# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1779 data_ylw3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H42 N4 O2 Si2 W' _chemical_formula_weight 658.65 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.299(3) _cell_length_b 16.059(3) _cell_length_c 22.341(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5847.7(20) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used IP _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour RED _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method ? _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 4.058 _exptl_absorpt_correction_type ABSCOR _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 1.187 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ROTATION ANODE' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'RIGAKU RAX-IIC' _diffrn_measurement_method 'IP' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15760 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.54 _reflns_number_total 4963 _reflns_number_observed 4543 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'BIOTEX' _computing_cell_refinement 'BIOTEX' _computing_data_reduction 'BIOTEX' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00291(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4963 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_obs 0.0609 _refine_ls_wR_factor_all 0.1812 _refine_ls_wR_factor_obs 0.1751 _refine_ls_goodness_of_fit_all 1.106 _refine_ls_goodness_of_fit_obs 1.125 _refine_ls_restrained_S_all 1.106 _refine_ls_restrained_S_obs 1.125 _refine_ls_shift/esd_max -0.020 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.124907(6) 0.990879(8) 0.127117(4) 0.05478(5) Uani 1 d . . Si1 Si 0.22437(4) 0.97625(4) -0.01080(3) 0.0623(2) Uani 1 d . . Si2 Si 0.01465(5) 1.00659(4) 0.26131(4) 0.0619(2) Uani 1 d . . O1 O 0.18388(11) 1.05632(11) 0.16858(8) 0.0744(6) Uani 1 d . . O2 O 0.06982(11) 1.05447(11) 0.08168(7) 0.0725(6) Uani 1 d . . N1 N 0.20329(11) 0.94241(12) 0.06249(8) 0.0580(6) Uani 1 d . . N2 N 0.20939(12) 0.87988(11) 0.15095(9) 0.0608(6) Uani 1 d . . N3 N 0.04193(11) 0.95736(12) 0.19369(8) 0.0579(6) Uani 1 d . . N4 N 0.03767(12) 0.87808(13) 0.11212(9) 0.0610(6) Uani 1 d . . C1 C 0.24162(15) 0.88160(14) 0.09561(10) 0.0588(7) Uani 1 d . . C2 C 0.3026(2) 0.8241(2) 0.07913(12) 0.0741(9) Uani 1 d . . H2A H 0.3653(17) 0.8409(20) 0.0362(14) 0.134(13) Uiso 1 d . . C3 C 0.3278(2) 0.7677(2) 0.12215(11) 0.0834(10) Uani 1 d . . H3A H 0.3680(2) 0.7288(2) 0.11253(11) 0.100 Uiso 1 calc R . C4 C 0.2953(2) 0.7678(2) 0.17815(12) 0.0800(9) Uani 1 d . . H4A H 0.3132(2) 0.7294(2) 0.20646(12) 0.096 Uiso 1 calc R . C5 C 0.2359(2) 0.8250(2) 0.19270(11) 0.0687(8) Uani 1 d . . C6 C 0.2006(2) 0.8325(2) 0.25375(12) 0.0875(9) Uani 1 d . . H6B H 0.1486(2) 0.8048(2) 0.25059(12) 0.105 Uiso 1 d R . H6C H 0.1880(2) 0.8905(2) 0.25801(12) 0.105 Uiso 1 d R . H6A H 0.2198(2) 0.8171(2) 0.29110(12) 0.172(14) Uiso 1 d R . C7 C 0.2534(2) 0.8854(2) -0.05841(11) 0.0995(11) Uani 1 d . . H7B H 0.2046(2) 0.8655(2) -0.07782(11) 0.119 Uiso 1 d R . H7C H 0.2715(2) 0.8420(2) -0.03202(11) 0.119 Uiso 1 d R . H7A H 0.2797(2) 0.8897(2) -0.07773(11) 0.060(7) Uiso 1 d R . C8 C 0.1294(2) 1.0203(2) -0.0429(2) 0.0853(12) Uani 1 d . . H8B H 0.0840(2) 0.9830(2) -0.0377(2) 0.102 Uiso 1 d R . H8C H 0.1366(2) 1.0302(2) -0.0849(2) 0.102 Uiso 1 d R . H8A H 0.1171(2) 1.0812(2) -0.0188(2) 0.150(14) Uiso 1 d R . C9 C 0.3069(2) 1.0578(2) -0.00845(13) 0.0817(10) Uani 1 d . . C10 C 0.2836(2) 1.1278(2) 0.0325(2) 0.1183(14) Uani 1 d . . H10A H 0.2427(2) 1.1613(2) 0.0131(2) 0.142 Uiso 1 d R . H10C H 0.3450(2) 1.1678(2) 0.0417(2) 0.085(8) Uiso 1 d R . H10B H 0.2685(2) 1.1196(2) 0.0822(2) 0.172(15) Uiso 1 d R . C11 C 0.3245(3) 1.0928(2) -0.0709(2) 0.128(2) Uani 1 d . . H11A H 0.3410(3) 1.0484(2) -0.0971(2) 0.193 Uiso 1 calc R . H11B H 0.3677(3) 1.1333(2) -0.0684(2) 0.193 Uiso 1 calc R . H11C H 0.2759(3) 1.1187(2) -0.0865(2) 0.193 Uiso 1 calc R . C12 C 0.3870(3) 1.0216(3) 0.0170(3) 0.154(2) Uani 1 d . . H12B H 0.4196(3) 1.0686(3) 0.0290(3) 0.184 Uiso 1 d R . H12C H 0.4157(3) 0.9952(3) -0.0154(3) 0.184 Uiso 1 d R . H12A H 0.3871(3) 0.9830(3) 0.0501(3) 0.169(19) Uiso 1 d R . C13 C 0.00204(14) 0.8924(2) 0.16496(10) 0.0592(7) Uani 1 d . . C14 C -0.0637(2) 0.8448(2) 0.18485(12) 0.0734(9) Uani 1 d . . H14A H -0.0885(12) 0.8456(11) 0.2186(7) 0.039(5) Uiso 1 d . . C15 C -0.0930(2) 0.7833(2) 0.14789(14) 0.0881(10) Uani 1 d . . H15A H -0.1376(2) 0.7512(2) 0.15977(14) 0.106 Uiso 1 calc R . C16 C -0.0562(2) 0.7689(2) 0.09299(12) 0.0802(10) Uani 1 d . . H16A H -0.0779(14) 0.7272(12) 0.0600(8) 0.063(6) Uiso 1 d . . C17 C 0.0089(2) 0.8185(2) 0.07482(11) 0.0654(8) Uani 1 d . . C18 C 0.0478(2) 0.8105(2) 0.01461(12) 0.0832(10) Uani 1 d . . H18B H 0.0972(2) 0.7789(2) 0.02052(12) 0.100 Uiso 1 d R . H18C H 0.0642(2) 0.8653(2) 0.00220(12) 0.100 Uiso 1 d R . H18A H 0.0259(2) 0.7919(2) -0.00976(12) 0.154(15) Uiso 1 d R . C19 C 0.1055(2) 1.0614(2) 0.29133(12) 0.0795(10) Uani 1 d . . H19B H 0.1186(2) 1.1082(2) 0.26629(12) 0.095 Uiso 1 d R . H19C H 0.1513(2) 1.0238(2) 0.29036(12) 0.095 Uiso 1 d R . H19A H 0.0980(2) 1.0796(2) 0.32977(12) 0.077(8) Uiso 1 d R . C20 C -0.0177(2) 0.9281(2) 0.31774(12) 0.0873(10) Uani 1 d . . H20B H -0.0013(2) 0.9476(2) 0.35659(12) 0.105 Uiso 1 d R . H20C H 0.0112(2) 0.8771(2) 0.31019(12) 0.105 Uiso 1 d R . H20A H -0.0731(2) 0.9169(2) 0.31857(12) 0.101(9) Uiso 1 d R . C21 C -0.0686(2) 1.0856(2) 0.24790(12) 0.0780(9) Uani 1 d . . C22 C -0.0904(2) 1.1269(2) 0.30685(14) 0.1009(12) Uani 1 d . . H22B H -0.1476(2) 1.1378(2) 0.30034(14) 0.121 Uiso 1 d R . H22C H -0.0642(2) 1.1799(2) 0.30137(14) 0.121 Uiso 1 d R . H22A H -0.0887(2) 1.1214(2) 0.34988(14) 0.282(27) Uiso 1 d R . C23 C -0.1485(2) 1.0397(3) 0.2256(2) 0.1163(14) Uani 1 d . . H23B H -0.1370(2) 1.0109(3) 0.1889(2) 0.174 Uiso 1 calc R . H23C H -0.1911(2) 1.0799(3) 0.2190(2) 0.174 Uiso 1 calc R . H23D H -0.1660(2) 1.0005(3) 0.2554(2) 0.174 Uiso 1 calc R . C24 C -0.0400(2) 1.1498(2) 0.20216(14) 0.1153(13) Uani 1 d . . H24B H 0.0090(2) 1.1751(2) 0.21775(14) 0.138 Uiso 1 d R . H24C H -0.0813(2) 1.1924(2) 0.20099(14) 0.138 Uiso 1 d R . H24A H -0.0286(2) 1.1334(2) 0.16096(14) 0.087(8) Uiso 1 d 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 W1 0.04518(9) 0.05556(9) 0.06361(8) 0.00252(3) 0.00149(4) 0.00111(4) Si1 0.0493(4) 0.0724(4) 0.0653(4) -0.0024(3) 0.0044(3) 0.0100(3) Si2 0.0460(4) 0.0723(4) 0.0675(4) 0.0024(3) 0.0021(3) -0.0053(3) O1 0.0607(11) 0.0738(11) 0.0887(11) -0.0072(9) 0.0117(9) -0.0129(9) O2 0.0579(10) 0.0811(11) 0.0783(10) 0.0062(9) 0.0126(9) 0.0165(9) N1 0.0466(10) 0.0609(11) 0.0665(11) 0.0017(8) -0.0071(8) 0.0177(9) N2 0.0516(11) 0.0560(10) 0.0748(11) 0.0034(9) -0.0134(9) 0.0035(9) N3 0.0400(10) 0.0637(11) 0.0699(11) 0.0012(9) 0.0003(9) -0.0088(9) N4 0.0511(12) 0.0610(12) 0.0710(11) -0.0021(9) -0.0049(9) -0.0030(10) C1 0.0477(13) 0.0557(13) 0.0729(13) -0.0041(10) -0.0011(11) 0.0003(10) C2 0.0542(15) 0.0661(14) 0.102(2) -0.0098(13) -0.0128(13) 0.0162(12) C3 0.076(2) 0.078(2) 0.097(2) -0.0137(12) -0.0239(14) 0.021(2) C4 0.065(2) 0.074(2) 0.101(2) 0.0087(13) -0.0258(14) 0.0014(13) C5 0.060(2) 0.0613(14) 0.0843(15) 0.0093(11) -0.0196(12) -0.0073(12) C6 0.091(2) 0.085(2) 0.087(2) 0.0312(14) -0.010(2) -0.0061(15) C7 0.106(2) 0.123(2) 0.069(2) -0.0102(15) 0.013(2) 0.033(2) C8 0.062(2) 0.116(2) 0.078(2) 0.011(2) 0.0031(14) 0.0167(15) C9 0.068(2) 0.092(2) 0.085(2) 0.0022(14) 0.0091(14) -0.006(2) C10 0.131(3) 0.104(2) 0.120(2) -0.018(2) 0.041(2) -0.030(2) C11 0.143(3) 0.135(3) 0.108(2) 0.004(2) 0.047(2) -0.026(3) C12 0.080(3) 0.161(4) 0.219(6) 0.025(4) -0.025(3) -0.032(3) C13 0.0458(13) 0.0641(13) 0.0678(13) 0.0070(11) -0.0059(10) 0.0004(10) C14 0.059(2) 0.078(2) 0.084(2) 0.0056(13) -0.0034(13) -0.0180(13) C15 0.065(2) 0.083(2) 0.116(2) 0.018(2) -0.008(2) -0.0280(15) C16 0.071(2) 0.072(2) 0.098(2) -0.0054(14) -0.0171(14) -0.0024(14) C17 0.0590(15) 0.0522(13) 0.0851(15) 0.0033(11) -0.0179(12) 0.0032(11) C18 0.081(2) 0.068(2) 0.101(2) -0.0198(13) -0.008(2) 0.0013(15) C19 0.068(2) 0.095(2) 0.075(2) -0.0134(15) -0.0028(13) -0.015(2) C20 0.074(2) 0.110(2) 0.078(2) 0.0194(15) 0.0088(14) -0.018(2) C21 0.066(2) 0.096(2) 0.0717(15) -0.0062(14) 0.0003(14) 0.0047(14) C22 0.088(2) 0.114(2) 0.100(2) -0.024(2) 0.020(2) 0.017(2) C23 0.073(2) 0.153(3) 0.124(3) -0.032(2) -0.029(2) 0.024(2) C24 0.126(3) 0.120(2) 0.100(2) 0.028(2) 0.031(2) 0.057(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O2 1.697(2) . ? W1 O1 1.699(2) . ? W1 N3 2.081(2) . ? W1 N1 2.079(2) . ? W1 N2 2.315(2) . ? W1 N4 2.327(2) . ? Si1 N1 1.759(2) . ? Si1 C8 1.847(3) . ? Si1 C9 1.878(3) . ? Si1 C7 1.866(3) . ? Si2 N3 1.762(2) . ? Si2 C21 1.881(3) . ? Si2 C19 1.849(3) . ? Si2 C20 1.858(3) . ? N1 C1 1.375(3) . ? N2 C1 1.344(3) . ? N2 C5 1.354(3) . ? N3 C13 1.387(3) . ? N4 C17 1.353(3) . ? N4 C13 1.336(3) . ? C1 C2 1.406(3) . ? C2 C3 1.382(4) . ? C3 C4 1.359(4) . ? C4 C5 1.374(4) . ? C5 C6 1.485(4) . ? C9 C10 1.499(4) . ? C9 C12 1.538(5) . ? C9 C11 1.532(5) . ? C13 C14 1.389(4) . ? C14 C15 1.373(4) . ? C15 C16 1.384(4) . ? C16 C17 1.387(4) . ? C17 C18 1.493(4) . ? C21 C23 1.577(5) . ? C21 C22 1.516(4) . ? C21 C24 1.525(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 W1 O1 104.67(9) . . ? O2 W1 N3 103.85(8) . . ? O1 W1 N3 97.93(8) . . ? O2 W1 N1 97.76(8) . . ? O1 W1 N1 105.22(8) . . ? N3 W1 N1 143.01(8) . . ? O2 W1 N2 156.33(8) . . ? O1 W1 N2 90.82(8) . . ? N3 W1 N2 91.32(7) . . ? N1 W1 N2 60.38(7) . . ? O2 W1 N4 93.38(8) . . ? O1 W1 N4 154.92(8) . . ? N3 W1 N4 60.30(7) . . ? N1 W1 N4 89.08(7) . . ? N2 W1 N4 78.30(7) . . ? N1 Si1 C8 108.43(13) . . ? N1 Si1 C9 109.22(12) . . ? C8 Si1 C9 110.11(14) . . ? N1 Si1 C7 109.78(11) . . ? C8 Si1 C7 106.90(15) . . ? C9 Si1 C7 112.30(14) . . ? N3 Si2 C21 110.37(11) . . ? N3 Si2 C19 108.81(11) . . ? C21 Si2 C19 108.32(13) . . ? N3 Si2 C20 110.41(12) . . ? C21 Si2 C20 111.15(13) . . ? C19 Si2 C20 107.68(13) . . ? C1 N1 Si1 129.1(2) . . ? C1 N1 W1 99.88(14) . . ? Si1 N1 W1 130.60(10) . . ? C1 N2 C5 121.5(2) . . ? C1 N2 W1 90.29(14) . . ? C5 N2 W1 148.1(2) . . ? C13 N3 Si2 128.0(2) . . ? C13 N3 W1 99.70(14) . . ? Si2 N3 W1 131.35(11) . . ? C17 N4 C13 121.0(2) . . ? C17 N4 W1 148.3(2) . . ? C13 N4 W1 90.26(14) . . ? N2 C1 N1 109.4(2) . . ? N2 C1 C2 120.3(2) . . ? N1 C1 C2 130.3(2) . . ? C3 C2 C1 117.2(2) . . ? C4 C3 C2 121.6(3) . . ? C3 C4 C5 119.6(3) . . ? N2 C5 C4 119.8(2) . . ? N2 C5 C6 117.2(2) . . ? C4 C5 C6 123.0(2) . . ? C10 C9 C12 105.8(3) . . ? C10 C9 C11 109.2(3) . . ? C12 C9 C11 108.5(3) . . ? C10 C9 Si1 111.0(2) . . ? C12 C9 Si1 110.8(2) . . ? C11 C9 Si1 111.4(2) . . ? N4 C13 N3 109.6(2) . . ? N4 C13 C14 121.6(2) . . ? N3 C13 C14 128.9(2) . . ? C15 C14 C13 118.1(2) . . ? C16 C15 C14 120.1(3) . . ? C17 C16 C15 119.7(3) . . ? N4 C17 C16 119.4(2) . . ? N4 C17 C18 117.9(2) . . ? C16 C17 C18 122.7(2) . . ? C23 C21 C22 106.6(3) . . ? C23 C21 C24 110.9(3) . . ? C22 C21 C24 111.0(2) . . ? C23 C21 Si2 109.3(2) . . ? C22 C21 Si2 109.0(2) . . ? C24 C21 Si2 110.0(2) . . ? _refine_diff_density_max 0.916 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.092 data_yl2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 Mo N4 O2 Si2' _chemical_formula_weight 570.74 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' 'O' 'O' 0.0106 0.0060 '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' 'Mo' 'Mo' -1.6832 0.6857 '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+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.342(3) _cell_length_b 16.007(3) _cell_length_c 22.218(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5812(2) _cell_formula_units_Z 8 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 0.560 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8239 _exptl_absorpt_correction_T_max 0.8774 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 3746 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1064 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.66 _reflns_number_total 3746 _reflns_number_gt 3050 _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^)+(0.1201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3746 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.2051 _refine_ls_wR_factor_gt 0.1887 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.014 _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 Mo1 Mo 0.124334(15) 0.99000(2) 0.127080(14) 0.06365(10) Uani 1 1 d . . . Si1 Si 0.22349(5) 0.97477(7) -0.01118(5) 0.0719(3) Uani 1 1 d . . . Si2 Si 0.01463(6) 1.00478(7) 0.26169(5) 0.0707(3) Uani 1 1 d . . . O1 O 0.18257(13) 1.05470(16) 0.16917(11) 0.0802(8) Uani 1 1 d . . . O2 O 0.06994(13) 1.05373(16) 0.08123(10) 0.0797(8) Uani 1 1 d . . . N1 N 0.20307(14) 0.94260(17) 0.06217(11) 0.0658(8) Uani 1 1 d . . . N2 N 0.20945(13) 0.87934(17) 0.15165(12) 0.0669(8) Uani 1 1 d . . . N3 N 0.04174(14) 0.95646(19) 0.19371(11) 0.0647(8) Uani 1 1 d . . . N4 N 0.03675(14) 0.87710(18) 0.11147(12) 0.0684(8) Uani 1 1 d . . . C1 C 0.24068(17) 0.8813(2) 0.09575(15) 0.0682(10) Uani 1 1 d . . . C2 C 0.30334(19) 0.8250(3) 0.07929(17) 0.0828(12) Uani 1 1 d . . . H2 H 0.333(2) 0.839(3) 0.0343(18) 0.144(15) Uiso 1 1 d . . . C3 C 0.3297(2) 0.7703(3) 0.12174(18) 0.0943(14) Uani 1 1 d . . . H3 H 0.3592(18) 0.728(3) 0.1164(13) 0.089(11) Uiso 1 1 d . . . C4 C 0.2965(2) 0.7684(3) 0.17788(18) 0.0909(13) Uani 1 1 d . . . H4 H 0.3148(14) 0.7367(19) 0.2064(10) 0.055(7) Uiso 1 1 d . . . C5 C 0.23711(18) 0.8251(2) 0.19261(16) 0.0779(11) Uani 1 1 d . . . C6 C 0.2001(2) 0.8318(3) 0.25456(18) 0.1005(14) Uani 1 1 d . . . H6A H 0.2142 0.8021 0.2806 0.158(18) Uiso 1 1 d R . . H6B H 0.1421 0.8249 0.2499 0.190 Uiso 1 1 d R . . H6C H 0.2090 0.8882 0.2679 0.190 Uiso 1 1 d R . . C7 C 0.2543(3) 0.8863(3) -0.05935(17) 0.1041(15) Uani 1 1 d . . . H7A H 0.2612 0.8966 -0.1003 0.085(10) Uiso 1 1 d R . . H7B H 0.2073 0.8503 -0.0581 0.102 Uiso 1 1 d R . . H7C H 0.3095 0.8412 -0.0432 0.19(2) Uiso 1 1 d R . . C8 C 0.1300(2) 1.0231(3) -0.04325(19) 0.1007(15) Uani 1 1 d . . . H8B H 0.1086 0.9887 -0.0750 0.121 Uiso 1 1 d R . . H8C H 0.1451 1.0759 -0.0605 0.121 Uiso 1 1 d R . . H8A H 0.0984 1.0298 -0.0210 0.17(2) Uiso 1 1 d R . . C9 C 0.3066(2) 1.0551(3) -0.00926(18) 0.0948(14) Uani 1 1 d . . . C10 C 0.2818(3) 1.1271(3) 0.0336(2) 0.140(2) Uani 1 1 d . . . H10A H 0.2435 1.1631 0.0108 0.18(2) Uiso 1 1 d R . . H10B H 0.2713 1.1031 0.0735 0.19(2) Uiso 1 1 d R . . H10C H 0.3305 1.1599 0.0382 0.222 Uiso 1 1 d R . . C11 C 0.3180(3) 1.0921(4) -0.0733(2) 0.139(2) Uani 1 1 d . . . H11A H 0.2667 1.1060 -0.1133 0.18(2) Uiso 1 1 d R . . H11B H 0.3585 1.0571 -0.0918 0.212 Uiso 1 1 d R . . H11C H 0.3444 1.1448 -0.0662 0.212 Uiso 1 1 d R . . C12 C 0.3856(2) 1.0190(3) 0.0139(3) 0.162(3) Uani 1 1 d . . . H12A H 0.3867 0.9889 0.0381 0.093(13) Uiso 1 1 d R . . H12B H 0.4173 1.0664 0.0264 0.112 Uiso 1 1 d R . . H12C H 0.4138 0.9946 -0.0197 0.112 Uiso 1 1 d R . . C13 C 0.00301(17) 0.8909(2) 0.16537(16) 0.0685(10) Uani 1 1 d . . . C14 C -0.0637(2) 0.8441(3) 0.18537(16) 0.0808(12) Uani 1 1 d . . . H14 H -0.0915(12) 0.8511(14) 0.2216(9) 0.032(6) Uiso 1 1 d . . . C15 C -0.0938(2) 0.7836(3) 0.14618(19) 0.0889(13) Uani 1 1 d . . . H15 H -0.121(2) 0.750(4) 0.168(2) 0.17(2) Uiso 1 1 d . . . C16 C -0.0572(2) 0.7677(3) 0.09147(18) 0.0891(13) Uani 1 1 d . . . H16 H -0.079(2) 0.735(3) 0.0545(14) 0.116(13) Uiso 1 1 d . . . C17 C 0.00718(18) 0.8174(2) 0.07457(16) 0.0741(11) Uani 1 1 d . . . C18 C 0.0468(2) 0.8072(3) 0.01555(17) 0.0977(14) Uani 1 1 d . . . H18A H 0.0324 0.7822 -0.0005 0.095(12) Uiso 1 1 d R . . H18B H 0.1029 0.7926 0.0229 0.114 Uiso 1 1 d R . . H18C H 0.0462 0.8604 -0.0044 0.114 Uiso 1 1 d R . . C19 C 0.1053(2) 1.0602(3) 0.29056(17) 0.0841(13) Uani 1 1 d . . . H19A H 0.165(2) 1.025(3) 0.2834(17) 0.118(14) Uiso 1 1 d . . . H19B H 0.1212(15) 1.098(2) 0.2663(12) 0.071(10) Uiso 1 1 d . . . H19C H 0.0883(19) 1.080(2) 0.3310(14) 0.092(11) Uiso 1 1 d . . . C20 C -0.0171(2) 0.9279(3) 0.31803(16) 0.1056(16) Uani 1 1 d . . . H20A H 0.0010 0.9568 0.3652 0.118(14) Uiso 1 1 d R . . H20B H 0.0087 0.9020 0.3294 0.047(8) Uiso 1 1 d R . . H20C H -0.0724 0.9084 0.3141 0.057 Uiso 1 1 d R . . C21 C -0.0702(2) 1.0831(3) 0.24863(17) 0.0856(13) Uani 1 1 d . . . C22 C -0.0893(2) 1.1282(3) 0.30631(18) 0.1119(17) Uani 1 1 d . . . H22A H -0.0985 1.1089 0.3215 0.139(17) Uiso 1 1 d R . . H22B H -0.1414 1.1710 0.2995 0.077(9) Uiso 1 1 d R . . H22C H -0.0417 1.1582 0.3197 0.092 Uiso 1 1 d R . . C23 C -0.14837(19) 1.0385(2) 0.22682(15) 0.1246(19) Uani 1 1 d . . . H23A H -0.1565 1.0036 0.2881 0.102(13) Uiso 1 1 d R . . H23B H -0.1406 0.9972 0.1960 0.122 Uiso 1 1 d R . . H23C H -0.1906 1.0774 0.2161 0.122 Uiso 1 1 d R . . C24 C -0.04205(19) 1.1473(2) 0.20212(15) 0.1171(16) Uani 1 1 d R . . H24A H -0.0636 1.1897 0.1964 0.171(19) Uiso 1 1 d R . . H24B H -0.0301 1.1257 0.1465 0.156(17) Uiso 1 1 d R . . H24C H 0.0186 1.1864 0.2501 0.20(2) Uiso 1 1 d 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 Mo1 0.05044(15) 0.0526(2) 0.0879(2) 0.00213(13) 0.00213(13) 0.00142(10) Si1 0.0589(5) 0.0716(6) 0.0851(6) -0.0005(5) 0.0047(5) 0.0122(4) Si2 0.0578(5) 0.0677(7) 0.0867(6) 0.0036(5) 0.0013(5) -0.0055(4) O1 0.0700(13) 0.0674(17) 0.1031(15) -0.0044(13) 0.0082(13) -0.0134(11) O2 0.0685(12) 0.0728(17) 0.0977(15) 0.0152(12) 0.0039(13) 0.0169(11) N1 0.0543(13) 0.0638(19) 0.0793(16) 0.0017(13) -0.0057(13) 0.0096(12) N2 0.0505(12) 0.0546(17) 0.0955(17) 0.0125(13) -0.0087(13) 0.0025(12) N3 0.0484(12) 0.0659(18) 0.0796(16) 0.0026(13) 0.0026(12) -0.0041(12) N4 0.0501(12) 0.0591(18) 0.0959(17) -0.0089(14) -0.0115(13) -0.0010(12) C1 0.0476(14) 0.057(2) 0.100(2) 0.0061(16) -0.0022(16) 0.0023(14) C2 0.0637(18) 0.079(3) 0.105(2) -0.008(2) -0.0031(18) 0.0194(18) C3 0.080(2) 0.074(3) 0.128(3) -0.006(2) -0.030(2) 0.0212(19) C4 0.076(2) 0.061(3) 0.136(3) 0.019(2) -0.041(2) 0.0030(18) C5 0.0581(16) 0.067(2) 0.108(2) 0.0054(19) -0.0243(17) -0.0090(16) C6 0.100(2) 0.092(3) 0.110(3) 0.029(2) -0.003(2) -0.003(2) C7 0.110(3) 0.105(4) 0.097(3) -0.014(2) 0.025(2) 0.010(3) C8 0.093(3) 0.120(3) 0.089(3) 0.015(2) 0.002(2) 0.034(2) C9 0.071(2) 0.120(4) 0.094(2) 0.005(2) 0.012(2) -0.010(2) C10 0.175(4) 0.107(4) 0.137(4) -0.019(3) 0.049(3) -0.045(3) C11 0.152(4) 0.124(5) 0.141(3) 0.021(3) 0.037(3) -0.026(3) C12 0.081(3) 0.134(5) 0.271(8) 0.039(5) -0.012(4) -0.032(3) C13 0.0518(15) 0.053(2) 0.101(2) 0.0019(18) -0.0113(16) -0.0036(14) C14 0.0657(18) 0.078(3) 0.098(2) 0.0106(19) 0.0017(19) -0.0104(18) C15 0.0667(19) 0.070(3) 0.130(3) 0.009(2) -0.008(2) -0.0131(18) C16 0.071(2) 0.079(3) 0.117(3) 0.004(2) -0.022(2) -0.0078(19) C17 0.0618(17) 0.055(2) 0.105(2) -0.0009(19) -0.0125(17) 0.0092(15) C18 0.101(3) 0.067(3) 0.125(3) -0.021(2) -0.006(3) 0.004(2) C19 0.0666(18) 0.102(3) 0.083(2) 0.003(2) 0.0016(19) -0.012(2) C20 0.088(2) 0.126(4) 0.102(3) 0.026(3) -0.002(2) -0.029(3) C21 0.0679(19) 0.098(3) 0.091(2) -0.012(2) 0.0029(19) 0.002(2) C22 0.084(2) 0.127(4) 0.124(3) -0.033(3) 0.001(2) 0.020(3) C23 0.069(2) 0.157(4) 0.148(4) -0.043(4) -0.029(3) 0.026(3) C24 0.144(3) 0.092(3) 0.115(3) 0.016(3) 0.014(3) 0.050(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 Mo1 O1 1.689(2) . ? Mo1 O2 1.694(2) . ? Mo1 N3 2.074(2) . ? Mo1 N1 2.076(2) . ? Mo1 N2 2.317(3) . ? Mo1 N4 2.331(3) . ? Si1 N1 1.741(3) . ? Si1 C7 1.845(4) . ? Si1 C8 1.855(4) . ? Si1 C9 1.871(4) . ? Si2 N3 1.754(3) . ? Si2 C20 1.830(4) . ? Si2 C19 1.842(4) . ? Si2 C21 1.892(4) . ? N1 C1 1.378(4) . ? N2 C5 1.336(4) . ? N2 C1 1.343(4) . ? N3 C13 1.378(4) . ? N4 C13 1.337(4) . ? N4 C17 1.349(5) . ? C1 C2 1.412(5) . ? C2 C3 1.357(6) . ? C3 C4 1.361(6) . ? C4 C5 1.368(5) . ? C5 C6 1.507(5) . ? C9 C12 1.505(6) . ? C9 C10 1.548(6) . ? C9 C11 1.552(6) . ? C13 C14 1.396(5) . ? C14 C15 1.393(5) . ? C15 C16 1.379(6) . ? C16 C17 1.371(5) . ? C17 C18 1.471(5) . ? C21 C22 1.503(5) . ? C21 C24 1.528(5) . ? C21 C23 1.542(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 105.04(12) . . ? O1 Mo1 N3 97.48(11) . . ? O2 Mo1 N3 104.10(10) . . ? O1 Mo1 N1 105.04(10) . . ? O2 Mo1 N1 97.33(11) . . ? N3 Mo1 N1 143.56(11) . . ? O1 Mo1 N2 90.00(10) . . ? O2 Mo1 N2 156.51(10) . . ? N3 Mo1 N2 91.41(10) . . ? N1 Mo1 N2 60.81(10) . . ? O1 Mo1 N4 154.64(11) . . ? O2 Mo1 N4 93.16(11) . . ? N3 Mo1 N4 60.39(10) . . ? N1 Mo1 N4 89.65(10) . . ? N2 Mo1 N4 79.11(9) . . ? N1 Si1 C7 111.60(16) . . ? N1 Si1 C8 108.96(16) . . ? C7 Si1 C8 108.80(19) . . ? N1 Si1 C9 108.73(16) . . ? C7 Si1 C9 110.05(19) . . ? C8 Si1 C9 108.6(2) . . ? N3 Si2 C20 111.35(17) . . ? N3 Si2 C19 108.01(15) . . ? C20 Si2 C19 108.27(18) . . ? N3 Si2 C21 110.20(15) . . ? C20 Si2 C21 110.05(18) . . ? C19 Si2 C21 108.89(19) . . ? C1 N1 Si1 129.2(2) . . ? C1 N1 Mo1 99.26(19) . . ? Si1 N1 Mo1 131.35(15) . . ? C5 N2 C1 121.1(3) . . ? C5 N2 Mo1 149.3(2) . . ? C1 N2 Mo1 89.58(18) . . ? C13 N3 Si2 127.8(2) . . ? C13 N3 Mo1 99.8(2) . . ? Si2 N3 Mo1 131.67(16) . . ? C13 N4 C17 120.9(3) . . ? C13 N4 Mo1 89.5(2) . . ? C17 N4 Mo1 149.3(2) . . ? N2 C1 N1 110.3(3) . . ? N2 C1 C2 120.0(3) . . ? N1 C1 C2 129.7(3) . . ? C3 C2 C1 117.5(3) . . ? C2 C3 C4 121.6(4) . . ? C3 C4 C5 119.2(4) . . ? N2 C5 C4 120.5(3) . . ? N2 C5 C6 116.1(3) . . ? C4 C5 C6 123.4(3) . . ? C12 C9 C10 107.5(4) . . ? C12 C9 C11 110.8(4) . . ? C10 C9 C11 108.1(4) . . ? C12 C9 Si1 111.5(3) . . ? C10 C9 Si1 109.6(3) . . ? C11 C9 Si1 109.2(3) . . ? N4 C13 N3 110.2(3) . . ? N4 C13 C14 121.3(3) . . ? N3 C13 C14 128.5(3) . . ? C15 C14 C13 116.8(3) . . ? C16 C15 C14 121.7(3) . . ? C17 C16 C15 117.9(4) . . ? N4 C17 C16 121.3(3) . . ? N4 C17 C18 117.6(3) . . ? C16 C17 C18 121.1(4) . . ? C22 C21 C24 108.4(4) . . ? C22 C21 C23 108.6(3) . . ? C24 C21 C23 110.4(3) . . ? C22 C21 Si2 109.8(3) . . ? C24 C21 Si2 109.2(2) . . ? C23 C21 Si2 110.4(3) . . ? _diffrn_measured_fraction_theta_max 0.681 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.681 _refine_diff_density_max 0.451 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.096 data_ylw1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 N4 O2 Si2 W' _chemical_formula_weight 574.49 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' 'O' 'O' 0.0106 0.0060 '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' 'W' 'W' -0.8490 6.8722 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.965(3) _cell_length_b 11.848(2) _cell_length_c 14.239(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.91(3) _cell_angle_gamma 90.00 _cell_volume 2333.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 5.071 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.6167 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'AFC7R Rigaku' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4590 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.05 _reflns_number_total 4590 _reflns_number_gt 3968 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'AFC7R Rigaku' _computing_cell_refinement 'AFC7R Rigaku' _computing_data_reduction 'Siemens PC' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens shelxtl' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00022(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4590 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.176 _refine_ls_shift/su_mean 0.016 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 W1 W 0.738267(12) 0.074706(13) 0.021665(11) 0.04601(6) Uani 1 1 d . . . Si1 Si 0.68498(11) -0.19164(11) 0.09988(10) 0.0598(3) Uani 1 1 d . . . Si2 Si 0.79015(11) 0.35269(11) -0.04163(10) 0.0599(3) Uani 1 1 d . . . O1 O 0.8223(3) 0.1110(3) 0.1160(3) 0.0689(10) Uani 1 1 d . . . O2 O 0.6293(3) 0.0940(3) 0.0626(2) 0.0643(9) Uani 1 1 d . . . N1 N 0.7369(3) -0.1005(4) 0.0240(3) 0.0556(12) Uani 1 1 d . . . N2 N 0.8459(3) -0.0254(3) -0.0587(3) 0.0548(10) Uani 1 1 d . . . N3 N 0.7527(3) 0.2129(3) -0.0642(3) 0.0530(9) Uani 1 1 d . . . N4 N 0.6640(3) 0.0727(3) -0.1340(3) 0.0479(10) Uani 1 1 d . . . C1 C 0.8030(3) -0.1229(4) -0.0343(3) 0.0522(11) Uani 1 1 d . . . C2 C 0.8296(4) -0.2253(5) -0.0709(4) 0.0709(15) Uani 1 1 d . . . H2A H 0.7992 -0.2920 -0.0571 0.085 Uiso 1 1 calc R . . C3 C 0.9009(4) -0.2261(5) -0.1271(4) 0.0804(17) Uani 1 1 d . . . H3A H 0.9202 -0.2945 -0.1506 0.096 Uiso 1 1 calc R . . C4 C 0.9446(4) -0.1289(6) -0.1499(4) 0.0806(18) Uani 1 1 d . . . H4A H 0.9937 -0.1307 -0.1878 0.097 Uiso 1 1 calc R . . C5 C 0.9140(3) -0.0254(5) -0.1148(4) 0.0652(14) Uani 1 1 d . . . C6 C 0.9557(4) 0.0841(5) -0.1375(4) 0.0782(19) Uani 1 1 d . . . H6A H 0.9252 0.1437 -0.1069 0.117 Uiso 1 1 calc R . . H6B H 0.9453 0.0955 -0.2049 0.117 Uiso 1 1 calc R . . H6C H 1.0239 0.0842 -0.1155 0.117 Uiso 1 1 calc R . . C7 C 0.6693(6) -0.1106(5) 0.2082(4) 0.098(2) Uani 1 1 d . . . H7A H 0.7307 -0.0814 0.2364 0.147 Uiso 1 1 calc R . . H7B H 0.6437 -0.1592 0.2526 0.147 Uiso 1 1 calc R . . H7C H 0.6254 -0.0492 0.1917 0.147 Uiso 1 1 calc R . . C8 C 0.5704(5) -0.2494(6) 0.0430(5) 0.107(2) Uani 1 1 d . . . H8A H 0.5809 -0.2908 -0.0127 0.161 Uiso 1 1 calc R . . H8B H 0.5258 -0.1889 0.0254 0.161 Uiso 1 1 calc R . . H8C H 0.5441 -0.2989 0.0863 0.161 Uiso 1 1 calc R . . C9 C 0.7700(5) -0.3105(5) 0.1362(4) 0.089(2) Uani 1 1 d . . . H9A H 0.8305 -0.2807 0.1663 0.133 Uiso 1 1 calc R . . H9B H 0.7804 -0.3532 0.0813 0.133 Uiso 1 1 calc R . . H9C H 0.7427 -0.3586 0.1799 0.133 Uiso 1 1 calc R . . C10 C 0.6972(3) 0.1778(4) -0.1479(3) 0.0521(11) Uani 1 1 d . . . C11 C 0.6760(4) 0.2339(4) -0.2334(3) 0.0645(14) Uani 1 1 d . . . H11A H 0.7005 0.3056 -0.2420 0.077 Uiso 1 1 calc R . . C12 C 0.6183(4) 0.1809(5) -0.3045(3) 0.0652(14) Uani 1 1 d . . . H12A H 0.6018 0.2174 -0.3623 0.078 Uiso 1 1 calc R . . C13 C 0.5835(4) 0.0728(4) -0.2919(4) 0.0648(15) Uani 1 1 d . . . H13A H 0.5444 0.0366 -0.3410 0.078 Uiso 1 1 calc R . . C14 C 0.6078(3) 0.0202(4) -0.2058(3) 0.0521(11) Uani 1 1 d . . . C15 C 0.5707(4) -0.0944(4) -0.1844(4) 0.0624(13) Uani 1 1 d . . . H15A H 0.5962 -0.1155 -0.1207 0.094 Uiso 1 1 calc R . . H15B H 0.5907 -0.1485 -0.2279 0.094 Uiso 1 1 calc R . . H15C H 0.5013 -0.0926 -0.1907 0.094 Uiso 1 1 calc R . . C16 C 0.8778(6) 0.3984(5) -0.1211(5) 0.091(2) Uani 1 1 d . . . H16A H 0.9339 0.3509 -0.1112 0.136 Uiso 1 1 calc R . . H16B H 0.8964 0.4753 -0.1071 0.136 Uiso 1 1 calc R . . H16C H 0.8483 0.3928 -0.1859 0.136 Uiso 1 1 calc R . . C17 C 0.6815(5) 0.4438(5) -0.0594(5) 0.085(2) Uani 1 1 d . . . H17A H 0.6509 0.4373 -0.1238 0.128 Uiso 1 1 calc R . . H17B H 0.7001 0.5208 -0.0464 0.128 Uiso 1 1 calc R . . H17C H 0.6372 0.4205 -0.0173 0.128 Uiso 1 1 calc R . . C18 C 0.8483(4) 0.3663(5) 0.0831(4) 0.0775(17) Uani 1 1 d . . . H18A H 0.9049 0.3195 0.0930 0.116 Uiso 1 1 calc R . . H18B H 0.8037 0.3428 0.1249 0.116 Uiso 1 1 calc R . . H18C H 0.8663 0.4435 0.0959 0.116 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 W1 0.05438(12) 0.03510(11) 0.04933(11) -0.00075(6) 0.00990(9) 0.00200(6) Si1 0.0704(8) 0.0405(6) 0.0691(7) 0.0084(6) 0.0119(6) 0.0019(6) Si2 0.0697(7) 0.0389(6) 0.0713(7) 0.0007(6) 0.0099(6) -0.0101(6) O1 0.076(2) 0.0615(19) 0.0672(19) -0.0089(18) 0.0042(17) -0.0057(19) O2 0.083(2) 0.0484(16) 0.0669(19) 0.0033(14) 0.0293(17) 0.0148(16) N1 0.059(3) 0.0379(18) 0.070(3) -0.0016(15) 0.011(2) 0.0057(15) N2 0.0505(19) 0.054(2) 0.060(2) -0.0066(18) 0.0094(16) 0.0047(17) N3 0.060(2) 0.0406(19) 0.0564(19) -0.0020(16) 0.0019(16) -0.0009(16) N4 0.052(2) 0.0356(19) 0.057(2) -0.0024(13) 0.0126(16) -0.0005(13) C1 0.049(2) 0.047(2) 0.061(2) -0.004(2) 0.0093(18) 0.012(2) C2 0.079(3) 0.056(3) 0.079(3) -0.023(2) 0.014(3) 0.008(3) C3 0.075(3) 0.069(3) 0.101(4) -0.026(3) 0.024(3) 0.010(3) C4 0.066(3) 0.098(4) 0.080(3) -0.012(3) 0.018(3) 0.018(3) C5 0.047(2) 0.088(4) 0.062(3) -0.004(3) 0.013(2) -0.006(3) C6 0.057(3) 0.105(5) 0.076(3) 0.005(3) 0.022(3) -0.007(3) C7 0.167(6) 0.056(3) 0.085(3) -0.005(3) 0.066(3) 0.002(4) C8 0.082(4) 0.107(4) 0.125(5) 0.060(4) -0.012(4) -0.033(3) C9 0.111(5) 0.071(3) 0.078(3) 0.008(3) -0.007(3) 0.024(3) C10 0.059(2) 0.044(2) 0.054(2) -0.0011(19) 0.0083(18) -0.006(2) C11 0.072(3) 0.056(3) 0.065(3) 0.014(2) 0.011(2) 0.004(2) C12 0.075(3) 0.067(3) 0.055(2) 0.009(2) 0.010(2) 0.001(3) C13 0.067(3) 0.063(3) 0.064(3) -0.008(2) 0.004(2) -0.003(2) C14 0.056(2) 0.048(2) 0.054(2) -0.0040(19) 0.0131(18) -0.0056(19) C15 0.066(3) 0.049(2) 0.073(3) -0.008(2) 0.013(2) -0.009(2) C16 0.106(5) 0.060(3) 0.109(5) 0.006(3) 0.030(4) -0.020(3) C17 0.113(5) 0.048(3) 0.092(4) -0.001(3) 0.005(4) 0.005(3) C18 0.077(3) 0.054(3) 0.097(4) -0.009(3) -0.006(3) -0.016(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 W1 O1 1.712(4) . ? W1 O2 1.718(4) . ? W1 N3 2.070(4) . ? W1 N1 2.076(5) . ? W1 N4 2.315(4) . ? W1 N2 2.333(4) . ? Si1 N1 1.754(4) . ? Si1 C8 1.825(7) . ? Si1 C7 1.855(6) . ? Si1 C9 1.868(6) . ? Si2 N3 1.753(4) . ? Si2 C17 1.851(7) . ? Si2 C18 1.855(6) . ? Si2 C16 1.858(8) . ? N1 C1 1.349(6) . ? N2 C5 1.324(6) . ? N2 C1 1.368(6) . ? N3 C10 1.393(6) . ? N4 C14 1.351(6) . ? N4 C10 1.352(5) . ? C1 C2 1.391(7) . ? C2 C3 1.362(9) . ? C3 C4 1.363(9) . ? C4 C5 1.412(9) . ? C5 C6 1.477(8) . ? C10 C11 1.383(6) . ? C11 C12 1.358(7) . ? C12 C13 1.391(7) . ? C13 C14 1.377(7) . ? C14 C15 1.499(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O2 104.13(18) . . ? O1 W1 N3 98.77(17) . . ? O2 W1 N3 104.96(16) . . ? O1 W1 N1 104.23(16) . . ? O2 W1 N1 96.72(15) . . ? N3 W1 N1 143.32(14) . . ? O1 W1 N4 157.22(16) . . ? O2 W1 N4 91.44(16) . . ? N3 W1 N4 60.62(13) . . ? N1 W1 N4 90.06(12) . . ? O1 W1 N2 95.39(16) . . ? O2 W1 N2 153.37(15) . . ? N3 W1 N2 89.47(15) . . ? N1 W1 N2 60.49(14) . . ? N4 W1 N2 76.08(13) . . ? N1 Si1 C8 111.7(3) . . ? N1 Si1 C7 107.4(3) . . ? C8 Si1 C7 111.5(4) . . ? N1 Si1 C9 109.5(3) . . ? C8 Si1 C9 109.0(3) . . ? C7 Si1 C9 107.6(3) . . ? N3 Si2 C17 107.9(2) . . ? N3 Si2 C18 109.7(2) . . ? C17 Si2 C18 108.9(3) . . ? N3 Si2 C16 111.6(3) . . ? C17 Si2 C16 110.0(3) . . ? C18 Si2 C16 108.6(3) . . ? C1 N1 Si1 129.3(4) . . ? C1 N1 W1 100.3(3) . . ? Si1 N1 W1 129.1(2) . . ? C5 N2 C1 121.9(5) . . ? C5 N2 W1 149.4(4) . . ? C1 N2 W1 88.3(3) . . ? C10 N3 Si2 123.8(3) . . ? C10 N3 W1 100.4(3) . . ? Si2 N3 W1 133.6(2) . . ? C14 N4 C10 119.3(4) . . ? C14 N4 W1 150.0(3) . . ? C10 N4 W1 90.8(3) . . ? N1 C1 N2 110.5(4) . . ? N1 C1 C2 129.9(5) . . ? N2 C1 C2 119.6(5) . . ? C3 C2 C1 118.7(5) . . ? C4 C3 C2 121.4(6) . . ? C3 C4 C5 118.8(5) . . ? N2 C5 C4 119.5(6) . . ? N2 C5 C6 118.0(5) . . ? C4 C5 C6 122.5(5) . . ? N4 C10 C11 122.3(4) . . ? N4 C10 N3 108.2(4) . . ? C11 C10 N3 129.5(4) . . ? C12 C11 C10 117.9(5) . . ? C11 C12 C13 120.8(5) . . ? C14 C13 C12 119.0(5) . . ? N4 C14 C13 120.8(4) . . ? N4 C14 C15 116.4(4) . . ? C13 C14 C15 122.8(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.151 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.129 data_lhk15 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H30 Mo N4 O2 Si2' _chemical_formula_weight 486.58 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 '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' 'Mo' 'Mo' -1.6832 0.6857 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.931(3) _cell_length_b 11.888(2) _cell_length_c 14.295(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.38(3) _cell_angle_gamma 90.00 _cell_volume 2347.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used IP _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour golden _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method ? _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_T_max 1.068 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 RAX-IIC _diffrn_measurement_method IP _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7569 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.59 _reflns_number_total 4261 _reflns_number_observed 4074 _reflns_observed_criterion >2sigma(I) _computing_data_collection BIOTEX _computing_cell_refinement BIOTEX _computing_data_reduction BIOTEX _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+0.6492P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0122(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4261 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_obs 0.0372 _refine_ls_wR_factor_all 0.1390 _refine_ls_wR_factor_obs 0.1364 _refine_ls_goodness_of_fit_all 1.095 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.095 _refine_ls_restrained_S_obs 1.099 _refine_ls_shift/esd_max 0.006 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.738013(11) 0.075119(12) 0.020525(10) 0.05450(5) Uani 1 d . . Si1 Si 0.68660(4) -0.19119(5) 0.09897(4) 0.0670(2) Uani 1 d . . Si2 Si 0.78892(4) 0.35298(5) -0.04347(4) 0.0685(2) Uani 1 d . . O1 O 0.82119(11) 0.11278(13) 0.11199(10) 0.0752(4) Uani 1 d . . O2 O 0.62954(10) 0.09087(11) 0.06068(10) 0.0693(4) Uani 1 d . . N1 N 0.73764(10) -0.0996(2) 0.02336(10) 0.0625(5) Uani 1 d . . N2 N 0.84653(10) -0.02464(15) -0.05963(11) 0.0632(4) Uani 1 d . . N3 N 0.75136(11) 0.21346(13) -0.06554(10) 0.0613(4) Uani 1 d . . N4 N 0.66327(11) 0.07307(11) -0.13647(11) 0.0551(4) Uani 1 d . . C1 C 0.80603(13) -0.1224(2) -0.03586(13) 0.0606(5) Uani 1 d . . C2 C 0.83000(15) -0.2246(2) -0.07396(15) 0.0744(6) Uani 1 d . . H2B H 0.79831(15) -0.2907(2) -0.06118(15) 0.089 Uiso 1 calc R . C3 C 0.9020(2) -0.2249(2) -0.1311(2) 0.0897(7) Uani 1 d . . H3A H 0.9215(2) -0.2924(2) -0.1555(2) 0.108 Uiso 1 calc R . C4 C 0.9459(2) -0.1255(2) -0.1525(2) 0.0872(7) Uani 1 d . . H4A H 0.9951(2) -0.1264(2) -0.1908(2) 0.105 Uiso 1 calc R . C5 C 0.91636(13) -0.0249(2) -0.11691(14) 0.0713(6) Uani 1 d . . C6 C 0.9582(2) 0.0864(2) -0.1381(2) 0.0896(8) Uani 1 d . . H6A H 0.9273(2) 0.1447(2) -0.1062(2) 0.134 Uiso 1 calc R . H6B H 0.9477(2) 0.0997(2) -0.2048(2) 0.134 Uiso 1 calc R . H6C H 1.0264(2) 0.0866(2) -0.1167(2) 0.134 Uiso 1 calc R . C7 C 0.6714(2) -0.1105(2) 0.2074(2) 0.1100(9) Uani 1 d . . H7A H 0.7330(2) -0.0818(2) 0.2349(2) 0.165 Uiso 1 calc R . H7B H 0.6457(2) -0.1591(2) 0.2518(2) 0.165 Uiso 1 calc R . H7C H 0.6276(2) -0.0491(2) 0.1916(2) 0.165 Uiso 1 calc R . C8 C 0.5693(2) -0.2478(2) 0.0442(2) 0.1214(10) Uani 1 d . . H8A H 0.5258(2) -0.1867(2) 0.0261(2) 0.182 Uiso 1 calc R . H8B H 0.5423(2) -0.2950(2) 0.0887(2) 0.182 Uiso 1 calc R . H8C H 0.5788(2) -0.2910(2) -0.0106(2) 0.182 Uiso 1 calc R . C9 C 0.7699(2) -0.3098(2) 0.1336(2) 0.0904(8) Uani 1 d . . H9A H 0.8311(2) -0.2810(2) 0.1621(2) 0.136 Uiso 1 calc R . H9B H 0.7791(2) -0.3530(2) 0.0787(2) 0.136 Uiso 1 calc R . H9C H 0.7426(2) -0.3570(2) 0.1779(2) 0.136 Uiso 1 calc R . C10 C 0.69669(13) 0.1778(2) -0.14780(12) 0.0591(5) Uani 1 d . . C11 C 0.67490(15) 0.2357(2) -0.23403(14) 0.0705(6) Uani 1 d . . H11A H 0.69827(15) 0.3078(2) -0.24222(14) 0.085 Uiso 1 calc R . C12 C 0.6180(2) 0.1813(2) -0.30518(14) 0.0746(6) Uani 1 d . . H12A H 0.6025(2) 0.2171(2) -0.36300(14) 0.090 Uiso 1 calc R . C13 C 0.5828(2) 0.0738(2) -0.2927(2) 0.0708(6) Uani 1 d . . H13A H 0.5434(2) 0.0382(2) -0.3413(2) 0.085 Uiso 1 calc R . C14 C 0.60702(13) 0.0203(2) -0.20701(13) 0.0590(5) Uani 1 d . . C15 C 0.5720(2) -0.0949(2) -0.1862(2) 0.0705(6) Uani 1 d . . H15A H 0.5974(2) -0.1157(2) -0.1229(2) 0.106 Uiso 1 calc R . H15B H 0.5936(2) -0.1478(2) -0.2297(2) 0.106 Uiso 1 calc R . H15C H 0.5026(2) -0.0951(2) -0.1925(2) 0.106 Uiso 1 calc R . C16 C 0.8768(2) 0.3990(2) -0.1257(2) 0.1007(9) Uani 1 d . . H16A H 0.8468(2) 0.3922(2) -0.1897(2) 0.151 Uiso 1 calc R . H16B H 0.9334(2) 0.3523(2) -0.1163(2) 0.151 Uiso 1 calc R . H16C H 0.8949(2) 0.4759(2) -0.1128(2) 0.151 Uiso 1 calc R . C17 C 0.6782(2) 0.4440(2) -0.0602(2) 0.0869(8) Uani 1 d . . H17A H 0.6473(2) 0.4370(2) -0.1239(2) 0.130 Uiso 1 calc R . H17B H 0.6965(2) 0.5209(2) -0.0478(2) 0.130 Uiso 1 calc R . H17C H 0.6343(2) 0.4206(2) -0.0174(2) 0.130 Uiso 1 calc R . C18 C 0.8485(2) 0.3668(2) 0.0799(2) 0.0870(8) Uani 1 d . . H18A H 0.9053(2) 0.3203(2) 0.0886(2) 0.131 Uiso 1 calc R . H18B H 0.8045(2) 0.3435(2) 0.1225(2) 0.131 Uiso 1 calc R . H18C H 0.8666(2) 0.4438(2) 0.0922(2) 0.131 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.05884(10) 0.04883(9) 0.05588(9) -0.00052(6) 0.00757(8) 0.00205(6) Si1 0.0748(3) 0.0533(3) 0.0721(3) 0.0074(2) 0.0066(3) 0.0014(2) Si2 0.0724(3) 0.0546(3) 0.0779(3) 0.0005(3) 0.0073(3) -0.0093(2) O1 0.0827(9) 0.0727(8) 0.0672(7) -0.0038(7) -0.0017(7) -0.0028(8) O2 0.0728(8) 0.0633(7) 0.0747(8) -0.0002(6) 0.0211(6) 0.0075(6) N1 0.0636(9) 0.0572(8) 0.0680(10) -0.0009(7) 0.0134(8) 0.0074(6) N2 0.0537(8) 0.0732(10) 0.0626(8) -0.0023(8) 0.0068(6) 0.0060(7) N3 0.0682(8) 0.0555(8) 0.0595(8) 0.0023(7) 0.0051(7) -0.0066(7) N4 0.0556(8) 0.0534(8) 0.0563(8) 0.0013(6) 0.0069(6) 0.0013(6) C1 0.0566(9) 0.0620(10) 0.0627(10) -0.0001(9) 0.0052(8) 0.0068(8) C2 0.0768(12) 0.0644(11) 0.0824(12) -0.0138(10) 0.0120(10) 0.0117(10) C3 0.0773(13) 0.0933(15) 0.0991(15) -0.0281(13) 0.0132(11) 0.0161(12) C4 0.0627(10) 0.122(2) 0.0786(12) -0.0196(14) 0.0175(9) 0.0153(12) C5 0.0524(9) 0.0957(14) 0.0652(10) 0.0007(11) 0.0050(8) 0.0006(10) C6 0.0677(12) 0.115(2) 0.0892(15) 0.0103(13) 0.0210(11) -0.0065(12) C7 0.175(2) 0.0743(14) 0.0929(14) 0.0131(13) 0.0634(14) 0.011(2) C8 0.086(2) 0.133(2) 0.137(2) 0.062(2) -0.016(2) -0.029(2) C9 0.112(2) 0.0703(13) 0.0847(14) 0.0104(11) -0.0036(13) 0.0170(12) C10 0.0601(9) 0.0569(10) 0.0604(9) -0.0011(8) 0.0084(7) 0.0028(8) C11 0.0784(12) 0.0642(11) 0.0686(11) 0.0093(9) 0.0082(9) -0.0018(10) C12 0.0872(13) 0.0742(12) 0.0613(10) 0.0103(10) 0.0051(9) 0.0012(11) C13 0.0702(12) 0.0776(13) 0.0623(11) -0.0009(9) 0.0002(9) -0.0052(9) C14 0.0548(9) 0.0625(10) 0.0606(9) -0.0012(8) 0.0106(7) 0.0015(8) C15 0.0750(12) 0.0644(10) 0.0707(11) -0.0085(9) 0.0041(10) -0.0121(9) C16 0.100(2) 0.0852(14) 0.121(2) 0.000(2) 0.0297(15) -0.0268(13) C17 0.097(2) 0.0666(12) 0.095(2) 0.0007(12) 0.0027(13) 0.0085(12) C18 0.0865(14) 0.0673(13) 0.102(2) -0.0069(12) -0.0087(12) -0.0093(11) _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 Mo1 O1 1.6921(15) . ? Mo1 O2 1.694(2) . ? Mo1 N3 2.076(2) . ? Mo1 N1 2.077(2) . ? Mo1 N2 2.334(2) . ? Mo1 N4 2.350(2) . ? Si1 N1 1.748(2) . ? Si1 C8 1.846(3) . ? Si1 C9 1.852(2) . ? Si1 C7 1.858(3) . ? Si2 N3 1.755(2) . ? Si2 C18 1.857(2) . ? Si2 C17 1.873(3) . ? Si2 C16 1.883(3) . ? N1 C1 1.380(2) . ? N2 C5 1.350(3) . ? N2 C1 1.354(3) . ? N3 C10 1.383(2) . ? N4 C10 1.346(2) . ? N4 C14 1.350(2) . ? C1 C2 1.390(3) . ? C2 C3 1.373(3) . ? C3 C4 1.382(4) . ? C4 C5 1.383(4) . ? C5 C6 1.493(3) . ? C10 C11 1.410(3) . ? C11 C12 1.369(3) . ? C12 C13 1.389(3) . ? C13 C14 1.383(3) . ? C14 C15 1.497(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 105.13(7) . . ? O1 Mo1 N3 98.26(7) . . ? O2 Mo1 N3 105.36(7) . . ? O1 Mo1 N1 104.63(7) . . ? O2 Mo1 N1 95.70(6) . . ? N3 Mo1 N1 143.52(6) . . ? O1 Mo1 N2 95.24(7) . . ? O2 Mo1 N2 152.17(6) . . ? N3 Mo1 N2 89.92(6) . . ? N1 Mo1 N2 60.33(6) . . ? O1 Mo1 N4 156.38(6) . . ? O2 Mo1 N4 91.13(7) . . ? N3 Mo1 N4 60.31(5) . . ? N1 Mo1 N4 90.36(5) . . ? N2 Mo1 N4 76.19(5) . . ? N1 Si1 C8 111.91(11) . . ? N1 Si1 C9 110.42(10) . . ? C8 Si1 C9 109.01(12) . . ? N1 Si1 C7 107.07(10) . . ? C8 Si1 C7 110.61(15) . . ? C9 Si1 C7 107.74(12) . . ? N3 Si2 C18 109.93(9) . . ? N3 Si2 C17 107.53(10) . . ? C18 Si2 C17 109.28(12) . . ? N3 Si2 C16 111.40(10) . . ? C18 Si2 C16 108.62(12) . . ? C17 Si2 C16 110.07(12) . . ? C1 N1 Si1 128.65(15) . . ? C1 N1 Mo1 100.41(12) . . ? Si1 N1 Mo1 129.56(9) . . ? C5 N2 C1 120.4(2) . . ? C5 N2 Mo1 149.5(2) . . ? C1 N2 Mo1 89.76(11) . . ? C10 N3 Si2 124.15(13) . . ? C10 N3 Mo1 100.34(11) . . ? Si2 N3 Mo1 133.56(8) . . ? C10 N4 C14 121.1(2) . . ? C10 N4 Mo1 89.29(10) . . ? C14 N4 Mo1 149.55(12) . . ? N2 C1 N1 109.2(2) . . ? N2 C1 C2 121.6(2) . . ? N1 C1 C2 129.2(2) . . ? C3 C2 C1 117.7(2) . . ? C2 C3 C4 120.6(2) . . ? C3 C4 C5 119.8(2) . . ? N2 C5 C4 119.8(2) . . ? N2 C5 C6 116.8(2) . . ? C4 C5 C6 123.4(2) . . ? N4 C10 N3 110.0(2) . . ? N4 C10 C11 121.2(2) . . ? N3 C10 C11 128.8(2) . . ? C12 C11 C10 117.3(2) . . ? C11 C12 C13 121.3(2) . . ? C14 C13 C12 119.1(2) . . ? N4 C14 C13 120.0(2) . . ? N4 C14 C15 116.7(2) . . ? C13 C14 C15 123.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 Si1 N1 C1 -96.2(2) . . . . ? C9 Si1 N1 C1 25.4(2) . . . . ? C7 Si1 N1 C1 142.4(2) . . . . ? C8 Si1 N1 Mo1 99.89(14) . . . . ? C9 Si1 N1 Mo1 -138.50(11) . . . . ? C7 Si1 N1 Mo1 -21.47(15) . . . . ? O1 Mo1 N1 C1 -91.33(11) . . . . ? O2 Mo1 N1 C1 161.38(11) . . . . ? N3 Mo1 N1 C1 35.7(2) . . . . ? N2 Mo1 N1 C1 -3.63(9) . . . . ? N4 Mo1 N1 C1 70.22(11) . . . . ? O1 Mo1 N1 Si1 75.93(11) . . . . ? O2 Mo1 N1 Si1 -31.35(11) . . . . ? N3 Mo1 N1 Si1 -156.99(9) . . . . ? N2 Mo1 N1 Si1 163.64(12) . . . . ? N4 Mo1 N1 Si1 -122.52(10) . . . . ? O1 Mo1 N2 C5 -80.3(2) . . . . ? O2 Mo1 N2 C5 142.3(2) . . . . ? N3 Mo1 N2 C5 17.9(2) . . . . ? N1 Mo1 N2 C5 175.8(3) . . . . ? N4 Mo1 N2 C5 77.3(2) . . . . ? O1 Mo1 N2 C1 107.51(11) . . . . ? O2 Mo1 N2 C1 -29.8(2) . . . . ? N3 Mo1 N2 C1 -154.20(10) . . . . ? N1 Mo1 N2 C1 3.64(9) . . . . ? N4 Mo1 N2 C1 -94.84(10) . . . . ? C18 Si2 N3 C10 173.7(2) . . . . ? C17 Si2 N3 C10 54.8(2) . . . . ? C16 Si2 N3 C10 -65.8(2) . . . . ? C18 Si2 N3 Mo1 12.9(2) . . . . ? C17 Si2 N3 Mo1 -105.98(14) . . . . ? C16 Si2 N3 Mo1 133.34(14) . . . . ? O1 Mo1 N3 C10 170.42(12) . . . . ? O2 Mo1 N3 C10 -81.32(12) . . . . ? N1 Mo1 N3 C10 41.7(2) . . . . ? N2 Mo1 N3 C10 75.14(11) . . . . ? N4 Mo1 N3 C10 1.03(10) . . . . ? O1 Mo1 N3 Si2 -25.63(13) . . . . ? O2 Mo1 N3 Si2 82.63(13) . . . . ? N1 Mo1 N3 Si2 -154.37(10) . . . . ? N2 Mo1 N3 Si2 -120.91(12) . . . . ? N4 Mo1 N3 Si2 164.98(15) . . . . ? O1 Mo1 N4 C10 -28.1(2) . . . . ? O2 Mo1 N4 C10 106.04(11) . . . . ? N3 Mo1 N4 C10 -1.04(10) . . . . ? N1 Mo1 N4 C10 -158.26(11) . . . . ? N2 Mo1 N4 C10 -99.00(11) . . . . ? O1 Mo1 N4 C14 155.5(2) . . . . ? O2 Mo1 N4 C14 -70.4(2) . . . . ? N3 Mo1 N4 C14 -177.5(3) . . . . ? N1 Mo1 N4 C14 25.3(2) . . . . ? N2 Mo1 N4 C14 84.6(2) . . . . ? C5 N2 C1 N1 179.57(15) . . . . ? Mo1 N2 C1 N1 -5.04(13) . . . . ? C5 N2 C1 C2 -4.2(3) . . . . ? Mo1 N2 C1 C2 171.2(2) . . . . ? Si1 N1 C1 N2 -161.67(12) . . . . ? Mo1 N1 C1 N2 5.76(15) . . . . ? Si1 N1 C1 C2 22.5(3) . . . . ? Mo1 N1 C1 C2 -170.1(2) . . . . ? N2 C1 C2 C3 5.1(3) . . . . ? N1 C1 C2 C3 -179.6(2) . . . . ? C1 C2 C3 C4 -2.6(3) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C1 N2 C5 C4 0.8(3) . . . . ? Mo1 N2 C5 C4 -170.0(2) . . . . ? C1 N2 C5 C6 -179.0(2) . . . . ? Mo1 N2 C5 C6 10.2(3) . . . . ? C3 C4 C5 N2 1.5(3) . . . . ? C3 C4 C5 C6 -178.7(2) . . . . ? C14 N4 C10 N3 179.3(2) . . . . ? Mo1 N4 C10 N3 1.45(14) . . . . ? C14 N4 C10 C11 -0.6(3) . . . . ? Mo1 N4 C10 C11 -178.5(2) . . . . ? Si2 N3 C10 N4 -167.66(13) . . . . ? Mo1 N3 C10 N4 -1.7(2) . . . . ? Si2 N3 C10 C11 12.3(3) . . . . ? Mo1 N3 C10 C11 178.3(2) . . . . ? N4 C10 C11 C12 0.5(3) . . . . ? N3 C10 C11 C12 -179.5(2) . . . . ? C10 C11 C12 C13 0.3(3) . . . . ? C11 C12 C13 C14 -0.9(3) . . . . ? C10 N4 C14 C13 0.0(3) . . . . ? Mo1 N4 C14 C13 175.8(2) . . . . ? C10 N4 C14 C15 -178.7(2) . . . . ? Mo1 N4 C14 C15 -2.8(3) . . . . ? C12 C13 C14 N4 0.7(3) . . . . ? C12 C13 C14 C15 179.3(2) . . . . ? _refine_diff_density_max 0.459 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.079