data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H46 Al Cl Li N3 O Si3' _chemical_formula_weight 474.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5500(2) _cell_length_b 16.0631(3) _cell_length_c 15.9430(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.4070(10) _cell_angle_gamma 90.00 _cell_volume 2955.28(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9959 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 32.79 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.293 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8880 _exptl_absorpt_correction_T_max 0.9752 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 36805 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 32.58 _reflns_number_total 10684 _reflns_number_gt 7311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.4595P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 10684 _refine_ls_number_parameters 313 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.30314(4) 0.20385(2) 0.53487(2) 0.01774(9) Uani 1 1 d . A . Li1 Li 0.2801(2) 0.34740(17) 0.61177(15) 0.0285(5) Uani 1 1 d . . . Cl1 Cl 0.33802(4) 0.12229(2) 0.63928(2) 0.03214(10) Uani 1 1 d . . . Si1 Si 0.55050(3) 0.29907(2) 0.55031(2) 0.01953(9) Uani 1 1 d . . . Si2 Si 0.04361(4) 0.23294(3) 0.59473(3) 0.03410(12) Uani 1 1 d . . . Si3 Si 0.29570(4) 0.06387(3) 0.38641(3) 0.02612(10) Uani 1 1 d . A . N1 N 0.40096(10) 0.29666(7) 0.53642(6) 0.0172(2) Uani 1 1 d . A . N2 N 0.16827(10) 0.26706(8) 0.54887(7) 0.0220(2) Uani 1 1 d . A . N3 N 0.29701(12) 0.16109(7) 0.43020(7) 0.0241(2) Uani 1 1 d . . . C1 C 0.35598(12) 0.35173(8) 0.46633(8) 0.0201(3) Uani 1 1 d . A . H1A H 0.4206 0.3642 0.4294 0.024 Uiso 1 1 calc R . . H1B H 0.3307 0.4051 0.4907 0.024 Uiso 1 1 calc R . . C2 C 0.14534(13) 0.30507(10) 0.46357(9) 0.0266(3) Uani 1 1 d . . . H2A H 0.1091 0.3603 0.4706 0.032 Uiso 1 1 calc R A . H2B H 0.0890 0.2696 0.4315 0.032 Uiso 1 1 calc R . . C3 C 0.28969(16) 0.23214(9) 0.37122(8) 0.0300(3) Uani 1 1 d . A . H3A H 0.2326 0.2186 0.3252 0.036 Uiso 1 1 calc R . . H3B H 0.3660 0.2395 0.3461 0.036 Uiso 1 1 calc R . . C4 C 0.25429(12) 0.31561(8) 0.41194(8) 0.0209(3) Uani 1 1 d . A . C5 C 0.22609(15) 0.37773(10) 0.34103(9) 0.0303(3) Uani 1 1 d . . . H5A H 0.1568 0.3592 0.3087 0.045 Uiso 1 1 calc R A . H5B H 0.2916 0.3810 0.3040 0.045 Uiso 1 1 calc R . . H5C H 0.2118 0.4328 0.3650 0.045 Uiso 1 1 calc R . . C11 C 0.62244(14) 0.25610(12) 0.45636(10) 0.0357(4) Uani 1 1 d . A . H11A H 0.5973 0.1985 0.4468 0.053 Uiso 1 1 calc R . . H11B H 0.7067 0.2576 0.4662 0.053 Uiso 1 1 calc R . . H11C H 0.6009 0.2898 0.4069 0.053 Uiso 1 1 calc R . . C12 C 0.59922(14) 0.40927(10) 0.56673(11) 0.0335(4) Uani 1 1 d . A . H12A H 0.5612 0.4329 0.6151 0.050 Uiso 1 1 calc R . . H12B H 0.5786 0.4421 0.5165 0.050 Uiso 1 1 calc R . . H12C H 0.6834 0.4105 0.5772 0.050 Uiso 1 1 calc R . . C13 C 0.59745(14) 0.23710(11) 0.64452(9) 0.0295(3) Uani 1 1 d . A . H13A H 0.5625 0.2604 0.6943 0.044 Uiso 1 1 calc R . . H13B H 0.6821 0.2391 0.6519 0.044 Uiso 1 1 calc R . . H13C H 0.5725 0.1792 0.6369 0.044 Uiso 1 1 calc R . . C21 C -0.07300(18) 0.3130(2) 0.58019(17) 0.0732(8) Uani 1 1 d . A . H21A H -0.0427 0.3676 0.5976 0.110 Uiso 1 1 calc R . . H21B H -0.1385 0.2982 0.6144 0.110 Uiso 1 1 calc R . . H21C H -0.0990 0.3151 0.5209 0.110 Uiso 1 1 calc R . . C22 C 0.07001(17) 0.21788(15) 0.70954(11) 0.0479(5) Uani 1 1 d . A . H22A H 0.1350 0.1794 0.7194 0.072 Uiso 1 1 calc R . . H22B H 0.0003 0.1947 0.7337 0.072 Uiso 1 1 calc R . . H22C H 0.0886 0.2716 0.7360 0.072 Uiso 1 1 calc R . . C23 C -0.0080(2) 0.13265(16) 0.54709(13) 0.0666(8) Uani 1 1 d . A . H23A H 0.0490 0.0888 0.5601 0.100 Uiso 1 1 calc R . . H23B H -0.0177 0.1391 0.4861 0.100 Uiso 1 1 calc R . . H23C H -0.0825 0.1174 0.5701 0.100 Uiso 1 1 calc R . . C31 C 0.15689(16) 0.04569(11) 0.32402(11) 0.0383(4) Uani 1 1 d . . . H31A H 0.0914 0.0513 0.3607 0.057 Uiso 1 1 calc R A . H31B H 0.1572 -0.0105 0.3001 0.057 Uiso 1 1 calc R . . H31C H 0.1495 0.0867 0.2786 0.057 Uiso 1 1 calc R . . C32 C 0.41676(17) 0.05145(12) 0.31297(12) 0.0445(4) Uani 1 1 d . . . H32A H 0.4909 0.0620 0.3433 0.067 Uiso 1 1 calc R A . H32B H 0.4067 0.0912 0.2667 0.067 Uiso 1 1 calc R . . H32C H 0.4161 -0.0053 0.2905 0.067 Uiso 1 1 calc R . . C33 C 0.31032(16) -0.01713(10) 0.46969(11) 0.0368(4) Uani 1 1 d . . . H33A H 0.2467 -0.0115 0.5081 0.055 Uiso 1 1 calc R A . H33B H 0.3845 -0.0100 0.5010 0.055 Uiso 1 1 calc R . . H33C H 0.3074 -0.0725 0.4438 0.055 Uiso 1 1 calc R . . O1 O 0.2665(11) 0.4385(6) 0.6857(6) 0.048(2) Uani 0.360(7) 1 d PU A 2 C6 C 0.2523(9) 0.5237(4) 0.6572(4) 0.054(2) Uani 0.360(7) 1 d PU A 2 H6A H 0.3234 0.5444 0.6317 0.065 Uiso 0.360(7) 1 calc PR A 2 H6B H 0.2326 0.5609 0.7040 0.065 Uiso 0.360(7) 1 calc PR A 2 C7 C 0.1458(7) 0.5170(5) 0.5880(3) 0.0372(16) Uani 0.360(7) 1 d PU A 2 H7A H 0.1038 0.5700 0.5851 0.056 Uiso 0.360(7) 1 calc PR A 2 H7B H 0.0930 0.4725 0.6040 0.056 Uiso 0.360(7) 1 calc PR A 2 H7C H 0.1762 0.5044 0.5329 0.056 Uiso 0.360(7) 1 calc PR A 2 C8 C 0.3208(12) 0.4337(6) 0.7674(7) 0.070(3) Uani 0.360(7) 1 d PU A 2 H8A H 0.2701 0.4597 0.8085 0.084 Uiso 0.360(7) 1 calc PR A 2 H8B H 0.3947 0.4650 0.7683 0.084 Uiso 0.360(7) 1 calc PR A 2 C9 C 0.3438(14) 0.3480(7) 0.7916(8) 0.057(4) Uani 0.360(7) 1 d PU A 2 H9A H 0.3314 0.3412 0.8517 0.086 Uiso 0.360(7) 1 calc PR A 2 H9B H 0.4242 0.3340 0.7803 0.086 Uiso 0.360(7) 1 calc PR A 2 H9C H 0.2913 0.3110 0.7593 0.086 Uiso 0.360(7) 1 calc PR A 2 O1A O 0.2646(6) 0.4291(4) 0.6956(4) 0.0581(12) Uani 0.640(7) 1 d PU A 1 C6A C 0.1906(4) 0.5051(3) 0.6824(3) 0.0606(11) Uani 0.640(7) 1 d PU A 1 H6AA H 0.1228 0.4995 0.7179 0.073 Uiso 0.640(7) 1 calc PR A 1 H6AB H 0.2357 0.5537 0.7034 0.073 Uiso 0.640(7) 1 calc PR A 1 C7A C 0.1534(10) 0.5214(6) 0.6089(7) 0.166(4) Uani 0.640(7) 1 d PU A 1 H7AA H 0.1032 0.5705 0.6097 0.250 Uiso 0.640(7) 1 calc PR A 1 H7AB H 0.1092 0.4738 0.5862 0.250 Uiso 0.640(7) 1 calc PR A 1 H7AC H 0.2190 0.5325 0.5734 0.250 Uiso 0.640(7) 1 calc PR A 1 C8A C 0.2890(5) 0.4152(5) 0.7808(4) 0.0677(16) Uani 0.640(7) 1 d PU A 1 H8AA H 0.2158 0.4115 0.8108 0.081 Uiso 0.640(7) 1 calc PR A 1 H8AB H 0.3351 0.4621 0.8049 0.081 Uiso 0.640(7) 1 calc PR A 1 C9A C 0.3561(8) 0.3351(6) 0.7915(5) 0.073(2) Uani 0.640(7) 1 d PU A 1 H9AA H 0.3849 0.3299 0.8500 0.109 Uiso 0.640(7) 1 calc PR A 1 H9AB H 0.4217 0.3355 0.7545 0.109 Uiso 0.640(7) 1 calc PR A 1 H9AC H 0.3053 0.2879 0.7771 0.109 Uiso 0.640(7) 1 calc PR A 1 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 Al1 0.0222(2) 0.01474(19) 0.01618(17) 0.00264(13) -0.00040(14) -0.00406(15) Li1 0.0307(14) 0.0294(14) 0.0258(12) -0.0069(10) 0.0051(10) -0.0015(11) Cl1 0.0404(2) 0.02828(19) 0.02729(17) 0.01457(14) -0.00426(15) -0.00702(16) Si1 0.01818(18) 0.01930(18) 0.02102(17) 0.00227(13) -0.00034(13) -0.00134(14) Si2 0.0216(2) 0.0519(3) 0.0289(2) 0.00359(19) 0.00155(16) -0.0128(2) Si3 0.0320(2) 0.01647(19) 0.0298(2) -0.00560(14) 0.00006(16) -0.00185(16) N1 0.0190(5) 0.0150(5) 0.0176(5) 0.0031(4) -0.0010(4) -0.0026(4) N2 0.0192(5) 0.0253(6) 0.0213(5) 0.0015(4) -0.0001(4) -0.0037(5) N3 0.0394(7) 0.0133(5) 0.0194(5) 0.0008(4) -0.0013(5) -0.0032(5) C1 0.0216(6) 0.0157(6) 0.0227(6) 0.0045(5) -0.0015(5) -0.0030(5) C2 0.0217(7) 0.0276(8) 0.0298(7) 0.0074(6) -0.0068(5) -0.0033(6) C3 0.0544(10) 0.0196(7) 0.0159(6) -0.0002(5) -0.0003(6) -0.0031(7) C4 0.0287(7) 0.0163(6) 0.0171(5) 0.0036(4) -0.0039(5) -0.0044(5) C5 0.0433(9) 0.0219(7) 0.0246(6) 0.0071(5) -0.0098(6) -0.0049(7) C11 0.0279(8) 0.0508(11) 0.0286(7) -0.0019(7) 0.0052(6) 0.0072(8) C12 0.0250(8) 0.0254(8) 0.0494(9) 0.0042(7) -0.0058(7) -0.0077(6) C13 0.0251(7) 0.0336(8) 0.0294(7) 0.0061(6) -0.0041(6) 0.0004(6) C21 0.0232(10) 0.114(2) 0.0832(17) 0.0297(16) 0.0157(10) 0.0107(12) C22 0.0342(10) 0.0801(16) 0.0302(8) 0.0030(9) 0.0114(7) -0.0085(10) C23 0.0674(15) 0.0851(18) 0.0475(11) -0.0033(11) 0.0054(10) -0.0576(14) C31 0.0453(10) 0.0293(9) 0.0395(9) -0.0111(7) -0.0081(7) -0.0028(8) C32 0.0475(11) 0.0372(10) 0.0495(10) -0.0168(8) 0.0120(8) -0.0025(8) C33 0.0411(10) 0.0161(7) 0.0526(10) 0.0023(6) -0.0059(8) -0.0015(7) O1 0.089(5) 0.025(2) 0.030(3) -0.003(2) -0.020(3) 0.022(3) C6 0.091(5) 0.028(3) 0.045(3) -0.002(2) 0.004(3) 0.007(3) C7 0.056(4) 0.032(3) 0.024(2) -0.0097(18) 0.0136(19) 0.027(3) C8 0.121(8) 0.037(3) 0.048(4) -0.011(3) -0.039(5) 0.014(5) C9 0.090(10) 0.033(3) 0.045(5) 0.014(3) -0.043(6) -0.014(4) O1A 0.061(3) 0.065(3) 0.050(2) -0.0405(17) 0.0215(18) -0.0115(18) C6A 0.066(2) 0.046(2) 0.072(2) -0.0369(16) 0.0364(19) -0.0169(17) C7A 0.212(10) 0.121(8) 0.163(6) 0.072(6) -0.033(7) -0.024(6) C8A 0.049(2) 0.107(4) 0.047(2) -0.049(2) 0.0123(16) -0.014(2) C9A 0.044(3) 0.123(6) 0.052(3) -0.030(3) 0.002(2) -0.009(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 Al1 N3 1.8032(12) . ? Al1 N1 1.8701(11) . ? Al1 N2 1.8805(13) . ? Al1 Cl1 2.1433(5) . ? Al1 Li1 2.630(3) . ? Li1 O1A 1.887(6) . ? Li1 O1 1.891(11) . ? Li1 N1 2.049(3) . ? Li1 N2 2.057(3) . ? Li1 C1 2.514(3) . ? Si1 N1 1.7326(12) . ? Si1 C13 1.8635(15) . ? Si1 C12 1.8725(16) . ? Si1 C11 1.8748(16) . ? Si2 N2 1.7311(12) . ? Si2 C22 1.8587(18) . ? Si2 C23 1.868(2) . ? Si2 C21 1.869(2) . ? Si3 N3 1.7105(12) . ? Si3 C33 1.8615(17) . ? Si3 C32 1.8717(19) . ? Si3 C31 1.8737(17) . ? N1 C1 1.5008(16) . ? N2 C2 1.5039(17) . ? N3 C3 1.4789(18) . ? C1 C4 1.5435(19) . ? C2 C4 1.542(2) . ? C3 C4 1.552(2) . ? C4 C5 1.5325(18) . ? O1 C8 1.423(12) . ? O1 C6 1.448(10) . ? C6 C7 1.622(11) . ? C8 C9 1.450(13) . ? O1A C8A 1.393(8) . ? O1A C6A 1.500(7) . ? C6A C7A 1.258(9) . ? C8A C9A 1.508(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Al1 N1 108.43(5) . . ? N3 Al1 N2 108.36(6) . . ? N1 Al1 N2 94.07(5) . . ? N3 Al1 Cl1 118.99(4) . . ? N1 Al1 Cl1 112.53(4) . . ? N2 Al1 Cl1 111.56(4) . . ? N3 Al1 Li1 139.86(7) . . ? N1 Al1 Li1 50.79(7) . . ? N2 Al1 Li1 51.01(7) . . ? Cl1 Al1 Li1 101.14(6) . . ? O1A Li1 O1 6.7(4) . . ? O1A Li1 N1 141.2(3) . . ? O1 Li1 N1 138.6(4) . . ? O1A Li1 N2 134.9(3) . . ? O1 Li1 N2 136.3(4) . . ? N1 Li1 N2 83.91(10) . . ? O1A Li1 C1 132.9(2) . . ? O1 Li1 C1 126.5(4) . . ? N1 Li1 C1 36.64(6) . . ? N2 Li1 C1 78.68(9) . . ? O1A Li1 Al1 162.6(2) . . ? O1 Li1 Al1 169.2(3) . . ? N1 Li1 Al1 45.02(6) . . ? N2 Li1 Al1 45.29(6) . . ? C1 Li1 Al1 63.15(6) . . ? N1 Si1 C13 110.23(6) . . ? N1 Si1 C12 109.34(7) . . ? C13 Si1 C12 108.47(7) . . ? N1 Si1 C11 111.26(7) . . ? C13 Si1 C11 108.88(8) . . ? C12 Si1 C11 108.61(8) . . ? N2 Si2 C22 110.62(7) . . ? N2 Si2 C23 111.00(9) . . ? C22 Si2 C23 108.94(11) . . ? N2 Si2 C21 109.72(9) . . ? C22 Si2 C21 107.41(11) . . ? C23 Si2 C21 109.06(13) . . ? N3 Si3 C33 110.37(7) . . ? N3 Si3 C32 111.01(8) . . ? C33 Si3 C32 108.90(9) . . ? N3 Si3 C31 110.59(7) . . ? C33 Si3 C31 108.64(8) . . ? C32 Si3 C31 107.24(9) . . ? C1 N1 Si1 113.21(8) . . ? C1 N1 Al1 105.66(8) . . ? Si1 N1 Al1 128.17(7) . . ? C1 N1 Li1 88.80(11) . . ? Si1 N1 Li1 128.05(9) . . ? Al1 N1 Li1 84.19(9) . . ? C2 N2 Si2 113.11(9) . . ? C2 N2 Al1 103.13(9) . . ? Si2 N2 Al1 125.94(7) . . ? C2 N2 Li1 105.62(11) . . ? Si2 N2 Li1 120.61(9) . . ? Al1 N2 Li1 83.70(9) . . ? C3 N3 Si3 116.47(9) . . ? C3 N3 Al1 107.06(9) . . ? Si3 N3 Al1 136.46(7) . . ? N1 C1 C4 115.36(10) . . ? N1 C1 Li1 54.56(9) . . ? C4 C1 Li1 102.79(10) . . ? N2 C2 C4 114.25(11) . . ? N3 C3 C4 114.19(11) . . ? C5 C4 C2 108.21(12) . . ? C5 C4 C1 107.63(11) . . ? C2 C4 C1 111.11(11) . . ? C5 C4 C3 107.79(11) . . ? C2 C4 C3 111.33(12) . . ? C1 C4 C3 110.61(12) . . ? C8 O1 C6 112.3(9) . . ? C8 O1 Li1 118.9(6) . . ? C6 O1 Li1 123.1(6) . . ? O1 C6 C7 103.0(7) . . ? O1 C8 C9 111.4(9) . . ? C8A O1A C6A 111.0(5) . . ? C8A O1A Li1 123.9(4) . . ? C6A O1A Li1 122.4(4) . . ? C7A C6A O1A 118.1(6) . . ? O1A C8A C9A 109.2(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 32.58 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.449 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.061 #===END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H44 Al N3 Si3' _chemical_formula_weight 545.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8773(3) _cell_length_b 11.8618(4) _cell_length_c 13.7028(5) _cell_angle_alpha 105.722(2) _cell_angle_beta 93.966(2) _cell_angle_gamma 96.701(2) _cell_volume 1526.28(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 8497 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 30.47 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9307 _exptl_absorpt_correction_T_max 0.9828 _exptl_absorpt_process_details 'SADABS, Scheldrick 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 44963 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 30.53 _reflns_number_total 9305 _reflns_number_gt 7058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.6057P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 9305 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.26639(4) 0.26725(4) 0.26323(3) 0.01456(9) Uani 1 1 d . . . Si1 Si 0.45123(4) 0.49979(3) 0.28600(3) 0.01432(8) Uani 1 1 d . . . Si2 Si 0.57929(4) 0.26286(3) 0.23770(3) 0.01466(8) Uani 1 1 d . . . Si3 Si 0.37924(4) 0.30766(3) 0.07423(3) 0.01472(8) Uani 1 1 d . . . N1 N 0.30431(12) 0.42912(10) 0.31427(9) 0.0158(2) Uani 1 1 d . . . N2 N 0.44704(12) 0.22490(11) 0.31554(9) 0.0171(2) Uani 1 1 d . . . N3 N 0.27124(12) 0.21880(10) 0.12461(9) 0.0166(2) Uani 1 1 d . . . C1 C 0.51537(13) 0.37996(11) 0.18566(10) 0.0136(2) Uani 1 1 d . . . H1A H 0.5942 0.4183 0.1586 0.016 Uiso 1 1 calc R . . C2 C 0.42794(18) 0.63398(13) 0.24249(12) 0.0246(3) Uani 1 1 d . . . H2A H 0.3914 0.6917 0.2960 0.037 Uiso 1 1 calc R . . H2B H 0.3638 0.6110 0.1804 0.037 Uiso 1 1 calc R . . H2C H 0.5165 0.6693 0.2284 0.037 Uiso 1 1 calc R . . C3 C 0.57803(15) 0.56340(13) 0.40251(11) 0.0214(3) Uani 1 1 d . . . H3A H 0.5474 0.6336 0.4465 0.032 Uiso 1 1 calc R . . H3B H 0.6681 0.5856 0.3819 0.032 Uiso 1 1 calc R . . H3C H 0.5847 0.5042 0.4399 0.032 Uiso 1 1 calc R . . C4 C 0.74685(15) 0.31518(14) 0.31769(12) 0.0224(3) Uani 1 1 d . . . H4A H 0.7773 0.2500 0.3407 0.034 Uiso 1 1 calc R . . H4B H 0.7365 0.3805 0.3770 0.034 Uiso 1 1 calc R . . H4C H 0.8150 0.3426 0.2774 0.034 Uiso 1 1 calc R . . C5 C 0.59947(18) 0.12275(14) 0.14181(12) 0.0263(3) Uani 1 1 d . . . H5A H 0.6433 0.0716 0.1758 0.039 Uiso 1 1 calc R . . H5B H 0.6566 0.1405 0.0907 0.039 Uiso 1 1 calc R . . H5C H 0.5091 0.0823 0.1084 0.039 Uiso 1 1 calc R . . C6 C 0.45435(16) 0.22237(14) -0.04100(11) 0.0228(3) Uani 1 1 d . . . H6A H 0.3853 0.2005 -0.1003 0.034 Uiso 1 1 calc R . . H6B H 0.4829 0.1506 -0.0287 0.034 Uiso 1 1 calc R . . H6C H 0.5340 0.2716 -0.0541 0.034 Uiso 1 1 calc R . . C7 C 0.29378(16) 0.41643(13) 0.02262(11) 0.0212(3) Uani 1 1 d . . . H7A H 0.2275 0.3735 -0.0360 0.032 Uiso 1 1 calc R . . H7B H 0.3632 0.4681 0.0011 0.032 Uiso 1 1 calc R . . H7C H 0.2462 0.4643 0.0758 0.032 Uiso 1 1 calc R . . C8 C 0.11754(16) 0.19378(15) 0.32352(12) 0.0247(3) Uani 1 1 d . . . H8A H 0.0320 0.2231 0.3084 0.037 Uiso 1 1 calc R . . H8B H 0.1401 0.2139 0.3975 0.037 Uiso 1 1 calc R . . H8C H 0.1063 0.1077 0.2947 0.037 Uiso 1 1 calc R . . C11 C 0.22089(15) 0.49749(13) 0.38626(11) 0.0193(3) Uani 1 1 d . . . H11A H 0.2812 0.5668 0.4322 0.023 Uiso 1 1 calc R . . H11B H 0.1845 0.4478 0.4287 0.023 Uiso 1 1 calc R . . C12 C 0.10098(14) 0.54145(12) 0.33876(10) 0.0159(3) Uani 1 1 d . . . C13 C 0.03505(15) 0.62741(13) 0.40064(11) 0.0201(3) Uani 1 1 d . . . H13A H 0.0656 0.6575 0.4713 0.024 Uiso 1 1 calc R . . C14 C -0.07500(16) 0.66957(14) 0.36006(12) 0.0232(3) Uani 1 1 d . . . H14A H -0.1184 0.7288 0.4028 0.028 Uiso 1 1 calc R . . C15 C -0.12156(15) 0.62508(14) 0.25693(12) 0.0229(3) Uani 1 1 d . . . H15A H -0.1970 0.6535 0.2291 0.027 Uiso 1 1 calc R . . C16 C -0.05736(15) 0.53928(14) 0.19515(11) 0.0216(3) Uani 1 1 d . . . H16A H -0.0890 0.5085 0.1247 0.026 Uiso 1 1 calc R . . C17 C 0.05372(15) 0.49765(13) 0.23586(11) 0.0183(3) Uani 1 1 d . . . H17A H 0.0974 0.4389 0.1928 0.022 Uiso 1 1 calc R . . C21 C 0.42938(16) 0.10277(13) 0.32883(12) 0.0215(3) Uani 1 1 d . . . H21A H 0.4042 0.0451 0.2609 0.026 Uiso 1 1 calc R . . H21B H 0.3516 0.0956 0.3697 0.026 Uiso 1 1 calc R . . C22 C 0.55350(16) 0.06861(13) 0.37973(11) 0.0200(3) Uani 1 1 d . . . C23 C 0.61330(19) 0.13328(14) 0.47593(12) 0.0275(3) Uani 1 1 d . . . H23A H 0.5771 0.2018 0.5113 0.033 Uiso 1 1 calc R . . C24 C 0.7260(2) 0.09913(16) 0.52165(14) 0.0348(4) Uani 1 1 d . . . H24A H 0.7669 0.1448 0.5874 0.042 Uiso 1 1 calc R . . C25 C 0.77817(19) -0.00133(19) 0.47116(16) 0.0394(5) Uani 1 1 d . . . H25A H 0.8556 -0.0246 0.5016 0.047 Uiso 1 1 calc R . . C26 C 0.7168(2) -0.06761(19) 0.37611(16) 0.0454(5) Uani 1 1 d . . . H26A H 0.7513 -0.1374 0.3414 0.054 Uiso 1 1 calc R . . C27 C 0.6049(2) -0.03259(16) 0.33113(13) 0.0340(4) Uani 1 1 d . . . H27A H 0.5632 -0.0791 0.2659 0.041 Uiso 1 1 calc R . . C31 C 0.18340(15) 0.11351(13) 0.05684(11) 0.0196(3) Uani 1 1 d . . . H31A H 0.1392 0.0671 0.0991 0.024 Uiso 1 1 calc R . . H31B H 0.2418 0.0631 0.0133 0.024 Uiso 1 1 calc R . . C32 C 0.07281(15) 0.14322(13) -0.01103(12) 0.0206(3) Uani 1 1 d . . . C33 C -0.02955(17) 0.20604(15) 0.03152(14) 0.0291(3) Uani 1 1 d . . . H33A H -0.0312 0.2288 0.1034 0.035 Uiso 1 1 calc R . . C34 C -0.12930(19) 0.23575(16) -0.02995(17) 0.0390(4) Uani 1 1 d . . . H34A H -0.1982 0.2790 0.0002 0.047 Uiso 1 1 calc R . . C35 C -0.1287(2) 0.20266(17) -0.13475(17) 0.0410(5) Uani 1 1 d . . . H35A H -0.1969 0.2232 -0.1766 0.049 Uiso 1 1 calc R . . C36 C -0.0286(2) 0.13954(16) -0.17817(14) 0.0349(4) Uani 1 1 d . . . H36A H -0.0279 0.1164 -0.2501 0.042 Uiso 1 1 calc R . . C37 C 0.07126(17) 0.10980(14) -0.11680(12) 0.0252(3) Uani 1 1 d . . . H37A H 0.1395 0.0660 -0.1474 0.030 Uiso 1 1 calc R . . H1 H 0.469(2) 0.2735(19) 0.3803(17) 0.044(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.01253(19) 0.0175(2) 0.01522(19) 0.00686(16) 0.00266(15) 0.00256(15) Si1 0.01584(18) 0.01388(17) 0.01393(17) 0.00475(14) 0.00098(13) 0.00328(13) Si2 0.01384(17) 0.01607(18) 0.01647(18) 0.00678(14) 0.00388(13) 0.00519(14) Si3 0.01586(18) 0.01644(18) 0.01251(17) 0.00554(14) 0.00154(13) 0.00134(14) N1 0.0139(5) 0.0177(5) 0.0160(5) 0.0036(4) 0.0027(4) 0.0048(4) N2 0.0167(6) 0.0191(6) 0.0188(6) 0.0098(5) 0.0030(4) 0.0045(4) N3 0.0169(6) 0.0163(5) 0.0157(5) 0.0051(4) 0.0011(4) -0.0020(4) C1 0.0131(6) 0.0144(6) 0.0145(6) 0.0058(5) 0.0022(5) 0.0020(5) C2 0.0349(9) 0.0180(7) 0.0228(7) 0.0082(6) 0.0005(6) 0.0064(6) C3 0.0208(7) 0.0229(7) 0.0183(7) 0.0039(6) -0.0003(5) 0.0007(6) C4 0.0153(7) 0.0293(8) 0.0260(7) 0.0129(6) 0.0007(6) 0.0057(6) C5 0.0367(9) 0.0225(7) 0.0242(8) 0.0081(6) 0.0097(7) 0.0146(7) C6 0.0268(8) 0.0258(7) 0.0154(6) 0.0048(6) 0.0049(6) 0.0029(6) C7 0.0235(7) 0.0237(7) 0.0182(7) 0.0102(6) -0.0014(5) 0.0026(6) C8 0.0187(7) 0.0309(8) 0.0276(8) 0.0129(6) 0.0067(6) 0.0018(6) C11 0.0183(7) 0.0245(7) 0.0155(6) 0.0039(5) 0.0021(5) 0.0086(5) C12 0.0132(6) 0.0176(6) 0.0177(6) 0.0062(5) 0.0022(5) 0.0026(5) C13 0.0179(7) 0.0223(7) 0.0195(7) 0.0035(6) 0.0028(5) 0.0051(5) C14 0.0200(7) 0.0222(7) 0.0280(8) 0.0051(6) 0.0048(6) 0.0096(6) C15 0.0181(7) 0.0265(8) 0.0282(8) 0.0126(6) 0.0020(6) 0.0082(6) C16 0.0199(7) 0.0277(8) 0.0195(7) 0.0097(6) 0.0006(5) 0.0059(6) C17 0.0177(7) 0.0205(7) 0.0183(7) 0.0060(5) 0.0039(5) 0.0063(5) C21 0.0227(7) 0.0191(7) 0.0251(7) 0.0105(6) 0.0017(6) 0.0029(6) C22 0.0235(7) 0.0194(7) 0.0235(7) 0.0135(6) 0.0077(6) 0.0075(6) C23 0.0393(9) 0.0199(7) 0.0257(8) 0.0081(6) 0.0032(7) 0.0094(7) C24 0.0401(10) 0.0316(9) 0.0330(9) 0.0167(7) -0.0098(8) -0.0037(8) C25 0.0280(9) 0.0563(12) 0.0513(12) 0.0384(10) 0.0069(8) 0.0184(9) C26 0.0646(14) 0.0471(12) 0.0394(11) 0.0201(9) 0.0177(10) 0.0421(11) C27 0.0510(11) 0.0305(9) 0.0237(8) 0.0080(7) 0.0028(7) 0.0183(8) C31 0.0203(7) 0.0170(6) 0.0194(7) 0.0040(5) -0.0011(5) -0.0013(5) C32 0.0177(7) 0.0166(6) 0.0252(7) 0.0058(6) -0.0023(5) -0.0041(5) C33 0.0216(8) 0.0275(8) 0.0347(9) 0.0046(7) -0.0007(7) 0.0006(6) C34 0.0230(9) 0.0303(9) 0.0600(13) 0.0087(9) -0.0064(8) 0.0049(7) C35 0.0331(10) 0.0320(9) 0.0579(13) 0.0213(9) -0.0189(9) -0.0023(8) C36 0.0401(10) 0.0305(9) 0.0327(9) 0.0167(7) -0.0117(8) -0.0099(8) C37 0.0265(8) 0.0216(7) 0.0257(8) 0.0082(6) -0.0018(6) -0.0045(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N3 1.8351(12) . ? Al1 N1 1.8397(12) . ? Al1 C8 1.9654(15) . ? Al1 N2 2.0438(13) . ? Si1 N1 1.7113(12) . ? Si1 C2 1.8769(15) . ? Si1 C3 1.8807(15) . ? Si1 C1 1.8930(14) . ? Si2 N2 1.8337(12) . ? Si2 C5 1.8597(16) . ? Si2 C4 1.8619(15) . ? Si2 C1 1.8750(13) . ? Si3 N3 1.7202(12) . ? Si3 C6 1.8812(15) . ? Si3 C7 1.8825(15) . ? Si3 C1 1.9005(13) . ? N1 C11 1.4644(18) . ? N2 C21 1.5003(18) . ? N3 C31 1.4772(18) . ? C11 C12 1.5231(19) . ? C12 C17 1.3898(19) . ? C12 C13 1.3948(19) . ? C13 C14 1.391(2) . ? C14 C15 1.392(2) . ? C15 C16 1.383(2) . ? C16 C17 1.396(2) . ? C21 C22 1.518(2) . ? C22 C27 1.378(2) . ? C22 C23 1.383(2) . ? C23 C24 1.393(2) . ? C24 C25 1.382(3) . ? C25 C26 1.381(3) . ? C26 C27 1.388(3) . ? C31 C32 1.520(2) . ? C32 C33 1.393(2) . ? C32 C37 1.394(2) . ? C33 C34 1.390(2) . ? C34 C35 1.383(3) . ? C35 C36 1.381(3) . ? C36 C37 1.389(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Al1 N1 111.83(5) . . ? N3 Al1 C8 119.00(6) . . ? N1 Al1 C8 114.40(7) . . ? N3 Al1 N2 102.00(5) . . ? N1 Al1 N2 98.49(5) . . ? C8 Al1 N2 108.06(6) . . ? N1 Si1 C2 114.67(7) . . ? N1 Si1 C3 111.34(6) . . ? C2 Si1 C3 102.12(7) . . ? N1 Si1 C1 103.52(6) . . ? C2 Si1 C1 112.80(7) . . ? C3 Si1 C1 112.75(6) . . ? N2 Si2 C5 106.52(7) . . ? N2 Si2 C4 109.86(6) . . ? C5 Si2 C4 106.53(8) . . ? N2 Si2 C1 104.99(6) . . ? C5 Si2 C1 115.96(7) . . ? C4 Si2 C1 112.75(7) . . ? N3 Si3 C6 112.98(7) . . ? N3 Si3 C7 114.56(7) . . ? C6 Si3 C7 101.79(7) . . ? N3 Si3 C1 102.15(6) . . ? C6 Si3 C1 112.06(7) . . ? C7 Si3 C1 113.75(6) . . ? C11 N1 Si1 118.99(10) . . ? C11 N1 Al1 122.18(10) . . ? Si1 N1 Al1 118.52(7) . . ? C21 N2 Si2 118.55(10) . . ? C21 N2 Al1 111.64(9) . . ? Si2 N2 Al1 107.99(6) . . ? C31 N3 Si3 120.24(9) . . ? C31 N3 Al1 123.36(9) . . ? Si3 N3 Al1 116.32(6) . . ? Si2 C1 Si1 113.01(7) . . ? Si2 C1 Si3 109.29(7) . . ? Si1 C1 Si3 111.84(7) . . ? N1 C11 C12 115.68(11) . . ? C17 C12 C13 118.76(13) . . ? C17 C12 C11 122.17(12) . . ? C13 C12 C11 119.06(12) . . ? C14 C13 C12 120.72(14) . . ? C13 C14 C15 120.07(14) . . ? C16 C15 C14 119.60(14) . . ? C15 C16 C17 120.26(14) . . ? C12 C17 C16 120.59(13) . . ? N2 C21 C22 115.65(12) . . ? C27 C22 C23 118.63(15) . . ? C27 C22 C21 119.38(14) . . ? C23 C22 C21 121.92(14) . . ? C22 C23 C24 120.84(15) . . ? C25 C24 C23 119.88(17) . . ? C26 C25 C24 119.45(16) . . ? C25 C26 C27 120.20(17) . . ? C22 C27 C26 120.97(17) . . ? N3 C31 C32 113.51(12) . . ? C33 C32 C37 118.16(15) . . ? C33 C32 C31 120.45(14) . . ? C37 C32 C31 121.39(14) . . ? C34 C33 C32 120.77(17) . . ? C35 C34 C33 120.32(18) . . ? C36 C35 C34 119.62(17) . . ? C35 C36 C37 120.13(17) . . ? C36 C37 C32 121.00(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.422 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.059 #===END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H53 Al2 N3 Si3' _chemical_formula_weight 618.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 39.9056(13) _cell_length_b 9.3888(3) _cell_length_c 19.4839(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7299.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7195 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 27.41 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78291 _diffrn_reflns_av_R_equivalents 0.0873 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.26 _reflns_number_total 17704 _reflns_number_gt 13114 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.4417P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.09(8) _refine_ls_number_reflns 17704 _refine_ls_number_parameters 747 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.76406(2) 0.39738(9) 0.99051(4) 0.01376(18) Uani 1 1 d . . . Al2 Al 0.73013(2) 0.59815(9) 0.91513(5) 0.01576(18) Uani 1 1 d . . . Si1 Si 0.76559(2) 0.35555(8) 0.83041(4) 0.01395(17) Uani 1 1 d . . . Si2 Si 0.80974(2) 0.60836(8) 0.90869(4) 0.01501(17) Uani 1 1 d . . . Si3 Si 0.82805(2) 0.49732(9) 0.75791(4) 0.01665(17) Uani 1 1 d . . . N1 N 0.73930(6) 0.3919(2) 0.90364(12) 0.0130(5) Uani 1 1 d . . . N2 N 0.77371(6) 0.5971(2) 0.96458(12) 0.0140(5) Uani 1 1 d . . . N3 N 0.82389(6) 0.3539(3) 0.70155(12) 0.0207(6) Uani 1 1 d . . . H3A H 0.8080 0.3669 0.6708 0.025 Uiso 1 1 calc R . . C1 C 0.80523(7) 0.4629(3) 0.84158(13) 0.0143(6) Uani 1 1 d . . . H1A H 0.8202 0.3886 0.8619 0.017 Uiso 1 1 calc R . . C2 C 0.77711(8) 0.1637(3) 0.83000(16) 0.0204(6) Uani 1 1 d . . . H2A H 0.7569 0.1059 0.8237 0.031 Uiso 1 1 calc R . . H2B H 0.7877 0.1389 0.8737 0.031 Uiso 1 1 calc R . . H2C H 0.7928 0.1451 0.7923 0.031 Uiso 1 1 calc R . . C3 C 0.74051(8) 0.3899(3) 0.75136(15) 0.0191(7) Uani 1 1 d . . . H3B H 0.7196 0.3353 0.7534 0.029 Uiso 1 1 calc R . . H3C H 0.7534 0.3606 0.7109 0.029 Uiso 1 1 calc R . . H3D H 0.7353 0.4917 0.7482 0.029 Uiso 1 1 calc R . . C4 C 0.81311(8) 0.7957(3) 0.87564(16) 0.0208(7) Uani 1 1 d . . . H4A H 0.8162 0.8612 0.9143 0.031 Uiso 1 1 calc R . . H4B H 0.7926 0.8207 0.8509 0.031 Uiso 1 1 calc R . . H4C H 0.8323 0.8030 0.8445 0.031 Uiso 1 1 calc R . . C5 C 0.84886(8) 0.5747(3) 0.95892(15) 0.0207(7) Uani 1 1 d . . . H5A H 0.8483 0.6303 1.0015 0.031 Uiso 1 1 calc R . . H5B H 0.8684 0.6029 0.9316 0.031 Uiso 1 1 calc R . . H5C H 0.8504 0.4731 0.9700 0.031 Uiso 1 1 calc R . . C6 C 0.80985(8) 0.6485(3) 0.70814(15) 0.0210(7) Uani 1 1 d . . . H6A H 0.8191 0.6485 0.6616 0.032 Uiso 1 1 calc R . . H6B H 0.8154 0.7386 0.7309 0.032 Uiso 1 1 calc R . . H6C H 0.7854 0.6379 0.7058 0.032 Uiso 1 1 calc R . . C7 C 0.87349(8) 0.5277(4) 0.77700(16) 0.0250(7) Uani 1 1 d . . . H7A H 0.8864 0.5223 0.7343 0.037 Uiso 1 1 calc R . . H7B H 0.8814 0.4547 0.8090 0.037 Uiso 1 1 calc R . . H7C H 0.8764 0.6221 0.7976 0.037 Uiso 1 1 calc R . . C11 C 0.71023(7) 0.2969(3) 0.90432(14) 0.0154(6) Uani 1 1 d . . . C12 C 0.68003(8) 0.3366(3) 0.87428(16) 0.0226(7) Uani 1 1 d . . . H12A H 0.6783 0.4259 0.8516 0.027 Uiso 1 1 calc R . . C13 C 0.65249(8) 0.2471(4) 0.87719(17) 0.0297(8) Uani 1 1 d . . . H13A H 0.6320 0.2760 0.8565 0.036 Uiso 1 1 calc R . . C14 C 0.65427(8) 0.1162(4) 0.90977(18) 0.0311(8) Uani 1 1 d . . . C15 C 0.68454(9) 0.0755(3) 0.93895(16) 0.0255(7) Uani 1 1 d . . . H15A H 0.6863 -0.0143 0.9611 0.031 Uiso 1 1 calc R . . C16 C 0.71222(8) 0.1645(3) 0.93611(15) 0.0196(7) Uani 1 1 d . . . H16A H 0.7328 0.1348 0.9561 0.023 Uiso 1 1 calc R . . C17 C 0.62361(10) 0.0203(4) 0.9147(2) 0.0499(11) Uani 1 1 d . . . H17A H 0.6099 0.0314 0.8732 0.075 Uiso 1 1 calc R . . H17B H 0.6104 0.0470 0.9550 0.075 Uiso 1 1 calc R . . H17C H 0.6308 -0.0791 0.9189 0.075 Uiso 1 1 calc R . . C21 C 0.77507(7) 0.6987(3) 1.02130(14) 0.0145(6) Uani 1 1 d . . . C22 C 0.76080(8) 0.8335(3) 1.01438(16) 0.0198(7) Uani 1 1 d . . . H22A H 0.7516 0.8615 0.9715 0.024 Uiso 1 1 calc R . . C23 C 0.75996(9) 0.9271(3) 1.06940(15) 0.0236(7) Uani 1 1 d . . . H23A H 0.7498 1.0178 1.0636 0.028 Uiso 1 1 calc R . . C24 C 0.77355(9) 0.8919(3) 1.13262(16) 0.0244(7) Uani 1 1 d . . . C25 C 0.78825(8) 0.7564(3) 1.13905(15) 0.0221(7) Uani 1 1 d . . . H25A H 0.7978 0.7290 1.1817 0.027 Uiso 1 1 calc R . . C26 C 0.78902(7) 0.6621(3) 1.08430(15) 0.0167(6) Uani 1 1 d . . . H26A H 0.7992 0.5714 1.0899 0.020 Uiso 1 1 calc R . . C27 C 0.77349(12) 0.9958(4) 1.19123(18) 0.0436(11) Uani 1 1 d . . . H27A H 0.7513 1.0396 1.1951 0.065 Uiso 1 1 calc R . . H27B H 0.7903 1.0699 1.1829 0.065 Uiso 1 1 calc R . . H27C H 0.7788 0.9456 1.2339 0.065 Uiso 1 1 calc R . . C31 C 0.84021(7) 0.2229(3) 0.69445(15) 0.0169(6) Uani 1 1 d . . . C32 C 0.86131(8) 0.1674(3) 0.74503(16) 0.0242(7) Uani 1 1 d . . . H32A H 0.8641 0.2173 0.7871 0.029 Uiso 1 1 calc R . . C33 C 0.87819(9) 0.0401(3) 0.73450(17) 0.0261(7) Uani 1 1 d . . . H33A H 0.8926 0.0055 0.7695 0.031 Uiso 1 1 calc R . . C34 C 0.87476(8) -0.0384(3) 0.67477(17) 0.0229(7) Uani 1 1 d . . . C35 C 0.85296(8) 0.0140(3) 0.62600(17) 0.0268(7) Uani 1 1 d . . . H35A H 0.8494 -0.0390 0.5851 0.032 Uiso 1 1 calc R . . C36 C 0.83601(8) 0.1417(3) 0.63485(15) 0.0232(7) Uani 1 1 d . . . H36A H 0.8213 0.1745 0.5999 0.028 Uiso 1 1 calc R . . C37 C 0.89469(9) -0.1727(3) 0.6616(2) 0.0341(9) Uani 1 1 d . . . H37A H 0.9094 -0.1917 0.7008 0.051 Uiso 1 1 calc R . . H37B H 0.9083 -0.1605 0.6201 0.051 Uiso 1 1 calc R . . H37C H 0.8793 -0.2530 0.6552 0.051 Uiso 1 1 calc R . . C41 C 0.80278(7) 0.2706(3) 1.00420(17) 0.0209(7) Uani 1 1 d . . . H41A H 0.7949 0.1731 1.0121 0.031 Uiso 1 1 calc R . . H41B H 0.8157 0.3029 1.0440 0.031 Uiso 1 1 calc R . . H41C H 0.8170 0.2727 0.9633 0.031 Uiso 1 1 calc R . . C42 C 0.73207(8) 0.3869(3) 1.06732(15) 0.0196(7) Uani 1 1 d . . . H42A H 0.7367 0.3017 1.0948 0.029 Uiso 1 1 calc R . . H42B H 0.7092 0.3819 1.0492 0.029 Uiso 1 1 calc R . . H42C H 0.7344 0.4718 1.0962 0.029 Uiso 1 1 calc R . . C43 C 0.69154(8) 0.6365(3) 0.97592(17) 0.0242(7) Uani 1 1 d . . . H43A H 0.6771 0.7088 0.9549 0.036 Uiso 1 1 calc R . . H43B H 0.6996 0.6713 1.0204 0.036 Uiso 1 1 calc R . . H43C H 0.6787 0.5486 0.9827 0.036 Uiso 1 1 calc R . . C44 C 0.72847(8) 0.7168(3) 0.83215(16) 0.0239(7) Uani 1 1 d . . . H44A H 0.7075 0.6989 0.8076 0.036 Uiso 1 1 calc R . . H44B H 0.7475 0.6932 0.8023 0.036 Uiso 1 1 calc R . . H44C H 0.7297 0.8175 0.8451 0.036 Uiso 1 1 calc R . . Al3 Al 1.00668(2) 1.11985(9) 1.01026(5) 0.01710(19) Uani 1 1 d . . . Al4 Al 0.97352(2) 0.92656(9) 0.92733(4) 0.01606(19) Uani 1 1 d . . . Si6 Si 0.96254(2) 0.89243(8) 1.08714(4) 0.01786(18) Uani 1 1 d . . . Si7 Si 0.92921(2) 1.16261(8) 1.00072(4) 0.01608(17) Uani 1 1 d . . . Si8 Si 0.89026(2) 1.01609(9) 1.12207(5) 0.0228(2) Uani 1 1 d . . . N6 N 0.99341(6) 0.9163(2) 1.02026(12) 0.0157(5) Uani 1 1 d . . . N7 N 0.96655(6) 1.1310(2) 0.95089(12) 0.0141(5) Uani 1 1 d . . . N8 N 0.87099(7) 1.1794(3) 1.13632(13) 0.0247(6) Uani 1 1 d . . . H8A H 0.8530 1.1953 1.1114 0.030 Uiso 1 1 calc R . . C51 C 0.93209(7) 1.0447(3) 1.07918(15) 0.0169(6) Uani 1 1 d . . . H51A H 0.9424 1.1133 1.1123 0.020 Uiso 1 1 calc R . . C52 C 0.98331(9) 0.9021(4) 1.17266(16) 0.0269(8) Uani 1 1 d . . . H52A H 0.9947 0.9941 1.1774 0.040 Uiso 1 1 calc R . . H52B H 0.9997 0.8250 1.1767 0.040 Uiso 1 1 calc R . . H52C H 0.9664 0.8925 1.2089 0.040 Uiso 1 1 calc R . . C53 C 0.94419(9) 0.7102(3) 1.08052(18) 0.0284(8) Uani 1 1 d . . . H53A H 0.9303 0.7041 1.0392 0.043 Uiso 1 1 calc R . . H53B H 0.9304 0.6910 1.1211 0.043 Uiso 1 1 calc R . . H53C H 0.9623 0.6398 1.0778 0.043 Uiso 1 1 calc R . . C54 C 0.92856(8) 1.3535(3) 1.02746(16) 0.0235(7) Uani 1 1 d . . . H54A H 0.9269 1.4143 0.9867 0.035 Uiso 1 1 calc R . . H54B H 0.9492 1.3761 1.0523 0.035 Uiso 1 1 calc R . . H54C H 0.9092 1.3705 1.0574 0.035 Uiso 1 1 calc R . . C55 C 0.89163(8) 1.1386(4) 0.94470(16) 0.0264(7) Uani 1 1 d . . . H55A H 0.8926 1.2064 0.9065 0.040 Uiso 1 1 calc R . . H55B H 0.8713 1.1556 0.9716 0.040 Uiso 1 1 calc R . . H55C H 0.8913 1.0412 0.9266 0.040 Uiso 1 1 calc R . . C56 C 0.89370(10) 0.9229(4) 1.20689(19) 0.0389(9) Uani 1 1 d . . . H56A H 0.8719 0.9251 1.2302 0.058 Uiso 1 1 calc R . . H56B H 0.9105 0.9712 1.2354 0.058 Uiso 1 1 calc R . . H56C H 0.9005 0.8238 1.1995 0.058 Uiso 1 1 calc R . . C57 C 0.86104(9) 0.9118(4) 1.0664(2) 0.0366(9) Uani 1 1 d . . . H57A H 0.8381 0.9466 1.0729 0.055 Uiso 1 1 calc R . . H57B H 0.8622 0.8108 1.0790 0.055 Uiso 1 1 calc R . . H57C H 0.8675 0.9233 1.0182 0.055 Uiso 1 1 calc R . . C61 C 1.02146(7) 0.8172(3) 1.02889(15) 0.0173(6) Uani 1 1 d . . . C62 C 1.04880(8) 0.8519(3) 1.06981(15) 0.0206(7) Uani 1 1 d . . . H62A H 1.0489 0.9395 1.0942 0.025 Uiso 1 1 calc R . . C63 C 1.07605(8) 0.7605(3) 1.07555(16) 0.0249(7) Uani 1 1 d . . . H63A H 1.0946 0.7874 1.1031 0.030 Uiso 1 1 calc R . . C64 C 1.07654(8) 0.6295(3) 1.04150(17) 0.0244(7) Uani 1 1 d . . . C65 C 1.04889(8) 0.5934(3) 1.00199(17) 0.0257(7) Uani 1 1 d . . . H65A H 1.0485 0.5045 0.9787 0.031 Uiso 1 1 calc R . . C66 C 1.02154(8) 0.6856(3) 0.99587(16) 0.0198(7) Uani 1 1 d . . . H66A H 1.0028 0.6582 0.9689 0.024 Uiso 1 1 calc R . . C67 C 1.10659(9) 0.5319(4) 1.0468(2) 0.0394(9) Uani 1 1 d . . . H67A H 1.0993 0.4327 1.0422 0.059 Uiso 1 1 calc R . . H67B H 1.1174 0.5452 1.0914 0.059 Uiso 1 1 calc R . . H67C H 1.1225 0.5545 1.0101 0.059 Uiso 1 1 calc R . . C71 C 0.96784(7) 1.2282(3) 0.89249(15) 0.0166(6) Uani 1 1 d . . . C72 C 0.98368(8) 1.3603(3) 0.89800(16) 0.0210(7) Uani 1 1 d . . . H72A H 0.9936 1.3874 0.9403 0.025 Uiso 1 1 calc R . . C73 C 0.98509(8) 1.4521(3) 0.84270(17) 0.0252(7) Uani 1 1 d . . . H73A H 0.9965 1.5403 0.8473 0.030 Uiso 1 1 calc R . . C74 C 0.97006(9) 1.4180(3) 0.78033(17) 0.0270(8) Uani 1 1 d . . . C75 C 0.95393(8) 1.2867(3) 0.77522(16) 0.0240(7) Uani 1 1 d . . . H75A H 0.9435 1.2607 0.7332 0.029 Uiso 1 1 calc R . . C76 C 0.95285(8) 1.1932(3) 0.83032(16) 0.0206(7) Uani 1 1 d . . . H76A H 0.9417 1.1043 0.8255 0.025 Uiso 1 1 calc R . . C77 C 0.97184(11) 1.5172(4) 0.71972(19) 0.0403(10) Uani 1 1 d . . . H77A H 0.9652 1.6132 0.7340 0.060 Uiso 1 1 calc R . . H77B H 0.9566 1.4836 0.6837 0.060 Uiso 1 1 calc R . . H77C H 0.9948 1.5193 0.7020 0.060 Uiso 1 1 calc R . . C81 C 0.87971(8) 1.2899(3) 1.18156(15) 0.0215(7) Uani 1 1 d . . . C82 C 0.90973(9) 1.2871(4) 1.21856(16) 0.0270(8) Uani 1 1 d . . . H82A H 0.9248 1.2101 1.2119 0.032 Uiso 1 1 calc R . . C83 C 0.91805(9) 1.3943(4) 1.26488(17) 0.0318(8) Uani 1 1 d . . . H83A H 0.9386 1.3891 1.2894 0.038 Uiso 1 1 calc R . . C84 C 0.89647(11) 1.5098(4) 1.27571(18) 0.0368(9) Uani 1 1 d . . . C85 C 0.86741(11) 1.5138(4) 1.23756(18) 0.0381(10) Uani 1 1 d . . . H85A H 0.8528 1.5929 1.2427 0.046 Uiso 1 1 calc R . . C86 C 0.85874(9) 1.4062(3) 1.19186(17) 0.0313(8) Uani 1 1 d . . . H86A H 0.8382 1.4122 1.1673 0.038 Uiso 1 1 calc R . . C87 C 0.90487(15) 1.6227(4) 1.3286(2) 0.0641(15) Uani 1 1 d . . . H87A H 0.8892 1.7024 1.3243 0.096 Uiso 1 1 calc R . . H87B H 0.9278 1.6570 1.3211 0.096 Uiso 1 1 calc R . . H87C H 0.9031 1.5818 1.3748 0.096 Uiso 1 1 calc R . . C91 C 1.00783(8) 1.2390(3) 1.09322(16) 0.0234(7) Uani 1 1 d . . . H91A H 1.0122 1.3381 1.0803 0.035 Uiso 1 1 calc R . . H91B H 1.0257 1.2054 1.1238 0.035 Uiso 1 1 calc R . . H91C H 0.9862 1.2328 1.1169 0.035 Uiso 1 1 calc R . . C92 C 1.04792(8) 1.1429(4) 0.95708(18) 0.0285(8) Uani 1 1 d . . . H92A H 1.0650 1.1892 0.9856 0.043 Uiso 1 1 calc R . . H92B H 1.0434 1.2019 0.9166 0.043 Uiso 1 1 calc R . . H92C H 1.0560 1.0493 0.9424 0.043 Uiso 1 1 calc R . . C93 C 1.00671(9) 0.9017(3) 0.85402(16) 0.0274(8) Uani 1 1 d . . . H93A H 0.9979 0.8358 0.8194 0.041 Uiso 1 1 calc R . . H93B H 1.0275 0.8629 0.8734 0.041 Uiso 1 1 calc R . . H93C H 1.0114 0.9941 0.8326 0.041 Uiso 1 1 calc R . . C94 C 0.93294(8) 0.8121(3) 0.91162(18) 0.0274(7) Uani 1 1 d . . . H94A H 0.9386 0.7107 0.9143 0.041 Uiso 1 1 calc R . . H94B H 0.9238 0.8336 0.8661 0.041 Uiso 1 1 calc R . . H94C H 0.9162 0.8351 0.9467 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0164(5) 0.0132(4) 0.0118(4) 0.0007(3) -0.0004(4) -0.0014(4) Al2 0.0163(4) 0.0151(4) 0.0159(4) 0.0017(4) 0.0004(4) 0.0003(4) Si1 0.0169(4) 0.0144(4) 0.0106(4) -0.0019(3) -0.0001(3) -0.0021(3) Si2 0.0162(4) 0.0138(4) 0.0150(4) -0.0025(3) 0.0017(3) -0.0019(3) Si3 0.0170(4) 0.0187(4) 0.0143(4) -0.0013(3) 0.0020(3) -0.0007(4) N1 0.0124(11) 0.0125(12) 0.0140(12) 0.0006(10) -0.0013(10) -0.0033(10) N2 0.0175(13) 0.0124(12) 0.0122(12) -0.0028(9) 0.0001(10) 0.0000(10) N3 0.0221(14) 0.0244(14) 0.0157(13) -0.0060(11) -0.0029(11) 0.0073(11) C1 0.0185(16) 0.0157(14) 0.0087(14) -0.0036(11) -0.0010(11) -0.0011(12) C2 0.0240(16) 0.0198(15) 0.0173(15) -0.0026(13) -0.0011(14) -0.0022(13) C3 0.0232(17) 0.0234(16) 0.0109(15) -0.0025(12) -0.0027(12) -0.0055(13) C4 0.0258(17) 0.0178(16) 0.0189(16) -0.0019(12) 0.0054(14) -0.0056(14) C5 0.0201(17) 0.0257(17) 0.0164(16) -0.0045(13) 0.0024(13) -0.0072(14) C6 0.0264(17) 0.0203(16) 0.0163(16) 0.0031(12) 0.0004(13) -0.0014(14) C7 0.0231(17) 0.0322(19) 0.0197(17) 0.0018(14) 0.0045(14) -0.0002(15) C11 0.0171(15) 0.0166(15) 0.0125(14) -0.0012(12) 0.0016(12) -0.0060(12) C12 0.0204(17) 0.0249(17) 0.0226(17) 0.0007(13) -0.0033(13) -0.0031(14) C13 0.0164(17) 0.041(2) 0.0315(19) 0.0017(16) -0.0056(15) -0.0083(15) C14 0.0285(18) 0.038(2) 0.0266(18) -0.0035(16) 0.0045(16) -0.0162(16) C15 0.036(2) 0.0228(17) 0.0178(16) 0.0019(13) 0.0012(14) -0.0090(15) C16 0.0233(17) 0.0181(15) 0.0173(15) 0.0009(13) 0.0023(13) -0.0022(13) C17 0.038(2) 0.059(3) 0.052(3) 0.000(2) -0.002(2) -0.029(2) C21 0.0167(15) 0.0146(14) 0.0123(14) -0.0028(11) 0.0053(11) -0.0039(12) C22 0.0241(17) 0.0167(15) 0.0184(16) 0.0026(12) 0.0019(13) -0.0011(13) C23 0.040(2) 0.0107(15) 0.0199(17) -0.0002(12) 0.0069(15) 0.0014(14) C24 0.037(2) 0.0205(16) 0.0160(16) -0.0034(13) 0.0112(14) -0.0062(15) C25 0.0325(19) 0.0186(16) 0.0153(16) 0.0007(12) 0.0025(14) -0.0050(14) C26 0.0195(16) 0.0140(14) 0.0167(15) 0.0019(12) 0.0001(13) -0.0030(12) C27 0.085(3) 0.0241(18) 0.0215(19) -0.0078(16) 0.011(2) 0.005(2) C31 0.0150(15) 0.0182(15) 0.0176(15) 0.0010(12) 0.0015(12) -0.0017(12) C32 0.0273(18) 0.0244(17) 0.0211(17) -0.0003(14) -0.0066(14) 0.0030(15) C33 0.0248(18) 0.0250(18) 0.0286(18) 0.0057(14) -0.0074(15) 0.0008(15) C34 0.0170(16) 0.0216(17) 0.0302(18) 0.0046(14) 0.0063(14) -0.0003(14) C35 0.0304(19) 0.0269(18) 0.0233(17) -0.0077(15) 0.0014(15) 0.0008(15) C36 0.0251(18) 0.0275(17) 0.0172(17) -0.0021(13) -0.0034(13) 0.0026(14) C37 0.032(2) 0.0201(17) 0.051(2) 0.0020(16) 0.0047(18) 0.0012(16) C41 0.0217(16) 0.0183(15) 0.0226(16) 0.0002(13) -0.0058(14) 0.0012(13) C42 0.0263(18) 0.0182(15) 0.0143(15) 0.0028(12) 0.0019(13) -0.0038(13) C43 0.0213(17) 0.0249(17) 0.0265(18) 0.0010(14) 0.0028(14) 0.0017(14) C44 0.0268(18) 0.0213(16) 0.0235(17) 0.0038(14) -0.0023(15) 0.0024(14) Al3 0.0162(5) 0.0142(4) 0.0209(5) -0.0009(4) -0.0008(4) 0.0000(4) Al4 0.0189(5) 0.0145(4) 0.0148(5) -0.0016(3) -0.0009(4) 0.0020(4) Si6 0.0230(5) 0.0138(4) 0.0168(4) 0.0002(3) 0.0013(4) 0.0019(4) Si7 0.0153(4) 0.0159(4) 0.0170(4) -0.0004(3) 0.0001(3) 0.0022(3) Si8 0.0234(5) 0.0209(5) 0.0240(5) -0.0007(4) 0.0076(4) -0.0024(4) N6 0.0166(13) 0.0122(12) 0.0181(13) 0.0009(10) 0.0004(10) 0.0021(10) N7 0.0171(13) 0.0116(12) 0.0137(13) 0.0001(9) 0.0026(10) 0.0026(10) N8 0.0171(14) 0.0288(15) 0.0282(16) -0.0053(12) 0.0010(11) -0.0002(12) C51 0.0187(15) 0.0156(14) 0.0165(15) -0.0018(12) 0.0008(13) -0.0026(12) C52 0.0313(19) 0.0291(18) 0.0204(17) 0.0027(14) 0.0014(14) 0.0085(15) C53 0.036(2) 0.0164(16) 0.0327(19) 0.0046(14) 0.0062(17) 0.0003(14) C54 0.0299(18) 0.0170(16) 0.0237(17) 0.0000(13) 0.0035(14) 0.0042(14) C55 0.0188(17) 0.0355(19) 0.0249(18) -0.0033(14) -0.0015(14) 0.0053(15) C56 0.043(2) 0.037(2) 0.037(2) 0.0094(17) 0.0209(18) 0.0055(18) C57 0.031(2) 0.032(2) 0.047(2) -0.0122(17) 0.0111(17) -0.0131(17) C61 0.0158(15) 0.0163(15) 0.0197(16) 0.0032(12) 0.0015(12) 0.0046(13) C62 0.0247(17) 0.0155(15) 0.0215(16) 0.0005(12) -0.0053(13) 0.0037(13) C63 0.0236(17) 0.0257(17) 0.0253(17) 0.0042(14) -0.0062(14) 0.0017(14) C64 0.0228(18) 0.0228(17) 0.0275(18) 0.0059(14) 0.0007(14) 0.0073(14) C65 0.0332(19) 0.0164(15) 0.0276(18) 0.0017(14) -0.0017(15) 0.0016(14) C66 0.0198(16) 0.0187(15) 0.0209(17) -0.0012(13) -0.0030(14) 0.0019(13) C67 0.037(2) 0.034(2) 0.047(2) 0.0024(17) -0.0051(19) 0.0153(18) C71 0.0173(15) 0.0171(15) 0.0154(15) 0.0026(12) 0.0031(12) 0.0055(12) C72 0.0274(17) 0.0165(16) 0.0191(16) 0.0027(12) 0.0013(13) -0.0007(13) C73 0.0277(18) 0.0197(16) 0.0281(19) 0.0062(14) 0.0041(15) -0.0004(14) C74 0.0310(19) 0.0264(18) 0.0235(18) 0.0088(14) 0.0074(15) 0.0082(15) C75 0.0216(17) 0.0321(19) 0.0183(17) 0.0010(14) -0.0017(13) 0.0061(15) C76 0.0219(16) 0.0184(15) 0.0214(16) -0.0010(13) 0.0013(14) 0.0015(13) C77 0.048(2) 0.039(2) 0.034(2) 0.0189(17) 0.0043(18) -0.0027(19) C81 0.0208(17) 0.0284(17) 0.0154(16) 0.0000(13) 0.0074(13) 0.0011(14) C82 0.0264(19) 0.0301(19) 0.0246(18) -0.0040(14) 0.0036(14) 0.0001(15) C83 0.035(2) 0.038(2) 0.0222(18) -0.0041(16) 0.0006(16) -0.0097(17) C84 0.066(3) 0.0205(18) 0.0237(19) 0.0000(15) 0.0022(19) -0.0051(18) C85 0.064(3) 0.0208(19) 0.030(2) -0.0003(15) 0.0060(19) 0.0119(19) C86 0.039(2) 0.0319(19) 0.0228(17) 0.0018(15) 0.0012(16) 0.0083(17) C87 0.122(5) 0.035(2) 0.035(2) -0.0064(19) -0.018(3) -0.005(3) C91 0.0215(17) 0.0210(16) 0.0276(18) -0.0049(14) -0.0053(15) -0.0010(14) C92 0.0213(18) 0.0246(18) 0.040(2) 0.0056(15) 0.0039(16) 0.0003(14) C93 0.035(2) 0.0255(18) 0.0213(17) -0.0013(14) 0.0052(15) 0.0066(16) C94 0.0299(18) 0.0193(16) 0.0330(19) -0.0047(14) -0.0054(16) 0.0009(14) _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 Al1 N1 1.961(2) . ? Al1 C41 1.969(3) . ? Al1 C42 1.969(3) . ? Al1 N2 1.980(2) . ? Al1 Al2 2.7466(12) . ? Al2 C44 1.965(3) . ? Al2 C43 1.976(3) . ? Al2 N1 1.984(2) . ? Al2 N2 1.988(3) . ? Si1 N1 1.803(2) . ? Si1 C2 1.859(3) . ? Si1 C3 1.865(3) . ? Si1 C1 1.888(3) . ? Si2 N2 1.807(3) . ? Si2 C5 1.869(3) . ? Si2 C4 1.878(3) . ? Si2 C1 1.899(3) . ? Si3 N3 1.745(3) . ? Si3 C6 1.867(3) . ? Si3 C7 1.873(3) . ? Si3 C1 1.895(3) . ? N1 C11 1.463(3) . ? N2 C21 1.461(3) . ? N3 C31 1.398(4) . ? C11 C16 1.390(4) . ? C11 C12 1.391(4) . ? C12 C13 1.385(4) . ? C13 C14 1.385(5) . ? C14 C15 1.388(5) . ? C14 C17 1.522(5) . ? C15 C16 1.386(4) . ? C21 C26 1.391(4) . ? C21 C22 1.394(4) . ? C22 C23 1.387(4) . ? C23 C24 1.386(4) . ? C24 C25 1.406(4) . ? C24 C27 1.502(4) . ? C25 C26 1.387(4) . ? C31 C32 1.397(4) . ? C31 C36 1.400(4) . ? C32 C33 1.387(4) . ? C33 C34 1.384(4) . ? C34 C35 1.379(4) . ? C34 C37 1.513(4) . ? C35 C36 1.388(4) . ? Al3 C92 1.957(3) . ? Al3 C91 1.966(3) . ? Al3 N7 1.978(3) . ? Al3 N6 1.993(2) . ? Al3 Al4 2.7666(12) . ? Al4 C93 1.962(3) . ? Al4 C94 1.967(3) . ? Al4 N6 1.979(3) . ? Al4 N7 1.993(2) . ? Si6 N6 1.807(3) . ? Si6 C52 1.863(3) . ? Si6 C53 1.865(3) . ? Si6 C51 1.883(3) . ? Si7 N7 1.803(3) . ? Si7 C54 1.867(3) . ? Si7 C55 1.869(3) . ? Si7 C51 1.891(3) . ? Si8 N8 1.737(3) . ? Si8 C57 1.869(4) . ? Si8 C56 1.875(4) . ? Si8 C51 1.886(3) . ? N6 C61 1.465(4) . ? N7 C71 1.460(3) . ? N8 C81 1.405(4) . ? C61 C62 1.390(4) . ? C61 C66 1.392(4) . ? C62 C63 1.390(4) . ? C63 C64 1.397(4) . ? C64 C65 1.387(5) . ? C64 C67 1.513(4) . ? C65 C66 1.398(4) . ? C71 C76 1.390(4) . ? C71 C72 1.396(4) . ? C72 C73 1.381(4) . ? C73 C74 1.392(5) . ? C74 C75 1.394(5) . ? C74 C77 1.506(4) . ? C75 C76 1.387(4) . ? C81 C86 1.390(4) . ? C81 C82 1.399(5) . ? C82 C83 1.392(5) . ? C83 C84 1.401(5) . ? C84 C85 1.378(5) . ? C84 C87 1.516(5) . ? C85 C86 1.391(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 N1 Al1 C41 119.77(12) . . ? N1 Al1 C42 109.16(12) . . ? C41 Al1 C42 112.06(14) . . ? N1 Al1 N2 84.41(10) . . ? C41 Al1 N2 117.04(12) . . ? C42 Al1 N2 111.55(12) . . ? N1 Al1 Al2 46.21(7) . . ? C41 Al1 Al2 150.97(10) . . ? C42 Al1 Al2 96.96(10) . . ? N2 Al1 Al2 46.32(7) . . ? C44 Al2 C43 111.32(14) . . ? C44 Al2 N1 117.84(12) . . ? C43 Al2 N1 112.93(12) . . ? C44 Al2 N2 115.54(12) . . ? C43 Al2 N2 113.08(13) . . ? N1 Al2 N2 83.59(10) . . ? C44 Al2 Al1 147.77(10) . . ? C43 Al2 Al1 100.88(10) . . ? N1 Al2 Al1 45.52(7) . . ? N2 Al2 Al1 46.07(7) . . ? N1 Si1 C2 109.30(13) . . ? N1 Si1 C3 107.97(12) . . ? C2 Si1 C3 107.25(14) . . ? N1 Si1 C1 107.17(11) . . ? C2 Si1 C1 108.09(14) . . ? C3 Si1 C1 116.91(14) . . ? N2 Si2 C5 109.83(12) . . ? N2 Si2 C4 108.57(13) . . ? C5 Si2 C4 106.16(14) . . ? N2 Si2 C1 107.30(12) . . ? C5 Si2 C1 108.54(13) . . ? C4 Si2 C1 116.36(13) . . ? N3 Si3 C6 102.88(13) . . ? N3 Si3 C7 109.55(14) . . ? C6 Si3 C7 111.34(15) . . ? N3 Si3 C1 111.35(12) . . ? C6 Si3 C1 112.93(14) . . ? C7 Si3 C1 108.69(13) . . ? C11 N1 Si1 110.67(18) . . ? C11 N1 Al1 114.06(18) . . ? Si1 N1 Al1 113.26(12) . . ? C11 N1 Al2 116.61(18) . . ? Si1 N1 Al2 112.41(12) . . ? Al1 N1 Al2 88.27(10) . . ? C21 N2 Si2 112.82(18) . . ? C21 N2 Al1 115.64(17) . . ? Si2 N2 Al1 111.35(12) . . ? C21 N2 Al2 113.33(18) . . ? Si2 N2 Al2 113.81(12) . . ? Al1 N2 Al2 87.61(10) . . ? C31 N3 Si3 134.1(2) . . ? Si1 C1 Si3 113.23(14) . . ? Si1 C1 Si2 122.86(15) . . ? Si3 C1 Si2 115.10(15) . . ? C16 C11 C12 118.5(3) . . ? C16 C11 N1 120.2(3) . . ? C12 C11 N1 121.3(3) . . ? C13 C12 C11 120.5(3) . . ? C12 C13 C14 121.1(3) . . ? C13 C14 C15 118.4(3) . . ? C13 C14 C17 120.8(3) . . ? C15 C14 C17 120.8(3) . . ? C16 C15 C14 120.8(3) . . ? C15 C16 C11 120.7(3) . . ? C26 C21 C22 118.2(3) . . ? C26 C21 N2 121.4(2) . . ? C22 C21 N2 120.3(3) . . ? C23 C22 C21 120.7(3) . . ? C24 C23 C22 121.8(3) . . ? C23 C24 C25 117.3(3) . . ? C23 C24 C27 121.4(3) . . ? C25 C24 C27 121.4(3) . . ? C26 C25 C24 121.2(3) . . ? C25 C26 C21 120.8(3) . . ? C32 C31 N3 122.6(3) . . ? C32 C31 C36 117.0(3) . . ? N3 C31 C36 120.4(3) . . ? C33 C32 C31 120.7(3) . . ? C34 C33 C32 122.3(3) . . ? C35 C34 C33 116.9(3) . . ? C35 C34 C37 120.8(3) . . ? C33 C34 C37 122.3(3) . . ? C34 C35 C36 122.0(3) . . ? C35 C36 C31 121.0(3) . . ? C92 Al3 C91 110.65(15) . . ? C92 Al3 N7 111.43(13) . . ? C91 Al3 N7 118.02(12) . . ? C92 Al3 N6 112.42(13) . . ? C91 Al3 N6 118.12(13) . . ? N7 Al3 N6 83.84(10) . . ? C92 Al3 Al4 99.53(11) . . ? C91 Al3 Al4 149.82(10) . . ? N7 Al3 Al4 46.06(7) . . ? N6 Al3 Al4 45.65(7) . . ? C93 Al4 C94 112.18(15) . . ? C93 Al4 N6 112.93(13) . . ? C94 Al4 N6 116.47(13) . . ? C93 Al4 N7 112.10(12) . . ? C94 Al4 N7 116.54(12) . . ? N6 Al4 N7 83.82(10) . . ? C93 Al4 Al3 100.39(11) . . ? C94 Al4 Al3 147.43(11) . . ? N6 Al4 Al3 46.06(7) . . ? N7 Al4 Al3 45.62(7) . . ? N6 Si6 C52 109.61(14) . . ? N6 Si6 C53 109.35(13) . . ? C52 Si6 C53 106.35(16) . . ? N6 Si6 C51 106.65(12) . . ? C52 Si6 C51 108.88(14) . . ? C53 Si6 C51 115.93(15) . . ? N7 Si7 C54 108.67(13) . . ? N7 Si7 C55 109.20(13) . . ? C54 Si7 C55 105.52(15) . . ? N7 Si7 C51 106.79(12) . . ? C54 Si7 C51 109.71(14) . . ? C55 Si7 C51 116.76(14) . . ? N8 Si8 C57 106.19(16) . . ? N8 Si8 C56 107.64(15) . . ? C57 Si8 C56 108.22(18) . . ? N8 Si8 C51 109.68(13) . . ? C57 Si8 C51 111.70(15) . . ? C56 Si8 C51 113.10(16) . . ? C61 N6 Si6 111.05(18) . . ? C61 N6 Al4 116.24(18) . . ? Si6 N6 Al4 113.11(13) . . ? C61 N6 Al3 114.67(18) . . ? Si6 N6 Al3 111.74(12) . . ? Al4 N6 Al3 88.30(10) . . ? C71 N7 Si7 110.22(18) . . ? C71 N7 Al3 117.41(19) . . ? Si7 N7 Al3 111.27(12) . . ? C71 N7 Al4 114.71(18) . . ? Si7 N7 Al4 113.46(12) . . ? Al3 N7 Al4 88.33(10) . . ? C81 N8 Si8 130.0(2) . . ? Si6 C51 Si8 115.26(15) . . ? Si6 C51 Si7 123.38(16) . . ? Si8 C51 Si7 112.83(15) . . ? C62 C61 C66 118.1(3) . . ? C62 C61 N6 121.1(3) . . ? C66 C61 N6 120.8(3) . . ? C61 C62 C63 121.0(3) . . ? C62 C63 C64 121.1(3) . . ? C65 C64 C63 117.9(3) . . ? C65 C64 C67 121.3(3) . . ? C63 C64 C67 120.8(3) . . ? C64 C65 C66 121.1(3) . . ? C61 C66 C65 120.8(3) . . ? C76 C71 C72 118.2(3) . . ? C76 C71 N7 121.1(3) . . ? C72 C71 N7 120.8(3) . . ? C73 C72 C71 120.9(3) . . ? C72 C73 C74 121.3(3) . . ? C73 C74 C75 117.7(3) . . ? C73 C74 C77 121.5(3) . . ? C75 C74 C77 120.9(3) . . ? C76 C75 C74 121.2(3) . . ? C75 C76 C71 120.8(3) . . ? C86 C81 C82 117.1(3) . . ? C86 C81 N8 121.4(3) . . ? C82 C81 N8 121.4(3) . . ? C83 C82 C81 121.7(3) . . ? C82 C83 C84 120.7(3) . . ? C85 C84 C83 117.2(3) . . ? C85 C84 C87 122.3(4) . . ? C83 C84 C87 120.5(4) . . ? C84 C85 C86 122.3(3) . . ? C81 C86 C85 120.9(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.322 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.066 #===END data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H45 Al2 N3 Si4' _chemical_formula_weight 589.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 36.562(3) _cell_length_b 9.5547(9) _cell_length_c 19.4147(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.698(6) _cell_angle_gamma 90.00 _cell_volume 6664.4(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9262 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 29.92 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 0.253 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9413 _exptl_absorpt_correction_T_max 0.9860 _exptl_absorpt_process_details 'SADABS, Scheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 54156 _diffrn_reflns_av_R_equivalents 0.1652 _diffrn_reflns_av_sigmaI/netI 0.2286 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 33.39 _reflns_number_total 12328 _reflns_number_gt 4845 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 12328 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2428 _refine_ls_R_factor_gt 0.1117 _refine_ls_wR_factor_ref 0.2942 _refine_ls_wR_factor_gt 0.2386 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si0 Si 0.08920(3) 0.36617(14) 0.57336(6) 0.0218(3) Uani 1 1 d . . . Si1 Si 0.11429(3) 0.48527(14) 0.48836(6) 0.0212(3) Uani 1 1 d . . . Si2 Si 0.13878(3) 0.33674(14) 0.66950(6) 0.0230(3) Uani 1 1 d . . . Si3 Si 0.05435(3) 0.53600(15) 0.61885(6) 0.0232(3) Uani 1 1 d . . . Al1 Al 0.13778(3) 0.65517(15) 0.63396(6) 0.0207(3) Uani 1 1 d . . . Al2 Al 0.19307(4) 0.50991(16) 0.58741(6) 0.0230(3) Uani 1 1 d . . . N1 N 0.14681(9) 0.6051(4) 0.53866(17) 0.0207(8) Uani 1 1 d . . . N2 N 0.16802(10) 0.4903(4) 0.66755(17) 0.0219(8) Uani 1 1 d . . . N3 N 0.09039(10) 0.6500(4) 0.65347(18) 0.0220(8) Uani 1 1 d . . . C0 C 0.07863(13) 0.5840(6) 0.4260(2) 0.0304(11) Uani 1 1 d . . . H0A H 0.0902 0.6253 0.3891 0.046 Uiso 1 1 calc R . . H0B H 0.0682 0.6584 0.4512 0.046 Uiso 1 1 calc R . . H0C H 0.0587 0.5201 0.4048 0.046 Uiso 1 1 calc R . . C1 C 0.06733(13) 0.1942(5) 0.5399(2) 0.0281(11) Uani 1 1 d . . . H1A H 0.0510 0.2089 0.4944 0.042 Uiso 1 1 calc R . . H1B H 0.0528 0.1572 0.5734 0.042 Uiso 1 1 calc R . . H1C H 0.0869 0.1273 0.5345 0.042 Uiso 1 1 calc R . . C2 C 0.13663(13) 0.3660(5) 0.4327(2) 0.0304(11) Uani 1 1 d . . . H2A H 0.1477 0.4214 0.3992 0.046 Uiso 1 1 calc R . . H2B H 0.1179 0.3025 0.4070 0.046 Uiso 1 1 calc R . . H2C H 0.1561 0.3114 0.4624 0.046 Uiso 1 1 calc R . . C3 C 0.16334(14) 0.1692(5) 0.6598(3) 0.0337(12) Uani 1 1 d . . . H3A H 0.1848 0.1600 0.6981 0.051 Uiso 1 1 calc R . . H3B H 0.1719 0.1687 0.6149 0.051 Uiso 1 1 calc R . . H3C H 0.1463 0.0907 0.6614 0.051 Uiso 1 1 calc R . . C4 C 0.12415(13) 0.3365(6) 0.7565(2) 0.0287(11) Uani 1 1 d . . . H4A H 0.1458 0.3175 0.7933 0.043 Uiso 1 1 calc R . . H4B H 0.1053 0.2638 0.7571 0.043 Uiso 1 1 calc R . . H4C H 0.1137 0.4280 0.7647 0.043 Uiso 1 1 calc R . . C5 C 0.02916(13) 0.4528(6) 0.6838(2) 0.0374(13) Uani 1 1 d . . . H5A H 0.0129 0.5221 0.7000 0.056 Uiso 1 1 calc R . . H5B H 0.0473 0.4182 0.7239 0.056 Uiso 1 1 calc R . . H5C H 0.0141 0.3745 0.6616 0.056 Uiso 1 1 calc R . . C6 C 0.01683(13) 0.6389(6) 0.5611(2) 0.0306(11) Uani 1 1 d . . . H6A H 0.0095 0.7182 0.5875 0.046 Uiso 1 1 calc R . . H6B H -0.0048 0.5784 0.5456 0.046 Uiso 1 1 calc R . . H6C H 0.0262 0.6736 0.5202 0.046 Uiso 1 1 calc R . . C11 C 0.15441(11) 0.7192(5) 0.49336(19) 0.0196(9) Uani 1 1 d . . . C12 C 0.13402(12) 0.8420(5) 0.4872(2) 0.0238(10) Uani 1 1 d . . . H12A H 0.1155 0.8554 0.5151 0.029 Uiso 1 1 calc R . . C13 C 0.14022(13) 0.9460(6) 0.4408(2) 0.0280(11) Uani 1 1 d . . . H13A H 0.1259 1.0296 0.4375 0.034 Uiso 1 1 calc R . . C14 C 0.16720(13) 0.9298(5) 0.3987(2) 0.0262(10) Uani 1 1 d . . . C15 C 0.18790(12) 0.8078(5) 0.4061(2) 0.0267(11) Uani 1 1 d . . . H15A H 0.2068 0.7950 0.3790 0.032 Uiso 1 1 calc R . . C16 C 0.18163(12) 0.7031(5) 0.4528(2) 0.0229(10) Uani 1 1 d . . . H16A H 0.1961 0.6200 0.4567 0.028 Uiso 1 1 calc R . . C17 C 0.17302(16) 1.0407(6) 0.3467(3) 0.0391(13) Uani 1 1 d . . . H17A H 0.1985 1.0344 0.3377 0.059 Uiso 1 1 calc R . . H17B H 0.1691 1.1333 0.3659 0.059 Uiso 1 1 calc R . . H17C H 0.1553 1.0267 0.3028 0.059 Uiso 1 1 calc R . . C21 C 0.19581(12) 0.4975(5) 0.7333(2) 0.0242(10) Uani 1 1 d . . . C22 C 0.22659(12) 0.4109(6) 0.7430(2) 0.0276(11) Uani 1 1 d . . . H22A H 0.2305 0.3501 0.7064 0.033 Uiso 1 1 calc R . . C23 C 0.24707(13) 0.5010(6) 0.8598(2) 0.0285(11) Uani 1 1 d . . . C24 C 0.25198(13) 0.4120(6) 0.8063(2) 0.0301(11) Uani 1 1 d . . . H24A H 0.2728 0.3509 0.8126 0.036 Uiso 1 1 calc R . . C25 C 0.21676(12) 0.5917(6) 0.8486(2) 0.0303(11) Uani 1 1 d . . . H25A H 0.2134 0.6557 0.8844 0.036 Uiso 1 1 calc R . . C26 C 0.19124(12) 0.5899(5) 0.7856(2) 0.0254(10) Uani 1 1 d . . . H26A H 0.1707 0.6524 0.7786 0.030 Uiso 1 1 calc R . . C27 C 0.27279(13) 0.4956(6) 0.9308(2) 0.0353(13) Uani 1 1 d . . . H27A H 0.2968 0.4556 0.9255 0.053 Uiso 1 1 calc R . . H27B H 0.2616 0.4372 0.9628 0.053 Uiso 1 1 calc R . . H27C H 0.2766 0.5905 0.9500 0.053 Uiso 1 1 calc R . . C31 C 0.07968(12) 0.7612(5) 0.6958(2) 0.0235(10) Uani 1 1 d . . . C32 C 0.07461(13) 0.8970(5) 0.6727(2) 0.0281(11) Uani 1 1 d . . . H32A H 0.0792 0.9201 0.6276 0.034 Uiso 1 1 calc R . . C33 C 0.06284(13) 1.0023(6) 0.7138(2) 0.0301(11) Uani 1 1 d . . . H33A H 0.0600 1.0955 0.6965 0.036 Uiso 1 1 calc R . . C34 C 0.05524(13) 0.9711(6) 0.7796(2) 0.0292(11) Uani 1 1 d . . . C35 C 0.06051(14) 0.8350(6) 0.8034(2) 0.0350(12) Uani 1 1 d . . . H35A H 0.0556 0.8120 0.8484 0.042 Uiso 1 1 calc R . . C36 C 0.07276(13) 0.7317(6) 0.7635(2) 0.0313(12) Uani 1 1 d . . . H36A H 0.0766 0.6396 0.7818 0.038 Uiso 1 1 calc R . . C37 C 0.04240(15) 1.0854(6) 0.8249(3) 0.0400(14) Uani 1 1 d . . . H37A H 0.0208 1.0522 0.8433 0.060 Uiso 1 1 calc R . . H37B H 0.0356 1.1694 0.7964 0.060 Uiso 1 1 calc R . . H37C H 0.0626 1.1080 0.8639 0.060 Uiso 1 1 calc R . . H1 H 0.1560(10) 0.789(4) 0.647(2) 0.012(10) Uiso 1 1 d . . . H2 H 0.2034(14) 0.382(6) 0.560(3) 0.046(16) Uiso 1 1 d . . . H3 H 0.2219(11) 0.624(5) 0.607(2) 0.024(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si0 0.0276(7) 0.0269(8) 0.0118(5) 0.0012(5) 0.0060(4) -0.0012(5) Si1 0.0253(6) 0.0287(8) 0.0102(5) -0.0005(5) 0.0048(4) -0.0010(5) Si2 0.0291(7) 0.0272(8) 0.0129(5) 0.0020(5) 0.0045(5) 0.0006(5) Si3 0.0266(7) 0.0317(9) 0.0127(5) -0.0022(5) 0.0073(5) -0.0012(5) Al1 0.0250(7) 0.0279(9) 0.0098(6) 0.0002(5) 0.0047(5) -0.0003(6) Al2 0.0258(7) 0.0311(9) 0.0129(6) 0.0012(5) 0.0058(5) 0.0017(6) N1 0.0266(19) 0.024(2) 0.0128(16) 0.0026(14) 0.0064(14) -0.0004(16) N2 0.027(2) 0.026(2) 0.0120(16) -0.0022(14) 0.0035(14) 0.0033(16) N3 0.0241(19) 0.029(2) 0.0143(17) -0.0031(15) 0.0062(13) 0.0001(16) C0 0.032(3) 0.040(3) 0.019(2) 0.006(2) 0.0025(18) -0.001(2) C1 0.039(3) 0.028(3) 0.018(2) 0.0013(18) 0.0072(19) 0.000(2) C2 0.038(3) 0.034(3) 0.020(2) -0.006(2) 0.0095(19) -0.007(2) C3 0.040(3) 0.028(3) 0.034(3) 0.005(2) 0.009(2) 0.001(2) C4 0.031(2) 0.042(3) 0.014(2) 0.0067(19) 0.0050(17) 0.001(2) C5 0.033(3) 0.059(4) 0.023(2) 0.001(2) 0.013(2) -0.003(2) C6 0.027(2) 0.040(3) 0.024(2) -0.003(2) 0.0020(18) 0.004(2) C11 0.026(2) 0.025(3) 0.0070(17) 0.0003(15) 0.0028(15) -0.0028(18) C12 0.033(2) 0.028(3) 0.0118(19) 0.0004(17) 0.0074(16) -0.001(2) C13 0.034(3) 0.035(3) 0.015(2) 0.0020(19) 0.0069(18) 0.002(2) C14 0.038(3) 0.031(3) 0.0096(19) -0.0039(17) 0.0061(17) -0.007(2) C15 0.031(3) 0.038(3) 0.0123(19) -0.0040(18) 0.0077(17) -0.004(2) C16 0.026(2) 0.030(3) 0.0131(19) -0.0046(17) 0.0038(16) -0.0003(19) C17 0.058(4) 0.042(4) 0.021(2) 0.009(2) 0.018(2) 0.002(3) C21 0.023(2) 0.041(3) 0.0091(18) 0.0027(18) 0.0043(15) -0.001(2) C22 0.029(2) 0.038(3) 0.017(2) 0.002(2) 0.0079(17) 0.004(2) C23 0.027(2) 0.043(3) 0.017(2) 0.006(2) 0.0045(17) -0.004(2) C24 0.027(2) 0.042(3) 0.022(2) 0.008(2) 0.0038(18) 0.004(2) C25 0.031(3) 0.045(4) 0.014(2) 0.002(2) 0.0030(17) -0.002(2) C26 0.026(2) 0.034(3) 0.018(2) 0.0034(19) 0.0063(17) 0.004(2) C27 0.033(3) 0.060(4) 0.012(2) 0.007(2) 0.0005(18) -0.003(2) C31 0.024(2) 0.031(3) 0.0150(19) -0.0027(18) 0.0019(16) 0.0007(19) C32 0.040(3) 0.028(3) 0.019(2) -0.0013(19) 0.0088(19) -0.004(2) C33 0.039(3) 0.029(3) 0.023(2) -0.004(2) 0.007(2) 0.000(2) C34 0.027(2) 0.039(3) 0.020(2) -0.006(2) 0.0015(18) 0.004(2) C35 0.047(3) 0.044(4) 0.015(2) -0.004(2) 0.007(2) 0.005(2) C36 0.042(3) 0.039(3) 0.014(2) 0.001(2) 0.0059(18) 0.007(2) C37 0.048(3) 0.047(4) 0.026(3) -0.009(2) 0.009(2) 0.005(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 Si0 C1 1.889(5) . ? Si0 Si1 2.3285(17) . ? Si0 Si3 2.3355(18) . ? Si0 Si2 2.3646(17) . ? Si1 N1 1.802(4) . ? Si1 C2 1.861(5) . ? Si1 C0 1.863(5) . ? Si2 N2 1.820(4) . ? Si2 C3 1.862(5) . ? Si2 C4 1.864(4) . ? Si3 N3 1.745(4) . ? Si3 C5 1.872(5) . ? Si3 C6 1.880(5) . ? Al1 N3 1.842(4) . ? Al1 N2 1.965(4) . ? Al1 N1 1.997(3) . ? Al1 Al2 2.7398(19) . ? Al1 H1 1.44(4) . ? Al2 N2 1.955(4) . ? Al2 N1 1.997(4) . ? Al2 H2 1.41(5) . ? Al2 H3 1.51(4) . ? N1 C11 1.460(5) . ? N2 C21 1.478(5) . ? N3 C31 1.441(6) . ? C0 H0A 0.9800 . ? C0 H0B 0.9800 . ? C0 H0C 0.9800 . ? 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 . ? C11 C12 1.384(6) . ? C11 C16 1.388(6) . ? C12 C13 1.388(6) . ? C12 H12A 0.9500 . ? C13 C14 1.402(6) . ? C13 H13A 0.9500 . ? C14 C15 1.383(7) . ? C14 C17 1.505(7) . ? C15 C16 1.397(6) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C21 C26 1.379(6) . ? C21 C22 1.381(6) . ? C22 C24 1.396(6) . ? C22 H22A 0.9500 . ? C23 C24 1.380(7) . ? C23 C25 1.392(7) . ? C23 C27 1.518(6) . ? C24 H24A 0.9500 . ? C25 C26 1.395(6) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C31 C32 1.374(7) . ? C31 C36 1.412(6) . ? C32 C33 1.400(6) . ? C32 H32A 0.9500 . ? C33 C34 1.389(6) . ? C33 H33A 0.9500 . ? C34 C35 1.382(7) . ? C34 C37 1.530(7) . ? C35 C36 1.380(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 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 C1 Si0 Si1 112.23(15) . . ? C1 Si0 Si3 120.58(16) . . ? Si1 Si0 Si3 104.05(7) . . ? C1 Si0 Si2 112.43(16) . . ? Si1 Si0 Si2 105.81(6) . . ? Si3 Si0 Si2 100.15(6) . . ? N1 Si1 C2 112.8(2) . . ? N1 Si1 C0 110.0(2) . . ? C2 Si1 C0 105.2(2) . . ? N1 Si1 Si0 103.50(12) . . ? C2 Si1 Si0 112.70(17) . . ? C0 Si1 Si0 112.83(16) . . ? N2 Si2 C3 113.3(2) . . ? N2 Si2 C4 106.8(2) . . ? C3 Si2 C4 108.4(2) . . ? N2 Si2 Si0 104.77(13) . . ? C3 Si2 Si0 109.63(17) . . ? C4 Si2 Si0 114.11(15) . . ? N3 Si3 C5 115.9(2) . . ? N3 Si3 C6 108.6(2) . . ? C5 Si3 C6 103.2(2) . . ? N3 Si3 Si0 98.83(13) . . ? C5 Si3 Si0 109.33(19) . . ? C6 Si3 Si0 121.80(16) . . ? N3 Al1 N2 113.78(17) . . ? N3 Al1 N1 120.52(16) . . ? N2 Al1 N1 86.32(15) . . ? N3 Al1 Al2 146.54(14) . . ? N2 Al1 Al2 45.52(10) . . ? N1 Al1 Al2 46.69(11) . . ? N3 Al1 H1 114.2(15) . . ? N2 Al1 H1 116.0(15) . . ? N1 Al1 H1 103.0(16) . . ? Al2 Al1 H1 99.3(15) . . ? N2 Al2 N1 86.58(15) . . ? N2 Al2 Al1 45.81(11) . . ? N1 Al2 Al1 46.69(10) . . ? N2 Al2 H2 114(2) . . ? N1 Al2 H2 119(2) . . ? Al1 Al2 H2 146(2) . . ? N2 Al2 H3 106.3(17) . . ? N1 Al2 H3 106.3(17) . . ? Al1 Al2 H3 94.5(17) . . ? H2 Al2 H3 120(3) . . ? C11 N1 Si1 109.2(3) . . ? C11 N1 Al1 117.5(3) . . ? Si1 N1 Al1 116.64(18) . . ? C11 N1 Al2 112.7(3) . . ? Si1 N1 Al2 112.5(2) . . ? Al1 N1 Al2 86.62(14) . . ? C21 N2 Si2 109.4(3) . . ? C21 N2 Al2 109.5(3) . . ? Si2 N2 Al2 117.23(19) . . ? C21 N2 Al1 120.2(3) . . ? Si2 N2 Al1 110.90(18) . . ? Al2 N2 Al1 88.67(15) . . ? C31 N3 Si3 114.5(3) . . ? C31 N3 Al1 117.6(3) . . ? Si3 N3 Al1 127.5(2) . . ? Si1 C0 H0A 109.5 . . ? Si1 C0 H0B 109.5 . . ? H0A C0 H0B 109.5 . . ? Si1 C0 H0C 109.5 . . ? H0A C0 H0C 109.5 . . ? H0B C0 H0C 109.5 . . ? Si0 C1 H1A 109.5 . . ? Si0 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si0 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 . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 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 . . ? Si3 C5 H5A 109.5 . . ? Si3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si3 C6 H6A 109.5 . . ? Si3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C11 C16 118.5(4) . . ? C12 C11 N1 121.7(4) . . ? C16 C11 N1 119.7(4) . . ? C11 C12 C13 120.9(4) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C12 C13 C14 121.2(5) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C15 C14 C13 117.6(4) . . ? C15 C14 C17 121.4(4) . . ? C13 C14 C17 121.0(5) . . ? C14 C15 C16 121.3(4) . . ? C14 C15 H15A 119.4 . . ? C16 C15 H15A 119.4 . . ? C11 C16 C15 120.6(4) . . ? C11 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? 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 . . ? C26 C21 C22 119.3(4) . . ? C26 C21 N2 120.5(4) . . ? C22 C21 N2 120.2(4) . . ? C21 C22 C24 120.5(4) . . ? C21 C22 H22A 119.7 . . ? C24 C22 H22A 119.7 . . ? C24 C23 C25 118.5(4) . . ? C24 C23 C27 121.2(5) . . ? C25 C23 C27 120.3(4) . . ? C23 C24 C22 120.6(5) . . ? C23 C24 H24A 119.7 . . ? C22 C24 H24A 119.7 . . ? C23 C25 C26 120.9(5) . . ? C23 C25 H25A 119.6 . . ? C26 C25 H25A 119.6 . . ? C21 C26 C25 120.1(4) . . ? C21 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? 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 . . ? C32 C31 C36 117.1(4) . . ? C32 C31 N3 123.0(4) . . ? C36 C31 N3 119.9(4) . . ? C31 C32 C33 122.0(4) . . ? C31 C32 H32A 119.0 . . ? C33 C32 H32A 119.0 . . ? C34 C33 C32 120.3(5) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C35 C34 C33 118.1(4) . . ? C35 C34 C37 121.2(4) . . ? C33 C34 C37 120.7(5) . . ? C36 C35 C34 121.6(5) . . ? C36 C35 H35A 119.2 . . ? C34 C35 H35A 119.2 . . ? C35 C36 C31 120.9(5) . . ? C35 C36 H36A 119.6 . . ? C31 C36 H36A 119.6 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 33.39 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.514 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.156 #===END data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H84 N6 Si8 Sm2' _chemical_formula_weight 1366.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.9744(6) _cell_length_b 14.4707(6) _cell_length_c 18.2232(8) _cell_angle_alpha 84.707(3) _cell_angle_beta 80.305(3) _cell_angle_gamma 63.979(2) _cell_volume 3263.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 1.967 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5173 _exptl_absorpt_correction_T_max 0.8978 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71422 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_sigmaI/netI 0.1192 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 33.19 _reflns_number_total 24333 _reflns_number_gt 16555 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+231.2692P] 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 24333 _refine_ls_number_parameters 672 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1572 _refine_ls_R_factor_gt 0.1167 _refine_ls_wR_factor_ref 0.3049 _refine_ls_wR_factor_gt 0.2874 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.211 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 1.74293(4) 0.36143(4) 0.22225(3) 0.01148(12) Uani 1 1 d . . . Sm2 Sm 1.75560(4) 0.64394(4) 0.24596(3) 0.01279(12) Uani 1 1 d . . . Si1 Si 1.5102(3) 0.4125(2) 0.32214(19) 0.0157(6) Uani 1 1 d . . . Si2 Si 1.6448(3) 0.2703(3) 0.3751(2) 0.0197(7) Uani 1 1 d . . . Si3 Si 1.5104(3) 0.3677(3) 0.20044(19) 0.0170(6) Uani 1 1 d . . . Si4 Si 1.5456(2) 0.5586(3) 0.31907(18) 0.0151(6) Uani 1 1 d . . . Si5 Si 1.9567(2) 0.6551(2) 0.31686(17) 0.0129(5) Uani 1 1 d . . . Si6 Si 1.9924(3) 0.4795(3) 0.3172(2) 0.0193(6) Uani 1 1 d . . . Si7 Si 1.9490(3) 0.7170(3) 0.1915(2) 0.0198(6) Uani 1 1 d . . . Si8 Si 1.7919(3) 0.7508(3) 0.39145(19) 0.0174(6) Uani 1 1 d . . . N2 N 1.7649(8) 0.2589(7) 0.3237(6) 0.0169(18) Uani 1 1 d . . . N3 N 1.6423(8) 0.3245(8) 0.1571(6) 0.0180(18) Uani 1 1 d . . . N4 N 1.6389(7) 0.5516(7) 0.2395(5) 0.0143(17) Uani 1 1 d . . . N6 N 1.9045(8) 0.4859(8) 0.2576(6) 0.0180(19) Uani 1 1 d . . . N7 N 1.8439(9) 0.7088(8) 0.1582(6) 0.020(2) Uani 1 1 d . . . N8 N 1.6970(8) 0.7569(7) 0.3397(6) 0.020(2) Uani 1 1 d . . . C1 C 1.3736(10) 0.4403(11) 0.3787(8) 0.024(2) Uani 1 1 d . . . H1A H 1.3631 0.3772 0.3846 0.035 Uiso 1 1 calc R . . H1B H 1.3170 0.4931 0.3528 0.035 Uiso 1 1 calc R . . H1C H 1.3702 0.4649 0.4278 0.035 Uiso 1 1 calc R . . C2 C 1.6378(12) 0.2906(12) 0.4757(8) 0.031(3) Uani 1 1 d . . . H2A H 1.5692 0.2948 0.5027 0.047 Uiso 1 1 calc R . . H2B H 1.6431 0.3548 0.4815 0.047 Uiso 1 1 calc R . . H2C H 1.6973 0.2330 0.4958 0.047 Uiso 1 1 calc R . . C3 C 1.6201(12) 0.1534(10) 0.3727(9) 0.030(3) Uani 1 1 d . . . H3A H 1.6515 0.1054 0.4130 0.045 Uiso 1 1 calc R . . H3B H 1.6533 0.1199 0.3247 0.045 Uiso 1 1 calc R . . H3C H 1.5424 0.1738 0.3792 0.045 Uiso 1 1 calc R . . C4 C 1.4602(12) 0.2643(12) 0.2088(10) 0.035(3) Uani 1 1 d . . . H4A H 1.3816 0.2960 0.2209 0.053 Uiso 1 1 calc R . . H4B H 1.4916 0.2149 0.2484 0.053 Uiso 1 1 calc R . . H4C H 1.4813 0.2286 0.1615 0.053 Uiso 1 1 calc R . . C5 C 1.4137(11) 0.4818(11) 0.1520(9) 0.028(3) Uani 1 1 d . . . H5A H 1.3403 0.5005 0.1776 0.043 Uiso 1 1 calc R . . H5B H 1.4182 0.4647 0.1003 0.043 Uiso 1 1 calc R . . H5C H 1.4319 0.5398 0.1526 0.043 Uiso 1 1 calc R . . C6 C 1.4117(11) 0.6766(11) 0.3227(8) 0.026(3) Uani 1 1 d . . . H6A H 1.3592 0.6664 0.3615 0.039 Uiso 1 1 calc R . . H6B H 1.3860 0.6874 0.2745 0.039 Uiso 1 1 calc R . . H6C H 1.4208 0.7369 0.3342 0.039 Uiso 1 1 calc R . . C7 C 1.6141(12) 0.5513(11) 0.4010(7) 0.026(3) Uani 1 1 d . . . H7A H 1.6108 0.6188 0.4085 0.039 Uiso 1 1 calc R . . H7B H 1.6895 0.5007 0.3917 0.039 Uiso 1 1 calc R . . H7C H 1.5778 0.5304 0.4457 0.039 Uiso 1 1 calc R . . C21 C 1.8605(10) 0.1757(9) 0.3454(7) 0.018(2) Uani 1 1 d . . . C22 C 1.9106(10) 0.1884(11) 0.4020(7) 0.024(2) Uani 1 1 d . . . H22A H 1.8807 0.2522 0.4267 0.029 Uiso 1 1 calc R . . C23 C 2.0046(11) 0.1073(12) 0.4222(8) 0.030(3) Uani 1 1 d . . . H23A H 2.0376 0.1167 0.4606 0.035 Uiso 1 1 calc R . . C24 C 2.0494(11) 0.0151(12) 0.3873(9) 0.031(3) Uani 1 1 d . . . C25 C 1.9993(12) 0.0019(11) 0.3326(10) 0.033(3) Uani 1 1 d . . . H25A H 2.0273 -0.0630 0.3098 0.039 Uiso 1 1 calc R . . C26 C 1.9072(10) 0.0839(11) 0.3103(8) 0.026(3) Uani 1 1 d . . . H26A H 1.8770 0.0751 0.2700 0.031 Uiso 1 1 calc R . . C27 C 2.1542(14) -0.0723(13) 0.4093(12) 0.048(5) Uani 1 1 d . . . H27A H 2.1457 -0.1364 0.4173 0.073 Uiso 1 1 calc R . . H27B H 2.1695 -0.0546 0.4552 0.073 Uiso 1 1 calc R . . H27C H 2.2139 -0.0814 0.3693 0.073 Uiso 1 1 calc R . . C31 C 1.6753(9) 0.2688(9) 0.0907(7) 0.017(2) Uani 1 1 d . . . C32 C 1.6615(11) 0.3150(10) 0.0200(7) 0.022(2) Uani 1 1 d . . . H32A H 1.6245 0.3878 0.0163 0.026 Uiso 1 1 calc R . . C33 C 1.6987(11) 0.2604(10) -0.0436(7) 0.023(2) Uani 1 1 d . . . H33A H 1.6863 0.2957 -0.0901 0.027 Uiso 1 1 calc R . . C34 C 1.7544(10) 0.1537(10) -0.0420(7) 0.021(2) Uani 1 1 d . . . C35 C 1.7707(10) 0.1037(9) 0.0273(7) 0.020(2) Uani 1 1 d . . . H35A H 1.8087 0.0309 0.0304 0.024 Uiso 1 1 calc R . . C36 C 1.7310(9) 0.1609(9) 0.0917(7) 0.019(2) Uani 1 1 d . . . H36A H 1.7419 0.1257 0.1384 0.023 Uiso 1 1 calc R . . C37 C 1.7965(13) 0.0913(12) -0.1136(8) 0.030(3) Uani 1 1 d . . . H37A H 1.7888 0.1381 -0.1569 0.045 Uiso 1 1 calc R . . H37B H 1.7550 0.0520 -0.1158 0.045 Uiso 1 1 calc R . . H37C H 1.8726 0.0438 -0.1138 0.045 Uiso 1 1 calc R . . C41 C 1.6042(9) 0.6180(9) 0.1776(7) 0.016(2) Uani 1 1 d . . . C42 C 1.5559(10) 0.7275(9) 0.1851(7) 0.018(2) Uani 1 1 d . . . H42A H 1.4938 0.7487 0.2263 0.021 Uiso 1 1 calc R . . C43 C 1.5283(10) 0.7923(9) 0.1246(7) 0.019(2) Uani 1 1 d . . . H43A H 1.4940 0.8643 0.1325 0.023 Uiso 1 1 calc R . . C44 C 1.5478(10) 0.7584(10) 0.0536(7) 0.021(2) Uani 1 1 d . . . C45 C 1.5979(10) 0.6507(10) 0.0434(7) 0.020(2) Uani 1 1 d . . . H45A H 1.6126 0.6240 -0.0050 0.024 Uiso 1 1 calc R . . C46 C 1.6261(10) 0.5833(9) 0.1051(7) 0.019(2) Uani 1 1 d . . . H46A H 1.6613 0.5114 0.0970 0.023 Uiso 1 1 calc R . . C47 C 1.5153(11) 0.8292(12) -0.0131(8) 0.028(3) Uani 1 1 d . . . H47A H 1.5085 0.8972 -0.0026 0.043 Uiso 1 1 calc R . . H47B H 1.4461 0.8354 -0.0234 0.043 Uiso 1 1 calc R . . H47C H 1.5702 0.8008 -0.0564 0.043 Uiso 1 1 calc R . . C51 C 2.0705(12) 0.6722(12) 0.3517(10) 0.035(3) Uani 1 1 d . . . H51A H 2.0761 0.6459 0.4031 0.052 Uiso 1 1 calc R . . H51B H 2.0545 0.7453 0.3499 0.052 Uiso 1 1 calc R . . H51C H 2.1386 0.6340 0.3199 0.052 Uiso 1 1 calc R . . C52 C 1.9648(14) 0.4258(11) 0.4124(8) 0.031(3) Uani 1 1 d . . . H52A H 1.9965 0.3506 0.4108 0.047 Uiso 1 1 calc R . . H52B H 1.8870 0.4526 0.4278 0.047 Uiso 1 1 calc R . . H52C H 1.9968 0.4463 0.4482 0.047 Uiso 1 1 calc R . . C53 C 2.1359(11) 0.4021(11) 0.2750(8) 0.027(3) Uiso 1 1 d . . . H53A H 2.1527 0.3288 0.2791 0.040 Uiso 1 1 calc R . . H53B H 2.1840 0.4153 0.3015 0.040 Uiso 1 1 calc R . . H53C H 2.1458 0.4220 0.2224 0.040 Uiso 1 1 calc R . . C54 C 2.0817(12) 0.6386(15) 0.1358(9) 0.038(4) Uani 1 1 d . . . H54A H 2.1396 0.6395 0.1591 0.056 Uiso 1 1 calc R . . H54B H 2.0840 0.6675 0.0851 0.056 Uiso 1 1 calc R . . H54C H 2.0911 0.5676 0.1340 0.056 Uiso 1 1 calc R . . C55 C 1.9356(14) 0.8506(13) 0.1863(9) 0.037(4) Uani 1 1 d . . . H55A H 1.9814 0.8567 0.2190 0.055 Uiso 1 1 calc R . . H55B H 1.8605 0.8982 0.2022 0.055 Uiso 1 1 calc R . . H55C H 1.9578 0.8676 0.1349 0.055 Uiso 1 1 calc R . . C56 C 1.7853(12) 0.8805(10) 0.4042(9) 0.031(3) Uani 1 1 d . . . H56A H 1.8307 0.8753 0.4413 0.046 Uiso 1 1 calc R . . H56B H 1.7107 0.9286 0.4212 0.046 Uiso 1 1 calc R . . H56C H 1.8109 0.9056 0.3567 0.046 Uiso 1 1 calc R . . C57 C 1.7790(13) 0.6933(11) 0.4889(7) 0.027(3) Uani 1 1 d . . . H57A H 1.8317 0.6966 0.5165 0.041 Uiso 1 1 calc R . . H57B H 1.7923 0.6213 0.4852 0.041 Uiso 1 1 calc R . . H57C H 1.7062 0.7322 0.5149 0.041 Uiso 1 1 calc R . . C61 C 1.9201(8) 0.4133(9) 0.2093(6) 0.0145(19) Uani 1 1 d . . . C62 C 1.9670(9) 0.3028(10) 0.2285(7) 0.018(2) Uani 1 1 d . . . H62A H 1.9959 0.2785 0.2768 0.021 Uiso 1 1 calc R . . C63 C 1.9759(9) 0.2309(9) 0.1781(7) 0.017(2) Uani 1 1 d . . . H63A H 2.0059 0.1566 0.1934 0.021 Uiso 1 1 calc R . . C64 C 1.9411(9) 0.2591(8) 0.1078(7) 0.016(2) Uani 1 1 d . . . C65 C 1.8934(9) 0.3648(9) 0.0899(7) 0.0154(19) Uani 1 1 d . . . H65A H 1.8671 0.3887 0.0407 0.018 Uiso 1 1 calc R . . C66 C 1.8863(9) 0.4362(8) 0.1397(6) 0.0140(19) Uani 1 1 d . . . H66A H 1.8550 0.5102 0.1235 0.017 Uiso 1 1 calc R . . C67 C 1.9651(11) 0.1801(10) 0.0516(8) 0.024(3) Uani 1 1 d . . . H67A H 2.0391 0.1583 0.0264 0.036 Uiso 1 1 calc R . . H67B H 1.9152 0.2096 0.0149 0.036 Uiso 1 1 calc R . . H67C H 1.9569 0.1206 0.0767 0.036 Uiso 1 1 calc R . . C71 C 1.8221(9) 0.7467(9) 0.0848(7) 0.017(2) Uani 1 1 d . . . C72 C 1.8631(10) 0.6781(9) 0.0250(7) 0.018(2) Uani 1 1 d . . . H72A H 1.9094 0.6078 0.0331 0.022 Uiso 1 1 calc R . . C73 C 1.8359(10) 0.7130(10) -0.0458(7) 0.019(2) Uani 1 1 d . . . H73A H 1.8637 0.6653 -0.0851 0.023 Uiso 1 1 calc R . . C74 C 1.7698(10) 0.8148(10) -0.0607(7) 0.019(2) Uani 1 1 d . . . C75 C 1.7317(9) 0.8818(9) -0.0022(7) 0.019(2) Uani 1 1 d . . . H75A H 1.6875 0.9525 -0.0112 0.022 Uiso 1 1 calc R . . C76 C 1.7563(10) 0.8486(9) 0.0704(7) 0.017(2) Uani 1 1 d . . . H76A H 1.7275 0.8965 0.1096 0.020 Uiso 1 1 calc R . . C77 C 1.7389(11) 0.8534(11) -0.1367(8) 0.026(3) Uani 1 1 d . . . H77A H 1.7602 0.7948 -0.1688 0.040 Uiso 1 1 calc R . . H77B H 1.7754 0.8960 -0.1585 0.040 Uiso 1 1 calc R . . H77C H 1.6608 0.8946 -0.1324 0.040 Uiso 1 1 calc R . . C81 C 1.5964(9) 0.8419(9) 0.3459(7) 0.019(2) Uani 1 1 d . . . C82 C 1.5188(11) 0.8625(10) 0.4085(7) 0.025(3) Uani 1 1 d . . . H82A H 1.5348 0.8182 0.4511 0.030 Uiso 1 1 calc R . . C83 C 1.4190(12) 0.9456(12) 0.4106(7) 0.030(3) Uani 1 1 d . . . H83A H 1.3671 0.9549 0.4536 0.036 Uiso 1 1 calc R . . C84 C 1.3921(10) 1.0166(10) 0.3510(7) 0.023(2) Uani 1 1 d . . . C85 C 1.4690(11) 0.9960(9) 0.2881(7) 0.022(2) Uani 1 1 d . . . H85A H 1.4535 1.0416 0.2462 0.027 Uiso 1 1 calc R . . C86 C 1.5667(9) 0.9115(8) 0.2846(6) 0.016(2) Uani 1 1 d . . . H86A H 1.6160 0.8993 0.2398 0.020 Uiso 1 1 calc R . . C87 C 1.2839(13) 1.1089(13) 0.3532(11) 0.042(4) Uani 1 1 d . . . H87A H 1.2480 1.1210 0.4048 0.064 Uiso 1 1 calc R . . H87B H 1.2393 1.0958 0.3232 0.064 Uiso 1 1 calc R . . H87C H 1.2942 1.1696 0.3332 0.064 Uiso 1 1 calc R . . C91 C 1.7195(19) 0.0766(18) 0.2464(13) 0.059(6) Uiso 1 1 d . . . C92 C 1.345(2) 0.585(2) 0.2383(16) 0.077(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0110(2) 0.0090(2) 0.0142(2) 0.00122(18) -0.00322(18) -0.00383(18) Sm2 0.0132(2) 0.0107(2) 0.0151(3) 0.00003(19) -0.00489(19) -0.00483(19) Si1 0.0146(13) 0.0126(13) 0.0191(15) 0.0006(11) -0.0020(11) -0.0054(11) Si2 0.0169(14) 0.0156(15) 0.0222(16) 0.0062(12) -0.0022(12) -0.0044(12) Si3 0.0164(14) 0.0163(14) 0.0200(15) 0.0008(12) -0.0049(12) -0.0081(12) Si4 0.0102(12) 0.0167(14) 0.0165(14) -0.0017(11) -0.0029(11) -0.0034(11) Si5 0.0120(12) 0.0136(13) 0.0136(13) -0.0027(10) -0.0044(10) -0.0047(11) Si6 0.0178(14) 0.0132(14) 0.0263(17) -0.0010(12) -0.0105(13) -0.0036(12) Si7 0.0191(15) 0.0247(17) 0.0191(15) 0.0026(13) -0.0043(12) -0.0127(13) Si8 0.0215(15) 0.0136(14) 0.0166(14) -0.0025(11) -0.0039(12) -0.0062(12) N2 0.014(4) 0.010(4) 0.021(5) 0.006(3) -0.005(4) -0.001(3) N3 0.017(4) 0.017(4) 0.018(5) -0.001(4) -0.002(4) -0.006(4) N4 0.011(4) 0.012(4) 0.016(4) -0.003(3) 0.001(3) -0.003(3) N6 0.014(4) 0.015(4) 0.025(5) -0.001(4) -0.011(4) -0.005(4) N7 0.023(5) 0.021(5) 0.025(5) 0.002(4) -0.011(4) -0.014(4) N8 0.021(5) 0.009(4) 0.025(5) -0.002(4) -0.006(4) -0.002(4) C1 0.018(5) 0.027(6) 0.028(6) -0.002(5) 0.000(5) -0.012(5) C2 0.031(7) 0.033(7) 0.019(6) -0.001(5) 0.002(5) -0.006(6) C3 0.031(7) 0.017(6) 0.042(8) 0.005(5) -0.001(6) -0.013(5) C4 0.027(7) 0.033(8) 0.054(10) -0.006(7) 0.003(7) -0.023(6) C5 0.018(6) 0.028(7) 0.037(8) 0.002(6) -0.011(5) -0.006(5) C6 0.026(6) 0.024(6) 0.022(6) -0.006(5) 0.006(5) -0.008(5) C7 0.034(7) 0.032(7) 0.014(5) 0.003(5) -0.014(5) -0.014(6) C21 0.020(5) 0.018(5) 0.015(5) 0.007(4) -0.005(4) -0.006(4) C22 0.020(5) 0.023(6) 0.023(6) 0.003(5) -0.007(5) -0.004(5) C23 0.018(6) 0.040(8) 0.026(7) 0.002(6) -0.013(5) -0.006(5) C24 0.020(6) 0.029(7) 0.038(8) 0.017(6) -0.001(5) -0.008(5) C25 0.023(6) 0.020(6) 0.044(9) 0.001(6) -0.001(6) -0.002(5) C26 0.014(5) 0.027(6) 0.026(6) 0.003(5) -0.007(5) 0.002(5) C27 0.029(8) 0.031(8) 0.063(12) 0.017(8) -0.010(8) 0.005(7) C31 0.011(4) 0.019(5) 0.020(5) -0.006(4) 0.002(4) -0.008(4) C32 0.026(6) 0.020(6) 0.022(6) 0.004(5) -0.006(5) -0.013(5) C33 0.026(6) 0.028(6) 0.018(5) 0.008(5) -0.006(5) -0.016(5) C34 0.017(5) 0.025(6) 0.025(6) -0.009(5) -0.002(4) -0.011(5) C35 0.017(5) 0.012(5) 0.027(6) -0.004(4) -0.003(4) -0.003(4) C36 0.017(5) 0.015(5) 0.029(6) 0.009(4) -0.010(4) -0.008(4) C37 0.038(8) 0.035(8) 0.026(7) -0.012(6) 0.001(6) -0.023(7) C41 0.011(4) 0.016(5) 0.025(6) -0.005(4) -0.013(4) -0.004(4) C42 0.018(5) 0.017(5) 0.019(5) 0.000(4) -0.003(4) -0.008(4) C43 0.020(5) 0.015(5) 0.024(6) 0.004(4) -0.010(4) -0.008(4) C44 0.022(5) 0.020(5) 0.023(6) 0.007(4) -0.010(5) -0.012(5) C45 0.020(5) 0.023(6) 0.018(5) -0.003(4) -0.004(4) -0.009(5) C46 0.021(5) 0.016(5) 0.021(5) -0.001(4) -0.009(4) -0.008(4) C47 0.026(6) 0.033(7) 0.031(7) 0.014(6) -0.015(6) -0.016(6) C51 0.030(7) 0.031(7) 0.047(9) 0.005(7) -0.016(7) -0.014(6) C52 0.047(9) 0.025(7) 0.026(7) 0.009(5) -0.020(6) -0.016(6) C54 0.025(7) 0.062(11) 0.025(7) -0.008(7) 0.004(5) -0.018(7) C55 0.045(9) 0.048(9) 0.037(8) 0.017(7) -0.019(7) -0.037(8) C56 0.031(7) 0.017(6) 0.045(9) -0.013(6) 0.003(6) -0.013(5) C57 0.040(8) 0.029(7) 0.019(6) 0.007(5) -0.009(5) -0.020(6) C61 0.010(4) 0.015(5) 0.018(5) -0.003(4) 0.002(4) -0.005(4) C62 0.014(5) 0.023(6) 0.018(5) 0.001(4) -0.004(4) -0.009(4) C63 0.013(4) 0.013(5) 0.028(6) 0.004(4) -0.004(4) -0.009(4) C64 0.014(5) 0.011(5) 0.022(5) -0.002(4) -0.003(4) -0.004(4) C65 0.014(4) 0.017(5) 0.019(5) 0.001(4) -0.003(4) -0.010(4) C66 0.017(5) 0.010(4) 0.016(5) 0.000(4) -0.003(4) -0.006(4) C67 0.023(6) 0.023(6) 0.031(7) -0.008(5) -0.002(5) -0.013(5) C71 0.017(5) 0.020(5) 0.018(5) -0.003(4) -0.005(4) -0.008(4) C72 0.020(5) 0.018(5) 0.016(5) -0.001(4) -0.002(4) -0.009(4) C73 0.024(5) 0.026(6) 0.013(5) 0.001(4) 0.000(4) -0.017(5) C74 0.018(5) 0.025(6) 0.017(5) -0.002(4) -0.002(4) -0.011(5) C75 0.016(5) 0.016(5) 0.022(5) 0.005(4) -0.005(4) -0.006(4) C76 0.020(5) 0.015(5) 0.016(5) 0.002(4) -0.007(4) -0.006(4) C77 0.021(6) 0.032(7) 0.027(6) 0.006(5) -0.007(5) -0.012(5) C81 0.011(4) 0.019(5) 0.030(6) -0.005(5) -0.008(4) -0.006(4) C82 0.028(6) 0.021(6) 0.020(6) 0.002(5) -0.003(5) -0.006(5) C83 0.026(6) 0.033(7) 0.016(6) 0.000(5) 0.001(5) -0.001(6) C84 0.022(6) 0.018(5) 0.025(6) -0.003(5) -0.014(5) -0.001(4) C85 0.029(6) 0.014(5) 0.019(5) 0.001(4) -0.011(5) -0.003(5) C86 0.016(5) 0.012(5) 0.013(5) -0.010(4) 0.005(4) 0.000(4) C87 0.027(7) 0.030(8) 0.050(10) 0.002(7) -0.007(7) 0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N2 2.236(10) . ? Sm1 N3 2.239(10) . ? Sm1 N4 2.507(9) . ? Sm1 C66 2.835(11) . ? Sm1 C61 2.854(11) . ? Sm1 C62 2.882(11) . ? Sm1 C65 2.933(11) . ? Sm1 C63 2.969(11) . ? Sm1 C64 3.039(12) . ? Sm1 Si1 3.253(3) . ? Sm1 Si3 3.301(3) . ? Sm1 Si2 3.316(4) . ? Sm2 N7 2.244(11) . ? Sm2 N8 2.265(10) . ? Sm2 N6 2.343(10) . ? Sm2 N4 2.543(10) . ? Sm2 C41 2.801(10) . ? Sm2 C42 2.884(12) . ? Sm2 Si7 3.289(3) . ? Sm2 Si5 3.355(3) . ? Sm2 Si8 3.402(3) . ? Si1 C1 1.899(13) . ? Si1 Si2 2.357(5) . ? Si1 Si3 2.367(5) . ? Si1 Si4 2.367(5) . ? Si2 N2 1.725(11) . ? Si2 C2 1.863(15) . ? Si2 C3 1.876(14) . ? Si3 N3 1.732(11) . ? Si3 C5 1.873(14) . ? Si3 C4 1.897(14) . ? Si4 N4 1.757(10) . ? Si4 C7 1.876(12) . ? Si4 C6 1.896(14) . ? Si5 C51 1.924(15) . ? Si5 Si8 2.358(5) . ? Si5 Si6 2.366(5) . ? Si5 Si7 2.377(5) . ? Si6 N6 1.740(10) . ? Si6 C53 1.880(14) . ? Si6 C52 1.885(15) . ? Si7 N7 1.734(10) . ? Si7 C55 1.853(16) . ? Si7 C54 1.868(15) . ? Si8 N8 1.720(11) . ? Si8 C56 1.873(13) . ? Si8 C57 1.905(13) . ? N2 C21 1.438(14) . ? N3 C31 1.411(15) . ? N4 C41 1.417(15) . ? N6 C61 1.352(15) . ? N7 C71 1.428(16) . ? N8 C81 1.399(15) . ? C21 C26 1.363(18) . ? C21 C22 1.408(18) . ? C22 C23 1.403(18) . ? C23 C24 1.37(2) . ? C24 C25 1.38(2) . ? C24 C27 1.54(2) . ? C25 C26 1.405(18) . ? C31 C32 1.399(17) . ? C31 C36 1.405(16) . ? C32 C33 1.357(19) . ? C33 C34 1.391(19) . ? C34 C35 1.398(19) . ? C34 C37 1.536(18) . ? C35 C36 1.388(18) . ? C41 C46 1.393(17) . ? C41 C42 1.433(16) . ? C42 C43 1.370(16) . ? C43 C44 1.369(18) . ? C44 C45 1.416(18) . ? C44 C47 1.508(18) . ? C45 C46 1.407(17) . ? C61 C66 1.389(16) . ? C61 C62 1.471(16) . ? C62 C63 1.402(17) . ? C63 C64 1.407(17) . ? C64 C65 1.406(16) . ? C64 C67 1.494(17) . ? C65 C66 1.398(15) . ? C71 C76 1.381(16) . ? C71 C72 1.412(16) . ? C72 C73 1.392(16) . ? C73 C74 1.383(18) . ? C74 C75 1.380(17) . ? C74 C77 1.506(18) . ? C75 C76 1.411(16) . ? C81 C82 1.389(18) . ? C81 C86 1.420(17) . ? C82 C83 1.383(19) . ? C83 C84 1.403(19) . ? C84 C85 1.387(19) . ? C84 C87 1.514(19) . ? C85 C86 1.372(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 N2 Sm1 N3 106.5(4) . . ? N2 Sm1 N4 118.1(3) . . ? N3 Sm1 N4 102.9(3) . . ? N2 Sm1 C66 129.1(3) . . ? N3 Sm1 C66 116.5(3) . . ? N4 Sm1 C66 78.3(3) . . ? N2 Sm1 C61 102.5(3) . . ? N3 Sm1 C61 143.8(4) . . ? N4 Sm1 C61 81.5(3) . . ? C66 Sm1 C61 28.3(3) . . ? N2 Sm1 C62 80.2(3) . . ? N3 Sm1 C62 138.9(4) . . ? N4 Sm1 C62 109.3(3) . . ? C66 Sm1 C62 49.6(3) . . ? C61 Sm1 C62 29.7(3) . . ? N2 Sm1 C65 131.9(3) . . ? N3 Sm1 C65 93.3(3) . . ? N4 Sm1 C65 98.5(3) . . ? C66 Sm1 C65 28.0(3) . . ? C61 Sm1 C65 50.7(3) . . ? C62 Sm1 C65 57.8(3) . . ? N2 Sm1 C63 83.9(3) . . ? N3 Sm1 C63 111.4(3) . . ? N4 Sm1 C63 131.6(3) . . ? C66 Sm1 C63 56.4(3) . . ? C61 Sm1 C63 50.7(3) . . ? C62 Sm1 C63 27.7(3) . . ? C65 Sm1 C63 48.0(3) . . ? N2 Sm1 C64 107.3(3) . . ? N3 Sm1 C64 91.3(3) . . ? N4 Sm1 C64 125.1(3) . . ? C66 Sm1 C64 48.7(3) . . ? C61 Sm1 C64 59.1(3) . . ? C62 Sm1 C64 49.2(3) . . ? C65 Sm1 C64 27.2(3) . . ? C63 Sm1 C64 27.1(3) . . ? N2 Sm1 Si1 70.4(3) . . ? N3 Sm1 Si1 71.0(3) . . ? N4 Sm1 Si1 69.9(2) . . ? C66 Sm1 Si1 148.1(2) . . ? C61 Sm1 Si1 140.8(2) . . ? C62 Sm1 Si1 144.3(2) . . ? C65 Sm1 Si1 156.8(2) . . ? C63 Sm1 Si1 153.3(2) . . ? C64 Sm1 Si1 159.9(2) . . ? N2 Sm1 Si3 95.5(3) . . ? N3 Sm1 Si3 29.2(3) . . ? N4 Sm1 Si3 85.2(2) . . ? C66 Sm1 Si3 135.2(2) . . ? C61 Sm1 Si3 161.2(2) . . ? C62 Sm1 Si3 165.3(3) . . ? C65 Sm1 Si3 119.0(2) . . ? C63 Sm1 Si3 138.3(2) . . ? C64 Sm1 Si3 120.5(2) . . ? Si1 Sm1 Si3 42.33(9) . . ? N2 Sm1 Si2 28.6(3) . . ? N3 Sm1 Si2 89.4(3) . . ? N4 Sm1 Si2 101.5(2) . . ? C66 Sm1 Si2 153.7(2) . . ? C61 Sm1 Si2 125.4(2) . . ? C62 Sm1 Si2 108.0(2) . . ? C65 Sm1 Si2 158.7(2) . . ? C63 Sm1 Si2 111.7(2) . . ? C64 Sm1 Si2 131.7(2) . . ? Si1 Sm1 Si2 42.03(8) . . ? Si3 Sm1 Si2 70.28(9) . . ? N7 Sm2 N8 103.4(4) . . ? N7 Sm2 N6 95.0(4) . . ? N8 Sm2 N6 118.4(4) . . ? N7 Sm2 N4 132.7(3) . . ? N8 Sm2 N4 114.8(4) . . ? N6 Sm2 N4 90.5(3) . . ? N7 Sm2 C41 106.5(4) . . ? N8 Sm2 C41 119.0(4) . . ? N6 Sm2 C41 110.4(3) . . ? N4 Sm2 C41 30.3(3) . . ? N7 Sm2 C42 97.0(4) . . ? N8 Sm2 C42 96.1(4) . . ? N6 Sm2 C42 139.4(3) . . ? N4 Sm2 C42 53.9(3) . . ? C41 Sm2 C42 29.2(3) . . ? N7 Sm2 Si7 29.5(3) . . ? N8 Sm2 Si7 87.6(3) . . ? N6 Sm2 Si7 80.8(3) . . ? N4 Sm2 Si7 157.3(2) . . ? C41 Sm2 Si7 135.8(3) . . ? C42 Sm2 Si7 123.9(2) . . ? N7 Sm2 Si5 71.4(3) . . ? N8 Sm2 Si5 66.9(3) . . ? N6 Sm2 Si5 64.7(2) . . ? N4 Sm2 Si5 148.7(2) . . ? C41 Sm2 Si5 174.0(2) . . ? C42 Sm2 Si5 155.4(2) . . ? Si7 Sm2 Si5 41.91(8) . . ? N7 Sm2 Si8 95.3(3) . . ? N8 Sm2 Si8 26.9(3) . . ? N6 Sm2 Si8 94.3(2) . . ? N4 Sm2 Si8 131.1(2) . . ? C41 Sm2 Si8 144.9(3) . . ? C42 Sm2 Si8 122.8(2) . . ? Si7 Sm2 Si8 70.77(9) . . ? Si5 Sm2 Si8 40.85(8) . . ? C1 Si1 Si2 109.7(5) . . ? C1 Si1 Si3 108.7(4) . . ? Si2 Si1 Si3 107.48(18) . . ? C1 Si1 Si4 109.9(4) . . ? Si2 Si1 Si4 110.05(18) . . ? Si3 Si1 Si4 110.91(17) . . ? C1 Si1 Sm1 178.5(4) . . ? Si2 Si1 Sm1 70.41(12) . . ? Si3 Si1 Sm1 69.91(11) . . ? Si4 Si1 Sm1 71.28(11) . . ? N2 Si2 C2 112.5(6) . . ? N2 Si2 C3 113.5(6) . . ? C2 Si2 C3 105.1(7) . . ? N2 Si2 Si1 105.4(3) . . ? C2 Si2 Si1 110.7(5) . . ? C3 Si2 Si1 109.7(5) . . ? N2 Si2 Sm1 38.3(3) . . ? C2 Si2 Sm1 131.8(5) . . ? C3 Si2 Sm1 121.2(5) . . ? Si1 Si2 Sm1 67.55(11) . . ? N3 Si3 C5 113.3(6) . . ? N3 Si3 C4 112.5(6) . . ? C5 Si3 C4 107.4(7) . . ? N3 Si3 Si1 105.9(4) . . ? C5 Si3 Si1 109.6(5) . . ? C4 Si3 Si1 108.0(6) . . ? N3 Si3 Sm1 39.0(3) . . ? C5 Si3 Sm1 118.9(5) . . ? C4 Si3 Sm1 132.3(5) . . ? Si1 Si3 Sm1 67.76(11) . . ? N4 Si4 C7 106.2(6) . . ? N4 Si4 C6 115.0(5) . . ? C7 Si4 C6 111.3(7) . . ? N4 Si4 Si1 108.0(4) . . ? C7 Si4 Si1 108.9(5) . . ? C6 Si4 Si1 107.4(5) . . ? N4 Si4 Sm1 46.9(3) . . ? C7 Si4 Sm1 99.0(5) . . ? C6 Si4 Sm1 149.0(5) . . ? Si1 Si4 Sm1 66.76(11) . . ? C51 Si5 Si8 109.4(6) . . ? C51 Si5 Si6 111.2(5) . . ? Si8 Si5 Si6 110.92(18) . . ? C51 Si5 Si7 108.0(5) . . ? Si8 Si5 Si7 109.86(17) . . ? Si6 Si5 Si7 107.42(17) . . ? C51 Si5 Sm2 174.8(5) . . ? Si8 Si5 Sm2 70.65(11) . . ? Si6 Si5 Sm2 73.20(11) . . ? Si7 Si5 Sm2 67.56(11) . . ? N6 Si6 C53 110.6(6) . . ? N6 Si6 C52 112.9(6) . . ? C53 Si6 C52 110.1(7) . . ? N6 Si6 Si5 99.8(4) . . ? C53 Si6 Si5 109.4(5) . . ? C52 Si6 Si5 113.7(5) . . ? N7 Si7 C55 111.9(6) . . ? N7 Si7 C54 111.7(7) . . ? C55 Si7 C54 105.9(8) . . ? N7 Si7 Si5 110.1(4) . . ? C55 Si7 Si5 109.4(5) . . ? C54 Si7 Si5 107.6(6) . . ? N7 Si7 Sm2 39.6(4) . . ? C55 Si7 Sm2 126.7(6) . . ? C54 Si7 Sm2 125.5(6) . . ? Si5 Si7 Sm2 70.53(11) . . ? N8 Si8 C56 112.3(6) . . ? N8 Si8 C57 113.6(6) . . ? C56 Si8 C57 106.2(7) . . ? N8 Si8 Si5 103.6(4) . . ? C56 Si8 Si5 107.5(5) . . ? C57 Si8 Si5 113.7(5) . . ? N8 Si8 Sm2 36.5(3) . . ? C56 Si8 Sm2 132.4(5) . . ? C57 Si8 Sm2 119.0(4) . . ? Si5 Si8 Sm2 68.51(11) . . ? C21 N2 Si2 116.0(8) . . ? C21 N2 Sm1 130.1(8) . . ? Si2 N2 Sm1 113.1(5) . . ? C31 N3 Si3 120.1(8) . . ? C31 N3 Sm1 128.1(8) . . ? Si3 N3 Sm1 111.8(5) . . ? C41 N4 Si4 119.6(8) . . ? C41 N4 Sm1 120.2(7) . . ? Si4 N4 Sm1 102.3(4) . . ? C41 N4 Sm2 85.0(6) . . ? Si4 N4 Sm2 116.0(5) . . ? Sm1 N4 Sm2 113.9(3) . . ? C61 N6 Si6 126.7(8) . . ? C61 N6 Sm2 115.4(7) . . ? Si6 N6 Sm2 117.3(5) . . ? C71 N7 Si7 119.1(8) . . ? C71 N7 Sm2 129.9(8) . . ? Si7 N7 Sm2 110.9(5) . . ? C81 N8 Si8 119.6(8) . . ? C81 N8 Sm2 122.3(8) . . ? Si8 N8 Sm2 116.6(5) . . ? C26 C21 C22 118.1(11) . . ? C26 C21 N2 121.3(11) . . ? C22 C21 N2 120.6(11) . . ? C23 C22 C21 120.3(13) . . ? C24 C23 C22 120.9(13) . . ? C23 C24 C25 118.9(13) . . ? C23 C24 C27 120.0(16) . . ? C25 C24 C27 121.1(16) . . ? C24 C25 C26 120.5(14) . . ? C21 C26 C25 121.2(13) . . ? C32 C31 C36 115.3(11) . . ? C32 C31 N3 123.7(11) . . ? C36 C31 N3 121.0(11) . . ? C33 C32 C31 122.9(12) . . ? C32 C33 C34 121.3(12) . . ? C33 C34 C35 118.1(11) . . ? C33 C34 C37 121.7(13) . . ? C35 C34 C37 120.2(12) . . ? C36 C35 C34 119.6(11) . . ? C35 C36 C31 122.8(11) . . ? C46 C41 N4 123.2(10) . . ? C46 C41 C42 115.6(11) . . ? N4 C41 C42 120.7(10) . . ? C46 C41 Sm2 122.8(8) . . ? N4 C41 Sm2 64.7(5) . . ? C42 C41 Sm2 78.7(6) . . ? C43 C42 C41 121.2(11) . . ? C43 C42 Sm2 128.3(8) . . ? C41 C42 Sm2 72.2(6) . . ? C42 C43 C44 123.3(12) . . ? C43 C44 C45 117.3(11) . . ? C43 C44 C47 123.6(12) . . ? C45 C44 C47 119.0(12) . . ? C46 C45 C44 120.0(11) . . ? C41 C46 C45 122.6(11) . . ? N6 C61 C66 123.4(10) . . ? N6 C61 C62 122.6(11) . . ? C66 C61 C62 113.9(10) . . ? N6 C61 Sm1 113.3(7) . . ? C66 C61 Sm1 75.1(6) . . ? C62 C61 Sm1 76.2(6) . . ? C63 C62 C61 120.5(11) . . ? C63 C62 Sm1 79.6(6) . . ? C61 C62 Sm1 74.1(6) . . ? C62 C63 C64 122.9(11) . . ? C62 C63 Sm1 72.7(6) . . ? C64 C63 Sm1 79.2(7) . . ? C65 C64 C63 117.0(10) . . ? C65 C64 C67 121.3(11) . . ? C63 C64 C67 121.3(11) . . ? C65 C64 Sm1 72.2(6) . . ? C63 C64 Sm1 73.7(7) . . ? C67 C64 Sm1 130.0(8) . . ? C66 C65 C64 120.0(11) . . ? C66 C65 Sm1 72.1(6) . . ? C64 C65 Sm1 80.6(7) . . ? C61 C66 C65 125.7(10) . . ? C61 C66 Sm1 76.7(6) . . ? C65 C66 Sm1 79.9(6) . . ? C76 C71 C72 118.0(11) . . ? C76 C71 N7 122.1(11) . . ? C72 C71 N7 119.8(11) . . ? C73 C72 C71 120.3(11) . . ? C74 C73 C72 122.1(12) . . ? C75 C74 C73 117.2(11) . . ? C75 C74 C77 120.0(12) . . ? C73 C74 C77 122.8(12) . . ? C74 C75 C76 122.0(11) . . ? C71 C76 C75 120.3(11) . . ? C82 C81 N8 124.2(12) . . ? C82 C81 C86 115.8(11) . . ? N8 C81 C86 120.0(11) . . ? C83 C82 C81 121.7(12) . . ? C82 C83 C84 122.0(13) . . ? C85 C84 C83 116.4(11) . . ? C85 C84 C87 121.1(13) . . ? C83 C84 C87 122.4(14) . . ? C86 C85 C84 121.9(11) . . ? C85 C86 C81 122.0(11) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 33.19 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 7.232 _refine_diff_density_min -5.385 _refine_diff_density_rms 0.363 #===END data_13 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57.20 H78.80 B N3 Si3 Zr' _chemical_formula_weight 994.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 43.7510(12) _cell_length_b 12.7618(4) _cell_length_c 26.9246(7) _cell_angle_alpha 90.00 _cell_angle_beta 127.374(2) _cell_angle_gamma 90.00 _cell_volume 11946.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8113 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.33 _exptl_crystal_description triangular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.221 _exptl_crystal_size_mid 0.157 _exptl_crystal_size_min 0.073 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4240 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS, Scheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 175125 _diffrn_reflns_av_R_equivalents 0.1306 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 28.28 _reflns_number_total 14811 _reflns_number_gt 9039 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+42.8728P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14811 _refine_ls_number_parameters 632 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1212 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.2172 _refine_ls_wR_factor_gt 0.1794 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.080846(11) 0.55406(3) 0.953737(19) 0.04017(13) Uani 1 1 d . . . B1 B 0.30693(13) 0.4851(4) 1.1688(2) 0.0380(10) Uani 1 1 d . . . Si1 Si 0.16578(3) 0.45229(10) 1.09614(5) 0.0394(3) Uani 1 1 d . . . Si2 Si 0.23008(3) 0.55158(9) 1.08495(5) 0.0320(2) Uani 1 1 d . . . Si3 Si 0.25594(4) 0.41328(10) 1.19630(5) 0.0424(3) Uani 1 1 d . . . N1 N 0.12734(9) 0.4514(3) 1.01598(15) 0.0369(7) Uani 1 1 d . . . N2 N 0.27507(9) 0.5124(3) 1.10562(14) 0.0344(7) Uani 1 1 d . . . N3 N 0.29891(10) 0.4622(3) 1.21259(15) 0.0373(7) Uani 1 1 d . . . C1 C 0.21444(11) 0.4454(3) 1.11300(17) 0.0349(8) Uani 1 1 d . . . H1A H 0.2124 0.3823 1.0891 0.042 Uiso 1 1 calc R . . C2 C 0.16111(14) 0.3321(4) 1.1312(2) 0.0522(12) Uani 1 1 d . . . H2A H 0.1346 0.3260 1.1170 0.078 Uiso 1 1 calc R . . H2B H 0.1786 0.3376 1.1769 0.078 Uiso 1 1 calc R . . H2C H 0.1677 0.2700 1.1181 0.078 Uiso 1 1 calc R . . C3 C 0.16246(13) 0.5715(4) 1.1327(2) 0.0491(11) Uani 1 1 d . . . H3A H 0.1618 0.6341 1.1110 0.074 Uiso 1 1 calc R . . H3B H 0.1849 0.5748 1.1769 0.074 Uiso 1 1 calc R . . H3C H 0.1389 0.5682 1.1295 0.074 Uiso 1 1 calc R . . C4 C 0.23526(12) 0.6803(3) 1.1228(2) 0.0424(9) Uani 1 1 d . . . H4A H 0.2521 0.6717 1.1683 0.064 Uiso 1 1 calc R . . H4B H 0.2099 0.7047 1.1087 0.064 Uiso 1 1 calc R . . H4C H 0.2465 0.7318 1.1112 0.064 Uiso 1 1 calc R . . C5 C 0.19775(11) 0.5679(3) 0.99821(17) 0.0373(9) Uani 1 1 d . . . H5A H 0.2055 0.6302 0.9871 0.056 Uiso 1 1 calc R . . H5B H 0.1711 0.5762 0.9833 0.056 Uiso 1 1 calc R . . H5C H 0.1996 0.5060 0.9787 0.056 Uiso 1 1 calc R . . C6 C 0.26026(16) 0.2684(4) 1.2077(3) 0.0670(15) Uani 1 1 d . . . H6A H 0.2810 0.2523 1.2516 0.100 Uiso 1 1 calc R . . H6B H 0.2661 0.2369 1.1811 0.100 Uiso 1 1 calc R . . H6C H 0.2360 0.2400 1.1962 0.100 Uiso 1 1 calc R . . C7 C 0.25245(16) 0.4704(5) 1.2563(2) 0.0629(15) Uani 1 1 d . . . H7A H 0.2746 0.4480 1.2979 0.094 Uiso 1 1 calc R . . H7B H 0.2287 0.4462 1.2488 0.094 Uiso 1 1 calc R . . H7C H 0.2522 0.5470 1.2537 0.094 Uiso 1 1 calc R . . C11 C 0.12236(11) 0.3498(3) 0.98850(17) 0.0350(8) Uani 1 1 d . . . C12 C 0.14465(11) 0.3143(3) 0.97062(18) 0.0362(8) Uani 1 1 d . . . H12A H 0.1648 0.3572 0.9780 0.043 Uiso 1 1 calc R . . C13 C 0.13776(12) 0.2175(3) 0.94231(19) 0.0419(10) Uani 1 1 d . . . H13A H 0.1532 0.1955 0.9304 0.050 Uiso 1 1 calc R . . C14 C 0.10874(12) 0.1515(3) 0.93083(19) 0.0434(10) Uani 1 1 d . . . C15 C 0.08710(13) 0.1859(4) 0.9495(2) 0.0472(10) Uani 1 1 d . . . H15A H 0.0674 0.1420 0.9430 0.057 Uiso 1 1 calc R . . C16 C 0.09347(12) 0.2829(3) 0.9774(2) 0.0423(10) Uani 1 1 d . . . H16A H 0.0779 0.3044 0.9892 0.051 Uiso 1 1 calc R . . C17 C 0.10145(15) 0.0471(4) 0.8993(2) 0.0599(13) Uani 1 1 d . . . H17A H 0.0854 0.0039 0.9052 0.090 Uiso 1 1 calc R . . H17B H 0.1260 0.0115 0.9176 0.090 Uiso 1 1 calc R . . H17C H 0.0882 0.0579 0.8545 0.090 Uiso 1 1 calc R . . C21 C 0.28190(11) 0.5200(3) 1.05994(17) 0.0345(8) Uani 1 1 d . . . C22 C 0.27568(13) 0.4341(4) 1.02363(19) 0.0438(10) Uani 1 1 d . . . H22A H 0.2657 0.3712 1.0276 0.053 Uiso 1 1 calc R . . C23 C 0.28398(14) 0.4394(4) 0.9811(2) 0.0565(13) Uani 1 1 d . . . H23A H 0.2794 0.3798 0.9563 0.068 Uiso 1 1 calc R . . C24 C 0.29877(13) 0.5302(5) 0.9745(2) 0.0534(13) Uani 1 1 d . . . C25 C 0.30397(13) 0.6154(4) 1.0099(2) 0.0504(11) Uani 1 1 d . . . H25A H 0.3137 0.6785 1.0056 0.061 Uiso 1 1 calc R . . C26 C 0.29540(12) 0.6123(4) 1.0518(2) 0.0435(10) Uani 1 1 d . . . H26A H 0.2988 0.6732 1.0749 0.052 Uiso 1 1 calc R . . C27 C 0.30988(18) 0.5336(6) 0.9310(3) 0.082(2) Uani 1 1 d . . . H27A H 0.3314 0.5824 0.9476 0.123 Uiso 1 1 calc R . . H27B H 0.2878 0.5572 0.8895 0.123 Uiso 1 1 calc R . . H27C H 0.3176 0.4635 0.9277 0.123 Uiso 1 1 calc R . . C31 C 0.33174(12) 0.4573(3) 1.27813(18) 0.0402(9) Uani 1 1 d . . . C32 C 0.34143(12) 0.5441(4) 1.3156(2) 0.0423(9) Uani 1 1 d . . . H32A H 0.3262 0.6058 1.2985 0.051 Uiso 1 1 calc R . . C33 C 0.37353(13) 0.5418(4) 1.3787(2) 0.0500(11) Uani 1 1 d . . . H33A H 0.3799 0.6021 1.4039 0.060 Uiso 1 1 calc R . . C34 C 0.39617(16) 0.4526(4) 1.4047(2) 0.0603(14) Uani 1 1 d . . . C35 C 0.38668(16) 0.3675(4) 1.3663(2) 0.0700(16) Uani 1 1 d . . . H35A H 0.4025 0.3068 1.3828 0.084 Uiso 1 1 calc R . . C36 C 0.35436(15) 0.3685(4) 1.3038(2) 0.0597(13) Uani 1 1 d . . . H36A H 0.3479 0.3079 1.2787 0.072 Uiso 1 1 calc R . . C37 C 0.43056(19) 0.4500(5) 1.4730(2) 0.083(2) Uani 1 1 d . . . H37A H 0.4494 0.3993 1.4792 0.124 Uiso 1 1 calc R . . H37B H 0.4222 0.4295 1.4982 0.124 Uiso 1 1 calc R . . H37C H 0.4424 0.5197 1.4860 0.124 Uiso 1 1 calc R . . C41 C 0.34931(12) 0.4838(4) 1.1902(2) 0.0491(11) Uani 1 1 d . . . H41A H 0.3667 0.5139 1.2321 0.074 Uiso 1 1 calc R . . H41B H 0.3506 0.5252 1.1609 0.074 Uiso 1 1 calc R . . H41C H 0.3570 0.4114 1.1907 0.074 Uiso 1 1 calc R . . C42 C 0.11368(13) 0.7088(4) 0.9860(2) 0.0478(11) Uani 1 1 d . . . H42A H 0.1384 0.6995 0.9935 0.072 Uiso 1 1 calc R . . H42B H 0.1182 0.7314 1.0248 0.072 Uiso 1 1 calc R . . H42C H 0.0985 0.7622 0.9537 0.072 Uiso 1 1 calc R . . C43 C -0.01207(13) 0.5189(4) 0.8137(2) 0.0516(11) Uani 1 1 d . . . H43A H -0.0163 0.4443 0.8181 0.062 Uiso 1 1 calc R . . H43B H -0.0299 0.5374 0.7689 0.062 Uiso 1 1 calc R . . C44 C -0.02078(13) 0.5874(5) 0.8507(3) 0.0595(13) Uani 1 1 d . . . H44A H -0.0250 0.6607 0.8358 0.071 Uiso 1 1 calc R . . H44B H -0.0446 0.5624 0.8434 0.071 Uiso 1 1 calc R . . C51 C 0.01152(13) 0.5836(4) 0.9187(2) 0.0553(12) Uani 1 1 d . . . C52 C 0.03515(14) 0.6662(5) 0.9580(3) 0.0586(13) Uani 1 1 d . . . H52A H 0.0301 0.7421 0.9464 0.070 Uiso 1 1 calc R . . C53 C 0.06230(15) 0.6277(5) 1.0197(3) 0.0615(15) Uani 1 1 d . . . H53A H 0.0792 0.6724 1.0576 0.074 Uiso 1 1 calc R . . C54 C 0.05452(13) 0.5225(5) 1.0203(2) 0.0562(13) Uani 1 1 d . . . C55 C 0.06829(15) 0.4459(5) 1.0678(3) 0.0663(16) Uani 1 1 d . . . H55A H 0.0896 0.4621 1.1095 0.080 Uiso 1 1 calc R . . C56 C 0.05155(17) 0.3497(6) 1.0550(3) 0.0706(16) Uani 1 1 d . . . H56A H 0.0605 0.3009 1.0878 0.085 Uiso 1 1 calc R . . C57 C 0.02023(16) 0.3219(5) 0.9914(3) 0.0676(15) Uani 1 1 d . . . H57A H 0.0087 0.2546 0.9829 0.081 Uiso 1 1 calc R . . C58 C 0.00690(14) 0.3903(5) 0.9437(3) 0.0588(13) Uani 1 1 d . . . H58A H -0.0132 0.3698 0.9020 0.071 Uiso 1 1 calc R . . C59 C 0.02299(13) 0.4927(5) 0.9562(2) 0.0546(13) Uani 1 1 d . . . C61 C 0.02873(12) 0.5339(4) 0.8369(2) 0.0420(10) Uani 1 1 d . . . C62 C 0.05651(12) 0.4533(3) 0.85612(19) 0.0408(9) Uani 1 1 d . . . H62A H 0.0508 0.3765 0.8503 0.049 Uiso 1 1 calc R . . C63 C 0.09109(12) 0.4991(3) 0.87315(18) 0.0381(9) Uani 1 1 d . . . H63A H 0.1139 0.4597 0.8827 0.046 Uiso 1 1 calc R . . C64 C 0.08486(11) 0.6089(3) 0.86116(18) 0.0382(9) Uani 1 1 d . . . C65 C 0.10751(12) 0.6900(3) 0.86321(19) 0.0430(10) Uani 1 1 d . . . H65A H 0.1329 0.6760 0.8771 0.052 Uiso 1 1 calc R . . C66 C 0.09261(13) 0.7889(4) 0.8450(2) 0.0523(11) Uani 1 1 d . . . H66A H 0.1075 0.8431 0.8450 0.063 Uiso 1 1 calc R . . C67 C 0.05520(14) 0.8111(4) 0.8260(2) 0.0565(12) Uani 1 1 d . . . H67A H 0.0457 0.8808 0.8146 0.068 Uiso 1 1 calc R . . C68 C 0.03243(13) 0.7354(4) 0.8238(2) 0.0508(11) Uani 1 1 d . . . H68A H 0.0075 0.7525 0.8113 0.061 Uiso 1 1 calc R . . C69 C 0.04621(12) 0.6304(3) 0.8401(2) 0.0428(10) Uani 1 1 d . . . C71A C 0.3084(4) 0.1938(10) 1.1239(7) 0.046(3) Uiso 0.328(6) 1 d PD A 1 H71A H 0.3029 0.2042 1.0831 0.069 Uiso 0.328(6) 1 calc PR A 1 H71B H 0.3276 0.2449 1.1538 0.069 Uiso 0.328(6) 1 calc PR A 1 H71C H 0.2847 0.2033 1.1197 0.069 Uiso 0.328(6) 1 calc PR A 1 C72A C 0.3229(5) 0.0892(11) 1.1459(6) 0.055(4) Uiso 0.328(6) 1 d PD A 1 H72A H 0.3032 0.0390 1.1147 0.066 Uiso 0.328(6) 1 calc PR A 1 H72B H 0.3459 0.0800 1.1474 0.066 Uiso 0.328(6) 1 calc PR A 1 C73A C 0.3329(5) 0.0621(12) 1.2045(7) 0.056(4) Uiso 0.328(6) 1 d PD A 1 H73A H 0.3090 0.0565 1.2008 0.067 Uiso 0.328(6) 1 calc PR A 1 H73B H 0.3484 0.1197 1.2341 0.067 Uiso 0.328(6) 1 calc PR A 1 C74A C 0.3561(5) -0.0430(11) 1.2329(8) 0.066(5) Uiso 0.328(6) 1 d PD A 1 H74A H 0.3755 -0.0476 1.2252 0.080 Uiso 0.328(6) 1 calc PR A 1 H74B H 0.3699 -0.0429 1.2787 0.080 Uiso 0.328(6) 1 calc PR A 1 C75A C 0.3291(4) -0.1401(11) 1.2038(7) 0.044(3) Uiso 0.328(6) 1 d PD A 1 H75A H 0.3092 -0.1357 1.2106 0.052 Uiso 0.328(6) 1 calc PR A 1 H75B H 0.3159 -0.1427 1.1582 0.052 Uiso 0.328(6) 1 calc PR A 1 C76A C 0.3526(5) -0.2343(11) 1.2340(8) 0.049(3) Uiso 0.328(6) 1 d PD A 1 H76A H 0.3358 -0.2960 1.2193 0.073 Uiso 0.328(6) 1 calc PR A 1 H76B H 0.3674 -0.2280 1.2794 0.073 Uiso 0.328(6) 1 calc PR A 1 H76C H 0.3703 -0.2420 1.2233 0.073 Uiso 0.328(6) 1 calc PR A 1 C71B C 0.3313(7) 0.155(2) 1.1570(12) 0.081(7) Uiso 0.272(6) 1 d PD A 2 H71D H 0.3200 0.2253 1.1500 0.121 Uiso 0.272(6) 1 calc PR A 2 H71E H 0.3263 0.1301 1.1184 0.121 Uiso 0.272(6) 1 calc PR A 2 H71F H 0.3591 0.1592 1.1901 0.121 Uiso 0.272(6) 1 calc PR A 2 C72B C 0.3136(7) 0.0813(14) 1.1765(12) 0.071(6) Uiso 0.272(6) 1 d PD A 2 H72C H 0.3193 0.1018 1.2169 0.085 Uiso 0.272(6) 1 calc PR A 2 H72D H 0.2854 0.0751 1.1442 0.085 Uiso 0.272(6) 1 calc PR A 2 C73B C 0.3341(5) -0.0162(12) 1.1820(8) 0.048(4) Uiso 0.272(6) 1 d PD A 2 H73C H 0.3622 -0.0065 1.2130 0.058 Uiso 0.272(6) 1 calc PR A 2 H73D H 0.3282 -0.0339 1.1412 0.058 Uiso 0.272(6) 1 calc PR A 2 C74B C 0.3207(7) -0.1027(15) 1.2026(12) 0.073(7) Uiso 0.272(6) 1 d PD A 2 H74C H 0.3267 -0.0816 1.2430 0.088 Uiso 0.272(6) 1 calc PR A 2 H74D H 0.2924 -0.1068 1.1719 0.088 Uiso 0.272(6) 1 calc PR A 2 C75B C 0.3360(4) -0.2090(13) 1.2103(7) 0.036(3) Uiso 0.272(6) 1 d PD A 2 H75C H 0.3234 -0.2579 1.2214 0.043 Uiso 0.272(6) 1 calc PR A 2 H75D H 0.3302 -0.2329 1.1704 0.043 Uiso 0.272(6) 1 calc PR A 2 C76B C 0.3776(5) -0.2097(18) 1.2595(9) 0.070(6) Uiso 0.272(6) 1 d PD A 2 H76D H 0.3858 -0.2802 1.2775 0.106 Uiso 0.272(6) 1 calc PR A 2 H76E H 0.3842 -0.1597 1.2922 0.106 Uiso 0.272(6) 1 calc PR A 2 H76F H 0.3908 -0.1898 1.2416 0.106 Uiso 0.272(6) 1 calc PR A 2 C81A C 0.4630(4) 0.5953(12) 1.3855(8) 0.053(4) Uiso 0.328(6) 1 d PD A 1 H81D H 0.4660 0.6716 1.3906 0.079 Uiso 0.328(6) 1 calc PR A 1 H81E H 0.4792 0.5617 1.4267 0.079 Uiso 0.328(6) 1 calc PR A 1 H81F H 0.4360 0.5769 1.3649 0.079 Uiso 0.328(6) 1 calc PR A 1 C82A C 0.4746(4) 0.5586(10) 1.3465(7) 0.045(3) Uiso 0.328(6) 1 d PD A 1 H82C H 0.5018 0.5775 1.3669 0.053 Uiso 0.328(6) 1 calc PR A 1 H82D H 0.4584 0.5925 1.3049 0.053 Uiso 0.328(6) 1 calc PR A 1 C83A C 0.4696(4) 0.4366(9) 1.3392(7) 0.042(3) Uiso 0.328(6) 1 d PD A 1 H83C H 0.4879 0.4021 1.3802 0.050 Uiso 0.328(6) 1 calc PR A 1 H83D H 0.4431 0.4170 1.3230 0.050 Uiso 0.328(6) 1 calc PR A 1 C84A C 0.4774(5) 0.4022(13) 1.2933(7) 0.061(4) Uiso 0.328(6) 1 d PD A 1 H84C H 0.5043 0.4202 1.3110 0.073 Uiso 0.328(6) 1 calc PR A 1 H84D H 0.4602 0.4414 1.2537 0.073 Uiso 0.328(6) 1 calc PR A 1 C85A C 0.4711(5) 0.2817(13) 1.2790(11) 0.073(5) Uiso 0.328(6) 1 d PD A 1 H85C H 0.4796 0.2636 1.2534 0.087 Uiso 0.328(6) 1 calc PR A 1 H85D H 0.4879 0.2433 1.3190 0.087 Uiso 0.328(6) 1 calc PR A 1 C86A C 0.4291(5) 0.2422(15) 1.2445(8) 0.057(4) Uiso 0.328(6) 1 d PD A 1 H86D H 0.4283 0.1660 1.2390 0.086 Uiso 0.328(6) 1 calc PR A 1 H86E H 0.4124 0.2761 1.2035 0.086 Uiso 0.328(6) 1 calc PR A 1 H86F H 0.4202 0.2594 1.2693 0.086 Uiso 0.328(6) 1 calc PR A 1 C81B C 0.4575(5) 0.5989(13) 1.3520(9) 0.049(4) Uiso 0.272(6) 1 d PD A 2 H81A H 0.4720 0.6493 1.3864 0.073 Uiso 0.272(6) 1 calc PR A 2 H81B H 0.4365 0.5692 1.3513 0.073 Uiso 0.272(6) 1 calc PR A 2 H81C H 0.4467 0.6345 1.3123 0.073 Uiso 0.272(6) 1 calc PR A 2 C82B C 0.4843(6) 0.5108(16) 1.3615(9) 0.066(6) Uiso 0.272(6) 1 d PD A 2 H82A H 0.5059 0.5415 1.3638 0.079 Uiso 0.272(6) 1 calc PR A 2 H82B H 0.4952 0.4753 1.4017 0.079 Uiso 0.272(6) 1 calc PR A 2 C84B C 0.4818(7) 0.3315(19) 1.3072(11) 0.087(7) Uiso 0.272(6) 1 d PD A 2 H84A H 0.4914 0.2888 1.3447 0.104 Uiso 0.272(6) 1 calc PR A 2 H84B H 0.5040 0.3494 1.3076 0.104 Uiso 0.272(6) 1 calc PR A 2 C83B C 0.4639(5) 0.4312(13) 1.3094(10) 0.057(5) Uiso 0.272(6) 1 d PD A 2 H83A H 0.4544 0.4700 1.2706 0.068 Uiso 0.272(6) 1 calc PR A 2 H83B H 0.4409 0.4093 1.3057 0.068 Uiso 0.272(6) 1 calc PR A 2 C85B C 0.4531(7) 0.2682(19) 1.2493(11) 0.075(6) Uiso 0.272(6) 1 d PD A 2 H85A H 0.4668 0.2116 1.2450 0.090 Uiso 0.272(6) 1 calc PR A 2 H85B H 0.4409 0.3141 1.2121 0.090 Uiso 0.272(6) 1 calc PR A 2 C86B C 0.4211(7) 0.219(2) 1.2511(14) 0.082(8) Uiso 0.272(6) 1 d PD A 2 H86A H 0.4034 0.1780 1.2129 0.123 Uiso 0.272(6) 1 calc PR A 2 H86B H 0.4068 0.2747 1.2539 0.123 Uiso 0.272(6) 1 calc PR A 2 H86C H 0.4329 0.1728 1.2875 0.123 Uiso 0.272(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0334(2) 0.0530(3) 0.0427(2) -0.01670(19) 0.02755(19) -0.00568(18) B1 0.036(2) 0.043(3) 0.032(2) -0.0001(19) 0.019(2) 0.0016(19) Si1 0.0433(6) 0.0511(7) 0.0375(6) -0.0106(5) 0.0316(5) -0.0100(5) Si2 0.0317(5) 0.0408(6) 0.0276(5) -0.0003(4) 0.0202(4) -0.0004(4) Si3 0.0479(7) 0.0518(7) 0.0323(6) 0.0026(5) 0.0268(5) -0.0041(5) N1 0.0373(17) 0.0468(19) 0.0387(17) -0.0133(15) 0.0294(15) -0.0079(15) N2 0.0344(17) 0.0455(19) 0.0300(16) 0.0037(14) 0.0230(14) 0.0020(14) N3 0.0409(18) 0.0424(19) 0.0280(15) 0.0012(14) 0.0206(15) 0.0014(15) C1 0.040(2) 0.044(2) 0.0305(18) -0.0045(16) 0.0264(17) -0.0058(17) C2 0.058(3) 0.069(3) 0.045(2) -0.010(2) 0.039(2) -0.020(2) C3 0.048(3) 0.067(3) 0.045(2) -0.021(2) 0.036(2) -0.012(2) C4 0.044(2) 0.045(2) 0.040(2) -0.0015(18) 0.027(2) -0.0024(19) C5 0.0329(19) 0.050(2) 0.0304(18) 0.0002(17) 0.0199(17) -0.0006(17) C6 0.066(3) 0.060(3) 0.064(3) 0.024(3) 0.034(3) -0.001(3) C7 0.056(3) 0.105(4) 0.035(2) -0.005(3) 0.031(2) -0.011(3) C11 0.036(2) 0.041(2) 0.0321(19) -0.0072(16) 0.0225(17) -0.0046(16) C12 0.0338(19) 0.045(2) 0.035(2) -0.0048(17) 0.0237(17) -0.0004(17) C13 0.039(2) 0.049(2) 0.041(2) -0.0073(19) 0.0260(19) 0.0055(18) C14 0.042(2) 0.041(2) 0.038(2) -0.0082(18) 0.0196(19) 0.0016(18) C15 0.043(2) 0.045(2) 0.052(3) -0.007(2) 0.028(2) -0.0103(19) C16 0.040(2) 0.050(3) 0.047(2) -0.0093(19) 0.031(2) -0.0088(19) C17 0.053(3) 0.049(3) 0.059(3) -0.016(2) 0.024(3) -0.001(2) C21 0.0290(18) 0.049(2) 0.0273(18) 0.0060(16) 0.0183(16) 0.0073(16) C22 0.044(2) 0.052(3) 0.037(2) 0.0036(19) 0.0260(19) 0.007(2) C23 0.055(3) 0.081(4) 0.038(2) 0.002(2) 0.030(2) 0.023(3) C24 0.041(2) 0.091(4) 0.034(2) 0.017(2) 0.026(2) 0.018(2) C25 0.043(2) 0.074(3) 0.039(2) 0.012(2) 0.027(2) 0.000(2) C26 0.044(2) 0.054(3) 0.040(2) 0.0033(19) 0.029(2) 0.000(2) C27 0.074(4) 0.144(6) 0.051(3) 0.020(3) 0.049(3) 0.027(4) C31 0.045(2) 0.046(2) 0.0272(18) 0.0050(17) 0.0205(18) 0.0025(19) C32 0.043(2) 0.046(2) 0.039(2) 0.0035(18) 0.0256(19) 0.0007(19) C33 0.047(3) 0.056(3) 0.039(2) -0.004(2) 0.022(2) -0.007(2) C34 0.063(3) 0.057(3) 0.036(2) 0.006(2) 0.017(2) -0.004(3) C35 0.067(4) 0.050(3) 0.050(3) 0.012(2) 0.014(3) 0.010(3) C36 0.067(3) 0.044(3) 0.041(2) 0.003(2) 0.019(2) 0.007(2) C37 0.081(4) 0.078(4) 0.037(3) 0.009(3) 0.008(3) 0.000(3) C41 0.039(2) 0.068(3) 0.037(2) 0.005(2) 0.021(2) 0.008(2) C42 0.042(2) 0.052(3) 0.053(3) -0.019(2) 0.030(2) -0.004(2) C43 0.041(2) 0.065(3) 0.052(3) -0.014(2) 0.030(2) -0.012(2) C44 0.037(2) 0.075(3) 0.073(3) -0.014(3) 0.037(3) -0.007(2) C51 0.040(2) 0.077(3) 0.063(3) -0.012(3) 0.038(2) -0.001(2) C52 0.044(3) 0.071(3) 0.073(3) -0.024(3) 0.041(3) -0.001(2) C53 0.054(3) 0.081(4) 0.071(3) -0.037(3) 0.050(3) -0.012(3) C54 0.042(2) 0.096(4) 0.049(3) -0.013(3) 0.037(2) -0.003(2) C55 0.048(3) 0.110(5) 0.065(3) -0.022(3) 0.048(3) -0.013(3) C56 0.067(3) 0.106(5) 0.072(4) 0.004(3) 0.060(3) 0.004(3) C57 0.058(3) 0.087(4) 0.089(4) -0.009(3) 0.060(3) -0.013(3) C58 0.045(3) 0.090(4) 0.064(3) -0.012(3) 0.045(3) -0.008(3) C59 0.044(2) 0.082(4) 0.059(3) -0.024(3) 0.042(2) -0.013(2) C61 0.036(2) 0.051(3) 0.041(2) -0.0129(19) 0.0243(19) -0.0049(18) C62 0.046(2) 0.043(2) 0.038(2) -0.0143(18) 0.0278(19) -0.0044(19) C63 0.039(2) 0.043(2) 0.036(2) -0.0077(18) 0.0252(18) 0.0018(18) C64 0.035(2) 0.046(2) 0.035(2) -0.0111(17) 0.0225(18) -0.0027(17) C65 0.034(2) 0.051(3) 0.040(2) -0.0066(19) 0.0201(18) -0.0072(19) C66 0.046(3) 0.047(3) 0.056(3) -0.010(2) 0.026(2) -0.012(2) C67 0.049(3) 0.043(3) 0.057(3) -0.007(2) 0.021(2) -0.003(2) C68 0.037(2) 0.056(3) 0.053(3) -0.008(2) 0.024(2) 0.001(2) C69 0.035(2) 0.044(2) 0.045(2) -0.0133(19) 0.0225(19) -0.0038(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N1 2.127(4) . ? Zr1 C42 2.282(4) . ? Zr1 C62 2.509(4) . ? Zr1 C52 2.517(4) . ? Zr1 C53 2.538(4) . ? Zr1 C61 2.541(4) . ? Zr1 C63 2.565(4) . ? Zr1 C51 2.600(4) . ? Zr1 C69 2.641(5) . ? Zr1 C54 2.685(4) . ? Zr1 C59 2.689(4) . ? Zr1 C64 2.695(4) . ? B1 N2 1.443(5) . ? B1 N3 1.448(6) . ? B1 C41 1.574(6) . ? Si1 N1 1.755(4) . ? Si1 C3 1.866(4) . ? Si1 C2 1.877(5) . ? Si1 C1 1.890(4) . ? Si2 N2 1.762(3) . ? Si2 C5 1.868(4) . ? Si2 C4 1.873(4) . ? Si2 C1 1.871(4) . ? Si3 N3 1.765(4) . ? Si3 C7 1.860(5) . ? Si3 C6 1.864(5) . ? Si3 C1 1.885(4) . ? N1 C11 1.443(5) . ? N2 C21 1.434(5) . ? N3 C31 1.450(5) . ? C11 C16 1.399(5) . ? C11 C12 1.399(5) . ? C12 C13 1.385(6) . ? C13 C14 1.393(6) . ? C14 C15 1.385(6) . ? C14 C17 1.507(6) . ? C15 C16 1.386(6) . ? C21 C22 1.381(6) . ? C21 C26 1.394(6) . ? C22 C23 1.396(6) . ? C23 C24 1.391(8) . ? C24 C25 1.371(7) . ? C24 C27 1.517(6) . ? C25 C26 1.389(6) . ? C31 C32 1.380(6) . ? C31 C36 1.382(6) . ? C32 C33 1.401(6) . ? C33 C34 1.388(7) . ? C34 C35 1.378(8) . ? C34 C37 1.512(7) . ? C35 C36 1.394(7) . ? C43 C61 1.504(6) . ? C43 C44 1.537(7) . ? C44 C51 1.488(7) . ? C51 C52 1.404(7) . ? C51 C59 1.415(8) . ? C52 C53 1.420(8) . ? C53 C54 1.388(8) . ? C54 C55 1.422(8) . ? C54 C59 1.461(7) . ? C55 C56 1.362(8) . ? C56 C57 1.444(8) . ? C57 C58 1.357(8) . ? C58 C59 1.425(8) . ? C61 C69 1.423(6) . ? C61 C62 1.428(6) . ? C62 C63 1.414(6) . ? C63 C64 1.427(6) . ? C64 C65 1.410(6) . ? C64 C69 1.447(6) . ? C65 C66 1.367(7) . ? C66 C67 1.416(7) . ? C67 C68 1.363(7) . ? C68 C69 1.425(7) . ? C71A C72A 1.441(15) . ? C72A C73A 1.402(15) . ? C73A C74A 1.572(16) . ? C74A C75A 1.557(15) . ? C75A C76A 1.467(15) . ? C71B C72B 1.504(18) . ? C72B C73B 1.488(17) . ? C73B C74B 1.503(17) . ? C74B C75B 1.469(17) . ? C75B C76B 1.465(16) . ? C81A C82A 1.494(15) . ? C82A C83A 1.568(14) . ? C83A C84A 1.534(15) . ? C84A C85A 1.568(16) . ? C85A C86A 1.556(16) . ? C81B C82B 1.531(17) . ? C82B C83B 1.508(17) . ? C84B C83B 1.514(18) . ? C84B C85B 1.511(18) . ? C85B C86B 1.562(18) . ? 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 Zr1 C42 98.80(15) . . ? N1 Zr1 C62 96.00(13) . . ? C42 Zr1 C62 127.70(16) . . ? N1 Zr1 C52 136.11(16) . . ? C42 Zr1 C52 79.87(16) . . ? C62 Zr1 C52 119.67(16) . . ? N1 Zr1 C53 103.65(16) . . ? C42 Zr1 C53 78.90(17) . . ? C62 Zr1 C53 144.08(15) . . ? C52 Zr1 C53 32.63(18) . . ? N1 Zr1 C61 128.59(13) . . ? C42 Zr1 C61 116.34(16) . . ? C62 Zr1 C61 32.85(14) . . ? C52 Zr1 C61 88.46(15) . . ? C53 Zr1 C61 118.43(16) . . ? N1 Zr1 C63 85.62(12) . . ? C42 Zr1 C63 99.56(15) . . ? C62 Zr1 C63 32.33(13) . . ? C52 Zr1 C63 138.16(16) . . ? C53 Zr1 C63 170.73(17) . . ? C61 Zr1 C63 53.92(13) . . ? N1 Zr1 C51 136.24(16) . . ? C42 Zr1 C51 109.80(17) . . ? C62 Zr1 C51 91.99(15) . . ? C52 Zr1 C51 31.79(16) . . ? C53 Zr1 C51 53.27(16) . . ? C61 Zr1 C51 66.00(15) . . ? C63 Zr1 C51 119.83(15) . . ? N1 Zr1 C69 137.88(12) . . ? C42 Zr1 C69 84.72(16) . . ? C62 Zr1 C69 52.81(14) . . ? C52 Zr1 C69 85.95(16) . . ? C53 Zr1 C69 118.10(17) . . ? C61 Zr1 C69 31.81(14) . . ? C63 Zr1 C69 52.64(13) . . ? C51 Zr1 C69 78.68(15) . . ? N1 Zr1 C54 88.53(14) . . ? C42 Zr1 C54 107.55(17) . . ? C62 Zr1 C54 122.76(16) . . ? C52 Zr1 C54 51.74(19) . . ? C53 Zr1 C54 30.66(18) . . ? C61 Zr1 C54 112.67(14) . . ? C63 Zr1 C54 152.83(16) . . ? C51 Zr1 C54 52.04(16) . . ? C69 Zr1 C54 130.65(14) . . ? N1 Zr1 C59 105.40(16) . . ? C42 Zr1 C59 128.85(15) . . ? C62 Zr1 C59 93.98(14) . . ? C52 Zr1 C59 51.61(18) . . ? C53 Zr1 C59 52.06(16) . . ? C61 Zr1 C59 81.40(14) . . ? C63 Zr1 C59 126.28(14) . . ? C51 Zr1 C59 30.97(17) . . ? C69 Zr1 C59 104.42(15) . . ? C54 Zr1 C59 31.56(14) . . ? N1 Zr1 C64 108.70(12) . . ? C42 Zr1 C64 75.41(15) . . ? C62 Zr1 C64 52.34(13) . . ? C52 Zr1 C64 113.17(17) . . ? C53 Zr1 C64 141.12(17) . . ? C61 Zr1 C64 52.72(13) . . ? C63 Zr1 C64 31.35(13) . . ? C51 Zr1 C64 110.10(15) . . ? C69 Zr1 C64 31.44(12) . . ? C54 Zr1 C64 162.08(14) . . ? C59 Zr1 C64 133.57(14) . . ? N2 B1 N3 118.1(4) . . ? N2 B1 C41 120.9(4) . . ? N3 B1 C41 121.0(4) . . ? N1 Si1 C3 109.3(2) . . ? N1 Si1 C2 107.35(19) . . ? C3 Si1 C2 109.5(2) . . ? N1 Si1 C1 113.20(16) . . ? C3 Si1 C1 110.39(19) . . ? C2 Si1 C1 107.0(2) . . ? N2 Si2 C5 106.24(16) . . ? N2 Si2 C4 109.50(18) . . ? C5 Si2 C4 109.37(19) . . ? N2 Si2 C1 106.21(17) . . ? C5 Si2 C1 113.63(18) . . ? C4 Si2 C1 111.65(18) . . ? N3 Si3 C7 106.4(2) . . ? N3 Si3 C6 108.8(2) . . ? C7 Si3 C6 107.4(3) . . ? N3 Si3 C1 109.27(16) . . ? C7 Si3 C1 114.9(2) . . ? C6 Si3 C1 109.9(2) . . ? C11 N1 Si1 111.7(3) . . ? C11 N1 Zr1 112.0(2) . . ? Si1 N1 Zr1 135.19(18) . . ? C21 N2 B1 118.2(3) . . ? C21 N2 Si2 119.0(2) . . ? B1 N2 Si2 122.4(3) . . ? B1 N3 C31 116.6(3) . . ? B1 N3 Si3 128.1(3) . . ? C31 N3 Si3 113.9(3) . . ? Si2 C1 Si3 108.3(2) . . ? Si2 C1 Si1 120.3(2) . . ? Si3 C1 Si1 115.27(19) . . ? C16 C11 C12 117.2(4) . . ? C16 C11 N1 119.6(3) . . ? C12 C11 N1 123.2(3) . . ? C13 C12 C11 120.9(4) . . ? C12 C13 C14 121.7(4) . . ? C15 C14 C13 117.3(4) . . ? C15 C14 C17 121.8(4) . . ? C13 C14 C17 120.8(4) . . ? C16 C15 C14 121.5(4) . . ? C15 C16 C11 121.3(4) . . ? C22 C21 C26 118.6(4) . . ? C22 C21 N2 120.0(4) . . ? C26 C21 N2 121.4(4) . . ? C21 C22 C23 120.3(5) . . ? C24 C23 C22 121.2(5) . . ? C25 C24 C23 117.7(4) . . ? C25 C24 C27 121.2(5) . . ? C23 C24 C27 121.0(5) . . ? C24 C25 C26 122.0(5) . . ? C25 C26 C21 120.1(4) . . ? C32 C31 C36 118.9(4) . . ? C32 C31 N3 119.5(4) . . ? C36 C31 N3 121.5(4) . . ? C31 C32 C33 120.4(4) . . ? C34 C33 C32 120.9(4) . . ? C35 C34 C33 118.0(4) . . ? C35 C34 C37 121.3(5) . . ? C33 C34 C37 120.7(5) . . ? C34 C35 C36 121.4(5) . . ? C31 C36 C35 120.3(5) . . ? C61 C43 C44 111.0(4) . . ? C51 C44 C43 110.8(4) . . ? C52 C51 C59 107.4(5) . . ? C52 C51 C44 128.1(5) . . ? C59 C51 C44 124.4(5) . . ? C52 C51 Zr1 70.8(2) . . ? C59 C51 Zr1 78.0(3) . . ? C44 C51 Zr1 118.6(3) . . ? C51 C52 C53 109.4(5) . . ? C51 C52 Zr1 77.4(3) . . ? C53 C52 Zr1 74.5(3) . . ? C54 C53 C52 108.2(5) . . ? C54 C53 Zr1 80.5(3) . . ? C52 C53 Zr1 72.9(3) . . ? C53 C54 C55 134.7(5) . . ? C53 C54 C59 107.5(5) . . ? C55 C54 C59 117.7(5) . . ? C53 C54 Zr1 68.8(3) . . ? C55 C54 Zr1 125.8(3) . . ? C59 C54 Zr1 74.4(2) . . ? C56 C55 C54 121.5(5) . . ? C55 C56 C57 120.0(6) . . ? C58 C57 C56 121.1(6) . . ? C57 C58 C59 120.0(5) . . ? C51 C59 C58 132.4(5) . . ? C51 C59 C54 107.5(5) . . ? C58 C59 C54 119.6(5) . . ? C51 C59 Zr1 71.1(3) . . ? C58 C59 Zr1 126.8(3) . . ? C54 C59 Zr1 74.1(2) . . ? C69 C61 C62 107.1(4) . . ? C69 C61 C43 126.5(4) . . ? C62 C61 C43 126.4(4) . . ? C69 C61 Zr1 78.0(2) . . ? C62 C61 Zr1 72.4(2) . . ? C43 C61 Zr1 118.2(3) . . ? C63 C62 C61 109.1(4) . . ? C63 C62 Zr1 76.0(2) . . ? C61 C62 Zr1 74.8(2) . . ? C62 C63 C64 108.2(4) . . ? C62 C63 Zr1 71.7(2) . . ? C64 C63 Zr1 79.4(2) . . ? C65 C64 C63 132.7(4) . . ? C65 C64 C69 120.2(4) . . ? C63 C64 C69 107.0(4) . . ? C65 C64 Zr1 126.4(3) . . ? C63 C64 Zr1 69.3(2) . . ? C69 C64 Zr1 72.2(2) . . ? C66 C65 C64 119.5(4) . . ? C65 C66 C67 120.6(4) . . ? C68 C67 C66 121.8(5) . . ? C67 C68 C69 119.5(4) . . ? C61 C69 C68 133.1(4) . . ? C61 C69 C64 108.5(4) . . ? C68 C69 C64 118.3(4) . . ? C61 C69 Zr1 70.2(3) . . ? C68 C69 Zr1 122.9(3) . . ? C64 C69 Zr1 76.4(2) . . ? C73A C72A C71A 116.7(13) . . ? C72A C73A C74A 115.3(13) . . ? C75A C74A C73A 111.4(13) . . ? C76A C75A C74A 108.1(12) . . ? C73B C72B C71B 98.8(17) . . ? C72B C73B C74B 107.8(15) . . ? C75B C74B C73B 119.0(17) . . ? C76B C75B C74B 110.0(17) . . ? C81A C82A C83A 108.5(11) . . ? C84A C83A C82A 107.6(11) . . ? C83A C84A C85A 112.7(14) . . ? C86A C85A C84A 115.6(15) . . ? C83B C82B C81B 112.2(16) . . ? C83B C84B C85B 111.3(19) . . ? C82B C83B C84B 125.1(17) . . ? C84B C85B C86B 113(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.973 _refine_diff_density_min -1.633 _refine_diff_density_rms 0.101 #===END