Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Nadia Carmen Mosch-Zanetti' _publ_contact_author_address ;Institute of Inorganic Chemistry University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; _publ_contact_author_email NMOESCH@GWDG.D loop_ _publ_author_name _publ_author_address G.Lyashenko ;Institute of Inorganic Chemistry University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; V.Jancik ;Institute of Inorganic Chemistry University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; A.Pal ;Institute of Inorganic Chemistry University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; R.Herbst-Irmer ;Institute of Inorganic Chemistry University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; N.C.Mosch-Zanetti ;Institute of Inorganic Chemistry University of G\"ottingen Tammannstr. 4 D-37077 G\"ottingen Germany ; data_compound3 _database_code_depnum_ccdc_archive 'CCDC 284752' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H40 Cl Mo N3 S Si' _chemical_formula_weight 622.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 '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 8.982(2) _cell_length_b 20.696(3) _cell_length_c 16.862(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.65(2) _cell_angle_gamma 90.00 _cell_volume 3069.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8369 _cell_measurement_theta_min 2.135 _cell_measurement_theta_max 59.006 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 5.464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4079 _exptl_absorpt_correction_T_max 0.6111 _exptl_absorpt_process_details ? _exptl_special_details ; Intensities are measured with a SMART 6000 area detector ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'mirror system' _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.602 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27816 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 59.05 _reflns_number_total 4397 _reflns_number_gt 4330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Proteum(Version 1.40, Bruker 2002)' _computing_cell_refinement 'Siemens SAINT (V. 7.01A, Siemens 2003)' _computing_data_reduction 'Siemens SAINT (V. 7.01A, Siemens 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (V. 6.12)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+3.2032P] 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 0.00115(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4397 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 Mo1 Mo 0.12484(2) 0.246155(8) 0.189713(11) 0.01087(10) Uani 1 1 d . . . Cl1 Cl 0.26196(8) 0.24225(3) 0.32620(4) 0.02675(18) Uani 1 1 d . . . S1 S 0.27098(6) 0.36280(3) 0.20004(4) 0.01694(16) Uani 1 1 d . . . Si1 Si -0.22691(7) 0.29964(3) 0.11495(4) 0.01613(17) Uani 1 1 d . . . N1 N -0.0279(2) 0.30532(9) 0.12114(11) 0.0118(4) Uani 1 1 d . . . C1 C 0.0303(3) 0.35088(11) 0.07281(13) 0.0130(5) Uani 1 1 d . . . C2 C 0.1665(3) 0.38379(11) 0.10268(14) 0.0157(5) Uani 1 1 d . . . N2 N 0.0112(2) 0.17904(9) 0.19990(11) 0.0152(4) Uani 1 1 d . . . N3 N 0.2502(2) 0.22261(9) 0.12761(11) 0.0146(4) Uani 1 1 d . . . C3 C 0.2237(3) 0.42911(12) 0.05545(17) 0.0258(6) Uani 1 1 d . . . H3A H 0.3163 0.4509 0.0768 0.031 Uiso 1 1 calc R . . C4 C 0.1466(3) 0.44246(13) -0.02201(17) 0.0329(7) Uani 1 1 d . . . H4A H 0.1835 0.4744 -0.0536 0.039 Uiso 1 1 calc R . . C5 C 0.0142(4) 0.40864(13) -0.05345(16) 0.0308(7) Uani 1 1 d . . . H5A H -0.0377 0.4168 -0.1074 0.037 Uiso 1 1 calc R . . C6 C -0.0428(3) 0.36348(12) -0.00765(14) 0.0212(6) Uani 1 1 d . . . H6A H -0.1327 0.3405 -0.0307 0.025 Uiso 1 1 calc R . . C7 C 0.2129(3) 0.42497(13) 0.26830(16) 0.0277(6) Uani 1 1 d . . . C8 C 0.0452(3) 0.41851(19) 0.2704(2) 0.0508(10) Uani 1 1 d . . . H8A H 0.0173 0.4512 0.3068 0.076 Uiso 1 1 calc R . . H8B H 0.0257 0.3754 0.2900 0.076 Uiso 1 1 calc R . . H8C H -0.0156 0.4247 0.2158 0.076 Uiso 1 1 calc R . . C9 C 0.3095(4) 0.41155(15) 0.35181(17) 0.0378(7) Uani 1 1 d . . . H9A H 0.2915 0.4453 0.3896 0.057 Uiso 1 1 calc R . . H9B H 0.4172 0.4114 0.3485 0.057 Uiso 1 1 calc R . . H9C H 0.2819 0.3694 0.3710 0.057 Uiso 1 1 calc R . . C10 C 0.2490(3) 0.49142(13) 0.23921(18) 0.0371(8) Uani 1 1 d . . . H10A H 0.2319 0.5241 0.2785 0.056 Uiso 1 1 calc R . . H10B H 0.1829 0.5003 0.1866 0.056 Uiso 1 1 calc R . . H10C H 0.3555 0.4928 0.2337 0.056 Uiso 1 1 calc R . . C11 C -0.3175(3) 0.38008(13) 0.08620(17) 0.0276(6) Uani 1 1 d . . . H11A H -0.3161 0.3892 0.0293 0.041 Uiso 1 1 calc R . . H11B H -0.2610 0.4138 0.1205 0.041 Uiso 1 1 calc R . . H11C H -0.4229 0.3793 0.0937 0.041 Uiso 1 1 calc R . . C12 C -0.2664(3) 0.28065(14) 0.21666(17) 0.0273(6) Uani 1 1 d . . . H12A H -0.2470 0.2347 0.2285 0.041 Uiso 1 1 calc R . . H12B H -0.3729 0.2905 0.2172 0.041 Uiso 1 1 calc R . . H12C H -0.2001 0.3068 0.2578 0.041 Uiso 1 1 calc R . . C13 C -0.3131(3) 0.23638(14) 0.04139(18) 0.0274(6) Uani 1 1 d . . . H13A H -0.2792 0.1936 0.0627 0.041 Uiso 1 1 calc R . . H13B H -0.2814 0.2433 -0.0103 0.041 Uiso 1 1 calc R . . H13C H -0.4241 0.2389 0.0329 0.041 Uiso 1 1 calc R . . C14 C -0.0526(3) 0.11853(11) 0.20711(15) 0.0165(5) Uani 1 1 d . . . C15 C -0.0752(3) 0.07565(11) 0.14079(15) 0.0176(5) Uani 1 1 d . . . C16 C -0.1403(3) 0.01589(12) 0.14894(17) 0.0234(6) Uani 1 1 d . . . H16A H -0.1598 -0.0128 0.1041 0.028 Uiso 1 1 calc R . . C17 C -0.1772(3) -0.00261(13) 0.22146(19) 0.0302(7) Uani 1 1 d . . . H17A H -0.2199 -0.0440 0.2265 0.036 Uiso 1 1 calc R . . C18 C -0.1518(3) 0.03920(13) 0.28638(19) 0.0315(7) Uani 1 1 d . . . H18A H -0.1767 0.0258 0.3360 0.038 Uiso 1 1 calc R . . C19 C -0.0907(3) 0.10050(12) 0.28147(16) 0.0238(6) Uani 1 1 d . . . C20 C -0.0235(3) 0.09261(13) 0.06402(15) 0.0260(6) Uani 1 1 d . . . H20A H -0.0645 0.0611 0.0219 0.039 Uiso 1 1 calc R . . H20B H 0.0878 0.0919 0.0738 0.039 Uiso 1 1 calc R . . H20C H -0.0601 0.1359 0.0463 0.039 Uiso 1 1 calc R . . C21 C -0.0625(4) 0.14473(14) 0.35350(17) 0.0360(7) Uani 1 1 d . . . H21A H -0.1017 0.1248 0.3979 0.054 Uiso 1 1 calc R . . H21B H -0.1143 0.1860 0.3388 0.054 Uiso 1 1 calc R . . H21C H 0.0470 0.1523 0.3708 0.054 Uiso 1 1 calc R . . C22 C 0.3145(3) 0.17787(11) 0.08275(14) 0.0147(5) Uani 1 1 d . . . C23 C 0.4207(3) 0.13305(11) 0.12354(15) 0.0184(5) Uani 1 1 d . . . C24 C 0.4817(3) 0.08851(12) 0.07714(17) 0.0247(6) Uani 1 1 d . . . H24A H 0.5529 0.0574 0.1033 0.030 Uiso 1 1 calc R . . C25 C 0.4405(3) 0.08877(12) -0.00634(17) 0.0270(6) Uani 1 1 d . . . H25A H 0.4832 0.0579 -0.0370 0.032 Uiso 1 1 calc R . . C26 C 0.3370(3) 0.13378(12) -0.04556(16) 0.0228(6) Uani 1 1 d . . . H26A H 0.3100 0.1335 -0.1030 0.027 Uiso 1 1 calc R . . C27 C 0.2723(3) 0.17922(11) -0.00246(15) 0.0177(5) Uani 1 1 d . . . C28 C 0.4678(3) 0.13436(12) 0.21416(16) 0.0253(6) Uani 1 1 d . . . H28A H 0.5413 0.0997 0.2320 0.038 Uiso 1 1 calc R . . H28B H 0.3783 0.1281 0.2383 0.038 Uiso 1 1 calc R . . H28C H 0.5147 0.1762 0.2314 0.038 Uiso 1 1 calc R . . C29 C 0.1605(3) 0.22854(13) -0.04422(15) 0.0237(6) Uani 1 1 d . . . H29A H 0.1468 0.2232 -0.1030 0.036 Uiso 1 1 calc R . . H29B H 0.1992 0.2720 -0.0290 0.036 Uiso 1 1 calc R . . H29C H 0.0627 0.2225 -0.0279 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01417(15) 0.01340(14) 0.00558(15) 0.00211(6) 0.00330(9) 0.00060(7) Cl1 0.0349(4) 0.0336(4) 0.0087(3) 0.0058(2) -0.0027(3) -0.0024(3) S1 0.0134(3) 0.0182(3) 0.0192(3) -0.0012(2) 0.0033(2) -0.0018(2) Si1 0.0135(3) 0.0175(3) 0.0173(4) -0.0007(3) 0.0026(3) -0.0005(3) N1 0.0139(10) 0.0139(10) 0.0074(9) 0.0007(8) 0.0016(8) 0.0006(8) C1 0.0207(12) 0.0115(11) 0.0087(12) 0.0002(9) 0.0075(10) 0.0056(10) C2 0.0178(12) 0.0154(12) 0.0171(13) 0.0038(10) 0.0115(10) 0.0048(10) N2 0.0193(10) 0.0168(10) 0.0100(10) 0.0052(8) 0.0043(8) 0.0031(8) N3 0.0156(10) 0.0162(10) 0.0121(10) 0.0025(8) 0.0027(8) 0.0014(8) C3 0.0277(14) 0.0195(13) 0.0364(17) 0.0060(12) 0.0214(13) 0.0037(11) C4 0.0507(19) 0.0234(14) 0.0347(17) 0.0149(13) 0.0329(15) 0.0126(14) C5 0.055(2) 0.0273(15) 0.0136(13) 0.0090(11) 0.0161(13) 0.0229(14) C6 0.0317(15) 0.0198(13) 0.0126(13) -0.0003(10) 0.0055(11) 0.0092(11) C7 0.0233(14) 0.0304(15) 0.0269(15) -0.0156(12) -0.0005(11) -0.0026(11) C8 0.0308(17) 0.077(3) 0.048(2) -0.0461(19) 0.0152(15) -0.0051(16) C9 0.0501(19) 0.0323(16) 0.0260(16) -0.0099(13) -0.0044(14) -0.0070(14) C10 0.0380(18) 0.0231(15) 0.0413(18) -0.0120(13) -0.0133(14) 0.0072(13) C11 0.0197(14) 0.0258(14) 0.0366(16) 0.0005(12) 0.0039(12) 0.0037(11) C12 0.0214(14) 0.0359(16) 0.0287(15) -0.0011(13) 0.0150(12) -0.0027(12) C13 0.0243(15) 0.0293(14) 0.0260(16) -0.0038(12) -0.0012(12) -0.0086(12) C14 0.0126(12) 0.0152(12) 0.0224(13) 0.0076(10) 0.0056(10) 0.0031(10) C15 0.0132(12) 0.0178(13) 0.0208(13) 0.0042(10) 0.0007(10) 0.0025(10) C16 0.0169(13) 0.0183(13) 0.0342(15) 0.0023(11) 0.0032(11) 0.0013(10) C17 0.0243(14) 0.0186(13) 0.0513(19) 0.0081(13) 0.0162(13) -0.0012(11) C18 0.0343(16) 0.0267(15) 0.0402(17) 0.0144(14) 0.0236(13) 0.0035(12) C19 0.0249(14) 0.0241(14) 0.0264(15) 0.0088(11) 0.0150(11) 0.0034(11) C20 0.0382(16) 0.0224(14) 0.0165(14) -0.0021(11) 0.0034(12) -0.0061(12) C21 0.057(2) 0.0348(16) 0.0237(16) 0.0058(12) 0.0248(14) 0.0004(14) C22 0.0140(12) 0.0142(12) 0.0181(13) 0.0007(10) 0.0085(10) -0.0025(10) C23 0.0150(12) 0.0158(12) 0.0256(14) 0.0040(10) 0.0068(10) -0.0029(10) C24 0.0210(13) 0.0166(13) 0.0382(17) 0.0065(12) 0.0103(12) 0.0058(11) C25 0.0288(15) 0.0200(14) 0.0372(17) -0.0037(12) 0.0188(13) 0.0044(12) C26 0.0292(14) 0.0207(13) 0.0226(14) -0.0020(11) 0.0149(12) -0.0008(11) C27 0.0188(13) 0.0177(12) 0.0193(13) 0.0015(10) 0.0101(10) -0.0004(10) C28 0.0245(14) 0.0218(13) 0.0278(15) 0.0064(11) 0.0010(11) 0.0024(11) C29 0.0329(15) 0.0291(14) 0.0112(13) 0.0031(11) 0.0092(11) 0.0077(13) _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 N2 1.7526(19) . ? Mo1 N3 1.7544(19) . ? Mo1 N1 2.0193(18) . ? Mo1 Cl1 2.3823(8) . ? Mo1 S1 2.7366(7) . ? S1 C2 1.773(2) . ? S1 C7 1.869(3) . ? Si1 N1 1.7734(19) . ? Si1 C13 1.861(3) . ? Si1 C12 1.862(3) . ? Si1 C11 1.874(3) . ? N1 C1 1.414(3) . ? C1 C2 1.402(3) . ? C1 C6 1.407(3) . ? C2 C3 1.394(3) . ? N2 C14 1.393(3) . ? N3 C22 1.393(3) . ? C3 C4 1.377(4) . ? C4 C5 1.389(4) . ? C5 C6 1.375(4) . ? C7 C10 1.517(4) . ? C7 C8 1.520(4) . ? C7 C9 1.523(4) . ? C14 C15 1.410(4) . ? C14 C19 1.415(3) . ? C15 C16 1.386(3) . ? C15 C20 1.503(3) . ? C16 C17 1.384(4) . ? C17 C18 1.378(4) . ? C18 C19 1.391(4) . ? C19 C21 1.501(4) . ? C22 C23 1.407(3) . ? C22 C27 1.410(3) . ? C23 C24 1.391(4) . ? C23 C28 1.501(4) . ? C24 C25 1.381(4) . ? C25 C26 1.386(4) . ? C26 C27 1.386(3) . ? C27 C29 1.503(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 N2 Mo1 N3 107.16(9) . . ? N2 Mo1 N1 101.24(8) . . ? N3 Mo1 N1 105.68(8) . . ? N2 Mo1 Cl1 94.37(6) . . ? N3 Mo1 Cl1 107.36(7) . . ? N1 Mo1 Cl1 137.11(5) . . ? N2 Mo1 S1 166.98(6) . . ? N3 Mo1 S1 85.74(7) . . ? N1 Mo1 S1 76.30(6) . . ? Cl1 Mo1 S1 79.67(2) . . ? C2 S1 C7 103.90(12) . . ? C2 S1 Mo1 89.99(8) . . ? C7 S1 Mo1 117.17(9) . . ? N1 Si1 C13 111.39(11) . . ? N1 Si1 C12 109.70(11) . . ? C13 Si1 C12 109.54(13) . . ? N1 Si1 C11 109.66(11) . . ? C13 Si1 C11 110.62(13) . . ? C12 Si1 C11 105.79(13) . . ? C1 N1 Si1 119.73(15) . . ? C1 N1 Mo1 116.55(14) . . ? Si1 N1 Mo1 123.62(10) . . ? C2 C1 C6 117.4(2) . . ? C2 C1 N1 121.0(2) . . ? C6 C1 N1 121.6(2) . . ? C3 C2 C1 121.2(2) . . ? C3 C2 S1 120.4(2) . . ? C1 C2 S1 118.30(17) . . ? C14 N2 Mo1 168.31(17) . . ? C22 N3 Mo1 153.56(16) . . ? C4 C3 C2 120.2(3) . . ? C3 C4 C5 119.3(2) . . ? C6 C5 C4 121.0(3) . . ? C5 C6 C1 120.9(3) . . ? C10 C7 C8 111.4(3) . . ? C10 C7 C9 110.2(2) . . ? C8 C7 C9 110.2(3) . . ? C10 C7 S1 108.7(2) . . ? C8 C7 S1 110.77(18) . . ? C9 C7 S1 105.43(19) . . ? N2 C14 C15 119.5(2) . . ? N2 C14 C19 119.5(2) . . ? C15 C14 C19 121.0(2) . . ? C16 C15 C14 118.6(2) . . ? C16 C15 C20 120.2(2) . . ? C14 C15 C20 121.1(2) . . ? C17 C16 C15 121.0(3) . . ? C18 C17 C16 119.8(2) . . ? C17 C18 C19 122.0(3) . . ? C18 C19 C14 117.5(2) . . ? C18 C19 C21 120.8(2) . . ? C14 C19 C21 121.6(2) . . ? N3 C22 C23 119.2(2) . . ? N3 C22 C27 119.0(2) . . ? C23 C22 C27 121.8(2) . . ? C24 C23 C22 117.8(2) . . ? C24 C23 C28 121.5(2) . . ? C22 C23 C28 120.7(2) . . ? C25 C24 C23 121.0(2) . . ? C24 C25 C26 120.3(2) . . ? C25 C26 C27 121.2(2) . . ? C26 C27 C22 117.7(2) . . ? C26 C27 C29 121.8(2) . . ? C22 C27 C29 120.5(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 N2 Mo1 S1 C2 -109.5(3) . . . . ? N3 Mo1 S1 C2 78.36(10) . . . . ? N1 Mo1 S1 C2 -28.92(9) . . . . ? Cl1 Mo1 S1 C2 -173.11(8) . . . . ? N2 Mo1 S1 C7 -3.9(3) . . . . ? N3 Mo1 S1 C7 -175.98(12) . . . . ? N1 Mo1 S1 C7 76.73(11) . . . . ? Cl1 Mo1 S1 C7 -67.46(10) . . . . ? C13 Si1 N1 C1 94.02(19) . . . . ? C12 Si1 N1 C1 -144.54(17) . . . . ? C11 Si1 N1 C1 -28.77(19) . . . . ? C13 Si1 N1 Mo1 -82.31(15) . . . . ? C12 Si1 N1 Mo1 39.13(15) . . . . ? C11 Si1 N1 Mo1 154.91(13) . . . . ? N2 Mo1 N1 C1 -153.98(15) . . . . ? N3 Mo1 N1 C1 -42.38(17) . . . . ? Cl1 Mo1 N1 C1 96.87(15) . . . . ? S1 Mo1 N1 C1 39.12(14) . . . . ? N2 Mo1 N1 Si1 22.45(13) . . . . ? N3 Mo1 N1 Si1 134.06(12) . . . . ? Cl1 Mo1 N1 Si1 -86.70(13) . . . . ? S1 Mo1 N1 Si1 -144.45(12) . . . . ? Si1 N1 C1 C2 142.96(18) . . . . ? Mo1 N1 C1 C2 -40.5(3) . . . . ? Si1 N1 C1 C6 -39.2(3) . . . . ? Mo1 N1 C1 C6 137.40(18) . . . . ? C6 C1 C2 C3 2.5(3) . . . . ? N1 C1 C2 C3 -179.5(2) . . . . ? C6 C1 C2 S1 -173.61(17) . . . . ? N1 C1 C2 S1 4.3(3) . . . . ? C7 S1 C2 C3 86.4(2) . . . . ? Mo1 S1 C2 C3 -155.51(19) . . . . ? C7 S1 C2 C1 -97.4(2) . . . . ? Mo1 S1 C2 C1 20.65(18) . . . . ? N3 Mo1 N2 C14 33.4(9) . . . . ? N1 Mo1 N2 C14 143.9(8) . . . . ? Cl1 Mo1 N2 C14 -76.3(8) . . . . ? S1 Mo1 N2 C14 -138.4(7) . . . . ? N2 Mo1 N3 C22 -4.3(4) . . . . ? N1 Mo1 N3 C22 -111.7(4) . . . . ? Cl1 Mo1 N3 C22 96.1(4) . . . . ? S1 Mo1 N3 C22 173.8(4) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? S1 C2 C3 C4 176.13(19) . . . . ? C2 C3 C4 C5 -2.3(4) . . . . ? C3 C4 C5 C6 1.8(4) . . . . ? C4 C5 C6 C1 0.9(4) . . . . ? C2 C1 C6 C5 -3.0(3) . . . . ? N1 C1 C6 C5 179.1(2) . . . . ? C2 S1 C7 C10 -57.7(2) . . . . ? Mo1 S1 C7 C10 -155.01(15) . . . . ? C2 S1 C7 C8 65.0(3) . . . . ? Mo1 S1 C7 C8 -32.3(3) . . . . ? C2 S1 C7 C9 -175.88(19) . . . . ? Mo1 S1 C7 C9 86.84(19) . . . . ? Mo1 N2 C14 C15 -67.4(9) . . . . ? Mo1 N2 C14 C19 111.3(8) . . . . ? N2 C14 C15 C16 -179.4(2) . . . . ? C19 C14 C15 C16 2.0(3) . . . . ? N2 C14 C15 C20 3.5(3) . . . . ? C19 C14 C15 C20 -175.1(2) . . . . ? C14 C15 C16 C17 -2.4(4) . . . . ? C20 C15 C16 C17 174.7(2) . . . . ? C15 C16 C17 C18 1.2(4) . . . . ? C16 C17 C18 C19 0.6(4) . . . . ? C17 C18 C19 C14 -1.0(4) . . . . ? C17 C18 C19 C21 -179.2(3) . . . . ? N2 C14 C19 C18 -178.9(2) . . . . ? C15 C14 C19 C18 -0.3(4) . . . . ? N2 C14 C19 C21 -0.7(4) . . . . ? C15 C14 C19 C21 177.9(2) . . . . ? Mo1 N3 C22 C23 -76.4(4) . . . . ? Mo1 N3 C22 C27 104.2(4) . . . . ? N3 C22 C23 C24 179.3(2) . . . . ? C27 C22 C23 C24 -1.3(3) . . . . ? N3 C22 C23 C28 -1.7(3) . . . . ? C27 C22 C23 C28 177.7(2) . . . . ? C22 C23 C24 C25 0.7(4) . . . . ? C28 C23 C24 C25 -178.3(2) . . . . ? C23 C24 C25 C26 0.1(4) . . . . ? C24 C25 C26 C27 -0.3(4) . . . . ? C25 C26 C27 C22 -0.4(4) . . . . ? C25 C26 C27 C29 179.7(2) . . . . ? N3 C22 C27 C26 -179.5(2) . . . . ? C23 C22 C27 C26 1.1(3) . . . . ? N3 C22 C27 C29 0.5(3) . . . . ? C23 C22 C27 C29 -178.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 59.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.494 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.069 data_compound1 _database_code_depnum_ccdc_archive 'CCDC 286078' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H44 N2 O2 S2 Si2 W' _chemical_formula_weight 720.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -5.4734 5.5774 '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 9.610(2) _cell_length_b 12.010(2) _cell_length_c 13.775(3) _cell_angle_alpha 85.31(3) _cell_angle_beta 82.58(3) _cell_angle_gamma 88.53(3) _cell_volume 1571(1) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6273 _cell_measurement_theta_min 4.72 _cell_measurement_theta_max 58.69 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 8.975 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2125 _exptl_absorpt_correction_T_max 0.9156 _exptl_absorpt_process_details ? _exptl_special_details ; Intensities were measured with a SMART 6000 area detector ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'mirror system' _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 5.602 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14658 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 58.86 _reflns_number_total 4390 _reflns_number_gt 4241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Proteum (v 1.40, Bruker 2002)' _computing_cell_refinement 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_data_reduction 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (v 6.12)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+1.1737P] 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 4390 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0168 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0400 _refine_ls_wR_factor_gt 0.0396 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.004 _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 S1 S 0.18232(6) 0.58177(4) 0.74056(4) 0.01868(13) Uani 1 1 d . . . Si1 Si 0.29091(7) 0.82598(5) 0.46435(5) 0.01971(14) Uani 1 1 d . . . O1 O 0.38414(17) 0.91486(13) 0.66629(12) 0.0229(4) Uani 1 1 d . . . N1 N 0.22108(19) 0.76510(15) 0.58174(14) 0.0186(4) Uani 1 1 d . . . C1 C 0.0856(2) 0.71875(18) 0.59577(17) 0.0182(5) Uani 1 1 d . . . W1 W 0.331722(10) 0.779187(8) 0.696640(7) 0.01789(5) Uani 1 1 d . . . S2 S 0.07204(6) 0.85714(4) 0.77636(4) 0.01878(13) Uani 1 1 d . . . O2 O 0.48094(16) 0.69993(13) 0.66654(12) 0.0239(4) Uani 1 1 d . . . C2 C 0.0525(2) 0.62870(19) 0.66631(17) 0.0180(5) Uani 1 1 d . . . N2 N 0.3315(2) 0.76036(16) 0.84627(14) 0.0220(4) Uani 1 1 d . . . Si2 Si 0.49469(7) 0.76648(6) 0.89226(5) 0.02804(16) Uani 1 1 d . . . C3 C -0.0822(2) 0.5852(2) 0.68407(18) 0.0224(5) Uani 1 1 d . . . H3A H -0.1019 0.5246 0.7323 0.027 Uiso 1 1 calc R . . C4 C -0.1873(3) 0.6292(2) 0.63251(19) 0.0260(6) Uani 1 1 d . . . H4A H -0.2788 0.5988 0.6440 0.031 Uiso 1 1 calc R . . C5 C -0.1567(3) 0.7188(2) 0.56357(18) 0.0244(5) Uani 1 1 d . . . H5A H -0.2286 0.7508 0.5284 0.029 Uiso 1 1 calc R . . C6 C -0.0234(2) 0.7623(2) 0.54518(17) 0.0211(5) Uani 1 1 d . . . H6A H -0.0053 0.8233 0.4971 0.025 Uiso 1 1 calc R . . C7 C 0.2760(3) 0.46639(19) 0.67469(18) 0.0230(5) Uani 1 1 d . . . C8 C 0.1741(3) 0.3694(2) 0.68244(19) 0.0281(6) Uani 1 1 d . . . H8A H 0.2224 0.3048 0.6535 0.042 Uiso 1 1 calc R . . H8B H 0.0944 0.3918 0.6471 0.042 Uiso 1 1 calc R . . H8C H 0.1402 0.3493 0.7517 0.042 Uiso 1 1 calc R . . C9 C 0.3989(3) 0.4350(2) 0.7321(2) 0.0320(6) Uani 1 1 d . . . H9A H 0.4498 0.3705 0.7049 0.048 Uiso 1 1 calc R . . H9B H 0.3634 0.4160 0.8013 0.048 Uiso 1 1 calc R . . H9C H 0.4625 0.4983 0.7270 0.048 Uiso 1 1 calc R . . C10 C 0.3240(3) 0.5023(2) 0.56764(19) 0.0276(6) Uani 1 1 d . . . H10A H 0.3703 0.4391 0.5353 0.041 Uiso 1 1 calc R . . H10B H 0.3902 0.5638 0.5635 0.041 Uiso 1 1 calc R . . H10C H 0.2426 0.5272 0.5350 0.041 Uiso 1 1 calc R . . C11 C 0.2342(3) 0.9750(2) 0.44699(19) 0.0262(6) Uani 1 1 d . . . H11A H 0.2676 1.0173 0.4972 0.039 Uiso 1 1 calc R . . H11B H 0.1316 0.9798 0.4530 0.039 Uiso 1 1 calc R . . H11C H 0.2738 1.0065 0.3817 0.039 Uiso 1 1 calc R . . C12 C 0.2375(3) 0.7425(2) 0.36681(18) 0.0275(6) Uani 1 1 d . . . H12A H 0.2672 0.6644 0.3785 0.041 Uiso 1 1 calc R . . H12B H 0.2820 0.7727 0.3024 0.041 Uiso 1 1 calc R . . H12C H 0.1352 0.7466 0.3685 0.041 Uiso 1 1 calc R . . C13 C 0.4859(3) 0.8219(2) 0.45210(19) 0.0261(6) Uani 1 1 d . . . H13A H 0.5180 0.8677 0.5003 0.039 Uiso 1 1 calc R . . H13B H 0.5240 0.8512 0.3858 0.039 Uiso 1 1 calc R . . H13C H 0.5187 0.7446 0.4638 0.039 Uiso 1 1 calc R . . C14 C 0.2088(3) 0.7333(2) 0.91005(18) 0.0219(5) Uani 1 1 d . . . C15 C 0.0777(3) 0.77531(19) 0.88863(17) 0.0210(5) Uani 1 1 d . . . C16 C -0.0467(3) 0.7430(2) 0.94645(18) 0.0248(5) Uani 1 1 d . . . H16A H -0.1340 0.7722 0.9296 0.030 Uiso 1 1 calc R . . C17 C -0.0433(3) 0.6687(2) 1.02819(19) 0.0313(6) Uani 1 1 d . . . H17A H -0.1277 0.6470 1.0682 0.038 Uiso 1 1 calc R . . C18 C 0.0848(3) 0.6265(2) 1.05082(19) 0.0335(6) Uani 1 1 d . . . H18A H 0.0878 0.5754 1.1069 0.040 Uiso 1 1 calc R . . C19 C 0.2083(3) 0.6574(2) 0.99339(18) 0.0281(6) Uani 1 1 d . . . H19A H 0.2948 0.6267 1.0105 0.034 Uiso 1 1 calc R . . C20 C 0.0829(3) 1.00568(19) 0.80545(18) 0.0235(5) Uani 1 1 d . . . C21 C 0.0936(3) 1.0710(2) 0.7051(2) 0.0307(6) Uani 1 1 d . . . H21A H 0.0852 1.1512 0.7138 0.046 Uiso 1 1 calc R . . H21B H 0.0179 1.0489 0.6697 0.046 Uiso 1 1 calc R . . H21C H 0.1844 1.0550 0.6674 0.046 Uiso 1 1 calc R . . C22 C 0.2097(3) 1.0252(2) 0.85771(19) 0.0282(6) Uani 1 1 d . . . H22A H 0.2089 1.1031 0.8743 0.042 Uiso 1 1 calc R . . H22B H 0.2961 1.0098 0.8144 0.042 Uiso 1 1 calc R . . H22C H 0.2057 0.9754 0.9180 0.042 Uiso 1 1 calc R . . C23 C -0.0541(3) 1.0336(2) 0.8681(2) 0.0296(6) Uani 1 1 d . . . H23A H -0.0522 1.1110 0.8856 0.044 Uiso 1 1 calc R . . H23B H -0.0652 0.9831 0.9281 0.044 Uiso 1 1 calc R . . H23C H -0.1329 1.0246 0.8310 0.044 Uiso 1 1 calc R . . C24 C 0.6113(3) 0.8651(2) 0.8104(2) 0.0373(7) Uani 1 1 d . . . H24A H 0.6367 0.8342 0.7467 0.056 Uiso 1 1 calc R . . H24B H 0.6965 0.8761 0.8404 0.056 Uiso 1 1 calc R . . H24C H 0.5622 0.9369 0.8010 0.056 Uiso 1 1 calc R . . C25 C 0.5836(3) 0.6262(2) 0.8984(2) 0.0360(7) Uani 1 1 d . . . H25A H 0.6047 0.6012 0.8321 0.054 Uiso 1 1 calc R . . H25B H 0.5217 0.5725 0.9393 0.054 Uiso 1 1 calc R . . H25C H 0.6711 0.6314 0.9272 0.054 Uiso 1 1 calc R . . C26 C 0.4667(3) 0.8215(3) 1.0165(2) 0.0456(8) Uani 1 1 d . . . H26A H 0.4106 0.8907 1.0137 0.068 Uiso 1 1 calc R . . H26B H 0.5577 0.8368 1.0371 0.068 Uiso 1 1 calc R . . H26C H 0.4172 0.7660 1.0637 0.068 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 S1 0.0178(3) 0.0149(3) 0.0227(3) 0.0009(2) -0.0014(2) -0.0011(2) Si1 0.0196(3) 0.0175(3) 0.0209(3) 0.0020(3) -0.0002(3) -0.0005(3) O1 0.0216(9) 0.0205(9) 0.0267(9) 0.0016(7) -0.0047(7) -0.0026(7) N1 0.0173(10) 0.0152(9) 0.0221(10) 0.0008(8) 0.0005(8) -0.0022(8) C1 0.0176(12) 0.0155(11) 0.0211(12) -0.0056(10) 0.0018(10) 0.0012(9) W1 0.01502(7) 0.01558(7) 0.02255(7) 0.00315(5) -0.00297(5) -0.00221(4) S2 0.0195(3) 0.0159(3) 0.0212(3) -0.0007(2) -0.0035(2) -0.0018(2) O2 0.0176(9) 0.0212(8) 0.0319(9) 0.0048(7) -0.0036(7) -0.0021(7) C2 0.0160(12) 0.0172(12) 0.0210(12) -0.0035(10) -0.0015(10) -0.0006(9) N2 0.0202(11) 0.0210(10) 0.0248(11) 0.0033(9) -0.0051(9) -0.0044(8) Si2 0.0237(4) 0.0287(4) 0.0327(4) 0.0080(3) -0.0127(3) -0.0072(3) C3 0.0202(13) 0.0211(12) 0.0244(13) -0.0009(10) 0.0025(10) -0.0041(10) C4 0.0163(13) 0.0308(14) 0.0311(14) -0.0042(12) -0.0014(11) -0.0048(10) C5 0.0190(13) 0.0283(13) 0.0270(13) -0.0052(11) -0.0059(10) 0.0029(10) C6 0.0233(13) 0.0193(12) 0.0204(12) -0.0015(10) -0.0023(10) 0.0018(10) C7 0.0217(13) 0.0145(11) 0.0315(14) -0.0013(10) 0.0007(11) 0.0010(10) C8 0.0330(15) 0.0179(12) 0.0311(14) -0.0032(11) 0.0051(12) -0.0028(11) C9 0.0270(14) 0.0230(13) 0.0447(16) 0.0008(12) -0.0038(12) 0.0052(11) C10 0.0256(14) 0.0207(13) 0.0336(14) -0.0022(11) 0.0073(11) -0.0005(10) C11 0.0276(14) 0.0217(13) 0.0274(13) 0.0046(11) -0.0007(11) 0.0003(11) C12 0.0280(14) 0.0281(14) 0.0249(13) -0.0014(11) 0.0011(11) 0.0003(11) C13 0.0246(13) 0.0239(13) 0.0277(13) 0.0035(11) 0.0015(11) -0.0020(10) C14 0.0237(13) 0.0194(12) 0.0235(13) -0.0013(10) -0.0058(10) -0.0052(10) C15 0.0257(13) 0.0189(12) 0.0181(12) -0.0001(10) -0.0026(10) -0.0032(10) C16 0.0243(13) 0.0242(13) 0.0260(13) -0.0040(11) -0.0018(11) -0.0028(10) C17 0.0296(15) 0.0350(15) 0.0272(14) 0.0014(12) 0.0034(11) -0.0091(12) C18 0.0416(17) 0.0345(15) 0.0228(14) 0.0098(12) -0.0042(12) -0.0061(13) C19 0.0298(15) 0.0276(14) 0.0270(14) 0.0058(11) -0.0083(11) -0.0015(11) C20 0.0276(14) 0.0164(12) 0.0282(13) -0.0051(10) -0.0071(11) -0.0029(10) C21 0.0367(15) 0.0196(13) 0.0357(15) 0.0031(11) -0.0066(12) -0.0027(11) C22 0.0297(14) 0.0241(13) 0.0328(14) -0.0079(11) -0.0070(11) -0.0049(11) C23 0.0294(14) 0.0240(13) 0.0370(15) -0.0102(12) -0.0050(12) 0.0006(11) C24 0.0278(15) 0.0357(15) 0.0501(17) 0.0140(14) -0.0200(13) -0.0130(12) C25 0.0234(14) 0.0389(16) 0.0447(17) 0.0158(13) -0.0111(12) -0.0062(12) C26 0.0482(19) 0.0489(18) 0.0444(18) 0.0006(15) -0.0240(15) -0.0118(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C2 1.766(2) . ? S1 C7 1.867(2) . ? S1 W1 2.7865(10) . ? Si1 N1 1.775(2) . ? Si1 C13 1.860(3) . ? Si1 C11 1.864(2) . ? Si1 C12 1.871(3) . ? O1 W1 1.7204(16) . ? N1 C1 1.413(3) . ? N1 W1 2.038(2) . ? C1 C6 1.400(3) . ? C1 C2 1.407(3) . ? W1 O2 1.7249(17) . ? W1 N2 2.055(2) . ? W1 S2 2.7660(10) . ? S2 C15 1.769(2) . ? S2 C20 1.869(2) . ? C2 C3 1.393(3) . ? N2 C14 1.405(3) . ? N2 Si2 1.771(2) . ? Si2 C24 1.858(3) . ? Si2 C26 1.869(3) . ? Si2 C25 1.870(3) . ? C3 C4 1.379(4) . ? C4 C5 1.387(4) . ? C5 C6 1.381(4) . ? C7 C10 1.518(4) . ? C7 C9 1.528(4) . ? C7 C8 1.529(3) . ? C14 C15 1.403(3) . ? C14 C19 1.406(3) . ? C15 C16 1.393(4) . ? C16 C17 1.382(4) . ? C17 C18 1.382(4) . ? C18 C19 1.380(4) . ? C20 C23 1.524(4) . ? C20 C21 1.525(4) . ? C20 C22 1.526(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 C2 S1 C7 104.35(11) . . ? C2 S1 W1 92.44(8) . . ? C7 S1 W1 110.09(8) . . ? N1 Si1 C13 109.82(11) . . ? N1 Si1 C11 111.14(11) . . ? C13 Si1 C11 107.67(12) . . ? N1 Si1 C12 109.55(11) . . ? C13 Si1 C12 107.20(12) . . ? C11 Si1 C12 111.37(12) . . ? C1 N1 Si1 119.99(16) . . ? C1 N1 W1 121.45(15) . . ? Si1 N1 W1 118.24(10) . . ? C6 C1 C2 116.7(2) . . ? C6 C1 N1 122.6(2) . . ? C2 C1 N1 120.6(2) . . ? O1 W1 O2 104.34(8) . . ? O1 W1 N1 97.33(8) . . ? O2 W1 N1 103.07(8) . . ? O1 W1 N2 103.37(8) . . ? O2 W1 N2 96.83(8) . . ? N1 W1 N2 146.65(8) . . ? O1 W1 S2 89.55(6) . . ? O2 W1 S2 165.07(5) . . ? N1 W1 S2 80.14(6) . . ? N2 W1 S2 74.23(6) . . ? O1 W1 S1 166.00(5) . . ? O2 W1 S1 88.60(6) . . ? N1 W1 S1 74.16(6) . . ? N2 W1 S1 79.93(6) . . ? S2 W1 S1 78.17(3) . . ? C15 S2 C20 105.99(11) . . ? C15 S2 W1 92.89(9) . . ? C20 S2 W1 110.55(9) . . ? C3 C2 C1 121.3(2) . . ? C3 C2 S1 120.67(18) . . ? C1 C2 S1 117.69(17) . . ? C14 N2 Si2 120.49(16) . . ? C14 N2 W1 121.50(15) . . ? Si2 N2 W1 117.76(11) . . ? N2 Si2 C24 109.50(11) . . ? N2 Si2 C26 109.52(13) . . ? C24 Si2 C26 107.50(15) . . ? N2 Si2 C25 111.33(12) . . ? C24 Si2 C25 108.53(14) . . ? C26 Si2 C25 110.37(14) . . ? C4 C3 C2 120.7(2) . . ? C3 C4 C5 118.6(2) . . ? C6 C5 C4 121.1(2) . . ? C5 C6 C1 121.5(2) . . ? C10 C7 C9 112.3(2) . . ? C10 C7 C8 110.2(2) . . ? C9 C7 C8 110.6(2) . . ? C10 C7 S1 111.95(16) . . ? C9 C7 S1 104.40(17) . . ? C8 C7 S1 107.25(16) . . ? C15 C14 N2 120.6(2) . . ? C15 C14 C19 116.5(2) . . ? N2 C14 C19 122.7(2) . . ? C16 C15 C14 121.8(2) . . ? C16 C15 S2 119.97(19) . . ? C14 C15 S2 117.71(18) . . ? C17 C16 C15 120.1(2) . . ? C16 C17 C18 119.0(2) . . ? C19 C18 C17 121.2(2) . . ? C18 C19 C14 121.3(2) . . ? C23 C20 C21 110.8(2) . . ? C23 C20 C22 111.5(2) . . ? C21 C20 C22 111.4(2) . . ? C23 C20 S2 106.89(17) . . ? C21 C20 S2 103.70(16) . . ? C22 C20 S2 112.19(17) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 58.86 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.420 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.058 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 286079' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H57 Mo N3 O S3 Si2' _chemical_formula_weight 796.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 '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 11.834(2) _cell_length_b 12.365(3) _cell_length_c 15.082(3) _cell_angle_alpha 78.65(3) _cell_angle_beta 76.75(3) _cell_angle_gamma 76.53(3) _cell_volume 2065(1) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8351 _cell_measurement_theta_min 3.72 _cell_measurement_theta_max 58.87 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 4.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7954 _exptl_absorpt_correction_T_max 0.9101 _exptl_absorpt_process_details ? _exptl_special_details ; Intensities were measured on a SMART 6000 area detector ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'mirror system' _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 5.602 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22428 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 58.87 _reflns_number_total 5702 _reflns_number_gt 5349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Proteum (v 1.40, Bruker 2002)' _computing_cell_refinement 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_data_reduction 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (v 6.12)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+1.1261P] 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 5702 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0513 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.261368(12) 0.683215(12) 0.762214(9) 0.01559(6) Uani 1 1 d . . . S1 S 0.24306(4) 0.98839(4) 0.83432(3) 0.02322(12) Uani 1 1 d . . . Si1 Si 0.45871(5) 0.77576(4) 0.57800(3) 0.02185(13) Uani 1 1 d . . . O1 O 0.40461(11) 0.70957(11) 0.67866(8) 0.0217(3) Uani 1 1 d . . . N1 N 0.22925(13) 0.73850(13) 0.86526(10) 0.0181(3) Uani 1 1 d . . . C1 C 0.4624(2) 0.6945(2) 0.48565(15) 0.0405(6) Uani 1 1 d . . . H1A H 0.3813 0.6945 0.4807 0.061 Uiso 1 1 calc R . . H1B H 0.5041 0.6169 0.5007 0.061 Uiso 1 1 calc R . . H1C H 0.5039 0.7292 0.4268 0.061 Uiso 1 1 calc R . . S2 S 0.09688(4) 0.82073(4) 0.51276(3) 0.02178(11) Uani 1 1 d . . . Si2 Si 0.15648(5) 0.47701(4) 0.72232(3) 0.01921(12) Uani 1 1 d . . . N2 N 0.14721(14) 0.75358(13) 0.70203(10) 0.0187(3) Uani 1 1 d . . . C2 C 0.61285(19) 0.7857(2) 0.57976(17) 0.0366(5) Uani 1 1 d . . . H2A H 0.6121 0.8247 0.6306 0.055 Uiso 1 1 calc R . . H2B H 0.6462 0.8278 0.5213 0.055 Uiso 1 1 calc R . . H2C H 0.6613 0.7099 0.5883 0.055 Uiso 1 1 calc R . . S3 S 0.43518(4) 0.53941(4) 0.86451(3) 0.01890(11) Uani 1 1 d . . . C3 C 0.36511(19) 0.91726(18) 0.55474(15) 0.0316(5) Uani 1 1 d . . . H3A H 0.2853 0.9094 0.5526 0.047 Uiso 1 1 calc R . . H3B H 0.3999 0.9568 0.4955 0.047 Uiso 1 1 calc R . . H3C H 0.3607 0.9604 0.6039 0.047 Uiso 1 1 calc R . . N3 N 0.21412(13) 0.53235(13) 0.79801(10) 0.0177(3) Uani 1 1 d . . . C4 C 0.18179(16) 0.79354(16) 0.94106(12) 0.0187(4) Uani 1 1 d . . . C5 C 0.18518(17) 0.90736(16) 0.93847(13) 0.0211(4) Uani 1 1 d . . . C6 C 0.13596(18) 0.95594(18) 1.01815(14) 0.0264(5) Uani 1 1 d . . . H6A H 0.1360 1.0330 1.0170 0.032 Uiso 1 1 calc R . . C7 C 0.08699(18) 0.89408(19) 1.09907(14) 0.0289(5) Uani 1 1 d . . . H7A H 0.0556 0.9282 1.1530 0.035 Uiso 1 1 calc R . . C8 C 0.08408(18) 0.78271(19) 1.10084(14) 0.0283(5) Uani 1 1 d . . . H8A H 0.0501 0.7404 1.1561 0.034 Uiso 1 1 calc R . . C9 C 0.13019(17) 0.73237(18) 1.02281(13) 0.0236(4) Uani 1 1 d . . . H9A H 0.1270 0.6559 1.0245 0.028 Uiso 1 1 calc R . . C10 C 0.39311(18) 0.99327(17) 0.84954(14) 0.0273(5) Uani 1 1 d . . . C11 C 0.4500(2) 1.04879(19) 0.75546(16) 0.0346(5) Uani 1 1 d . . . H11A H 0.5266 1.0634 0.7592 0.052 Uiso 1 1 calc R . . H11B H 0.3981 1.1200 0.7370 0.052 Uiso 1 1 calc R . . H11C H 0.4619 0.9986 0.7098 0.052 Uiso 1 1 calc R . . C12 C 0.3845(2) 1.0656(2) 0.92282(17) 0.0400(6) Uani 1 1 d . . . H12A H 0.4642 1.0726 0.9262 0.060 Uiso 1 1 calc R . . H12B H 0.3465 1.0303 0.9827 0.060 Uiso 1 1 calc R . . H12C H 0.3375 1.1405 0.9066 0.060 Uiso 1 1 calc R . . C13 C 0.4629(2) 0.87461(19) 0.87317(17) 0.0384(6) Uani 1 1 d . . . H13A H 0.5437 0.8783 0.8763 0.058 Uiso 1 1 calc R . . H13B H 0.4655 0.8300 0.8255 0.058 Uiso 1 1 calc R . . H13C H 0.4242 0.8393 0.9329 0.058 Uiso 1 1 calc R . . C14 C 0.03428(16) 0.81694(15) 0.69794(13) 0.0184(4) Uani 1 1 d . . . C15 C -0.00743(17) 0.84774(15) 0.61393(13) 0.0193(4) Uani 1 1 d . . . C16 C -0.12418(17) 0.90423(17) 0.61574(14) 0.0243(4) Uani 1 1 d . . . H16A H -0.1535 0.9252 0.5599 0.029 Uiso 1 1 calc R . . C17 C -0.19808(18) 0.93030(18) 0.69690(14) 0.0282(5) Uani 1 1 d . . . H17A H -0.2782 0.9665 0.6967 0.034 Uiso 1 1 calc R . . C18 C -0.15623(18) 0.90398(17) 0.77895(14) 0.0265(5) Uani 1 1 d . . . H18A H -0.2066 0.9240 0.8345 0.032 Uiso 1 1 calc R . . C19 C -0.04071(17) 0.84840(16) 0.77896(13) 0.0219(4) Uani 1 1 d . . . H19A H -0.0116 0.8312 0.8348 0.026 Uiso 1 1 calc R . . C20 C 0.02326(17) 0.77679(16) 0.43339(13) 0.0225(4) Uani 1 1 d . . . C21 C 0.12963(19) 0.72522(19) 0.36552(14) 0.0319(5) Uani 1 1 d . . . H21A H 0.1019 0.6988 0.3187 0.048 Uiso 1 1 calc R . . H21B H 0.1779 0.6617 0.3987 0.048 Uiso 1 1 calc R . . H21C H 0.1774 0.7821 0.3356 0.048 Uiso 1 1 calc R . . C22 C -0.04859(19) 0.68858(18) 0.48475(14) 0.0299(5) Uani 1 1 d . . . H22A H -0.0820 0.6622 0.4411 0.045 Uiso 1 1 calc R . . H22B H -0.1129 0.7216 0.5312 0.045 Uiso 1 1 calc R . . H22C H 0.0028 0.6250 0.5151 0.045 Uiso 1 1 calc R . . C23 C -0.05078(19) 0.87637(17) 0.38076(14) 0.0272(5) Uani 1 1 d . . . H23A H -0.0739 0.8510 0.3311 0.041 Uiso 1 1 calc R . . H23B H -0.0039 0.9348 0.3544 0.041 Uiso 1 1 calc R . . H23C H -0.1219 0.9071 0.4231 0.041 Uiso 1 1 calc R . . C24 C 0.22387(17) 0.47141(15) 0.88675(12) 0.0190(4) Uani 1 1 d . . . C25 C 0.32417(17) 0.46288(16) 0.92510(13) 0.0193(4) Uani 1 1 d . . . C26 C 0.33178(18) 0.40245(17) 1.01278(13) 0.0243(4) Uani 1 1 d . . . H26A H 0.4000 0.3973 1.0377 0.029 Uiso 1 1 calc R . . C27 C 0.24094(19) 0.34980(18) 1.06386(14) 0.0298(5) Uani 1 1 d . . . H27A H 0.2471 0.3078 1.1231 0.036 Uiso 1 1 calc R . . C28 C 0.14123(19) 0.35923(18) 1.02755(14) 0.0304(5) Uani 1 1 d . . . H28A H 0.0780 0.3244 1.0625 0.036 Uiso 1 1 calc R . . C29 C 0.13277(18) 0.41921(17) 0.94051(13) 0.0256(5) Uani 1 1 d . . . H29A H 0.0634 0.4249 0.9169 0.031 Uiso 1 1 calc R . . C30 C 0.55523(17) 0.43458(17) 0.80779(14) 0.0248(5) Uani 1 1 d . . . C31 C 0.65118(19) 0.5023(2) 0.76227(16) 0.0365(5) Uani 1 1 d . . . H31A H 0.7174 0.4552 0.7266 0.055 Uiso 1 1 calc R . . H31B H 0.6791 0.5272 0.8098 0.055 Uiso 1 1 calc R . . H31C H 0.6187 0.5681 0.7211 0.055 Uiso 1 1 calc R . . C32 C 0.5984(2) 0.33738(19) 0.87942(16) 0.0373(6) Uani 1 1 d . . . H32A H 0.6676 0.2873 0.8496 0.056 Uiso 1 1 calc R . . H32B H 0.5351 0.2953 0.9073 0.056 Uiso 1 1 calc R . . H32C H 0.6203 0.3671 0.9274 0.056 Uiso 1 1 calc R . . C33 C 0.5123(2) 0.3915(2) 0.73631(16) 0.0368(6) Uani 1 1 d . . . H33A H 0.5766 0.3367 0.7066 0.055 Uiso 1 1 calc R . . H33B H 0.4875 0.4546 0.6898 0.055 Uiso 1 1 calc R . . H33C H 0.4450 0.3552 0.7664 0.055 Uiso 1 1 calc R . . C34 C 0.19582(19) 0.31999(17) 0.74575(15) 0.0283(5) Uani 1 1 d . . . H34A H 0.1569 0.2934 0.8083 0.042 Uiso 1 1 calc R . . H34B H 0.2818 0.2961 0.7400 0.042 Uiso 1 1 calc R . . H34C H 0.1694 0.2882 0.7012 0.042 Uiso 1 1 calc R . . C35 C 0.23214(18) 0.51921(17) 0.60218(13) 0.0245(4) Uani 1 1 d . . . H35A H 0.2071 0.6004 0.5841 0.037 Uiso 1 1 calc R . . H35B H 0.2111 0.4787 0.5605 0.037 Uiso 1 1 calc R . . H35C H 0.3181 0.5008 0.5986 0.037 Uiso 1 1 calc R . . C36 C -0.00699(18) 0.52566(17) 0.73310(14) 0.0255(5) Uani 1 1 d . . . H36A H -0.0260 0.6081 0.7218 0.038 Uiso 1 1 calc R . . H36B H -0.0466 0.4986 0.7953 0.038 Uiso 1 1 calc R . . H36C H -0.0342 0.4959 0.6879 0.038 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 Mo1 0.01646(10) 0.01615(10) 0.01520(9) -0.00302(6) -0.00401(6) -0.00373(6) S1 0.0243(3) 0.0218(3) 0.0238(2) -0.0025(2) -0.0066(2) -0.0039(2) Si1 0.0204(3) 0.0239(3) 0.0209(3) -0.0024(2) -0.0013(2) -0.0070(2) O1 0.0202(7) 0.0240(8) 0.0209(7) -0.0026(6) -0.0037(6) -0.0051(5) N1 0.0187(9) 0.0175(9) 0.0188(8) -0.0019(7) -0.0052(7) -0.0039(6) C1 0.0482(15) 0.0466(15) 0.0272(12) -0.0116(11) 0.0062(11) -0.0185(12) S2 0.0197(3) 0.0286(3) 0.0187(2) -0.0054(2) -0.0058(2) -0.0044(2) Si2 0.0207(3) 0.0182(3) 0.0217(3) -0.0032(2) -0.0086(2) -0.0050(2) N2 0.0227(9) 0.0168(9) 0.0180(8) -0.0021(7) -0.0045(7) -0.0064(7) C2 0.0236(12) 0.0357(14) 0.0460(14) 0.0047(11) -0.0037(10) -0.0093(10) S3 0.0173(2) 0.0216(3) 0.0191(2) -0.00469(19) -0.00575(19) -0.00296(18) C3 0.0290(12) 0.0303(13) 0.0361(12) 0.0019(10) -0.0095(10) -0.0093(9) N3 0.0189(8) 0.0168(9) 0.0182(8) -0.0016(7) -0.0067(7) -0.0030(6) C4 0.0153(10) 0.0247(11) 0.0177(9) -0.0054(8) -0.0075(8) -0.0014(8) C5 0.0185(10) 0.0252(12) 0.0211(10) -0.0048(8) -0.0073(8) -0.0027(8) C6 0.0251(11) 0.0276(12) 0.0302(11) -0.0134(9) -0.0080(9) -0.0023(9) C7 0.0250(12) 0.0413(14) 0.0223(11) -0.0144(10) -0.0027(9) -0.0041(9) C8 0.0251(12) 0.0424(14) 0.0187(10) -0.0045(9) -0.0031(9) -0.0105(9) C9 0.0221(11) 0.0290(12) 0.0223(10) -0.0047(9) -0.0056(9) -0.0079(8) C10 0.0233(11) 0.0254(12) 0.0339(11) -0.0035(9) -0.0073(9) -0.0050(9) C11 0.0282(12) 0.0288(13) 0.0426(13) -0.0032(10) -0.0008(10) -0.0050(9) C12 0.0353(14) 0.0475(15) 0.0459(14) -0.0161(12) -0.0109(11) -0.0150(11) C13 0.0262(12) 0.0324(14) 0.0543(15) 0.0032(11) -0.0132(11) -0.0039(10) C14 0.0208(11) 0.0130(10) 0.0233(10) -0.0011(8) -0.0073(8) -0.0053(8) C15 0.0209(11) 0.0165(11) 0.0219(10) -0.0029(8) -0.0051(8) -0.0057(8) C16 0.0242(11) 0.0254(12) 0.0257(11) -0.0056(9) -0.0094(9) -0.0037(9) C17 0.0205(11) 0.0299(12) 0.0352(12) -0.0103(10) -0.0061(9) -0.0016(9) C18 0.0243(12) 0.0290(12) 0.0258(11) -0.0097(9) 0.0006(9) -0.0054(9) C19 0.0264(11) 0.0202(11) 0.0201(10) -0.0019(8) -0.0052(9) -0.0064(8) C20 0.0261(11) 0.0241(11) 0.0200(10) -0.0058(8) -0.0086(8) -0.0043(8) C21 0.0337(13) 0.0383(14) 0.0242(11) -0.0112(10) -0.0069(10) -0.0011(10) C22 0.0354(13) 0.0304(13) 0.0291(11) -0.0058(9) -0.0123(10) -0.0099(10) C23 0.0317(12) 0.0281(12) 0.0242(11) -0.0037(9) -0.0133(9) -0.0027(9) C24 0.0234(11) 0.0155(10) 0.0188(9) -0.0036(8) -0.0069(8) -0.0014(8) C25 0.0211(11) 0.0173(11) 0.0202(10) -0.0043(8) -0.0055(8) -0.0026(8) C26 0.0275(11) 0.0248(12) 0.0230(10) -0.0027(9) -0.0122(9) -0.0033(9) C27 0.0384(13) 0.0296(13) 0.0214(10) 0.0045(9) -0.0097(10) -0.0096(10) C28 0.0315(13) 0.0333(13) 0.0267(11) 0.0041(9) -0.0050(10) -0.0148(10) C29 0.0257(12) 0.0289(12) 0.0249(10) 0.0004(9) -0.0098(9) -0.0098(9) C30 0.0197(11) 0.0287(12) 0.0267(10) -0.0111(9) -0.0068(9) 0.0020(8) C31 0.0239(12) 0.0471(15) 0.0388(13) -0.0163(11) 0.0004(10) -0.0058(10) C32 0.0312(13) 0.0359(14) 0.0407(13) -0.0102(11) -0.0114(11) 0.0097(10) C33 0.0290(13) 0.0445(14) 0.0417(13) -0.0261(11) -0.0108(11) 0.0035(10) C34 0.0319(12) 0.0238(12) 0.0341(12) -0.0045(9) -0.0149(10) -0.0068(9) C35 0.0272(12) 0.0240(12) 0.0253(10) -0.0082(9) -0.0086(9) -0.0037(8) C36 0.0260(11) 0.0243(12) 0.0295(11) -0.0026(9) -0.0111(9) -0.0069(9) _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 N1 1.7474(15) . ? Mo1 N2 1.7634(16) . ? Mo1 O1 1.9195(14) . ? Mo1 N3 2.0088(16) . ? Mo1 S3 2.9058(11) . ? S1 C5 1.774(2) . ? S1 C10 1.858(2) . ? Si1 O1 1.6413(14) . ? Si1 C3 1.856(2) . ? Si1 C1 1.859(2) . ? Si1 C2 1.863(2) . ? N1 C4 1.385(2) . ? S2 C15 1.763(2) . ? S2 C20 1.8553(19) . ? Si2 N3 1.7660(15) . ? Si2 C35 1.860(2) . ? Si2 C36 1.866(2) . ? Si2 C34 1.870(2) . ? N2 C14 1.391(2) . ? S3 C25 1.773(2) . ? S3 C30 1.858(2) . ? N3 C24 1.416(2) . ? C4 C9 1.403(3) . ? C4 C5 1.410(3) . ? C5 C6 1.394(3) . ? C6 C7 1.387(3) . ? C7 C8 1.380(3) . ? C8 C9 1.381(3) . ? C10 C13 1.525(3) . ? C10 C12 1.526(3) . ? C10 C11 1.527(3) . ? C14 C19 1.400(3) . ? C14 C15 1.415(3) . ? C15 C16 1.392(3) . ? C16 C17 1.378(3) . ? C17 C18 1.389(3) . ? C18 C19 1.380(3) . ? C20 C22 1.520(3) . ? C20 C21 1.527(3) . ? C20 C23 1.531(3) . ? C24 C29 1.398(3) . ? C24 C25 1.409(3) . ? C25 C26 1.396(3) . ? C26 C27 1.386(3) . ? C27 C28 1.383(3) . ? C28 C29 1.388(3) . ? C30 C33 1.520(3) . ? C30 C31 1.524(3) . ? C30 C32 1.526(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 N1 Mo1 N2 106.07(7) . . ? N1 Mo1 O1 116.47(7) . . ? N2 Mo1 O1 104.69(7) . . ? N1 Mo1 N3 104.71(7) . . ? N2 Mo1 N3 98.27(7) . . ? O1 Mo1 N3 123.83(6) . . ? N1 Mo1 S3 76.94(6) . . ? N2 Mo1 S3 171.95(5) . . ? O1 Mo1 S3 80.06(5) . . ? N3 Mo1 S3 73.69(5) . . ? C5 S1 C10 103.39(9) . . ? O1 Si1 C3 110.36(9) . . ? O1 Si1 C1 109.83(9) . . ? C3 Si1 C1 108.62(11) . . ? O1 Si1 C2 107.72(9) . . ? C3 Si1 C2 111.29(11) . . ? C1 Si1 C2 108.99(12) . . ? Si1 O1 Mo1 144.40(8) . . ? C4 N1 Mo1 168.00(13) . . ? C15 S2 C20 108.76(9) . . ? N3 Si2 C35 108.66(8) . . ? N3 Si2 C36 112.45(9) . . ? C35 Si2 C36 109.94(10) . . ? N3 Si2 C34 108.60(8) . . ? C35 Si2 C34 106.32(10) . . ? C36 Si2 C34 110.65(10) . . ? C14 N2 Mo1 152.34(13) . . ? C25 S3 C30 105.08(9) . . ? C25 S3 Mo1 88.22(7) . . ? C30 S3 Mo1 120.04(7) . . ? C24 N3 Si2 119.73(12) . . ? C24 N3 Mo1 119.09(12) . . ? Si2 N3 Mo1 121.16(8) . . ? N1 C4 C9 118.12(17) . . ? N1 C4 C5 122.16(17) . . ? C9 C4 C5 119.71(17) . . ? C6 C5 C4 118.37(18) . . ? C6 C5 S1 121.03(16) . . ? C4 C5 S1 120.50(14) . . ? C7 C6 C5 121.4(2) . . ? C8 C7 C6 119.74(19) . . ? C7 C8 C9 120.43(19) . . ? C8 C9 C4 120.32(19) . . ? C13 C10 C12 111.46(19) . . ? C13 C10 C11 110.37(18) . . ? C12 C10 C11 109.95(18) . . ? C13 C10 S1 110.45(15) . . ? C12 C10 S1 110.54(15) . . ? C11 C10 S1 103.81(14) . . ? N2 C14 C19 119.33(16) . . ? N2 C14 C15 121.30(17) . . ? C19 C14 C15 119.35(17) . . ? C16 C15 C14 118.37(18) . . ? C16 C15 S2 124.57(15) . . ? C14 C15 S2 116.86(14) . . ? C17 C16 C15 121.33(18) . . ? C16 C17 C18 120.48(19) . . ? C19 C18 C17 119.31(19) . . ? C18 C19 C14 121.05(18) . . ? C22 C20 C21 110.58(17) . . ? C22 C20 C23 112.13(17) . . ? C21 C20 C23 108.87(16) . . ? C22 C20 S2 110.50(13) . . ? C21 C20 S2 101.48(13) . . ? C23 C20 S2 112.76(14) . . ? C29 C24 C25 117.42(17) . . ? C29 C24 N3 120.99(17) . . ? C25 C24 N3 121.58(17) . . ? C26 C25 C24 120.57(18) . . ? C26 C25 S3 120.21(15) . . ? C24 C25 S3 119.01(14) . . ? C27 C26 C25 120.73(18) . . ? C28 C27 C26 119.18(19) . . ? C27 C28 C29 120.52(19) . . ? C28 C29 C24 121.56(18) . . ? C33 C30 C31 111.01(18) . . ? C33 C30 C32 110.58(18) . . ? C31 C30 C32 111.32(18) . . ? C33 C30 S3 110.35(14) . . ? C31 C30 S3 103.01(14) . . ? C32 C30 S3 110.35(14) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 58.87 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.287 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.043 #=========================================================================== data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 292971' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H44 Mo N2 O2 S2 Si2' _chemical_formula_weight 632.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 '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 9.622(3) _cell_length_b 12.052(3) _cell_length_c 13.693(4) _cell_angle_alpha 85.060(10) _cell_angle_beta 82.800(10) _cell_angle_gamma 88.44(3) _cell_volume 1569.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14610 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 58.92 _exptl_crystal_description block _exptl_crystal_colour 'reddish brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 5.582 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4015 _exptl_absorpt_correction_T_max 0.6052 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'mirror system' _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 5.602 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14417 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 58.92 _reflns_number_total 4334 _reflns_number_gt 3684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Proteum (v 1.40, Bruker 2002)' _computing_cell_refinement 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_data_reduction 'Bruker AXS SAINT (v 7.01A, Bruker 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (v 6.12)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.5849P] 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 4334 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Mo1 Mo 0.16700(2) 0.219594(18) 0.303400(17) 0.01994(9) Uani 1 1 d . . . Si1 Si 0.20915(8) 0.17419(6) 0.53658(6) 0.02152(19) Uani 1 1 d . . . Si2 Si 0.00648(8) 0.23166(7) 0.10532(6) 0.0299(2) Uani 1 1 d . . . S1 S 0.31515(7) 0.41843(5) 0.25821(5) 0.02076(17) Uani 1 1 d . . . S2 S 0.42722(7) 0.14034(5) 0.22519(5) 0.02042(17) Uani 1 1 d . . . N1 N 0.2780(2) 0.23533(18) 0.41922(17) 0.0201(5) Uani 1 1 d . . . N2 N 0.1686(2) 0.23716(19) 0.15235(17) 0.0233(5) Uani 1 1 d . . . O1 O 0.01924(19) 0.29829(15) 0.33129(15) 0.0262(5) Uani 1 1 d . . . O2 O 0.11661(19) 0.08551(15) 0.33477(14) 0.0237(4) Uani 1 1 d . . . C1 C 0.2918(3) 0.2653(2) 0.0897(2) 0.0229(7) Uani 1 1 d . . . C2 C 0.4224(3) 0.2231(2) 0.1126(2) 0.0221(6) Uani 1 1 d . . . C3 C 0.5472(3) 0.2562(2) 0.0553(2) 0.0265(7) Uani 1 1 d . . . H3 H 0.6343 0.2271 0.0728 0.032 Uiso 1 1 calc R . . C4 C 0.5444(3) 0.3306(3) -0.0262(2) 0.0329(8) Uani 1 1 d . . . H4 H 0.6291 0.3530 -0.0654 0.039 Uiso 1 1 calc R . . C5 C 0.4166(3) 0.3728(3) -0.0507(2) 0.0359(8) Uani 1 1 d . . . H5 H 0.4142 0.4240 -0.1073 0.043 Uiso 1 1 calc R . . C6 C 0.2933(3) 0.3414(2) 0.0056(2) 0.0295(7) Uani 1 1 d . . . H6 H 0.2072 0.3718 -0.0126 0.035 Uiso 1 1 calc R . . C7 C 0.4167(3) -0.0073(2) 0.1951(2) 0.0244(7) Uani 1 1 d . . . C8 C 0.2905(3) -0.0261(2) 0.1414(2) 0.0294(7) Uani 1 1 d . . . H8A H 0.2959 0.0231 0.0803 0.044 Uiso 1 1 calc R . . H8B H 0.2041 -0.0096 0.1840 0.044 Uiso 1 1 calc R . . H8C H 0.2905 -0.1039 0.1256 0.044 Uiso 1 1 calc R . . C9 C 0.4061(3) -0.0733(2) 0.2954(2) 0.0315(7) Uani 1 1 d . . . H9A H 0.3156 -0.0572 0.3333 0.047 Uiso 1 1 calc R . . H9B H 0.4820 -0.0522 0.3312 0.047 Uiso 1 1 calc R . . H9C H 0.4139 -0.1531 0.2863 0.047 Uiso 1 1 calc R . . C10 C 0.5540(3) -0.0349(2) 0.1324(2) 0.0297(7) Uani 1 1 d . . . H10A H 0.5521 -0.1117 0.1144 0.045 Uiso 1 1 calc R . . H10B H 0.6325 -0.0267 0.1703 0.045 Uiso 1 1 calc R . . H10C H 0.5654 0.0161 0.0723 0.045 Uiso 1 1 calc R . . C11 C -0.1090(3) 0.1325(3) 0.1874(3) 0.0382(8) Uani 1 1 d . . . H11A H -0.0582 0.0619 0.1987 0.057 Uiso 1 1 calc R . . H11B H -0.1925 0.1192 0.1560 0.057 Uiso 1 1 calc R . . H11C H -0.1373 0.1640 0.2506 0.057 Uiso 1 1 calc R . . C12 C 0.0346(4) 0.1775(3) -0.0199(3) 0.0472(9) Uani 1 1 d . . . H12A H 0.0847 0.2329 -0.0671 0.071 Uiso 1 1 calc R . . H12B H -0.0563 0.1632 -0.0413 0.071 Uiso 1 1 calc R . . H12C H 0.0900 0.1082 -0.0169 0.071 Uiso 1 1 calc R . . C13 C -0.0832(3) 0.3709(3) 0.0988(3) 0.0377(8) Uani 1 1 d . . . H13A H -0.1083 0.3940 0.1657 0.057 Uiso 1 1 calc R . . H13B H -0.1682 0.3663 0.0668 0.057 Uiso 1 1 calc R . . H13C H -0.0201 0.4255 0.0603 0.057 Uiso 1 1 calc R . . C14 C 0.4454(3) 0.3713(2) 0.3330(2) 0.0199(6) Uani 1 1 d . . . C15 C 0.5801(3) 0.4146(2) 0.3149(2) 0.0234(7) Uani 1 1 d . . . H15 H 0.5995 0.4752 0.2663 0.028 Uiso 1 1 calc R . . C16 C 0.6851(3) 0.3705(2) 0.3666(2) 0.0280(7) Uani 1 1 d . . . H16 H 0.7764 0.4007 0.3547 0.034 Uiso 1 1 calc R . . C17 C 0.6559(3) 0.2815(2) 0.4363(2) 0.0256(7) Uani 1 1 d . . . H17 H 0.7282 0.2499 0.4717 0.031 Uiso 1 1 calc R . . C18 C 0.5233(3) 0.2380(2) 0.4550(2) 0.0218(6) Uani 1 1 d . . . H18 H 0.5061 0.1770 0.5034 0.026 Uiso 1 1 calc R . . C19 C 0.4134(3) 0.2812(2) 0.4045(2) 0.0191(6) Uani 1 1 d . . . C20 C 0.2225(3) 0.5333(2) 0.3245(2) 0.0245(7) Uani 1 1 d . . . C21 C 0.1755(3) 0.4972(2) 0.4320(2) 0.0303(7) Uani 1 1 d . . . H21A H 0.1286 0.5599 0.4644 0.045 Uiso 1 1 calc R . . H21B H 0.2573 0.4729 0.4649 0.045 Uiso 1 1 calc R . . H21C H 0.1103 0.4354 0.4363 0.045 Uiso 1 1 calc R . . C22 C 0.0995(3) 0.5653(2) 0.2666(3) 0.0345(8) Uani 1 1 d . . . H22A H 0.0339 0.5035 0.2739 0.052 Uiso 1 1 calc R . . H22B H 0.1344 0.5815 0.1966 0.052 Uiso 1 1 calc R . . H22C H 0.0514 0.6315 0.2921 0.052 Uiso 1 1 calc R . . C23 C 0.3246(3) 0.6301(2) 0.3162(2) 0.0294(7) Uani 1 1 d . . . H23A H 0.2766 0.6945 0.3451 0.044 Uiso 1 1 calc R . . H23B H 0.3579 0.6502 0.2464 0.044 Uiso 1 1 calc R . . H23C H 0.4045 0.6076 0.3516 0.044 Uiso 1 1 calc R . . C24 C 0.2625(3) 0.2569(2) 0.6350(2) 0.0285(7) Uani 1 1 d . . . H24A H 0.3647 0.2531 0.6334 0.043 Uiso 1 1 calc R . . H24B H 0.2186 0.2262 0.6998 0.043 Uiso 1 1 calc R . . H24C H 0.2323 0.3347 0.6234 0.043 Uiso 1 1 calc R . . C25 C 0.2655(3) 0.0253(2) 0.5544(2) 0.0287(7) Uani 1 1 d . . . H25A H 0.2312 -0.0167 0.5044 0.043 Uiso 1 1 calc R . . H25B H 0.2268 -0.0059 0.6204 0.043 Uiso 1 1 calc R . . H25C H 0.3680 0.0203 0.5479 0.043 Uiso 1 1 calc R . . C26 C 0.0144(3) 0.1787(2) 0.5484(2) 0.0282(7) Uani 1 1 d . . . H26A H -0.0181 0.2554 0.5342 0.042 Uiso 1 1 calc R . . H26B H -0.0236 0.1517 0.6158 0.042 Uiso 1 1 calc R . . H26C H -0.0178 0.1311 0.5014 0.042 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 Mo1 0.01594(14) 0.01733(13) 0.02640(15) 0.00096(10) -0.00363(9) -0.00181(9) Si1 0.0203(4) 0.0195(4) 0.0238(5) -0.0003(3) -0.0001(3) 0.0001(3) Si2 0.0246(5) 0.0300(5) 0.0362(5) 0.0071(4) -0.0139(4) -0.0072(4) S1 0.0189(4) 0.0166(4) 0.0265(4) -0.0008(3) -0.0020(3) -0.0007(3) S2 0.0205(4) 0.0175(4) 0.0240(4) -0.0028(3) -0.0046(3) -0.0013(3) N1 0.0154(12) 0.0181(12) 0.0267(14) -0.0020(11) -0.0016(10) -0.0017(10) N2 0.0197(13) 0.0227(13) 0.0276(14) 0.0025(11) -0.0051(10) -0.0042(10) O1 0.0183(11) 0.0237(11) 0.0357(12) 0.0016(9) -0.0026(9) -0.0006(8) O2 0.0217(11) 0.0206(10) 0.0288(12) 0.0016(9) -0.0050(8) -0.0037(8) C1 0.0261(17) 0.0195(15) 0.0242(17) -0.0032(13) -0.0053(13) -0.0056(13) C2 0.0261(17) 0.0198(15) 0.0213(16) -0.0019(13) -0.0049(12) -0.0033(13) C3 0.0255(17) 0.0262(16) 0.0285(18) -0.0038(15) -0.0039(13) -0.0036(13) C4 0.0287(19) 0.0359(18) 0.0323(19) 0.0000(16) 0.0024(14) -0.0074(15) C5 0.043(2) 0.0361(19) 0.0269(19) 0.0090(15) -0.0038(15) -0.0045(16) C6 0.0317(18) 0.0301(17) 0.0276(18) 0.0020(15) -0.0101(14) -0.0012(14) C7 0.0266(17) 0.0182(15) 0.0296(18) -0.0057(13) -0.0054(13) -0.0021(13) C8 0.0279(18) 0.0253(16) 0.0377(19) -0.0101(15) -0.0082(14) -0.0024(13) C9 0.0362(19) 0.0181(15) 0.041(2) -0.0019(15) -0.0088(15) -0.0010(14) C10 0.0293(18) 0.0229(16) 0.0392(19) -0.0119(14) -0.0074(14) 0.0029(13) C11 0.0261(18) 0.0344(19) 0.056(2) 0.0107(17) -0.0202(16) -0.0079(15) C12 0.050(2) 0.050(2) 0.047(2) -0.0028(18) -0.0256(18) -0.0115(18) C13 0.0248(18) 0.041(2) 0.047(2) 0.0123(17) -0.0131(15) -0.0067(15) C14 0.0173(15) 0.0196(15) 0.0231(16) -0.0046(13) -0.0018(12) 0.0001(12) C15 0.0196(16) 0.0213(15) 0.0283(17) -0.0020(13) 0.0015(13) -0.0024(12) C16 0.0162(16) 0.0334(18) 0.0346(19) -0.0065(15) -0.0009(13) -0.0041(13) C17 0.0187(16) 0.0297(17) 0.0299(18) -0.0060(15) -0.0077(13) 0.0026(13) C18 0.0226(16) 0.0195(15) 0.0240(17) -0.0053(13) -0.0029(12) 0.0029(12) C19 0.0192(15) 0.0166(14) 0.0212(16) -0.0065(13) 0.0012(12) 0.0005(12) C20 0.0234(16) 0.0166(15) 0.0318(18) -0.0024(13) 0.0024(13) 0.0020(12) C21 0.0264(17) 0.0232(16) 0.039(2) -0.0058(15) 0.0064(14) -0.0008(13) C22 0.0302(18) 0.0212(16) 0.052(2) -0.0026(15) -0.0050(15) 0.0067(14) C23 0.0341(18) 0.0168(15) 0.0360(19) -0.0068(14) 0.0048(14) -0.0036(13) C24 0.0293(18) 0.0297(17) 0.0253(17) -0.0010(14) -0.0003(13) 0.0021(14) C25 0.0310(18) 0.0250(16) 0.0287(18) 0.0030(14) -0.0019(14) -0.0006(14) C26 0.0260(17) 0.0259(16) 0.0313(18) -0.0007(14) 0.0013(13) -0.0014(13) _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 O2 1.7035(19) . ? Mo1 O1 1.7088(19) . ? Mo1 N1 2.044(2) . ? Mo1 N2 2.059(2) . ? Mo1 S2 2.7752(11) . ? Mo1 S1 2.8049(11) . ? Si1 N1 1.766(2) . ? Si1 C26 1.861(3) . ? Si1 C25 1.865(3) . ? Si1 C24 1.873(3) . ? Si2 N2 1.766(2) . ? Si2 C11 1.859(3) . ? Si2 C13 1.866(3) . ? Si2 C12 1.873(4) . ? S1 C14 1.768(3) . ? S1 C20 1.866(3) . ? S2 C2 1.767(3) . ? S2 C7 1.869(3) . ? N1 C19 1.413(3) . ? N2 C1 1.405(4) . ? C1 C2 1.405(4) . ? C1 C6 1.407(4) . ? C2 C3 1.398(4) . ? C3 C4 1.373(4) . ? C4 C5 1.387(5) . ? C5 C6 1.375(4) . ? C7 C9 1.520(4) . ? C7 C10 1.527(4) . ? C7 C8 1.527(4) . ? C14 C15 1.396(4) . ? C14 C19 1.412(4) . ? C15 C16 1.375(4) . ? C16 C17 1.383(4) . ? C17 C18 1.378(4) . ? C18 C19 1.399(4) . ? C20 C21 1.515(4) . ? C20 C22 1.528(4) . ? C20 C23 1.533(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 Mo1 O1 104.87(9) . . ? O2 Mo1 N1 97.34(9) . . ? O1 Mo1 N1 103.38(9) . . ? O2 Mo1 N2 103.51(9) . . ? O1 Mo1 N2 96.72(9) . . ? N1 Mo1 N2 146.14(9) . . ? O2 Mo1 S2 88.97(7) . . ? O1 Mo1 S2 165.04(7) . . ? N1 Mo1 S2 79.99(7) . . ? N2 Mo1 S2 74.10(7) . . ? O2 Mo1 S1 165.93(6) . . ? O1 Mo1 S1 88.08(7) . . ? N1 Mo1 S1 73.90(7) . . ? N2 Mo1 S1 79.93(6) . . ? S2 Mo1 S1 78.79(3) . . ? N1 Si1 C26 109.66(13) . . ? N1 Si1 C25 111.41(12) . . ? C26 Si1 C25 107.63(14) . . ? N1 Si1 C24 109.55(13) . . ? C26 Si1 C24 107.14(14) . . ? C25 Si1 C24 111.34(14) . . ? N2 Si2 C11 109.08(13) . . ? N2 Si2 C13 111.69(13) . . ? C11 Si2 C13 108.63(15) . . ? N2 Si2 C12 109.66(14) . . ? C11 Si2 C12 107.48(17) . . ? C13 Si2 C12 110.19(16) . . ? C14 S1 C20 104.15(13) . . ? C14 S1 Mo1 92.06(9) . . ? C20 S1 Mo1 110.42(9) . . ? C2 S2 C7 106.04(13) . . ? C2 S2 Mo1 92.44(10) . . ? C7 S2 Mo1 110.91(10) . . ? C19 N1 Si1 120.34(19) . . ? C19 N1 Mo1 121.38(18) . . ? Si1 N1 Mo1 117.82(12) . . ? C1 N2 Si2 121.00(19) . . ? C1 N2 Mo1 120.94(18) . . ? Si2 N2 Mo1 117.65(12) . . ? N2 C1 C2 120.5(3) . . ? N2 C1 C6 122.8(3) . . ? C2 C1 C6 116.6(3) . . ? C3 C2 C1 121.5(3) . . ? C3 C2 S2 120.0(2) . . ? C1 C2 S2 118.0(2) . . ? C4 C3 C2 120.2(3) . . ? C3 C4 C5 119.3(3) . . ? C6 C5 C4 120.9(3) . . ? C5 C6 C1 121.5(3) . . ? C9 C7 C10 110.7(2) . . ? C9 C7 C8 111.6(2) . . ? C10 C7 C8 111.3(2) . . ? C9 C7 S2 103.68(19) . . ? C10 C7 S2 107.00(19) . . ? C8 C7 S2 112.2(2) . . ? C15 C14 C19 121.1(3) . . ? C15 C14 S1 120.6(2) . . ? C19 C14 S1 118.0(2) . . ? C16 C15 C14 120.6(3) . . ? C15 C16 C17 119.1(3) . . ? C18 C17 C16 120.8(3) . . ? C17 C18 C19 121.8(3) . . ? C18 C19 C14 116.5(2) . . ? C18 C19 N1 123.0(3) . . ? C14 C19 N1 120.4(2) . . ? C21 C20 C22 112.5(2) . . ? C21 C20 C23 110.3(2) . . ? C22 C20 C23 110.3(2) . . ? C21 C20 S1 111.93(19) . . ? C22 C20 S1 104.3(2) . . ? C23 C20 S1 107.23(19) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 58.92 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.345 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.062