Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Abboud, Khalil A.' 'Boncella, James M.' 'Cameron, Thomas M.' _publ_contact_author_name 'Prof James M Boncella' _publ_contact_author_address ; Prof James M Boncella Department of Chemistry and Center for Catalysis University of Florida Gainesville FL 32611-7200 UNITED STATES OF AMERICA ; data_2 _database_code_CSD 159480 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H37 Mo N5 Si2' _chemical_formula_weight 595.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 15.5947(8) _cell_length_b 10.3170(5) _cell_length_c 18.4572(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2969.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Blocks _exptl_crystal_colour Brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.8636 _exptl_absorpt_correction_T_max 0.9478 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17849 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6777 _reflns_number_gt 6305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.475(18) _refine_ls_number_reflns 6777 _refine_ls_number_parameters 332 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0530 _refine_ls_wR_factor_gt 0.0517 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_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_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 Mo Mo 0.353963(8) 0.278006(12) 0.007509(8) 0.02166(4) Uani 1 1 d . . . N1 N 0.27161(9) 0.39283(14) 0.00554(11) 0.0284(3) Uani 1 1 d . . . C1 C 0.19342(11) 0.45872(16) 0.00168(15) 0.0305(4) Uani 1 1 d . . . C2 C 0.15173(14) 0.4733(2) -0.06441(16) 0.0395(6) Uani 1 1 d . . . H2A H 0.1764 0.4395 -0.1075 0.047 Uiso 1 1 calc R . . C3 C 0.07346(16) 0.5379(2) -0.0668(2) 0.0558(8) Uani 1 1 d . . . H3A H 0.0449 0.5475 -0.1120 0.067 Uiso 1 1 calc R . . C4 C 0.03707(15) 0.5875(2) -0.0062(2) 0.0583(9) Uani 1 1 d . . . H4A H -0.0172 0.6291 -0.0088 0.070 Uiso 1 1 calc R . . C5 C 0.07872(19) 0.5772(3) 0.0586(2) 0.0615(8) Uani 1 1 d . . . H5A H 0.0539 0.6141 0.1009 0.074 Uiso 1 1 calc R . . C6 C 0.15755(17) 0.5128(3) 0.06352(16) 0.0461(6) Uani 1 1 d . . . H6A H 0.1862 0.5061 0.1088 0.055 Uiso 1 1 calc R . . N2 N 0.36014(9) 0.16450(16) -0.08534(8) 0.0242(3) Uani 1 1 d . . . N3 N 0.31576(10) 0.09956(16) 0.04636(8) 0.0266(3) Uani 1 1 d . . . C7 C 0.34115(12) 0.03238(18) -0.07525(11) 0.0261(4) Uani 1 1 d . . . C8 C 0.31732(11) -0.00200(18) -0.00371(12) 0.0280(4) Uani 1 1 d . . . C9 C 0.29958(11) -0.13278(17) 0.01102(17) 0.0358(4) Uani 1 1 d . . . H9A H 0.2841 -0.1576 0.0588 0.043 Uiso 1 1 calc R . . C10 C 0.30413(14) -0.2270(2) -0.04288(15) 0.0402(5) Uani 1 1 d . . . H10A H 0.2902 -0.3145 -0.0320 0.048 Uiso 1 1 calc R . . C11 C 0.32862(15) -0.1933(2) -0.11156(14) 0.0400(5) Uani 1 1 d . . . H11A H 0.3326 -0.2578 -0.1482 0.048 Uiso 1 1 calc R . . C12 C 0.34772(13) -0.0644(2) -0.12781(13) 0.0341(4) Uani 1 1 d . . . H12A H 0.3655 -0.0421 -0.1754 0.041 Uiso 1 1 calc R . . Si1 Si 0.36662(4) 0.22486(6) -0.17390(3) 0.03103(12) Uani 1 1 d . . . C13 C 0.46725(17) 0.1755(3) -0.22222(14) 0.0514(6) Uani 1 1 d . . . H13A H 0.5172 0.2046 -0.1944 0.051 Uiso 1 1 calc R . . H13B H 0.4684 0.2153 -0.2704 0.051 Uiso 1 1 calc R . . H13C H 0.4687 0.0810 -0.2271 0.051 Uiso 1 1 calc R . . C14 C 0.27140(17) 0.1714(3) -0.22891(13) 0.0471(6) Uani 1 1 d . . . H14A H 0.2677 0.0765 -0.2284 0.047 Uiso 1 1 calc R . . H14B H 0.2779 0.2016 -0.2789 0.047 Uiso 1 1 calc R . . H14C H 0.2190 0.2081 -0.2081 0.047 Uiso 1 1 calc R . . C15 C 0.36623(17) 0.4060(2) -0.17612(12) 0.0426(5) Uani 1 1 d . . . H15A H 0.3241 0.4389 -0.1413 0.043 Uiso 1 1 calc R . . H15B H 0.3511 0.4357 -0.2249 0.043 Uiso 1 1 calc R . . H15C H 0.4233 0.4385 -0.1633 0.043 Uiso 1 1 calc R . . Si2 Si 0.26522(4) 0.07123(6) 0.13033(3) 0.03389(13) Uani 1 1 d . . . C16 C 0.24373(19) 0.2217(3) 0.18270(14) 0.0542(7) Uani 1 1 d . . . H16A H 0.2974 0.2537 0.2037 0.054 Uiso 1 1 calc R . . H16B H 0.2028 0.2029 0.2216 0.054 Uiso 1 1 calc R . . H16C H 0.2197 0.2877 0.1504 0.054 Uiso 1 1 calc R . . C17 C 0.33378(17) -0.0335(3) 0.19024(16) 0.0566(8) Uani 1 1 d . . . H17A H 0.3471 -0.1147 0.1651 0.057 Uiso 1 1 calc R . . H17B H 0.3028 -0.0526 0.2352 0.057 Uiso 1 1 calc R . . H17C H 0.3872 0.0122 0.2017 0.057 Uiso 1 1 calc R . . C18 C 0.15639(15) -0.0024(3) 0.11569(13) 0.0429(6) Uani 1 1 d . . . H18A H 0.1210 0.0571 0.0871 0.043 Uiso 1 1 calc R . . H18B H 0.1290 -0.0180 0.1627 0.043 Uiso 1 1 calc R . . H18C H 0.1625 -0.0847 0.0897 0.043 Uiso 1 1 calc R . . N4 N 0.41509(11) 0.31142(16) 0.10868(9) 0.0286(3) Uani 1 1 d . . . C19 C 0.40397(14) 0.4211(2) 0.14864(12) 0.0393(5) Uani 1 1 d . . . H19A H 0.3692 0.4887 0.1297 0.047 Uiso 1 1 calc R . . C20 C 0.44142(17) 0.4372(3) 0.21551(13) 0.0497(6) Uani 1 1 d . . . H20A H 0.4315 0.5144 0.2423 0.060 Uiso 1 1 calc R . . C21 C 0.49351(17) 0.3410(3) 0.24385(13) 0.0517(6) Uani 1 1 d . . . H21A H 0.5180 0.3494 0.2907 0.062 Uiso 1 1 calc R . . C22 C 0.50862(17) 0.2342(3) 0.20265(14) 0.0480(6) Uani 1 1 d . . . H22A H 0.5458 0.1682 0.2201 0.058 Uiso 1 1 calc R . . C23 C 0.47000(14) 0.2211(2) 0.13515(12) 0.0340(4) Uani 1 1 d . . . H23A H 0.4824 0.1467 0.1067 0.041 Uiso 1 1 calc R . . N5 N 0.46577(10) 0.37990(15) -0.02924(8) 0.0248(3) Uani 1 1 d . . . C24 C 0.53776(12) 0.3137(2) -0.04543(11) 0.0293(4) Uani 1 1 d . . . H24A H 0.5375 0.2221 -0.0401 0.035 Uiso 1 1 calc R . . C25 C 0.61222(13) 0.3732(2) -0.06950(12) 0.0345(4) Uani 1 1 d . . . H25A H 0.6616 0.3228 -0.0803 0.041 Uiso 1 1 calc R . . C26 C 0.61411(15) 0.5057(2) -0.07758(13) 0.0364(5) Uani 1 1 d . . . H26A H 0.6637 0.5482 -0.0956 0.044 Uiso 1 1 calc R . . C27 C 0.54155(14) 0.5751(2) -0.05867(12) 0.0375(5) Uani 1 1 d . . . H27A H 0.5412 0.6669 -0.0627 0.045 Uiso 1 1 calc R . . C28 C 0.46984(13) 0.51079(19) -0.03397(11) 0.0320(4) Uani 1 1 d . . . H28A H 0.4213 0.5602 -0.0197 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 Mo 0.01839(6) 0.02346(7) 0.02311(6) 0.00064(9) 0.00108(7) 0.00119(5) N1 0.0240(7) 0.0300(7) 0.0311(7) -0.0019(9) 0.0020(9) 0.0014(5) C1 0.0217(8) 0.0210(7) 0.0487(11) 0.0029(11) 0.0045(10) 0.0004(6) C2 0.0303(12) 0.0264(11) 0.0617(16) -0.0018(11) -0.0093(10) -0.0002(8) C3 0.0345(13) 0.0333(13) 0.100(2) 0.0077(14) -0.0270(15) -0.0001(10) C4 0.0259(10) 0.0316(11) 0.117(3) 0.0103(15) 0.0029(15) 0.0049(8) C5 0.0454(16) 0.0466(15) 0.093(2) 0.0073(16) 0.0324(16) 0.0133(12) C6 0.0432(14) 0.0401(14) 0.0552(15) 0.0061(12) 0.0103(12) 0.0107(10) N2 0.0239(8) 0.0239(7) 0.0247(7) 0.0006(6) 0.0030(6) -0.0024(6) N3 0.0236(8) 0.0309(8) 0.0251(8) 0.0037(7) 0.0018(6) -0.0008(6) C7 0.0208(9) 0.0252(9) 0.0323(9) 0.0007(8) -0.0007(7) -0.0002(7) C8 0.0175(7) 0.0279(8) 0.0388(13) 0.0030(8) -0.0007(8) 0.0016(6) C9 0.0272(8) 0.0313(9) 0.0489(11) 0.0107(12) 0.0023(12) -0.0012(7) C10 0.0288(11) 0.0242(10) 0.0677(15) 0.0030(10) -0.0005(11) -0.0012(8) C11 0.0344(11) 0.0289(11) 0.0568(14) -0.0098(10) -0.0041(11) 0.0013(9) C12 0.0304(10) 0.0309(11) 0.0410(12) -0.0043(9) -0.0004(9) 0.0018(8) Si1 0.0343(3) 0.0354(3) 0.0234(3) 0.0020(2) 0.0017(2) -0.0032(2) C13 0.0503(15) 0.0646(16) 0.0394(12) 0.0001(12) 0.0168(11) -0.0005(13) C14 0.0542(15) 0.0507(14) 0.0365(11) 0.0020(10) -0.0129(11) -0.0059(12) C15 0.0591(15) 0.0385(12) 0.0301(11) 0.0127(9) -0.0028(10) -0.0086(10) Si2 0.0262(3) 0.0492(3) 0.0262(2) 0.0107(2) 0.0006(2) -0.0054(2) C16 0.0521(16) 0.0739(19) 0.0365(12) -0.0055(12) 0.0178(12) -0.0112(13) C17 0.0392(14) 0.077(2) 0.0535(16) 0.0337(15) -0.0092(12) -0.0121(13) C18 0.0300(12) 0.0657(16) 0.0329(11) 0.0060(11) 0.0057(9) -0.0045(10) N4 0.0235(8) 0.0345(8) 0.0279(8) -0.0004(7) 0.0021(6) -0.0033(6) C19 0.0349(12) 0.0418(12) 0.0411(12) -0.0115(9) -0.0014(9) 0.0000(9) C20 0.0469(14) 0.0627(16) 0.0397(12) -0.0203(12) 0.0016(11) -0.0126(12) C21 0.0506(15) 0.0713(18) 0.0332(11) -0.0036(12) -0.0111(11) -0.0200(13) C22 0.0418(14) 0.0582(15) 0.0441(13) 0.0111(11) -0.0155(11) -0.0110(11) C23 0.0280(10) 0.0380(11) 0.0360(10) 0.0029(9) -0.0054(9) -0.0025(8) N5 0.0221(8) 0.0249(8) 0.0274(8) -0.0020(6) -0.0014(6) 0.0003(6) C24 0.0236(9) 0.0295(10) 0.0347(10) -0.0003(8) -0.0004(8) 0.0020(7) C25 0.0214(9) 0.0456(12) 0.0366(11) 0.0006(9) 0.0022(8) 0.0003(9) C26 0.0268(10) 0.0439(12) 0.0386(12) 0.0074(10) -0.0002(9) -0.0098(10) C27 0.0399(12) 0.0275(10) 0.0450(12) 0.0038(9) -0.0048(10) -0.0079(9) C28 0.0279(10) 0.0265(10) 0.0415(11) -0.0005(8) -0.0005(8) 0.0015(8) _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 Mo N1 1.7476(14) . ? Mo N3 2.0637(16) . ? Mo N2 2.0779(16) . ? Mo N4 2.1247(16) . ? Mo N5 2.1460(16) . ? N1 C1 1.398(2) . ? C1 C6 1.388(4) . ? C1 C2 1.391(4) . ? C2 C3 1.391(3) . ? C2 H2A 0.9500 . ? C3 C4 1.355(5) . ? C3 H3A 0.9500 . ? C4 C5 1.365(5) . ? C4 H4A 0.9500 . ? C5 C6 1.400(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? N2 C7 1.407(2) . ? N2 Si1 1.7520(17) . ? N3 C8 1.397(3) . ? N3 Si2 1.7631(16) . ? C7 C12 1.396(3) . ? C7 C8 1.417(3) . ? C8 C9 1.404(2) . ? C9 C10 1.393(4) . ? C9 H9A 0.9500 . ? C10 C11 1.369(4) . ? C10 H10A 0.9500 . ? C11 C12 1.396(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? Si1 C15 1.870(2) . ? Si1 C13 1.875(3) . ? Si1 C14 1.882(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? Si2 C16 1.859(3) . ? Si2 C18 1.879(2) . ? Si2 C17 1.880(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? N4 C23 1.356(3) . ? N4 C19 1.362(3) . ? C19 C20 1.375(3) . ? C19 H19A 0.9500 . ? C20 C21 1.385(4) . ? C20 H20A 0.9500 . ? C21 C22 1.359(4) . ? C21 H21A 0.9500 . ? C22 C23 1.390(3) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? N5 C24 1.348(2) . ? N5 C28 1.355(3) . ? C24 C25 1.387(3) . ? C24 H24A 0.9500 . ? C25 C26 1.375(3) . ? C25 H25A 0.9500 . ? C26 C27 1.384(3) . ? C26 H26A 0.9500 . ? C27 C28 1.378(3) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? 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 Mo N3 113.57(7) . . ? N1 Mo N2 113.51(8) . . ? N3 Mo N2 78.30(6) . . ? N1 Mo N4 103.77(8) . . ? N3 Mo N4 88.22(6) . . ? N2 Mo N4 142.70(6) . . ? N1 Mo N5 104.98(7) . . ? N3 Mo N5 141.39(6) . . ? N2 Mo N5 88.72(6) . . ? N4 Mo N5 80.43(6) . . ? C1 N1 Mo 166.35(13) . . ? C6 C1 C2 119.30(19) . . ? C6 C1 N1 120.3(2) . . ? C2 C1 N1 120.4(2) . . ? C1 C2 C3 119.4(3) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 119.7(2) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C1 C6 C5 119.4(3) . . ? C1 C6 H6A 120.3 . . ? C5 C6 H6A 120.3 . . ? C7 N2 Si1 118.68(13) . . ? C7 N2 Mo 115.27(12) . . ? Si1 N2 Mo 124.88(9) . . ? C8 N3 Si2 117.70(13) . . ? C8 N3 Mo 115.73(12) . . ? Si2 N3 Mo 125.62(9) . . ? C12 C7 N2 125.81(18) . . ? C12 C7 C8 119.22(18) . . ? N2 C7 C8 114.90(16) . . ? N3 C8 C9 126.1(2) . . ? N3 C8 C7 115.68(16) . . ? C9 C8 C7 118.2(2) . . ? C10 C9 C8 121.5(3) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C11 C10 C9 119.9(2) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 120.0(2) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C7 C12 C11 121.1(2) . . ? C7 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? N2 Si1 C15 112.06(9) . . ? N2 Si1 C13 113.30(11) . . ? C15 Si1 C13 105.28(12) . . ? N2 Si1 C14 110.71(10) . . ? C15 Si1 C14 106.19(12) . . ? C13 Si1 C14 108.91(13) . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 Si2 C16 113.53(10) . . ? N3 Si2 C18 110.15(9) . . ? C16 Si2 C18 104.44(13) . . ? N3 Si2 C17 110.99(11) . . ? C16 Si2 C17 106.05(15) . . ? C18 Si2 C17 111.47(12) . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C23 N4 C19 117.13(18) . . ? C23 N4 Mo 119.23(14) . . ? C19 N4 Mo 123.62(14) . . ? N4 C19 C20 122.2(2) . . ? N4 C19 H19A 118.9 . . ? C20 C19 H19A 118.9 . . ? C19 C20 C21 120.1(2) . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C22 C21 C20 118.1(2) . . ? C22 C21 H21A 120.9 . . ? C20 C21 H21A 120.9 . . ? C21 C22 C23 120.3(2) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? N4 C23 C22 121.9(2) . . ? N4 C23 H23A 119.0 . . ? C22 C23 H23A 119.0 . . ? C24 N5 C28 116.87(16) . . ? C24 N5 Mo 119.90(13) . . ? C28 N5 Mo 123.15(13) . . ? N5 C24 C25 122.96(19) . . ? N5 C24 H24A 118.5 . . ? C25 C24 H24A 118.5 . . ? C26 C25 C24 119.5(2) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C25 C26 C27 118.0(2) . . ? C25 C26 H26A 121.0 . . ? C27 C26 H26A 121.0 . . ? C28 C27 C26 119.8(2) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? N5 C28 C27 122.66(19) . . ? N5 C28 H28A 118.7 . . ? C27 C28 H28A 118.7 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.231 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.040 #===END data_3 _database_code_CSD 159481 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H63 Cl4 Mo2 N7 Si4' _chemical_formula_weight 1124.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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)/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 14.4655(8) _cell_length_b 23.572(1) _cell_length_c 15.9891(9) _cell_angle_alpha 90.00 _cell_angle_beta 104.390(1) _cell_angle_gamma 90.00 _cell_volume 5280.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plates _exptl_crystal_colour Green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8834 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37951 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12085 _reflns_number_gt 8378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^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 0.00001(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12085 _refine_ls_number_parameters 578 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.009 _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 -0.819766(18) -0.404693(10) 0.290018(15) 0.01864(7) Uani 1 1 d . . . Mo2 Mo -0.676467(18) -0.411105(10) 0.222669(16) 0.01949(7) Uani 1 1 d . . . Si1 Si -0.99934(6) -0.50111(4) 0.22547(5) 0.02428(19) Uani 1 1 d . . . Si2 Si -0.86119(7) -0.27108(4) 0.35562(6) 0.0300(2) Uani 1 1 d . . . Si3 Si -0.60125(7) -0.29178(4) 0.12829(6) 0.0310(2) Uani 1 1 d . . . Si4 Si -0.65977(7) -0.52611(4) 0.09044(6) 0.0311(2) Uani 1 1 d . . . N1 N -0.68732(17) -0.38152(10) 0.33757(15) 0.0222(5) Uani 1 1 d . . . N2 N -0.81907(17) -0.39262(10) 0.17484(15) 0.0207(5) Uani 1 1 d . . . N3 N -0.94456(17) -0.44417(10) 0.29237(15) 0.0213(5) Uani 1 1 d . . . N4 N -0.87794(18) -0.34469(10) 0.35570(16) 0.0242(6) Uani 1 1 d . . . N5 N -0.52697(18) -0.44459(11) 0.28487(18) 0.0292(6) Uani 1 1 d . . . N6 N -0.63094(18) -0.35485(11) 0.17424(16) 0.0255(6) Uani 1 1 d . . . N7 N -0.69183(18) -0.49237(10) 0.17616(16) 0.0227(5) Uani 1 1 d . . . C1 C -0.6273(2) -0.36040(13) 0.4133(2) 0.0250(7) Uani 1 1 d . . . C2 C -0.5396(2) -0.33581(14) 0.4125(2) 0.0337(8) Uani 1 1 d . . . H2A H -0.5190 -0.3349 0.3605 0.040 Uiso 1 1 calc R . . C3 C -0.4824(3) -0.31274(16) 0.4876(3) 0.0439(10) Uani 1 1 d . . . H3A H -0.4231 -0.2959 0.4865 0.053 Uiso 1 1 calc R . . C4 C -0.5105(3) -0.31400(17) 0.5632(3) 0.0504(11) Uani 1 1 d . . . H4A H -0.4716 -0.2973 0.6138 0.060 Uiso 1 1 calc R . . C5 C -0.5954(3) -0.33964(17) 0.5655(2) 0.0462(10) Uani 1 1 d . . . H5A H -0.6139 -0.3417 0.6184 0.055 Uiso 1 1 calc R . . C6 C -0.6539(3) -0.36253(15) 0.4911(2) 0.0351(8) Uani 1 1 d . . . H6A H -0.7126 -0.3798 0.4933 0.042 Uiso 1 1 calc R . . C7 C -0.8830(2) -0.37297(12) 0.09921(19) 0.0255(7) Uani 1 1 d . . . C8 C -0.8570(3) -0.37252(15) 0.0219(2) 0.0356(8) Uani 1 1 d . . . H8A H -0.7957 -0.3858 0.0194 0.043 Uiso 1 1 calc R . . C9 C -0.9207(3) -0.35250(16) -0.0527(2) 0.0492(11) Uani 1 1 d . . . H9A H -0.9024 -0.3520 -0.1058 0.059 Uiso 1 1 calc R . . C10 C -1.0098(3) -0.33353(16) -0.0498(3) 0.0534(12) Uani 1 1 d . . . H10A H -1.0533 -0.3204 -0.1009 0.064 Uiso 1 1 calc R . . C11 C -1.0353(3) -0.33363(16) 0.0266(3) 0.0489(11) Uani 1 1 d . . . H11A H -1.0967 -0.3202 0.0286 0.059 Uiso 1 1 calc R . . C12 C -0.9731(2) -0.35303(14) 0.1015(2) 0.0341(8) Uani 1 1 d . . . H12A H -0.9918 -0.3528 0.1544 0.041 Uiso 1 1 calc R . . C13 C -0.9803(2) -0.42378(13) 0.36026(19) 0.0230(7) Uani 1 1 d . . . C14 C -0.9459(2) -0.36959(13) 0.39270(19) 0.0231(7) Uani 1 1 d . . . C15 C -0.9811(2) -0.34561(14) 0.4589(2) 0.0315(8) Uani 1 1 d . . . H15A H -0.9599 -0.3090 0.4802 0.038 Uiso 1 1 calc R . . C16 C -1.0461(3) -0.37431(16) 0.4936(2) 0.0369(8) Uani 1 1 d . . . H16A H -1.0702 -0.3570 0.5375 0.044 Uiso 1 1 calc R . . C17 C -1.0764(2) -0.42824(15) 0.4646(2) 0.0362(8) Uani 1 1 d . . . H17A H -1.1197 -0.4482 0.4898 0.043 Uiso 1 1 calc R . . C18 C -1.0434(2) -0.45299(14) 0.3988(2) 0.0309(8) Uani 1 1 d . . . H18A H -1.0638 -0.4901 0.3797 0.037 Uiso 1 1 calc R . . C19 C -1.1307(2) -0.48834(16) 0.1947(2) 0.0424(9) Uani 1 1 d . . . H19A H -1.1573 -0.4965 0.2442 0.064 Uiso 1 1 calc R . . H19B H -1.1607 -0.5132 0.1464 0.064 Uiso 1 1 calc R . . H19C H -1.1433 -0.4486 0.1774 0.064 Uiso 1 1 calc R . . C20 C -0.9596(2) -0.50361(14) 0.12428(19) 0.0307(8) Uani 1 1 d . . . H20A H -0.9847 -0.4706 0.0886 0.046 Uiso 1 1 calc R . . H20B H -0.9834 -0.5384 0.0926 0.046 Uiso 1 1 calc R . . H20C H -0.8897 -0.5032 0.1379 0.046 Uiso 1 1 calc R . . C21 C -0.9758(3) -0.57200(14) 0.2789(2) 0.0355(8) Uani 1 1 d . . . H21A H -0.9099 -0.5834 0.2820 0.053 Uiso 1 1 calc R . . H21B H -1.0198 -0.6001 0.2453 0.053 Uiso 1 1 calc R . . H21C H -0.9854 -0.5697 0.3373 0.053 Uiso 1 1 calc R . . C22 C -0.7872(3) -0.25419(15) 0.2793(3) 0.0456(10) Uani 1 1 d . . . H22A H -0.7242 -0.2717 0.2995 0.068 Uiso 1 1 calc R . . H22B H -0.7800 -0.2130 0.2761 0.068 Uiso 1 1 calc R . . H22C H -0.8184 -0.2690 0.2219 0.068 Uiso 1 1 calc R . . C23 C -0.8017(3) -0.24041(16) 0.4636(2) 0.0466(10) Uani 1 1 d . . . H23A H -0.8352 -0.2531 0.5065 0.070 Uiso 1 1 calc R . . H23B H -0.8035 -0.1989 0.4602 0.070 Uiso 1 1 calc R . . H23C H -0.7351 -0.2532 0.4808 0.070 Uiso 1 1 calc R . . C24 C -0.9808(3) -0.23648(15) 0.3141(2) 0.0440(10) Uani 1 1 d . . . H24A H -1.0146 -0.2549 0.2602 0.066 Uiso 1 1 calc R . . H24B H -0.9718 -0.1962 0.3033 0.066 Uiso 1 1 calc R . . H24C H -1.0183 -0.2403 0.3571 0.066 Uiso 1 1 calc R . . C25 C -0.4550(3) -0.43724(16) 0.2470(3) 0.0457(10) Uani 1 1 d . . . H25A H -0.4646 -0.4133 0.1978 0.055 Uiso 1 1 calc R . . C26 C -0.3676(3) -0.4631(2) 0.2766(4) 0.0704(15) Uani 1 1 d . . . H26A H -0.3186 -0.4579 0.2473 0.084 Uiso 1 1 calc R . . C27 C -0.3525(3) -0.4964(2) 0.3493(4) 0.0734(16) Uani 1 1 d . . . H27A H -0.2925 -0.5143 0.3713 0.088 Uiso 1 1 calc R . . C28 C -0.4250(3) -0.50361(18) 0.3895(3) 0.0559(12) Uani 1 1 d . . . H28A H -0.4161 -0.5265 0.4397 0.067 Uiso 1 1 calc R . . C29 C -0.5112(3) -0.47690(15) 0.3557(2) 0.0382(9) Uani 1 1 d . . . H29A H -0.5613 -0.4817 0.3839 0.046 Uiso 1 1 calc R . . C30 C -0.5306(3) -0.24567(16) 0.2148(3) 0.0574(12) Uani 1 1 d . . . H30A H -0.5685 -0.2365 0.2560 0.086 Uiso 1 1 calc R . . H30B H -0.5137 -0.2106 0.1893 0.086 Uiso 1 1 calc R . . H30C H -0.4723 -0.2655 0.2448 0.086 Uiso 1 1 calc R . . C31 C -0.5280(3) -0.31158(18) 0.0531(3) 0.0685(14) Uani 1 1 d . . . H31A H -0.4717 -0.3328 0.0844 0.103 Uiso 1 1 calc R . . H31B H -0.5076 -0.2772 0.0282 0.103 Uiso 1 1 calc R . . H31C H -0.5658 -0.3353 0.0067 0.103 Uiso 1 1 calc R . . C32 C -0.7092(3) -0.25308(17) 0.0686(3) 0.0563(12) Uani 1 1 d . . . H32A H -0.7422 -0.2754 0.0183 0.084 Uiso 1 1 calc R . . H32B H -0.6905 -0.2163 0.0493 0.084 Uiso 1 1 calc R . . H32C H -0.7520 -0.2471 0.1066 0.084 Uiso 1 1 calc R . . C33 C -0.7133(2) -0.52084(12) 0.24680(19) 0.0227(6) Uani 1 1 d . . . C34 C -0.7584(2) -0.48962(12) 0.30210(19) 0.0213(6) Uani 1 1 d . . . C35 C -0.7607(2) -0.51424(13) 0.3811(2) 0.0282(7) Uani 1 1 d . . . H35A H -0.7855 -0.4927 0.4209 0.034 Uiso 1 1 calc R . . C36 C -0.7284(2) -0.56889(14) 0.4036(2) 0.0335(8) Uani 1 1 d . . . H36A H -0.7292 -0.5841 0.4585 0.040 Uiso 1 1 calc R . . C37 C -0.6948(2) -0.60099(14) 0.3448(2) 0.0359(8) Uani 1 1 d . . . H37A H -0.6776 -0.6395 0.3574 0.043 Uiso 1 1 calc R . . C38 C -0.6863(2) -0.57753(13) 0.2684(2) 0.0307(8) Uani 1 1 d . . . H38A H -0.6619 -0.5999 0.2294 0.037 Uiso 1 1 calc R . . C39 C -0.7576(3) -0.57462(16) 0.0363(2) 0.0471(10) Uani 1 1 d . . . H39A H -0.7689 -0.6026 0.0781 0.071 Uiso 1 1 calc R . . H39B H -0.7396 -0.5942 -0.0113 0.071 Uiso 1 1 calc R . . H39C H -0.8160 -0.5526 0.0137 0.071 Uiso 1 1 calc R . . C40 C -0.5455(3) -0.56627(17) 0.1243(3) 0.0529(11) Uani 1 1 d . . . H40A H -0.5048 -0.5487 0.1761 0.079 Uiso 1 1 calc R . . H40B H -0.5126 -0.5655 0.0776 0.079 Uiso 1 1 calc R . . H40C H -0.5589 -0.6056 0.1370 0.079 Uiso 1 1 calc R . . C41 C -0.6411(3) -0.47103(16) 0.0128(2) 0.0455(10) Uani 1 1 d . . . H41A H -0.7016 -0.4515 -0.0118 0.068 Uiso 1 1 calc R . . H41B H -0.6184 -0.4891 -0.0335 0.068 Uiso 1 1 calc R . . H41C H -0.5937 -0.4435 0.0430 0.068 Uiso 1 1 calc R . . C42 C -0.1996(3) -0.3377(2) 0.2975(3) 0.0753(15) Uani 1 1 d D . . H42A H -0.1843 -0.3784 0.3077 0.090 Uiso 1 1 calc R . . H42B H -0.1410 -0.3157 0.3230 0.090 Uiso 1 1 calc R . . Cl1 Cl -0.28753(12) -0.31916(8) 0.34942(10) 0.1024(5) Uani 1 1 d D . . Cl2 Cl -0.23371(13) -0.32518(7) 0.18687(8) 0.0976(5) Uani 1 1 d D . . C43 C -0.2598(18) -0.1686(6) -0.7557(10) 0.152(11) Uani 0.50 1 d PD A 1 H43A H -0.3111 -0.1927 -0.7436 0.182 Uiso 0.50 1 calc PR A 1 H43B H -0.2103 -0.1940 -0.7680 0.182 Uiso 0.50 1 calc PR A 1 Cl3 Cl -0.2108(3) -0.1289(2) -0.6665(2) 0.0877(12) Uani 0.50 1 d PD A 1 Cl4 Cl -0.3080(5) -0.1261(2) -0.8484(4) 0.095(2) Uani 0.50 1 d PD A 1 C44 C -0.2583(13) -0.1801(7) -0.7484(11) 0.051(4) Uiso 0.35 1 d PD B 3 H44A H -0.3044 -0.1939 -0.7165 0.061 Uiso 0.35 1 calc PR B 3 H44B H -0.2190 -0.2123 -0.7595 0.061 Uiso 0.35 1 calc PR B 3 Cl5 Cl -0.3179(7) -0.1444(4) -0.8474(6) 0.0539(16) Uiso 0.35 1 d PD B 3 Cl6 Cl -0.1882(5) -0.1256(3) -0.6938(4) 0.096(2) Uiso 0.35 1 d PD B 3 C45 C -0.225(3) -0.135(3) -0.7623(15) 0.15(2) Uiso 0.15 1 d PD C 2 H45A H -0.1631 -0.1450 -0.7754 0.184 Uiso 0.15 1 calc PR C 2 H45B H -0.2296 -0.0936 -0.7580 0.184 Uiso 0.15 1 calc PR C 2 Cl7 Cl -0.2352(8) -0.1685(5) -0.6669(7) 0.086(3) Uiso 0.15 1 d PD C 2 Cl8 Cl -0.3227(8) -0.1634(4) -0.8427(7) 0.061(4) Uiso 0.15 1 d PD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01906(14) 0.01717(13) 0.02062(13) 0.00001(10) 0.00667(10) 0.00004(11) Mo2 0.01965(14) 0.01760(13) 0.02234(14) 0.00108(10) 0.00733(10) -0.00031(11) Si1 0.0244(5) 0.0238(5) 0.0251(4) -0.0018(3) 0.0069(3) -0.0047(4) Si2 0.0337(5) 0.0188(4) 0.0388(5) -0.0028(4) 0.0113(4) 0.0009(4) Si3 0.0347(5) 0.0238(5) 0.0363(5) 0.0049(4) 0.0121(4) -0.0064(4) Si4 0.0400(6) 0.0243(5) 0.0351(5) -0.0023(4) 0.0213(4) -0.0001(4) N1 0.0233(14) 0.0206(13) 0.0231(13) 0.0005(10) 0.0065(10) -0.0004(11) N2 0.0234(14) 0.0164(12) 0.0232(13) -0.0009(10) 0.0075(10) 0.0006(10) N3 0.0185(13) 0.0207(13) 0.0257(13) -0.0010(10) 0.0076(10) -0.0004(10) N4 0.0260(15) 0.0210(13) 0.0264(14) -0.0021(11) 0.0079(11) 0.0013(11) N5 0.0224(15) 0.0251(15) 0.0385(16) -0.0012(12) 0.0049(12) 0.0037(11) N6 0.0239(14) 0.0253(14) 0.0280(14) 0.0051(11) 0.0077(11) -0.0021(11) N7 0.0253(14) 0.0200(13) 0.0255(13) -0.0007(10) 0.0117(11) -0.0010(11) C1 0.0276(18) 0.0175(15) 0.0273(17) -0.0015(12) 0.0018(13) 0.0040(13) C2 0.031(2) 0.0306(19) 0.0365(19) -0.0027(15) 0.0031(15) -0.0009(15) C3 0.030(2) 0.038(2) 0.054(2) -0.0106(18) -0.0069(17) -0.0009(17) C4 0.042(2) 0.050(2) 0.047(2) -0.021(2) -0.0113(19) 0.010(2) C5 0.048(3) 0.059(3) 0.0275(19) -0.0069(17) 0.0016(17) 0.015(2) C6 0.034(2) 0.039(2) 0.0315(19) -0.0027(15) 0.0062(15) 0.0037(16) C7 0.0282(18) 0.0174(15) 0.0271(16) 0.0014(12) -0.0002(13) -0.0039(13) C8 0.042(2) 0.035(2) 0.0284(18) 0.0022(15) 0.0057(15) -0.0065(17) C9 0.069(3) 0.045(2) 0.027(2) 0.0056(17) -0.0007(19) -0.019(2) C10 0.057(3) 0.040(2) 0.045(2) 0.0145(19) -0.023(2) -0.007(2) C11 0.036(2) 0.037(2) 0.062(3) 0.0111(19) -0.0093(19) 0.0056(17) C12 0.0283(19) 0.0295(19) 0.040(2) 0.0048(15) 0.0008(15) 0.0001(14) C13 0.0221(16) 0.0252(16) 0.0225(16) 0.0024(12) 0.0071(12) 0.0058(13) C14 0.0220(16) 0.0257(16) 0.0223(15) 0.0024(13) 0.0067(12) 0.0067(13) C15 0.039(2) 0.0268(17) 0.0301(18) -0.0045(14) 0.0107(15) 0.0058(15) C16 0.041(2) 0.045(2) 0.0299(18) -0.0001(16) 0.0199(16) 0.0080(18) C17 0.033(2) 0.045(2) 0.037(2) 0.0078(16) 0.0213(16) 0.0044(17) C18 0.035(2) 0.0272(18) 0.0340(19) 0.0013(14) 0.0159(15) -0.0009(15) C19 0.030(2) 0.050(2) 0.045(2) -0.0037(18) 0.0043(16) -0.0053(17) C20 0.038(2) 0.0291(18) 0.0254(17) -0.0043(14) 0.0085(14) -0.0075(15) C21 0.047(2) 0.0269(18) 0.0326(19) -0.0001(14) 0.0101(16) -0.0069(16) C22 0.055(3) 0.0248(19) 0.066(3) 0.0073(18) 0.033(2) -0.0002(18) C23 0.046(2) 0.035(2) 0.056(3) -0.0118(18) 0.0078(19) -0.0052(18) C24 0.047(2) 0.033(2) 0.051(2) 0.0025(17) 0.0110(18) 0.0127(18) C25 0.027(2) 0.043(2) 0.070(3) 0.001(2) 0.0190(19) 0.0036(17) C26 0.027(2) 0.073(3) 0.116(4) 0.011(3) 0.026(2) 0.010(2) C27 0.031(3) 0.070(3) 0.110(4) -0.003(3) -0.001(3) 0.023(2) C28 0.047(3) 0.051(3) 0.057(3) 0.003(2) -0.011(2) 0.013(2) C29 0.035(2) 0.035(2) 0.040(2) 0.0017(16) 0.0007(16) 0.0025(16) C30 0.073(3) 0.035(2) 0.056(3) 0.0072(19) 0.001(2) -0.025(2) C31 0.087(4) 0.046(3) 0.095(4) 0.017(3) 0.064(3) -0.006(3) C32 0.053(3) 0.044(2) 0.066(3) 0.028(2) 0.003(2) -0.003(2) C33 0.0229(16) 0.0178(15) 0.0267(16) -0.0004(12) 0.0051(12) -0.0012(13) C34 0.0169(15) 0.0225(16) 0.0247(16) 0.0007(12) 0.0052(12) -0.0003(12) C35 0.0285(18) 0.0289(18) 0.0282(17) 0.0025(13) 0.0089(14) 0.0025(14) C36 0.038(2) 0.0321(19) 0.0304(18) 0.0126(15) 0.0084(15) 0.0044(16) C37 0.041(2) 0.0247(18) 0.043(2) 0.0125(15) 0.0124(16) 0.0076(16) C38 0.035(2) 0.0239(17) 0.0369(19) 0.0024(14) 0.0160(15) 0.0076(15) C39 0.063(3) 0.037(2) 0.045(2) -0.0163(17) 0.0207(19) -0.010(2) C40 0.052(3) 0.045(2) 0.075(3) 0.005(2) 0.041(2) 0.015(2) C41 0.067(3) 0.040(2) 0.040(2) -0.0007(17) 0.0338(19) -0.001(2) C42 0.046(3) 0.109(4) 0.065(3) 0.016(3) 0.003(2) 0.015(3) Cl1 0.0926(11) 0.1280(14) 0.0848(10) -0.0158(10) 0.0188(8) 0.0335(10) Cl2 0.1295(14) 0.0994(11) 0.0538(8) 0.0011(7) 0.0038(8) 0.0371(10) C43 0.29(3) 0.061(11) 0.131(17) -0.018(10) 0.103(17) -0.046(13) Cl3 0.073(2) 0.120(3) 0.062(2) -0.035(2) 0.0023(18) -0.012(2) Cl4 0.083(3) 0.122(6) 0.085(2) -0.006(3) 0.0306(19) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 1.866(2) . ? Mo1 N1 1.955(2) . ? Mo1 N3 2.040(2) . ? Mo1 N4 2.062(2) . ? Mo1 C34 2.179(3) . ? Mo1 Mo2 2.5669(4) . ? Mo2 N6 1.745(2) . ? Mo2 N1 2.007(2) . ? Mo2 N7 2.047(2) . ? Mo2 N2 2.061(2) . ? Mo2 N5 2.285(3) . ? Si1 N3 1.775(2) . ? Si1 C20 1.848(3) . ? Si1 C19 1.866(4) . ? Si1 C21 1.869(3) . ? Si2 N4 1.752(3) . ? Si2 C22 1.856(4) . ? Si2 C23 1.873(4) . ? Si2 C24 1.878(4) . ? Si3 N6 1.758(3) . ? Si3 C31 1.849(4) . ? Si3 C30 1.854(4) . ? Si3 C32 1.855(4) . ? Si4 N7 1.744(3) . ? Si4 C39 1.858(4) . ? Si4 C41 1.861(4) . ? Si4 C40 1.865(4) . ? N1 C1 1.394(4) . ? N2 C7 1.406(4) . ? N3 C13 1.398(4) . ? N4 C14 1.396(4) . ? N5 C29 1.337(4) . ? N5 C25 1.340(4) . ? N7 C33 1.413(4) . ? C1 C6 1.393(4) . ? C1 C2 1.397(5) . ? C2 C3 1.388(5) . ? C3 C4 1.367(6) . ? C4 C5 1.377(6) . ? C5 C6 1.386(5) . ? C7 C8 1.379(4) . ? C7 C12 1.394(5) . ? C8 C9 1.396(5) . ? C9 C10 1.376(6) . ? C10 C11 1.362(6) . ? C11 C12 1.384(5) . ? C13 C18 1.403(4) . ? C13 C14 1.421(4) . ? C14 C15 1.402(4) . ? C15 C16 1.382(5) . ? C16 C17 1.386(5) . ? C17 C18 1.387(4) . ? C25 C26 1.376(5) . ? C26 C27 1.374(7) . ? C27 C28 1.371(7) . ? C28 C29 1.382(5) . ? C33 C38 1.411(4) . ? C33 C34 1.426(4) . ? C34 C35 1.399(4) . ? C35 C36 1.387(4) . ? C36 C37 1.385(5) . ? C37 C38 1.374(4) . ? C42 Cl1 1.738(5) . ? C42 Cl2 1.740(5) . ? C43 Cl3 1.705(14) . ? C43 Cl4 1.781(14) . ? C44 Cl6 1.734(14) . ? C44 Cl5 1.811(15) . ? C45 Cl7 1.755(18) . ? C45 Cl8 1.787(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Mo1 N1 95.51(10) . . ? N2 Mo1 N3 108.04(10) . . ? N1 Mo1 N3 155.03(10) . . ? N2 Mo1 N4 120.07(10) . . ? N1 Mo1 N4 95.44(10) . . ? N3 Mo1 N4 80.12(10) . . ? N2 Mo1 C34 97.21(11) . . ? N1 Mo1 C34 83.32(10) . . ? N3 Mo1 C34 85.55(10) . . ? N4 Mo1 C34 142.57(10) . . ? N2 Mo1 Mo2 52.55(7) . . ? N1 Mo1 Mo2 50.52(7) . . ? N3 Mo1 Mo2 142.33(7) . . ? N4 Mo1 Mo2 136.76(7) . . ? C34 Mo1 Mo2 68.23(8) . . ? N6 Mo2 N1 105.44(11) . . ? N6 Mo2 N7 124.66(11) . . ? N1 Mo2 N7 129.16(10) . . ? N6 Mo2 N2 97.35(11) . . ? N1 Mo2 N2 88.13(10) . . ? N7 Mo2 N2 93.14(9) . . ? N6 Mo2 N5 92.00(11) . . ? N1 Mo2 N5 90.14(10) . . ? N7 Mo2 N5 80.82(9) . . ? N2 Mo2 N5 170.62(10) . . ? N6 Mo2 Mo1 125.07(9) . . ? N1 Mo2 Mo1 48.75(7) . . ? N7 Mo2 Mo1 100.46(7) . . ? N2 Mo2 Mo1 45.97(7) . . ? N5 Mo2 Mo1 127.84(7) . . ? N3 Si1 C20 111.24(13) . . ? N3 Si1 C19 108.05(15) . . ? C20 Si1 C19 107.00(16) . . ? N3 Si1 C21 113.42(13) . . ? C20 Si1 C21 108.09(16) . . ? C19 Si1 C21 108.83(17) . . ? N4 Si2 C22 108.39(15) . . ? N4 Si2 C23 114.43(15) . . ? C22 Si2 C23 108.41(18) . . ? N4 Si2 C24 108.36(15) . . ? C22 Si2 C24 107.76(17) . . ? C23 Si2 C24 109.30(17) . . ? N6 Si3 C31 107.30(16) . . ? N6 Si3 C30 109.30(15) . . ? C31 Si3 C30 109.5(2) . . ? N6 Si3 C32 111.64(16) . . ? C31 Si3 C32 109.6(2) . . ? C30 Si3 C32 109.5(2) . . ? N7 Si4 C39 109.03(15) . . ? N7 Si4 C41 108.46(15) . . ? C39 Si4 C41 109.80(18) . . ? N7 Si4 C40 113.15(16) . . ? C39 Si4 C40 109.92(19) . . ? C41 Si4 C40 106.42(18) . . ? C1 N1 Mo1 140.9(2) . . ? C1 N1 Mo2 138.1(2) . . ? Mo1 N1 Mo2 80.74(9) . . ? C7 N2 Mo1 137.3(2) . . ? C7 N2 Mo2 140.6(2) . . ? Mo1 N2 Mo2 81.48(9) . . ? C13 N3 Si1 122.1(2) . . ? C13 N3 Mo1 110.91(18) . . ? Si1 N3 Mo1 126.76(13) . . ? C14 N4 Si2 121.9(2) . . ? C14 N4 Mo1 110.29(19) . . ? Si2 N4 Mo1 127.23(14) . . ? C29 N5 C25 118.0(3) . . ? C29 N5 Mo2 120.6(2) . . ? C25 N5 Mo2 121.1(2) . . ? Mo2 N6 Si3 170.50(17) . . ? C33 N7 Si4 124.5(2) . . ? C33 N7 Mo2 100.34(18) . . ? Si4 N7 Mo2 133.33(14) . . ? C6 C1 N1 120.8(3) . . ? C6 C1 C2 118.4(3) . . ? N1 C1 C2 120.8(3) . . ? C3 C2 C1 120.1(4) . . ? C4 C3 C2 120.8(4) . . ? C3 C4 C5 119.7(3) . . ? C4 C5 C6 120.4(4) . . ? C5 C6 C1 120.4(4) . . ? C8 C7 C12 119.1(3) . . ? C8 C7 N2 120.4(3) . . ? C12 C7 N2 120.5(3) . . ? C7 C8 C9 120.0(4) . . ? C10 C9 C8 120.4(4) . . ? C11 C10 C9 119.7(3) . . ? C10 C11 C12 120.9(4) . . ? C11 C12 C7 120.0(4) . . ? N3 C13 C18 125.4(3) . . ? N3 C13 C14 115.4(3) . . ? C18 C13 C14 119.2(3) . . ? N4 C14 C15 125.2(3) . . ? N4 C14 C13 116.3(3) . . ? C15 C14 C13 118.6(3) . . ? C16 C15 C14 121.1(3) . . ? C15 C16 C17 120.3(3) . . ? C16 C17 C18 120.0(3) . . ? C17 C18 C13 120.7(3) . . ? N5 C25 C26 122.5(4) . . ? C27 C26 C25 119.0(4) . . ? C28 C27 C26 119.1(4) . . ? C27 C28 C29 118.8(4) . . ? N5 C29 C28 122.5(4) . . ? C38 C33 N7 122.9(3) . . ? C38 C33 C34 118.5(3) . . ? N7 C33 C34 118.4(3) . . ? C35 C34 C33 117.6(3) . . ? C35 C34 Mo1 111.1(2) . . ? C33 C34 Mo1 131.1(2) . . ? C36 C35 C34 122.5(3) . . ? C37 C36 C35 119.0(3) . . ? C38 C37 C36 120.5(3) . . ? C37 C38 C33 121.3(3) . . ? Cl1 C42 Cl2 112.8(2) . . ? Cl3 C43 Cl4 112.5(8) . . ? Cl6 C44 Cl5 100.7(8) . . ? Cl7 C45 Cl8 103.6(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.807 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.085