Si2 N3 Si1 127.64(14) . . ? Si2 N3 Na1 118.47(13) . . ? Si1 N3 Na1 101.26(11) . . ? Si2 N3 Na2 104.22(12) . . ? Si1 N3 Na2 116.74(13) . . ? Na1 N3 Na2 78.32(8) . . ? Si4 N4 Si3 126.19(14) . . ? Si4 N4 Na1 119.84(13) . . ? Si3 N4 Na1 102.55(12) . . ? Si4 N4 Na2 103.12(11) . . ? Si3 N4 Na2 117.35(13) . . ? Na1 N4 Na2 78.46(8) . . ? N1 C1 C7 109.1(3) . . ? N1 C1 C2 109.5(3) . . ? C7 C1 C2 111.6(3) . . ? N1 C1 C6 107.2(3) . . ? C7 C1 C6 109.7(3) . . ? C2 C1 C6 109.6(3) . . ? C3 C2 C1 112.8(3) . . ? C4 C3 C2 109.4(3) . . ? C3 C4 C5 113.5(3) . . ? N1 C5 C4 110.1(2) . . ? N1 C5 C8 107.6(3) . . ? C4 C5 C8 109.4(3) . . ? N1 C5 C9 108.2(3) . . ? C4 C5 C9 111.3(3) . . ? C8 C5 C9 110.1(3) . . ? N2 C10 C11 109.4(2) . . ? N2 C10 C15 107.3(3) . . ? C11 C10 C15 110.1(3) . . ? N2 C10 C16 108.3(3) . . ? C11 C10 C16 111.7(3) . . ? C15 C10 C16 109.9(3) . . ? C12 C11 C10 113.5(3) . . ? C13 C12 C11 109.1(3) . . ? C12 C13 C14 113.6(3) . . ? N2 C14 C13 109.1(2) . . ? N2 C14 C17 107.3(3) . . ? C13 C14 C17 110.0(3) . . ? N2 C14 C18 108.9(3) . . ? C13 C14 C18 112.5(3) . . ? C17 C14 C18 109.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Na1 O1 N1 79(2) . . . . ? N3 Na1 O1 N1 -102(2) . . . . ? Na2 Na1 O1 N1 52(4) . . . . ? Si1 Na1 O1 N1 -133(2) . . . . ? Si3 Na1 O1 N1 50(2) . . . . ? Si2 Na1 O1 N1 -73(2) . . . . ? N3 Na2 O2 N2 14.9(16) . . . . ? N4 Na2 O2 N2 -169.4(15) . . . . ? Na1 Na2 O2 N2 134(4) . . . . ? Si4 Na2 O2 N2 162.5(15) . . . . ? Si2 Na2 O2 N2 -14.5(16) . . . . ? Si1 Na2 O2 N2 45.1(16) . . . . ? Si3 Na2 O2 N2 -139.6(15) . . . . ? Na2 O2 N2 C10 166.5(14) . . . . ? Na2 O2 N2 C14 -34.2(17) . . . . ? C24 Si2 N3 Si1 -33.0(2) . . . . ? C22 Si2 N3 Si1 89.7(2) . . . . ? C23 Si2 N3 Si1 -152.04(19) . . . . ? Na2 Si2 N3 Si1 -141.4(2) . . . . ? Na1 Si2 N3 Si1 134.3(3) . . . . ? C24 Si2 N3 Na1 -167.36(16) . . . . ? C22 Si2 N3 Na1 -44.6(2) . . . . ? C23 Si2 N3 Na1 73.63(18) . . . . ? Na2 Si2 N3 Na1 84.26(13) . . . . ? C24 Si2 N3 Na2 108.38(17) . . . . ? C22 Si2 N3 Na2 -128.85(18) . . . . ? C23 Si2 N3 Na2 -10.63(17) . . . . ? Na1 Si2 N3 Na2 -84.26(13) . . . . ? C19 Si1 N3 Si2 -150.08(18) . . . . ? C21 Si1 N3 Si2 90.7(2) . . . . ? C20 Si1 N3 Si2 -33.1(2) . . . . ? Na1 Si1 N3 Si2 -140.1(2) . . . . ? Na2 Si1 N3 Si2 137.4(2) . . . . ? C19 Si1 N3 Na1 -9.96(16) . . . . ? C21 Si1 N3 Na1 -129.21(14) . . . . ? C20 Si1 N3 Na1 107.04(16) . . . . ? Na2 Si1 N3 Na1 -82.49(12) . . . . ? C19 Si1 N3 Na2 72.53(17) . . . . ? C21 Si1 N3 Na2 -46.72(18) . . . . ? C20 Si1 N3 Na2 -170.48(15) . . . . ? Na1 Si1 N3 Na2 82.49(12) . . . . ? O1 Na1 N3 Si2 78.88(19) . . . . ? N4 Na1 N3 Si2 -102.27(14) . . . . ? Na2 Na1 N3 Si2 -99.98(15) . . . . ? Si1 Na1 N3 Si2 144.7(2) . . . . ? Si3 Na1 N3 Si2 -72.43(14) . . . . ? O1 Na1 N3 Si1 -65.84(18) . . . . ? N4 Na1 N3 Si1 113.01(11) . . . . ? Na2 Na1 N3 Si1 115.30(13) . . . . ? Si3 Na1 N3 Si1 142.85(9) . . . . ? Si2 Na1 N3 Si1 -144.7(2) . . . . ? O1 Na1 N3 Na2 178.86(13) . . . . ? N4 Na1 N3 Na2 -2.29(10) . . . . ? Si1 Na1 N3 Na2 -115.30(13) . . . . ? Si3 Na1 N3 Na2 27.55(9) . . . . ? Si2 Na1 N3 Na2 99.98(15) . . . . ? O2 Na2 N3 Si2 -64.46(17) . . . . ? N4 Na2 N3 Si2 118.99(12) . . . . ? Na1 Na2 N3 Si2 116.73(13) . . . . ? Si4 Na2 N3 Si2 148.51(9) . . . . ? Si1 Na2 N3 Si2 -146.4(2) . . . . ? Si3 Na2 N3 Si2 93.39(10) . . . . ? O2 Na2 N3 Si1 81.96(18) . . . . ? N4 Na2 N3 Si1 -94.59(13) . . . . ? Na1 Na2 N3 Si1 -96.85(14) . . . . ? Si4 Na2 N3 Si1 -65.07(13) . . . . ? Si2 Na2 N3 Si1 146.4(2) . . . . ? Si3 Na2 N3 Si1 -120.19(11) . . . . ? O2 Na2 N3 Na1 178.81(12) . . . . ? N4 Na2 N3 Na1 2.26(10) . . . . ? Si4 Na2 N3 Na1 31.77(9) . . . . ? Si2 Na2 N3 Na1 -116.73(13) . . . . ? Si1 Na2 N3 Na1 96.85(14) . . . . ? Si3 Na2 N3 Na1 -23.34(8) . . . . ? C28 Si4 N4 Si3 88.5(2) . . . . ? C30 Si4 N4 Si3 -151.84(17) . . . . ? C29 Si4 N4 Si3 -33.7(2) . . . . ? Na2 Si4 N4 Si3 -139.0(2) . . . . ? C28 Si4 N4 Na1 -48.34(19) . . . . ? C30 Si4 N4 Na1 71.28(17) . . . . ? C29 Si4 N4 Na1 -170.58(15) . . . . ? Na2 Si4 N4 Na1 84.08(13) . . . . ? C28 Si4 N4 Na2 -132.42(15) . . . . ? C30 Si4 N4 Na2 -12.81(16) . . . . ? C29 Si4 N4 Na2 105.33(15) . . . . ? C26 Si3 N4 Si4 83.2(2) . . . . ? C25 Si3 N4 Si4 -39.9(2) . . . . ? C27 Si3 N4 Si4 -157.12(18) . . . . ? Na1 Si3 N4 Si4 -142.6(2) . . . . ? Na2 Si3 N4 Si4 134.0(2) . . . . ? C26 Si3 N4 Na1 -134.24(15) . . . . ? C25 Si3 N4 Na1 102.66(15) . . . . ? C27 Si3 N4 Na1 -14.52(16) . . . . ? Na2 Si3 N4 Na1 -83.36(13) . . . . ? C26 Si3 N4 Na2 -50.88(19) . . . . ? C25 Si3 N4 Na2 -173.98(14) . . . . ? C27 Si3 N4 Na2 68.84(17) . . . . ? Na1 Si3 N4 Na2 83.36(13) . . . . ? O1 Na1 N4 Si4 82.57(18) . . . . ? N3 Na1 N4 Si4 -96.35(14) . . . . ? Na2 Na1 N4 Si4 -98.63(14) . . . . ? Si1 Na1 N4 Si4 -65.33(14) . . . . ? Si3 Na1 N4 Si4 145.6(2) . . . . ? Si2 Na1 N4 Si4 -121.58(12) . . . . ? O1 Na1 N4 Si3 -63.02(17) . . . . ? N3 Na1 N4 Si3 118.06(12) . . . . ? Na2 Na1 N4 Si3 115.78(13) . . . . ? Si1 Na1 N4 Si3 149.08(9) . . . . ? Si2 Na1 N4 Si3 92.82(10) . . . . ? O1 Na1 N4 Na2 -178.80(12) . . . . ? N3 Na1 N4 Na2 2.28(10) . . . . ? Si1 Na1 N4 Na2 33.29(8) . . . . ? Si3 Na1 N4 Na2 -115.78(13) . . . . ? Si2 Na1 N4 Na2 -22.96(8) . . . . ? O2 Na2 N4 Si4 -60.57(17) . . . . ? N3 Na2 N4 Si4 116.01(12) . . . . ? Na1 Na2 N4 Si4 118.28(13) . . . . ? Si2 Na2 N4 Si4 144.67(9) . . . . ? Si1 Na2 N4 Si4 90.00(11) . . . . ? Si3 Na2 N4 Si4 -143.4(2) . . . . ? O2 Na2 N4 Si3 82.86(18) . . . . ? N3 Na2 N4 Si3 -100.55(14) . . . . ? Na1 Na2 N4 Si3 -98.28(14) . . . . ? Si4 Na2 N4 Si3 143.4(2) . . . . ? Si2 Na2 N4 Si3 -71.89(14) . . . . ? Si1 Na2 N4 Si3 -126.56(12) . . . . ? O2 Na2 N4 Na1 -178.86(12) . . . . ? N3 Na2 N4 Na1 -2.27(10) . . . . ? Si4 Na2 N4 Na1 -118.28(13) . . . . ? Si2 Na2 N4 Na1 26.39(9) . . . . ? Si1 Na2 N4 Na1 -28.29(7) . . . . ? Si3 Na2 N4 Na1 98.28(14) . . . . ? O1 N1 C1 C7 -70.0(3) . . . . ? C5 N1 C1 C7 88.4(4) . . . . ? O1 N1 C1 C2 167.6(3) . . . . ? C5 N1 C1 C2 -34.0(4) . . . . ? O1 N1 C1 C6 48.8(4) . . . . ? C5 N1 C1 C6 -152.8(3) . . . . ? N1 C1 C2 C3 45.8(4) . . . . ? C7 C1 C2 C3 -75.2(4) . . . . ? C6 C1 C2 C3 163.1(3) . . . . ? C1 C2 C3 C4 -61.0(4) . . . . ? C2 C3 C4 C5 60.4(4) . . . . ? O1 N1 C5 C4 -168.4(3) . . . . ? C1 N1 C5 C4 33.3(4) . . . . ? O1 N1 C5 C8 -49.2(4) . . . . ? C1 N1 C5 C8 152.5(3) . . . . ? O1 N1 C5 C9 69.7(3) . . . . ? C1 N1 C5 C9 -88.5(3) . . . . ? C3 C4 C5 N1 -44.6(4) . . . . ? C3 C4 C5 C8 -162.7(3) . . . . ? C3 C4 C5 C9 75.4(4) . . . . ? O2 N2 C10 C11 -166.4(3) . . . . ? C14 N2 C10 C11 36.3(4) . . . . ? O2 N2 C10 C15 -47.0(4) . . . . ? C14 N2 C10 C15 155.8(3) . . . . ? O2 N2 C10 C16 71.6(3) . . . . ? C14 N2 C10 C16 -85.6(3) . . . . ? N2 C10 C11 C12 -46.4(4) . . . . ? C15 C10 C11 C12 -164.1(3) . . . . ? C16 C10 C11 C12 73.5(3) . . . . ? C10 C11 C12 C13 60.3(4) . . . . ? C11 C12 C13 C14 -60.3(4) . . . . ? O2 N2 C14 C13 166.6(3) . . . . ? C10 N2 C14 C13 -36.2(4) . . . . ? O2 N2 C14 C17 47.5(3) . . . . ? C10 N2 C14 C17 -155.3(3) . . . . ? O2 N2 C14 C18 -70.4(3) . . . . ? C10 N2 C14 C18 86.9(4) . . . . ? C12 C13 C14 N2 46.2(4) . . . . ? C12 C13 C14 C17 163.7(3) . . . . ? C12 C13 C14 C18 -74.7(4) . . . . ? _refine_diff_density_max 0.427 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.068 #------------------------------------------------------------------------- #-----------------------------COMPOUND 5------------------------------------ #--------------------------------------------------------------------------- data_g24 _database_code_CSD 160886 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H126 Li N7 O4 Si6 Zn' _chemical_formula_weight 1178.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Zn' 'Zn' 0.2839 1.4301 '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 0.0060 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 11.8488(2) _cell_length_b 18.2495(2) _cell_length_c 33.7384(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.2150(6) _cell_angle_gamma 90.00 _cell_volume 7283.93(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11710 _cell_measurement_theta_min 1.27 _cell_measurement_theta_max 16.02 _exptl_crystal_description fragment _exptl_crystal_colour yellowed _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonious Kappa CCD' _diffrn_measurement_method 'phi + omega scans ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12611 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0792 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12611 _reflns_number_gt 8255 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Denzo & Collect (Otwinowski & Minor, 1997; Hooft & Nonius 1988) ; _computing_cell_refinement 'Denzo & Collect' _computing_data_reduction 'Denzo & Collect' _computing_structure_solution 'SIR-97 ' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+2.6373P] 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 12611 _refine_ls_number_parameters 692 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.52084(3) 0.335921(17) 0.358404(9) 0.02131(9) Uani 1 d . . . Si1 Si 0.49342(7) 0.17783(4) 0.31951(3) 0.0314(2) Uani 1 d . . . Si2 Si 0.55801(7) 0.18807(5) 0.40654(3) 0.0318(2) Uani 1 d . . . Si3 Si 0.77241(7) 0.35812(5) 0.33672(2) 0.0300(2) Uani 1 d . . . Si4 Si 0.59139(7) 0.45235(5) 0.29557(2) 0.0306(2) Uani 1 d . . . Si5 Si 0.44263(7) 0.45967(4) 0.41713(2) 0.0282(2) Uani 1 d . . . Si6 Si 0.26873(7) 0.35870(4) 0.37965(2) 0.0261(2) Uani 1 d . . . O1 O 0.00241(17) 0.28087(11) 0.15424(6) 0.0349(5) Uani 1 d . . . O2 O 0.25184(16) 0.32642(11) 0.11421(6) 0.0376(5) Uani 1 d . . . O3 O 0.02516(16) 0.41430(10) 0.10482(6) 0.0320(5) Uani 1 d . . . O4 O 0.06890(16) 0.24946(11) 0.06672(6) 0.0357(5) Uani 1 d . . . N1 N 0.52433(19) 0.22755(11) 0.36174(6) 0.0250(5) Uani 1 d . . . N2 N 0.63544(18) 0.38638(12) 0.32857(6) 0.0253(6) Uani 1 d . . . N3 N 0.40421(18) 0.39047(11) 0.38511(6) 0.0225(5) Uani 1 d . . . N4 N -0.0270(2) 0.22432(13) 0.17420(7) 0.0277(6) Uani 1 d . . . N5 N 0.3490(2) 0.34491(13) 0.10218(8) 0.0356(6) Uani 1 d . . . N6 N 0.01188(19) 0.48042(12) 0.11742(7) 0.0287(6) Uani 1 d . . . N7 N 0.00376(19) 0.20290(12) 0.04780(6) 0.0256(6) Uani 1 d . . . C1 C 0.4967(3) 0.23536(17) 0.27382(9) 0.0416(8) Uani 1 d . . . H1A H 0.4339 0.2703 0.2732 0.062 Uiso 1 calc R . . H1B H 0.4896 0.2038 0.2503 0.062 Uiso 1 calc R . . H1C H 0.5685 0.2621 0.2740 0.062 Uiso 1 calc R . . C2 C 0.3493(3) 0.13467(17) 0.31788(10) 0.0463(9) Uani 1 d . . . H2A H 0.3484 0.0952 0.3376 0.069 Uiso 1 calc R . . H2B H 0.3315 0.1145 0.2913 0.069 Uiso 1 calc R . . H2C H 0.2930 0.1718 0.3239 0.069 Uiso 1 calc R . . C3 C 0.5922(3) 0.09865(17) 0.31276(10) 0.0508(10) Uani 1 d . . . H3A H 0.6688 0.1172 0.3097 0.076 Uiso 1 calc R . . H3B H 0.5670 0.0709 0.2890 0.076 Uiso 1 calc R . . H3C H 0.5922 0.0666 0.3361 0.076 Uiso 1 calc R . . C4 C 0.4646(3) 0.10855(17) 0.41876(10) 0.0489(9) Uani 1 d . . . H4A H 0.3862 0.1254 0.4196 0.073 Uiso 1 calc R . . H4B H 0.4897 0.0882 0.4447 0.073 Uiso 1 calc R . . H4C H 0.4692 0.0706 0.3983 0.073 Uiso 1 calc R . . C5 C 0.7053(3) 0.14977(18) 0.41151(10) 0.0475(9) Uani 1 d . . . H5A H 0.7127 0.1101 0.3922 0.071 Uiso 1 calc R . . H5B H 0.7202 0.1306 0.4384 0.071 Uiso 1 calc R . . H5C H 0.7598 0.1886 0.4065 0.071 Uiso 1 calc R . . C6 C 0.5487(3) 0.25487(16) 0.44836(8) 0.0360(8) Uani 1 d . . . H6A H 0.5977 0.2970 0.4438 0.054 Uiso 1 calc R . . H6B H 0.5732 0.2310 0.4734 0.054 Uiso 1 calc R . . H6C H 0.4704 0.2716 0.4497 0.054 Uiso 1 calc R . . C7 C 0.7969(3) 0.26357(18) 0.31791(10) 0.0489(9) Uani 1 d . . . H7A H 0.7516 0.2286 0.3323 0.073 Uiso 1 calc R . . H7B H 0.8772 0.2512 0.3220 0.073 Uiso 1 calc R . . H7C H 0.7748 0.2613 0.2895 0.073 Uiso 1 calc R . . C8 C 0.8181(3) 0.35395(18) 0.39060(9) 0.0410(8) Uani 1 d . . . H8A H 0.8247 0.4038 0.4013 0.061 Uiso 1 calc R . . H8B H 0.8915 0.3293 0.3938 0.061 Uiso 1 calc R . . H8C H 0.7620 0.3266 0.4049 0.061 Uiso 1 calc R . . C9 C 0.8797(3) 0.4182(2) 0.31420(12) 0.0666(12) Uani 1 d . . . H9A H 0.8686 0.4168 0.2852 0.100 Uiso 1 calc R . . H9B H 0.9558 0.4007 0.3221 0.100 Uiso 1 calc R . . H9C H 0.8708 0.4687 0.3235 0.100 Uiso 1 calc R . . C10 C 0.6502(3) 0.44018(19) 0.24531(9) 0.0473(9) Uani 1 d . . . H10A H 0.7293 0.4560 0.2464 0.071 Uiso 1 calc R . . H10B H 0.6063 0.4697 0.2257 0.071 Uiso 1 calc R . . H10C H 0.6456 0.3884 0.2377 0.071 Uiso 1 calc R . . C11 C 0.4343(3) 0.45279(18) 0.28676(10) 0.0443(9) Uani 1 d . . . H11A H 0.4097 0.4063 0.2746 0.066 Uiso 1 calc R . . H11B H 0.4119 0.4933 0.2690 0.066 Uiso 1 calc R . . H11C H 0.3988 0.4590 0.3121 0.066 Uiso 1 calc R . . C12 C 0.6304(3) 0.54762(17) 0.31248(11) 0.0565(10) Uani 1 d . . . H12A H 0.5947 0.5583 0.3373 0.085 Uiso 1 calc R . . H12B H 0.6042 0.5830 0.2921 0.085 Uiso 1 calc R . . H12C H 0.7127 0.5512 0.3168 0.085 Uiso 1 calc R . . C13 C 0.3910(3) 0.44417(19) 0.46822(9) 0.0475(9) Uani 1 d . . . H13A H 0.3098 0.4336 0.4662 0.071 Uiso 1 calc R . . H13B H 0.4048 0.4882 0.4844 0.071 Uiso 1 calc R . . H13C H 0.4315 0.4026 0.4807 0.071 Uiso 1 calc R . . C14 C 0.5992(2) 0.47074(17) 0.42362(9) 0.0349(8) Uani 1 d . . . H14A H 0.6319 0.4280 0.4376 0.052 Uiso 1 calc R . . H14B H 0.6169 0.5151 0.4392 0.052 Uiso 1 calc R . . H14C H 0.6311 0.4750 0.3975 0.052 Uiso 1 calc R . . C15 C 0.3879(3) 0.55225(16) 0.40074(11) 0.0478(9) Uani 1 d . . . H15A H 0.4126 0.5630 0.3741 0.072 Uiso 1 calc R . . H15B H 0.4175 0.5897 0.4193 0.072 Uiso 1 calc R . . H15C H 0.3051 0.5522 0.4002 0.072 Uiso 1 calc R . . C16 C 0.2409(3) 0.27749(16) 0.41169(10) 0.0419(8) Uani 1 d . . . H16A H 0.2893 0.2366 0.4044 0.063 Uiso 1 calc R . . H16B H 0.1614 0.2631 0.4078 0.063 Uiso 1 calc R . . H16C H 0.2576 0.2903 0.4396 0.063 Uiso 1 calc R . . C17 C 0.2273(3) 0.33066(18) 0.32768(9) 0.0440(9) Uani 1 d . . . H17A H 0.2164 0.3744 0.3111 0.066 Uiso 1 calc R . . H17B H 0.1566 0.3027 0.3273 0.066 Uiso 1 calc R . . H17C H 0.2870 0.3001 0.3173 0.066 Uiso 1 calc R . . C18 C 0.1588(2) 0.42780(17) 0.39200(10) 0.0418(9) Uani 1 d . . . H18A H 0.1740 0.4453 0.4192 0.063 Uiso 1 calc R . . H18B H 0.0838 0.4050 0.3897 0.063 Uiso 1 calc R . . H18C H 0.1610 0.4692 0.3736 0.063 Uiso 1 calc R . . C19 C 0.0538(3) 0.19966(17) 0.20727(9) 0.0351(8) Uani 1 d . . . C20 C 0.0280(3) 0.11994(19) 0.21648(10) 0.0546(10) Uani 1 d . . . H20A H 0.0555 0.0888 0.1950 0.082 Uiso 1 calc R . . H20B H 0.0704 0.1060 0.2415 0.082 Uiso 1 calc R . . C21 C -0.0959(3) 0.1044(2) 0.22063(11) 0.0626(12) Uani 1 d . . . H21A H -0.1239 0.1335 0.2428 0.094 Uiso 1 calc R . . H21B H -0.1066 0.0518 0.2266 0.094 Uiso 1 calc R . . C22 C -0.1619(3) 0.12418(18) 0.18213(10) 0.0513(10) Uani 1 d . . . H22A H -0.2429 0.1130 0.1849 0.077 Uiso 1 calc R . . H22B H -0.1351 0.0933 0.1604 0.077 Uiso 1 calc R . . C23 C -0.1499(2) 0.20471(17) 0.17084(9) 0.0339(8) Uani 1 d . . . C24 C 0.0422(3) 0.2497(2) 0.24341(9) 0.0528(10) Uani 1 d . . . H24A H 0.0464 0.3010 0.2351 0.079 Uiso 1 calc R . . H24B H 0.1035 0.2393 0.2633 0.079 Uiso 1 calc R . . H24C H -0.0307 0.2407 0.2549 0.079 Uiso 1 calc R . . C25 C 0.1726(3) 0.20684(19) 0.19315(10) 0.0476(9) Uani 1 d . . . H25A H 0.1779 0.1801 0.1681 0.071 Uiso 1 calc R . . H25B H 0.2267 0.1863 0.2132 0.071 Uiso 1 calc R . . H25C H 0.1899 0.2587 0.1890 0.071 Uiso 1 calc R . . C26 C -0.2143(3) 0.2554(2) 0.19777(9) 0.0528(10) Uani 1 d . . . H26A H -0.1927 0.2444 0.2256 0.079 Uiso 1 calc R . . H26B H -0.2958 0.2477 0.1929 0.079 Uiso 1 calc R . . H26C H -0.1957 0.3065 0.1921 0.079 Uiso 1 calc R . . C27 C -0.1927(3) 0.21676(18) 0.12805(8) 0.0407(8) Uani 1 d . . . H27A H -0.1918 0.2693 0.1220 0.061 Uiso 1 calc R . . H27B H -0.2702 0.1982 0.1243 0.061 Uiso 1 calc R . . H27C H -0.1439 0.1907 0.1103 0.061 Uiso 1 calc R . . C28 C 0.3548(3) 0.3586(2) 0.05898(10) 0.0502(10) Uani 1 d . . . C29 C 0.4701(3) 0.3920(2) 0.05096(12) 0.0654(12) Uani 1 d . . . H29A H 0.4812 0.3889 0.0221 0.098 Uiso 1 calc R . . H29B H 0.4693 0.4445 0.0583 0.098 Uiso 1 calc R . . C30 C 0.5690(3) 0.3557(2) 0.07313(15) 0.0797(14) Uani 1 d . . . H30A H 0.5727 0.3033 0.0657 0.120 Uiso 1 calc R . . H30B H 0.6404 0.3795 0.0664 0.120 Uiso 1 calc R . . C31 C 0.5533(3) 0.3628(2) 0.11670(14) 0.0642(12) Uani 1 d . . . H31A H 0.5498 0.4155 0.1235 0.096 Uiso 1 calc R . . H31B H 0.6201 0.3417 0.1315 0.096 Uiso 1 calc R . . C32 C 0.4471(3) 0.32513(18) 0.13038(12) 0.0524(10) Uani 1 d . . . C33 C 0.2605(3) 0.4110(2) 0.04655(11) 0.0719(13) Uani 1 d . . . H33A H 0.1875 0.3864 0.0483 0.108 Uiso 1 calc R . . H33B H 0.2692 0.4269 0.0191 0.108 Uiso 1 calc R . . H33C H 0.2638 0.4538 0.0641 0.108 Uiso 1 calc R . . C34 C 0.3378(4) 0.2853(2) 0.03698(13) 0.0901(16) Uani 1 d . . . H34A H 0.4033 0.2535 0.0430 0.135 Uiso 1 calc R . . H34B H 0.3300 0.2942 0.0083 0.135 Uiso 1 calc R . . H34C H 0.2694 0.2613 0.0456 0.135 Uiso 1 calc R . . C35 C 0.4206(3) 0.3534(2) 0.17147(12) 0.0697(13) Uani 1 d . . . H35A H 0.4063 0.4063 0.1701 0.105 Uiso 1 calc R . . H35B H 0.4851 0.3438 0.1902 0.105 Uiso 1 calc R . . H35C H 0.3535 0.3283 0.1804 0.105 Uiso 1 calc R . . C36 C 0.4583(3) 0.2418(2) 0.13106(15) 0.0896(16) Uani 1 d . . . H36A H 0.3860 0.2199 0.1375 0.134 Uiso 1 calc R . . H36B H 0.5169 0.2275 0.1512 0.134 Uiso 1 calc R . . H36C H 0.4790 0.2245 0.1050 0.134 Uiso 1 calc R . . C37 C -0.0617(3) 0.52734(17) 0.09064(11) 0.0478(10) Uani 1 d . . . C38 C -0.0505(3) 0.60755(17) 0.10351(11) 0.0551(11) Uani 1 d . . . H38A H 0.0214 0.6272 0.0944 0.083 Uiso 1 calc R . . H38B H -0.1130 0.6359 0.0902 0.083 Uiso 1 calc R . . C39 C -0.0528(3) 0.61917(18) 0.14794(11) 0.0517(10) Uani 1 d . . . H39A H -0.0454 0.6720 0.1543 0.078 Uiso 1 calc R . . H39B H -0.1252 0.6013 0.1577 0.078 Uiso 1 calc R . . C40 C 0.0451(3) 0.57682(16) 0.16733(9) 0.0420(9) Uani 1 d . . . H40A H 0.0484 0.5864 0.1963 0.063 Uiso 1 calc R . . H40B H 0.1163 0.5951 0.1569 0.063 Uiso 1 calc R . . C41 C 0.0376(3) 0.49417(16) 0.16051(9) 0.0353(8) Uani 1 d . . . C42 C -0.1828(3) 0.5002(2) 0.09207(15) 0.0920(18) Uani 1 d . . . H42A H -0.1860 0.4480 0.0853 0.138 Uiso 1 calc R . . H42B H -0.2315 0.5278 0.0730 0.138 Uiso 1 calc R . . H42C H -0.2089 0.5073 0.1189 0.138 Uiso 1 calc R . . C43 C -0.0202(4) 0.52005(19) 0.04858(10) 0.0758(15) Uani 1 d . . . H43A H 0.0610 0.5306 0.0491 0.114 Uiso 1 calc R . . H43B H -0.0611 0.5548 0.0309 0.114 Uiso 1 calc R . . H43C H -0.0339 0.4700 0.0389 0.114 Uiso 1 calc R . . C44 C -0.0551(3) 0.45923(19) 0.18413(11) 0.0696(12) Uani 1 d . . . H44A H -0.1263 0.4857 0.1787 0.104 Uiso 1 calc R . . H44B H -0.0335 0.4618 0.2126 0.104 Uiso 1 calc R . . H44C H -0.0649 0.4079 0.1762 0.104 Uiso 1 calc R . . C45 C 0.1508(3) 0.45888(17) 0.17194(10) 0.0536(11) Uani 1 d . . . H45A H 0.1428 0.4054 0.1712 0.080 Uiso 1 calc R . . H45B H 0.1761 0.4743 0.1988 0.080 Uiso 1 calc R . . H45C H 0.2065 0.4741 0.1532 0.080 Uiso 1 calc R . . C46 C 0.0408(2) 0.12444(15) 0.04968(8) 0.0274(7) Uani 1 d . . . C47 C -0.0616(3) 0.07657(16) 0.03902(9) 0.0375(8) Uani 1 d . . . H47A H -0.0359 0.0255 0.0355 0.056 Uiso 1 calc R . . H47B H -0.1122 0.0771 0.0614 0.056 Uiso 1 calc R . . C48 C -0.1285(3) 0.10050(16) 0.00163(10) 0.0445(9) Uani 1 d . . . H48A H -0.0802 0.0980 -0.0213 0.067 Uiso 1 calc R . . H48B H -0.1939 0.0675 -0.0036 0.067 Uiso 1 calc R . . C49 C -0.1692(3) 0.17807(17) 0.00704(9) 0.0390(8) Uani 1 d . . . H49A H -0.2208 0.1789 0.0291 0.059 Uiso 1 calc R . . H49B H -0.2133 0.1933 -0.0174 0.059 Uiso 1 calc R . . C50 C -0.0748(3) 0.23368(15) 0.01577(8) 0.0305(7) Uani 1 d . . . C51 C 0.0864(3) 0.10870(17) 0.09206(9) 0.0471(9) Uani 1 d . . . H51A H 0.1565 0.1363 0.0976 0.071 Uiso 1 calc R . . H51B H 0.1017 0.0562 0.0950 0.071 Uiso 1 calc R . . H51C H 0.0303 0.1236 0.1108 0.071 Uiso 1 calc R . . C52 C 0.1364(3) 0.11158(16) 0.02136(9) 0.0387(8) Uani 1 d . . . H52A H 0.1055 0.1139 -0.0062 0.058 Uiso 1 calc R . . H52B H 0.1701 0.0632 0.0265 0.058 Uiso 1 calc R . . H52C H 0.1944 0.1495 0.0257 0.058 Uiso 1 calc R . . C53 C -0.1242(3) 0.30451(17) 0.03074(10) 0.0456(9) Uani 1 d . . . H53A H -0.1578 0.2956 0.0562 0.068 Uiso 1 calc R . . H53B H -0.1825 0.3224 0.0114 0.068 Uiso 1 calc R . . H53C H -0.0642 0.3413 0.0343 0.068 Uiso 1 calc R . . C54 C -0.0094(3) 0.24961(18) -0.02109(9) 0.0449(9) Uani 1 d . . . H54A H 0.0590 0.2776 -0.0134 0.067 Uiso 1 calc R . . H54B H -0.0570 0.2782 -0.0401 0.067 Uiso 1 calc R . . H54C H 0.0118 0.2033 -0.0334 0.067 Uiso 1 calc R . . Li1 Li 0.0890(4) 0.3177(3) 0.11094(14) 0.0286(11) Uani 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 Zn1 0.02067(18) 0.02267(18) 0.02073(18) -0.00116(15) 0.00241(13) -0.00191(15) Si1 0.0292(5) 0.0272(5) 0.0382(5) -0.0101(4) 0.0056(4) -0.0023(4) Si2 0.0326(5) 0.0282(5) 0.0351(5) 0.0069(4) 0.0057(4) 0.0013(4) Si3 0.0225(5) 0.0412(5) 0.0266(5) 0.0067(4) 0.0042(4) -0.0032(4) Si4 0.0323(5) 0.0302(5) 0.0295(5) 0.0082(4) 0.0042(4) -0.0017(4) Si5 0.0251(5) 0.0298(5) 0.0300(5) -0.0109(4) 0.0048(4) -0.0058(4) Si6 0.0200(4) 0.0264(5) 0.0319(5) -0.0076(4) 0.0016(4) -0.0025(3) O1 0.0393(13) 0.0279(12) 0.0386(13) 0.0009(10) 0.0113(10) -0.0008(10) O2 0.0207(12) 0.0432(14) 0.0489(14) -0.0068(11) 0.0014(10) -0.0010(10) O3 0.0394(13) 0.0188(11) 0.0375(12) -0.0061(9) 0.0000(10) 0.0065(9) O4 0.0338(12) 0.0342(12) 0.0390(13) -0.0177(10) 0.0020(10) -0.0064(10) N1 0.0256(13) 0.0203(13) 0.0295(14) 0.0005(11) 0.0059(10) 0.0019(11) N2 0.0241(13) 0.0268(14) 0.0250(13) 0.0028(11) 0.0029(10) -0.0019(11) N3 0.0214(13) 0.0223(13) 0.0239(13) -0.0023(10) 0.0018(10) -0.0015(10) N4 0.0335(15) 0.0260(14) 0.0239(14) -0.0008(11) 0.0049(11) 0.0001(11) N5 0.0233(15) 0.0289(15) 0.0545(18) -0.0103(13) 0.0029(13) -0.0018(12) N6 0.0288(14) 0.0214(14) 0.0357(15) -0.0046(12) 0.0005(12) 0.0030(11) N7 0.0266(14) 0.0256(14) 0.0245(13) -0.0063(11) 0.0007(11) -0.0022(11) C1 0.044(2) 0.047(2) 0.0340(19) -0.0125(16) 0.0020(16) -0.0057(17) C2 0.042(2) 0.039(2) 0.058(2) -0.0119(17) 0.0053(17) -0.0121(16) C3 0.050(2) 0.042(2) 0.061(2) -0.0223(18) 0.0057(18) 0.0010(17) C4 0.055(2) 0.033(2) 0.059(2) 0.0123(17) 0.0081(19) -0.0016(17) C5 0.044(2) 0.048(2) 0.050(2) 0.0086(17) 0.0004(17) 0.0128(17) C6 0.0347(19) 0.043(2) 0.0309(18) 0.0068(15) 0.0050(14) 0.0029(15) C7 0.034(2) 0.070(3) 0.043(2) -0.0111(19) 0.0077(16) 0.0145(18) C8 0.0320(19) 0.056(2) 0.0348(19) -0.0001(16) -0.0021(15) 0.0070(16) C9 0.030(2) 0.092(3) 0.078(3) 0.041(2) 0.0033(19) -0.008(2) C10 0.049(2) 0.061(2) 0.0323(19) 0.0143(17) 0.0055(16) 0.0007(18) C11 0.039(2) 0.051(2) 0.043(2) 0.0227(17) 0.0030(16) 0.0062(17) C12 0.067(3) 0.033(2) 0.070(3) 0.0055(19) 0.006(2) -0.0082(18) C13 0.038(2) 0.066(2) 0.039(2) -0.0247(18) 0.0105(16) -0.0168(18) C14 0.0331(18) 0.041(2) 0.0303(18) -0.0108(15) 0.0031(14) -0.0083(15) C15 0.040(2) 0.033(2) 0.070(3) -0.0143(18) -0.0023(18) -0.0037(16) C16 0.0297(18) 0.038(2) 0.058(2) -0.0013(17) 0.0077(16) -0.0091(15) C17 0.0314(19) 0.057(2) 0.043(2) -0.0143(17) 0.0010(15) -0.0088(17) C18 0.0230(18) 0.040(2) 0.062(2) -0.0118(17) -0.0016(16) -0.0036(15) C19 0.0350(19) 0.043(2) 0.0271(18) -0.0005(15) -0.0021(14) 0.0069(15) C20 0.068(3) 0.052(2) 0.041(2) 0.0147(18) -0.0119(19) 0.004(2) C21 0.077(3) 0.060(3) 0.049(2) 0.026(2) -0.010(2) -0.020(2) C22 0.056(2) 0.052(2) 0.045(2) 0.0145(18) -0.0057(18) -0.0226(19) C23 0.0275(18) 0.046(2) 0.0284(18) -0.0009(15) 0.0032(14) -0.0037(15) C24 0.048(2) 0.074(3) 0.035(2) -0.0170(19) -0.0060(17) 0.0065(19) C25 0.036(2) 0.060(2) 0.046(2) -0.0072(18) -0.0021(16) 0.0120(17) C26 0.039(2) 0.085(3) 0.036(2) -0.0048(19) 0.0088(16) 0.0024(19) C27 0.0337(19) 0.054(2) 0.0338(19) 0.0041(16) -0.0009(15) 0.0028(16) C28 0.040(2) 0.063(3) 0.048(2) -0.0178(19) 0.0120(17) -0.0106(18) C29 0.056(3) 0.077(3) 0.065(3) -0.016(2) 0.021(2) -0.031(2) C30 0.033(2) 0.081(3) 0.127(4) -0.024(3) 0.024(3) -0.021(2) C31 0.033(2) 0.051(3) 0.107(4) 0.000(2) -0.005(2) -0.0043(18) C32 0.0238(19) 0.039(2) 0.092(3) 0.010(2) -0.0094(19) 0.0006(15) C33 0.065(3) 0.104(4) 0.046(2) 0.020(2) -0.001(2) -0.007(3) C34 0.069(3) 0.112(4) 0.094(3) -0.069(3) 0.042(2) -0.048(3) C35 0.044(2) 0.090(3) 0.072(3) 0.017(2) -0.023(2) -0.012(2) C36 0.042(3) 0.046(3) 0.180(5) 0.028(3) -0.009(3) 0.0077(19) C37 0.047(2) 0.0247(19) 0.069(3) -0.0060(17) -0.0219(19) 0.0142(16) C38 0.059(3) 0.025(2) 0.078(3) -0.0122(18) -0.022(2) 0.0199(17) C39 0.043(2) 0.029(2) 0.085(3) -0.0238(19) 0.014(2) 0.0008(16) C40 0.057(2) 0.0308(19) 0.039(2) -0.0104(15) 0.0050(17) -0.0028(17) C41 0.048(2) 0.0302(19) 0.0288(18) -0.0080(14) 0.0103(15) -0.0037(15) C42 0.044(3) 0.048(3) 0.178(5) -0.040(3) -0.044(3) 0.012(2) C43 0.140(4) 0.040(2) 0.043(2) -0.0001(19) -0.028(3) 0.031(2) C44 0.101(3) 0.044(2) 0.069(3) -0.012(2) 0.055(2) -0.015(2) C45 0.077(3) 0.038(2) 0.043(2) -0.0087(17) -0.028(2) 0.0122(19) C46 0.0347(18) 0.0221(17) 0.0255(17) -0.0027(13) 0.0013(14) 0.0048(14) C47 0.045(2) 0.0228(18) 0.046(2) -0.0043(15) 0.0118(16) -0.0042(15) C48 0.039(2) 0.038(2) 0.056(2) -0.0133(17) -0.0066(17) -0.0113(16) C49 0.0337(19) 0.049(2) 0.0332(18) -0.0051(16) -0.0045(15) 0.0018(16) C50 0.0387(19) 0.0250(17) 0.0276(17) -0.0011(14) 0.0004(14) 0.0021(14) C51 0.062(2) 0.045(2) 0.034(2) 0.0005(16) -0.0045(17) 0.0212(18) C52 0.038(2) 0.0324(19) 0.046(2) -0.0124(16) 0.0087(16) 0.0015(15) C53 0.060(2) 0.035(2) 0.041(2) -0.0006(16) -0.0013(18) 0.0151(17) C54 0.058(2) 0.043(2) 0.0343(19) 0.0065(16) 0.0097(17) -0.0016(17) Li1 0.029(3) 0.028(3) 0.029(3) -0.002(2) 0.003(2) 0.003(2) _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 Zn1 N3 1.963(2) . ? Zn1 N2 1.964(2) . ? Zn1 N1 1.981(2) . ? Si1 N1 1.711(2) . ? Si1 C1 1.867(3) . ? Si1 C2 1.878(3) . ? Si1 C3 1.881(3) . ? Si2 N1 1.702(2) . ? Si2 C6 1.872(3) . ? Si2 C5 1.879(3) . ? Si2 C4 1.885(3) . ? Si3 N2 1.710(2) . ? Si3 C7 1.867(3) . ? Si3 C8 1.869(3) . ? Si3 C9 1.872(3) . ? Si4 N2 1.702(2) . ? Si4 C11 1.869(3) . ? Si4 C12 1.879(3) . ? Si4 C10 1.882(3) . ? Si5 N3 1.707(2) . ? Si5 C14 1.867(3) . ? Si5 C15 1.882(3) . ? Si5 C13 1.883(3) . ? Si6 N3 1.707(2) . ? Si6 C17 1.866(3) . ? Si6 C16 1.874(3) . ? Si6 C18 1.877(3) . ? O1 N4 1.291(3) . ? O1 Li1 1.951(5) . ? O2 N5 1.287(3) . ? O2 Li1 1.933(5) . ? O3 N6 1.292(3) . ? O3 Li1 1.926(5) . ? O4 N7 1.292(3) . ? O4 Li1 1.947(5) . ? N4 C19 1.498(3) . ? N4 C23 1.499(4) . ? N5 C28 1.484(4) . ? N5 C32 1.504(4) . ? N6 C41 1.490(4) . ? N6 C37 1.491(4) . ? N7 C50 1.495(3) . ? N7 C46 1.498(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? 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 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? 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 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C25 1.516(4) . ? C19 C20 1.522(4) . ? C19 C24 1.535(4) . ? C20 C21 1.510(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.522(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.527(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C27 1.519(4) . ? C23 C26 1.530(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.512(5) . ? C28 C29 1.534(5) . ? C28 C34 1.538(5) . ? C29 C30 1.508(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.498(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.527(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C36 1.527(5) . ? C32 C35 1.528(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.520(5) . ? C37 C38 1.530(4) . ? C37 C43 1.534(5) . ? C38 C39 1.516(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.513(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.528(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C45 1.518(4) . ? C41 C44 1.533(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.521(4) . ? C46 C51 1.527(4) . ? C46 C52 1.541(4) . ? C47 C48 1.516(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.510(4) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.527(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C53 1.517(4) . ? C50 C54 1.530(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn1 N2 121.48(9) . . ? N3 Zn1 N1 119.55(9) . . ? N2 Zn1 N1 118.97(9) . . ? N1 Si1 C1 112.07(12) . . ? N1 Si1 C2 113.48(14) . . ? C1 Si1 C2 105.83(15) . . ? N1 Si1 C3 113.74(13) . . ? C1 Si1 C3 106.85(16) . . ? C2 Si1 C3 104.18(15) . . ? N1 Si2 C6 111.89(12) . . ? N1 Si2 C5 114.03(14) . . ? C6 Si2 C5 105.58(14) . . ? N1 Si2 C4 114.13(13) . . ? C6 Si2 C4 106.05(15) . . ? C5 Si2 C4 104.37(15) . . ? N2 Si3 C7 112.86(13) . . ? N2 Si3 C8 112.90(13) . . ? C7 Si3 C8 104.53(14) . . ? N2 Si3 C9 114.70(14) . . ? C7 Si3 C9 106.35(18) . . ? C8 Si3 C9 104.61(16) . . ? N2 Si4 C11 111.92(13) . . ? N2 Si4 C12 113.24(13) . . ? C11 Si4 C12 105.68(16) . . ? N2 Si4 C10 112.98(13) . . ? C11 Si4 C10 105.84(15) . . ? C12 Si4 C10 106.59(16) . . ? N3 Si5 C14 112.48(12) . . ? N3 Si5 C15 113.77(12) . . ? C14 Si5 C15 105.14(14) . . ? N3 Si5 C13 112.29(13) . . ? C14 Si5 C13 106.30(14) . . ? C15 Si5 C13 106.24(16) . . ? N3 Si6 C17 113.02(13) . . ? N3 Si6 C16 113.63(12) . . ? C17 Si6 C16 106.23(15) . . ? N3 Si6 C18 114.10(12) . . ? C17 Si6 C18 104.09(14) . . ? C16 Si6 C18 104.87(15) . . ? N4 O1 Li1 146.6(2) . . ? N5 O2 Li1 155.7(2) . . ? N6 O3 Li1 151.0(2) . . ? N7 O4 Li1 147.4(2) . . ? Si2 N1 Si1 122.93(13) . . ? Si2 N1 Zn1 118.44(12) . . ? Si1 N1 Zn1 118.63(12) . . ? Si4 N2 Si3 124.89(14) . . ? Si4 N2 Zn1 118.13(12) . . ? Si3 N2 Zn1 116.95(12) . . ? Si6 N3 Si5 122.37(14) . . ? Si6 N3 Zn1 117.41(11) . . ? Si5 N3 Zn1 119.74(12) . . ? O1 N4 C19 116.7(2) . . ? O1 N4 C23 116.2(2) . . ? C19 N4 C23 124.2(2) . . ? O2 N5 C28 116.4(2) . . ? O2 N5 C32 114.3(3) . . ? C28 N5 C32 125.8(3) . . ? O3 N6 C41 117.2(2) . . ? O3 N6 C37 114.5(2) . . ? C41 N6 C37 125.1(2) . . ? O4 N7 C50 116.1(2) . . ? O4 N7 C46 116.3(2) . . ? C50 N7 C46 124.0(2) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5 . . ? Si3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si4 C10 H10A 109.5 . . ? Si4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si4 C11 H11A 109.5 . . ? Si4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si4 C12 H12A 109.5 . . ? Si4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si5 C13 H13A 109.5 . . ? Si5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si5 C14 H14A 109.5 . . ? Si5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si5 C15 H15A 109.5 . . ? Si5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si6 C16 H16A 109.5 . . ? Si6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si6 C17 H17A 109.5 . . ? Si6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si6 C18 H18A 109.5 . . ? Si6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C25 107.8(2) . . ? N4 C19 C20 108.2(2) . . ? C25 C19 C20 110.3(3) . . ? N4 C19 C24 109.3(2) . . ? C25 C19 C24 108.9(3) . . ? C20 C19 C24 112.2(3) . . ? C21 C20 C19 114.0(3) . . ? C21 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? C21 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C20 C21 C22 109.4(3) . . ? C20 C21 H21A 109.8 . . ? C22 C21 H21A 109.8 . . ? C20 C21 H21B 109.8 . . ? C22 C21 H21B 109.8 . . ? H21A C21 H21B 108.2 . . ? C21 C22 C23 113.0(3) . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N4 C23 C27 108.0(2) . . ? N4 C23 C22 108.3(2) . . ? C27 C23 C22 110.2(2) . . ? N4 C23 C26 109.0(2) . . ? C27 C23 C26 109.0(3) . . ? C22 C23 C26 112.2(3) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 H25A 109.5 . . ? C19 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C19 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N5 C28 C33 107.7(3) . . ? N5 C28 C29 109.3(3) . . ? C33 C28 C29 110.6(3) . . ? N5 C28 C34 108.4(3) . . ? C33 C28 C34 110.0(3) . . ? C29 C28 C34 110.7(3) . . ? C30 C29 C28 114.4(3) . . ? C30 C29 H29A 108.7 . . ? C28 C29 H29A 108.7 . . ? C30 C29 H29B 108.7 . . ? C28 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C31 C30 C29 108.2(3) . . ? C31 C30 H30A 110.1 . . ? C29 C30 H30A 110.1 . . ? C31 C30 H30B 110.1 . . ? C29 C30 H30B 110.1 . . ? H30A C30 H30B 108.4 . . ? C30 C31 C32 114.0(3) . . ? C30 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? C30 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? N5 C32 C36 108.1(3) . . ? N5 C32 C31 108.7(3) . . ? C36 C32 C31 112.4(3) . . ? N5 C32 C35 107.6(3) . . ? C36 C32 C35 110.2(3) . . ? C31 C32 C35 109.7(3) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C28 C34 H34A 109.5 . . ? C28 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C28 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N6 C37 C42 108.3(3) . . ? N6 C37 C38 109.8(2) . . ? C42 C37 C38 111.7(3) . . ? N6 C37 C43 107.7(3) . . ? C42 C37 C43 110.7(3) . . ? C38 C37 C43 108.6(3) . . ? C39 C38 C37 114.1(3) . . ? C39 C38 H38A 108.7 . . ? C37 C38 H38A 108.7 . . ? C39 C38 H38B 108.7 . . ? C37 C38 H38B 108.7 . . ? H38A C38 H38B 107.6 . . ? C40 C39 C38 107.5(3) . . ? C40 C39 H39A 110.2 . . ? C38 C39 H39A 110.2 . . ? C40 C39 H39B 110.2 . . ? C38 C39 H39B 110.2 . . ? H39A C39 H39B 108.5 . . ? C39 C40 C41 113.7(3) . . ? C39 C40 H40A 108.8 . . ? C41 C40 H40A 108.8 . . ? C39 C40 H40B 108.8 . . ? C41 C40 H40B 108.8 . . ? H40A C40 H40B 107.7 . . ? N6 C41 C45 107.8(2) . . ? N6 C41 C40 108.7(2) . . ? C45 C41 C40 109.7(3) . . ? N6 C41 C44 108.9(3) . . ? C45 C41 C44 109.9(3) . . ? C40 C41 C44 111.7(3) . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C37 C43 H43A 109.5 . . ? C37 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C37 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41 C45 H45A 109.5 . . ? C41 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N7 C46 C47 108.1(2) . . ? N7 C46 C51 107.9(2) . . ? C47 C46 C51 110.4(3) . . ? N7 C46 C52 110.1(2) . . ? C47 C46 C52 111.7(2) . . ? C51 C46 C52 108.5(2) . . ? C48 C47 C46 113.8(2) . . ? C48 C47 H47A 108.8 . . ? C46 C47 H47A 108.8 . . ? C48 C47 H47B 108.8 . . ? C46 C47 H47B 108.8 . . ? H47A C47 H47B 107.7 . . ? C49 C48 C47 109.0(2) . . ? C49 C48 H48A 109.9 . . ? C47 C48 H48A 109.9 . . ? C49 C48 H48B 109.9 . . ? C47 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? C48 C49 C50 114.2(3) . . ? C48 C49 H49A 108.7 . . ? C50 C49 H49A 108.7 . . ? C48 C49 H49B 108.7 . . ? C50 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? N7 C50 C53 108.4(2) . . ? N7 C50 C49 108.0(2) . . ? C53 C50 C49 109.8(3) . . ? N7 C50 C54 109.6(2) . . ? C53 C50 C54 109.3(3) . . ? C49 C50 C54 111.6(2) . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C46 C52 H52A 109.5 . . ? C46 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C46 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C50 C54 H54A 109.5 . . ? C50 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C50 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O3 Li1 O2 108.4(2) . . ? O3 Li1 O4 118.2(2) . . ? O2 Li1 O4 100.1(2) . . ? O3 Li1 O1 100.1(2) . . ? O2 Li1 O1 123.4(2) . . ? O4 Li1 O1 107.9(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Si2 N1 Si1 -164.61(15) . . . . ? C5 Si2 N1 Si1 75.6(2) . . . . ? C4 Si2 N1 Si1 -44.2(2) . . . . ? C6 Si2 N1 Zn1 15.41(19) . . . . ? C5 Si2 N1 Zn1 -104.33(17) . . . . ? C4 Si2 N1 Zn1 135.83(15) . . . . ? C1 Si1 N1 Si2 -165.30(16) . . . . ? C2 Si1 N1 Si2 74.9(2) . . . . ? C3 Si1 N1 Si2 -44.0(2) . . . . ? C1 Si1 N1 Zn1 14.68(19) . . . . ? C2 Si1 N1 Zn1 -105.12(16) . . . . ? C3 Si1 N1 Zn1 136.01(16) . . . . ? N3 Zn1 N1 Si2 -67.57(16) . . . . ? N2 Zn1 N1 Si2 112.03(14) . . . . ? N3 Zn1 N1 Si1 112.44(14) . . . . ? N2 Zn1 N1 Si1 -67.95(16) . . . . ? C11 Si4 N2 Si3 166.88(16) . . . . ? C12 Si4 N2 Si3 -73.8(2) . . . . ? C10 Si4 N2 Si3 47.5(2) . . . . ? C11 Si4 N2 Zn1 -10.81(19) . . . . ? C12 Si4 N2 Zn1 108.53(17) . . . . ? C10 Si4 N2 Zn1 -130.16(15) . . . . ? C7 Si3 N2 Si4 -109.89(18) . . . . ? C8 Si3 N2 Si4 131.84(17) . . . . ? C9 Si3 N2 Si4 12.1(2) . . . . ? C7 Si3 N2 Zn1 67.83(18) . . . . ? C8 Si3 N2 Zn1 -50.44(18) . . . . ? C9 Si3 N2 Zn1 -170.16(17) . . . . ? N3 Zn1 N2 Si4 -48.06(16) . . . . ? N1 Zn1 N2 Si4 132.34(13) . . . . ? N3 Zn1 N2 Si3 134.06(12) . . . . ? N1 Zn1 N2 Si3 -45.53(16) . . . . ? C17 Si6 N3 Si5 144.79(16) . . . . ? C16 Si6 N3 Si5 -94.05(18) . . . . ? C18 Si6 N3 Si5 26.1(2) . . . . ? C17 Si6 N3 Zn1 -43.21(18) . . . . ? C16 Si6 N3 Zn1 77.95(17) . . . . ? C18 Si6 N3 Zn1 -161.88(14) . . . . ? C14 Si5 N3 Si6 169.38(15) . . . . ? C15 Si5 N3 Si6 -71.2(2) . . . . ? C13 Si5 N3 Si6 49.5(2) . . . . ? C14 Si5 N3 Zn1 -2.44(18) . . . . ? C15 Si5 N3 Zn1 116.98(16) . . . . ? C13 Si5 N3 Zn1 -122.30(16) . . . . ? N2 Zn1 N3 Si6 135.13(12) . . . . ? N1 Zn1 N3 Si6 -45.28(16) . . . . ? N2 Zn1 N3 Si5 -52.65(16) . . . . ? N1 Zn1 N3 Si5 126.94(13) . . . . ? Li1 O1 N4 C19 83.6(4) . . . . ? Li1 O1 N4 C23 -114.8(4) . . . . ? Li1 O2 N5 C28 -19.7(7) . . . . ? Li1 O2 N5 C32 -179.9(5) . . . . ? Li1 O3 N6 C41 -19.3(6) . . . . ? Li1 O3 N6 C37 179.8(4) . . . . ? Li1 O4 N7 C50 88.5(4) . . . . ? Li1 O4 N7 C46 -112.3(4) . . . . ? O1 N4 C19 C25 -39.9(3) . . . . ? C23 N4 C19 C25 160.2(3) . . . . ? O1 N4 C19 C20 -159.2(3) . . . . ? C23 N4 C19 C20 40.9(4) . . . . ? O1 N4 C19 C24 78.3(3) . . . . ? C23 N4 C19 C24 -81.6(3) . . . . ? N4 C19 C20 C21 -47.6(4) . . . . ? C25 C19 C20 C21 -165.3(3) . . . . ? C24 C19 C20 C21 73.1(3) . . . . ? C19 C20 C21 C22 59.6(4) . . . . ? C20 C21 C22 C23 -59.6(4) . . . . ? O1 N4 C23 C27 39.1(3) . . . . ? C19 N4 C23 C27 -160.9(3) . . . . ? O1 N4 C23 C22 158.5(2) . . . . ? C19 N4 C23 C22 -41.5(4) . . . . ? O1 N4 C23 C26 -79.2(3) . . . . ? C19 N4 C23 C26 80.8(3) . . . . ? C21 C22 C23 N4 48.2(4) . . . . ? C21 C22 C23 C27 166.2(3) . . . . ? C21 C22 C23 C26 -72.2(4) . . . . ? O2 N5 C28 C33 50.5(4) . . . . ? C32 N5 C28 C33 -151.9(3) . . . . ? O2 N5 C28 C29 170.7(3) . . . . ? C32 N5 C28 C29 -31.7(4) . . . . ? O2 N5 C28 C34 -68.5(3) . . . . ? C32 N5 C28 C34 89.1(4) . . . . ? N5 C28 C29 C30 43.8(4) . . . . ? C33 C28 C29 C30 162.2(3) . . . . ? C34 C28 C29 C30 -75.6(4) . . . . ? C28 C29 C30 C31 -60.3(4) . . . . ? C29 C30 C31 C32 61.8(4) . . . . ? O2 N5 C32 C36 68.6(4) . . . . ? C28 N5 C32 C36 -89.4(4) . . . . ? O2 N5 C32 C31 -169.1(3) . . . . ? C28 N5 C32 C31 33.0(4) . . . . ? O2 N5 C32 C35 -50.4(3) . . . . ? C28 N5 C32 C35 151.7(3) . . . . ? C30 C31 C32 N5 -46.4(4) . . . . ? C30 C31 C32 C36 73.3(4) . . . . ? C30 C31 C32 C35 -163.8(3) . . . . ? O3 N6 C37 C42 70.3(4) . . . . ? C41 N6 C37 C42 -88.9(3) . . . . ? O3 N6 C37 C38 -167.5(3) . . . . ? C41 N6 C37 C38 33.3(4) . . . . ? O3 N6 C37 C43 -49.5(4) . . . . ? C41 N6 C37 C43 151.4(3) . . . . ? N6 C37 C38 C39 -44.3(4) . . . . ? C42 C37 C38 C39 75.9(4) . . . . ? C43 C37 C38 C39 -161.7(3) . . . . ? C37 C38 C39 C40 59.9(4) . . . . ? C38 C39 C40 C41 -62.4(4) . . . . ? O3 N6 C41 C45 47.3(3) . . . . ? C37 N6 C41 C45 -154.1(3) . . . . ? O3 N6 C41 C40 166.2(2) . . . . ? C37 N6 C41 C40 -35.2(4) . . . . ? O3 N6 C41 C44 -71.9(3) . . . . ? C37 N6 C41 C44 86.7(3) . . . . ? C39 C40 C41 N6 48.4(4) . . . . ? C39 C40 C41 C45 166.1(3) . . . . ? C39 C40 C41 C44 -71.7(4) . . . . ? O4 N7 C46 C47 160.4(2) . . . . ? C50 N7 C46 C47 -42.1(3) . . . . ? O4 N7 C46 C51 40.9(3) . . . . ? C50 N7 C46 C51 -161.6(3) . . . . ? O4 N7 C46 C52 -77.3(3) . . . . ? C50 N7 C46 C52 80.2(3) . . . . ? N7 C46 C47 C48 48.6(3) . . . . ? C51 C46 C47 C48 166.5(3) . . . . ? C52 C46 C47 C48 -72.6(3) . . . . ? C46 C47 C48 C49 -59.3(4) . . . . ? C47 C48 C49 C50 58.9(4) . . . . ? O4 N7 C50 C53 -42.1(3) . . . . ? C46 N7 C50 C53 160.4(3) . . . . ? O4 N7 C50 C49 -160.9(2) . . . . ? C46 N7 C50 C49 41.5(4) . . . . ? O4 N7 C50 C54 77.2(3) . . . . ? C46 N7 C50 C54 -80.3(3) . . . . ? C48 C49 C50 N7 -47.8(3) . . . . ? C48 C49 C50 C53 -165.9(3) . . . . ? C48 C49 C50 C54 72.8(3) . . . . ? N6 O3 Li1 O2 -59.7(6) . . . . ? N6 O3 Li1 O4 -172.5(4) . . . . ? N6 O3 Li1 O1 70.8(5) . . . . ? N5 O2 Li1 O3 -57.8(6) . . . . ? N5 O2 Li1 O4 66.6(6) . . . . ? N5 O2 Li1 O1 -174.0(4) . . . . ? N7 O4 Li1 O3 -81.6(5) . . . . ? N7 O4 Li1 O2 161.1(3) . . . . ? N7 O4 Li1 O1 30.9(5) . . . . ? N4 O1 Li1 O3 165.8(3) . . . . ? N4 O1 Li1 O2 -74.1(5) . . . . ? N4 O1 Li1 O4 41.6(5) . . . . ? _refine_diff_density_max 0.371 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.054 #===END