# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_address S.R.Dubberley ; Department of Chemistr,University of Oxford, Chemistry Research Laboratory,Mansfield Road,Oxford OX1 3TA, UK ; S.K.Ignatov ; University of Nizhnii Novgorod, 23, Gagarin Avenue, Nizhnii Novgorod 603600, Russia ; N.H.Rees ; Department of Chemistr,University of Oxford, Chemistry Research Laboratory,Mansfield Road,Oxford OX1 3TA, UK ; A.G.Razuvaev ; University of Nizhnii Novgorod, 23, Gagarin Avenue, Nizhnii Novgorod 603600, Russia ; P.Mountford ; Department of Chemistr,University of Oxford, Chemistry Research Laboratory,Mansfield Road,Oxford OX1 3TA, UK ; ; G.I.Nikonov ; ; Department of Chemistry, Moscow State University Leninskie Gory, Moscow 119899, Russia ; _publ_contact_author_name 'Dr Georgii Nikonov' _publ_contact_author_address ; Department of Chemistry Moscow State University Vorob'evy Gory Moscow 119992 RUSSIAN FEDERATION ; _publ_contact_author_email NIKONOV@ORG.CHEM.MSU.SU _publ_section_title ; Unexpected Features of Stretched Si-H...Mo beta-Agostic Interactions ; data_gin8 _database_code_depnum_ccdc_archive 'CCDC 226162' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2,6-dimethylphenylimido)bis(trimethylphosphine)(chloro) ((2,6-dimethylphenyl)(dimethylsilyl)amido)molybdenum (IV) ; _chemical_name_common ; (2,6-dimethylphenylimido)bis(trimethylphosphine)(chloro) ((2,6-dimethylphenyl)(dimethylsilyl)amido)molybdenum (IV) ; _chemical_melting_point ? _chemical_formula_moiety (2,6-Me2C6H3N)((2,6-Me2C6H3)(HMe2Si)N)MoCl(PMe3)2 _chemical_formula_sum 'C27 H50 Cl Mo N2 P2 Si' _chemical_formula_weight 624.11 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' P P 0.1023 0.0942 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.521(4) _cell_length_b 9.849(2) _cell_length_c 18.691(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.52(3) _cell_angle_gamma 90.00 _cell_volume 3268.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_type multy-scan _exptl_absorpt_correction_T_min 0.8943 _exptl_absorpt_correction_T_max 0.9750 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 0 _diffrn_reflns_number 25752 _diffrn_reflns_av_R_equivalents 0.0936 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 5.28 _diffrn_reflns_theta_max 27.52 _reflns_number_total 7435 _reflns_number_gt 4801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0552P)^2^+3.4618P] 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 7435 _refine_ls_number_parameters 300 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1285 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.201 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.18368(2) 0.67917(3) 0.192346(19) 0.02243(12) Uani 1 1 d . . . Si1 Si 0.16588(8) 0.47213(12) 0.09689(7) 0.0301(3) Uani 1 1 d . . . Cl1 Cl 0.12224(6) 0.51954(10) 0.26523(6) 0.0291(3) Uani 1 1 d . . . P1 P 0.27597(7) 0.74449(12) 0.31196(6) 0.0297(3) Uani 1 1 d . . . P2 P 0.07904(6) 0.81298(11) 0.21765(6) 0.0241(2) Uani 1 1 d . . . N1 N 0.2421(2) 0.5083(3) 0.1677(2) 0.0296(8) Uani 1 1 d . . . N2 N 0.2016(2) 0.8113(3) 0.13668(17) 0.0239(8) Uani 1 1 d . . . H H 0.116(2) 0.589(4) 0.109(2) 0.025(11) Uiso 1 1 d . . . C1 C 0.3148(3) 0.4541(5) 0.1935(3) 0.0349(11) Uani 1 1 d . . . C2 C 0.3305(3) 0.3487(5) 0.2472(3) 0.0426(13) Uani 1 1 d . . . C3 C 0.4036(3) 0.3000(6) 0.2739(3) 0.0593(16) Uani 1 1 d . . . H3A H 0.4138 0.2312 0.3094 0.071 Uiso 1 1 calc R . . C4 C 0.4610(4) 0.3506(7) 0.2493(4) 0.0696(19) Uani 1 1 d . . . H4A H 0.5097 0.3173 0.2683 0.084 Uiso 1 1 calc R . . C5 C 0.4460(3) 0.4512(7) 0.1961(4) 0.0634(17) Uani 1 1 d . . . H5A H 0.4851 0.4856 0.1794 0.076 Uiso 1 1 calc R . . C6 C 0.3738(3) 0.5026(5) 0.1668(3) 0.0439(13) Uani 1 1 d . . . C7 C 0.3579(3) 0.6119(6) 0.1076(3) 0.0593(16) Uani 1 1 d . . . H7A H 0.4039 0.6575 0.1084 0.089 Uiso 1 1 calc R . . H7B H 0.3228 0.6762 0.1172 0.089 Uiso 1 1 calc R . . H7C H 0.3367 0.5714 0.0594 0.089 Uiso 1 1 calc R . . C8 C 0.2693(3) 0.2898(5) 0.2760(4) 0.0565(16) Uani 1 1 d . . . H8A H 0.2914 0.2365 0.3197 0.085 Uiso 1 1 calc R . . H8B H 0.2372 0.2333 0.2383 0.085 Uiso 1 1 calc R . . H8C H 0.2402 0.3620 0.2884 0.085 Uiso 1 1 calc R . . C9 C 0.2036(3) 0.9148(4) 0.0859(2) 0.0272(10) Uani 1 1 d . . . C10 C 0.2671(3) 1.0000(4) 0.0979(3) 0.0354(11) Uani 1 1 d . . . C11 C 0.2672(3) 1.1019(5) 0.0459(3) 0.0434(13) Uani 1 1 d . . . H11A H 0.3081 1.1604 0.0540 0.052 Uiso 1 1 calc R . . C12 C 0.2073(4) 1.1167(5) -0.0172(3) 0.0473(15) Uani 1 1 d . . . H12A H 0.2082 1.1843 -0.0517 0.057 Uiso 1 1 calc R . . C13 C 0.1460(3) 1.0313(5) -0.0292(3) 0.0389(12) Uani 1 1 d . . . H13A H 0.1063 1.0412 -0.0725 0.047 Uiso 1 1 calc R . . C14 C 0.1421(3) 0.9314(4) 0.0212(2) 0.0317(11) Uani 1 1 d . . . C15 C 0.0740(3) 0.8406(5) 0.0050(2) 0.0393(12) Uani 1 1 d . . . H15A H 0.0377 0.8704 -0.0399 0.059 Uiso 1 1 calc R . . H15B H 0.0521 0.8446 0.0458 0.059 Uiso 1 1 calc R . . H15C H 0.0886 0.7489 -0.0013 0.059 Uiso 1 1 calc R . . C16 C 0.3349(3) 0.9828(6) 0.1647(3) 0.0534(15) Uani 1 1 d . . . H16A H 0.3332 0.8952 0.1867 0.080 Uiso 1 1 calc R . . H16B H 0.3348 1.0522 0.2008 0.080 Uiso 1 1 calc R . . H16C H 0.3800 0.9900 0.1493 0.080 Uiso 1 1 calc R . . C17 C 0.1712(3) 0.5018(5) 0.0001(3) 0.0477(14) Uani 1 1 d . . . H17A H 0.1637 0.4176 -0.0268 0.072 Uiso 1 1 calc R . . H17B H 0.2198 0.5379 0.0019 0.072 Uiso 1 1 calc R . . H17C H 0.1329 0.5653 -0.0246 0.072 Uiso 1 1 calc R . . C18 C 0.1115(3) 0.3152(5) 0.0994(3) 0.0416(12) Uani 1 1 d . . . H18A H 0.1138 0.2568 0.0590 0.062 Uiso 1 1 calc R . . H18B H 0.0600 0.3382 0.0946 0.062 Uiso 1 1 calc R . . H18C H 0.1325 0.2692 0.1460 0.062 Uiso 1 1 calc R . . C19 C 0.2657(3) 0.6594(6) 0.3943(3) 0.0494(14) Uani 1 1 d . . . H19A H 0.3037 0.6913 0.4374 0.074 Uiso 1 1 calc R . . H19B H 0.2712 0.5632 0.3892 0.074 Uiso 1 1 calc R . . H19C H 0.2167 0.6784 0.3999 0.074 Uiso 1 1 calc R . . C20 C 0.2781(3) 0.9218(5) 0.3390(3) 0.0470(13) Uani 1 1 d . . . H20A H 0.3157 0.9346 0.3858 0.071 Uiso 1 1 calc R . . H20B H 0.2298 0.9476 0.3438 0.071 Uiso 1 1 calc R . . H20C H 0.2901 0.9769 0.3015 0.071 Uiso 1 1 calc R . . C21 C 0.3745(3) 0.7115(6) 0.3207(3) 0.0483(14) Uani 1 1 d . . . H21A H 0.4048 0.7407 0.3689 0.073 Uiso 1 1 calc R . . H21B H 0.3892 0.7603 0.2826 0.073 Uiso 1 1 calc R . . H21C H 0.3818 0.6160 0.3151 0.073 Uiso 1 1 calc R . . C22 C 0.0726(3) 0.9902(4) 0.1895(2) 0.0325(11) Uani 1 1 d . . . H22A H 0.0308 1.0320 0.2017 0.049 Uiso 1 1 calc R . . H22B H 0.0653 0.9960 0.1366 0.049 Uiso 1 1 calc R . . H22C H 0.1183 1.0363 0.2152 0.049 Uiso 1 1 calc R . . C23 C -0.0136(3) 0.7467(4) 0.1686(2) 0.0306(10) Uani 1 1 d . . . H23A H -0.0518 0.8014 0.1801 0.046 Uiso 1 1 calc R . . H23B H -0.0179 0.6547 0.1840 0.046 Uiso 1 1 calc R . . H23C H -0.0201 0.7489 0.1158 0.046 Uiso 1 1 calc R . . C24 C 0.0687(3) 0.8282(5) 0.3113(2) 0.0335(11) Uani 1 1 d . . . H24A H 0.0255 0.8832 0.3098 0.050 Uiso 1 1 calc R . . H24B H 0.1129 0.8698 0.3435 0.050 Uiso 1 1 calc R . . H24C H 0.0621 0.7396 0.3299 0.050 Uiso 1 1 calc R . . C31 C 0.5576(8) 0.7835(11) 0.5110(7) 0.169(5) Uiso 1 1 d D . . H31A H 0.5451 0.8713 0.5264 0.254 Uiso 1 1 calc R . . H31B H 0.5562 0.7867 0.4593 0.254 Uiso 1 1 calc R . . H31C H 0.6072 0.7583 0.5405 0.254 Uiso 1 1 calc R . . C33 C 0.5269(5) 0.5679(9) 0.4970(6) 0.116(3) Uiso 1 1 d D . . H33A H 0.5784 0.5495 0.5259 0.139 Uiso 1 1 calc R . . H33B H 0.5266 0.5789 0.4453 0.139 Uiso 1 1 calc R . . C32 C 0.5048(7) 0.6865(11) 0.5211(6) 0.129(4) Uiso 1 1 d D . . H32B H 0.5060 0.6802 0.5732 0.155 Uiso 1 1 calc R . . H32A H 0.4541 0.7103 0.4919 0.155 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 0.0241(2) 0.02011(18) 0.0243(2) 0.00264(16) 0.00890(15) 0.00011(16) Si1 0.0357(8) 0.0253(6) 0.0318(7) -0.0015(5) 0.0134(6) -0.0012(6) Cl1 0.0316(6) 0.0252(5) 0.0335(6) 0.0051(4) 0.0142(5) -0.0017(4) P1 0.0295(7) 0.0300(6) 0.0289(6) 0.0038(5) 0.0068(5) -0.0046(5) P2 0.0275(6) 0.0221(5) 0.0238(5) 0.0013(5) 0.0091(5) 0.0017(5) N1 0.030(2) 0.0262(19) 0.036(2) 0.0020(16) 0.0151(18) 0.0021(16) N2 0.027(2) 0.0253(18) 0.0192(17) 0.0016(15) 0.0060(15) -0.0013(15) C1 0.031(3) 0.033(2) 0.041(3) -0.004(2) 0.012(2) 0.002(2) C2 0.039(3) 0.035(3) 0.055(3) 0.002(2) 0.015(3) 0.012(2) C3 0.044(4) 0.063(4) 0.067(4) 0.008(3) 0.010(3) 0.023(3) C4 0.034(4) 0.086(5) 0.085(5) 0.003(4) 0.011(3) 0.022(3) C5 0.033(3) 0.079(4) 0.087(5) -0.011(4) 0.030(3) -0.003(3) C6 0.036(3) 0.047(3) 0.053(3) -0.005(3) 0.020(3) -0.001(2) C7 0.053(4) 0.060(4) 0.079(4) 0.003(3) 0.042(3) -0.008(3) C8 0.054(4) 0.042(3) 0.076(4) 0.027(3) 0.021(3) 0.010(3) C9 0.039(3) 0.021(2) 0.025(2) 0.0015(18) 0.016(2) 0.0024(19) C10 0.042(3) 0.031(2) 0.038(3) 0.001(2) 0.020(2) -0.001(2) C11 0.061(4) 0.030(3) 0.052(3) 0.003(2) 0.036(3) -0.005(2) C12 0.086(5) 0.025(2) 0.044(3) 0.013(2) 0.039(3) 0.013(3) C13 0.064(4) 0.029(2) 0.029(2) 0.006(2) 0.020(2) 0.018(2) C14 0.047(3) 0.025(2) 0.027(2) 0.0006(19) 0.015(2) 0.007(2) C15 0.047(3) 0.043(3) 0.024(2) 0.002(2) 0.003(2) 0.010(2) C16 0.050(4) 0.050(3) 0.061(4) 0.007(3) 0.017(3) -0.019(3) C17 0.069(4) 0.039(3) 0.040(3) -0.001(2) 0.023(3) -0.007(3) C18 0.047(3) 0.033(3) 0.047(3) -0.008(2) 0.015(3) -0.006(2) C19 0.053(4) 0.060(3) 0.031(3) 0.012(2) 0.006(2) -0.012(3) C20 0.046(3) 0.038(3) 0.052(3) -0.007(2) 0.004(3) -0.009(2) C21 0.033(3) 0.064(4) 0.046(3) 0.002(3) 0.008(2) -0.004(3) C22 0.039(3) 0.025(2) 0.037(3) 0.001(2) 0.015(2) 0.004(2) C23 0.032(3) 0.027(2) 0.034(2) 0.000(2) 0.011(2) 0.004(2) C24 0.035(3) 0.039(3) 0.030(2) 0.002(2) 0.014(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 1.756(3) . ? Mo1 N1 2.122(3) . ? Mo1 P1 2.4821(15) . ? Mo1 P2 2.4975(12) . ? Mo1 Cl1 2.5503(11) . ? Mo1 Si1 2.6675(13) . ? Mo1 H 1.92(4) . ? Si1 N1 1.676(4) . ? Si1 C18 1.853(5) . ? Si1 C17 1.862(5) . ? Si1 H 1.54(4) . ? P1 C19 1.809(5) . ? P1 C20 1.815(5) . ? P1 C21 1.816(5) . ? P2 C22 1.818(4) . ? P2 C24 1.820(4) . ? P2 C23 1.822(5) . ? N1 C1 1.400(6) . ? N2 C9 1.400(5) . ? C1 C6 1.407(7) . ? C1 C2 1.416(7) . ? C2 C3 1.389(7) . ? C2 C8 1.501(7) . ? C3 C4 1.367(9) . ? C3 H3A 0.9300 . ? C4 C5 1.374(9) . ? C4 H4A 0.9300 . ? C5 C6 1.388(8) . ? C5 H5A 0.9300 . ? C6 C7 1.512(8) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.410(6) . ? C9 C14 1.415(6) . ? C10 C11 1.397(6) . ? C10 C16 1.507(7) . ? C11 C12 1.378(8) . ? C11 H11A 0.9300 . ? C12 C13 1.379(7) . ? C12 H12A 0.9300 . ? C13 C14 1.378(6) . ? C13 H13A 0.9300 . ? C14 C15 1.506(7) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C31 C32 1.417(11) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C33 C32 1.356(11) . ? C33 C33 1.692(17) 3_666 ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C32 H32B 0.9700 . ? C32 H32A 0.9700 . ? 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 105.35(14) . . ? N2 Mo1 P1 98.26(11) . . ? N1 Mo1 P1 97.94(11) . . ? N2 Mo1 P2 90.51(12) . . ? N1 Mo1 P2 158.63(10) . . ? P1 Mo1 P2 93.75(4) . . ? N2 Mo1 Cl1 164.11(12) . . ? N1 Mo1 Cl1 87.71(10) . . ? P1 Mo1 Cl1 88.64(4) . . ? P2 Mo1 Cl1 74.70(4) . . ? N2 Mo1 Si1 100.29(11) . . ? N1 Mo1 Si1 38.91(11) . . ? P1 Mo1 Si1 136.31(4) . . ? P2 Mo1 Si1 125.11(4) . . ? Cl1 Mo1 Si1 84.09(4) . . ? N2 Mo1 H 93.1(11) . . ? N1 Mo1 H 73.4(12) . . ? P1 Mo1 H 167.3(11) . . ? P2 Mo1 H 91.8(12) . . ? Cl1 Mo1 H 81.8(11) . . ? Si1 Mo1 H 34.5(12) . . ? N1 Si1 C18 120.0(2) . . ? N1 Si1 C17 117.9(2) . . ? C18 Si1 C17 109.6(2) . . ? N1 Si1 Mo1 52.67(12) . . ? C18 Si1 Mo1 125.84(16) . . ? C17 Si1 Mo1 119.93(16) . . ? N1 Si1 H 97.6(14) . . ? C18 Si1 H 105.4(15) . . ? C17 Si1 H 103.2(14) . . ? Mo1 Si1 H 45.0(14) . . ? C19 P1 C20 102.0(3) . . ? C19 P1 C21 100.8(3) . . ? C20 P1 C21 101.8(3) . . ? C19 P1 Mo1 115.71(18) . . ? C20 P1 Mo1 117.06(18) . . ? C21 P1 Mo1 116.85(18) . . ? C22 P2 C24 100.6(2) . . ? C22 P2 C23 102.9(2) . . ? C24 P2 C23 99.9(2) . . ? C22 P2 Mo1 116.25(15) . . ? C24 P2 Mo1 121.69(16) . . ? C23 P2 Mo1 112.72(14) . . ? C1 N1 Si1 134.7(3) . . ? C1 N1 Mo1 136.7(3) . . ? Si1 N1 Mo1 88.42(16) . . ? C9 N2 Mo1 170.7(3) . . ? N1 C1 C6 121.0(4) . . ? N1 C1 C2 120.5(4) . . ? C6 C1 C2 118.5(5) . . ? C3 C2 C1 119.3(5) . . ? C3 C2 C8 119.7(5) . . ? C1 C2 C8 120.9(5) . . ? C4 C3 C2 121.7(6) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 119.3(6) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C5 C6 C1 119.6(5) . . ? C5 C6 C7 121.0(5) . . ? C1 C6 C7 119.4(5) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C10 120.4(4) . . ? N2 C9 C14 119.6(4) . . ? C10 C9 C14 119.9(4) . . ? C11 C10 C9 118.8(5) . . ? C11 C10 C16 119.5(5) . . ? C9 C10 C16 121.7(4) . . ? C12 C11 C10 120.8(5) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C11 C12 C13 120.0(4) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 121.6(5) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C9 118.8(5) . . ? C13 C14 C15 119.3(4) . . ? C9 C14 C15 121.9(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P1 C19 H19A 109.5 . . ? P1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P1 C20 H20A 109.5 . . ? P1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P1 C21 H21A 109.5 . . ? P1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P2 C23 H23A 109.5 . . ? P2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? P2 C24 H24A 109.5 . . ? P2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? P2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C32 C33 C33 114.8(10) . 3_666 ? C32 C33 H33A 108.6 . . ? C33 C33 H33A 108.6 3_666 . ? C32 C33 H33B 108.6 . . ? C33 C33 H33B 108.6 3_666 . ? H33A C33 H33B 107.5 . . ? C33 C32 C31 104.6(9) . . ? C33 C32 H32B 110.8 . . ? C31 C32 H32B 110.8 . . ? C33 C32 H32A 110.8 . . ? C31 C32 H32A 110.8 . . ? H32B C32 H32A 108.9 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.029 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.103 #END# data_gin10 _database_code_depnum_ccdc_archive 'CCDC 226163' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2,6-dimethylphenylimido)(bis(trimethylphosphine))(chloro) ((2,6-dimethylphenyl)(chloromethylsilyl)amido)molybdenum (IV) ; _chemical_name_common ; (2,6-dimethylphenylimido)(bis(trimethylphosphine))(chloro) ((2,6-dimethylphenyl)(chloromethylsilyl)amido)molybdenum (IV) ; _chemical_melting_point ? _chemical_formula_moiety (2,6-Me2C6H3N)((2,6-Me2C6H3)(HMeClSi)N)MoCl(PMe3)2 _chemical_formula_sum 'C26 H47 Cl2 Mo N2 P2 Si' _chemical_formula_weight 644.53 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' P P 0.1023 0.0942 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.403(4) _cell_length_b 9.920(2) _cell_length_c 18.548(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.78(3) _cell_angle_gamma 90.00 _cell_volume 3258.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8464 _exptl_absorpt_correction_T_max 0.9788 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 'not measured' _diffrn_standards_decay_% 0 _diffrn_reflns_number 13541 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.1112 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.27 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7696 _reflns_number_gt 4729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0459P)^2^+5.1402P] 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 7696 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.054 _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 Mo1 Mo 0.31633(2) 0.82226(4) 0.80956(2) 0.02229(12) Uani 1 1 d . . . Si1 Si 0.33763(8) 1.03068(12) 0.90296(7) 0.0301(3) Uani 1 1 d . . . H H 0.3838(19) 0.909(3) 0.8948(19) 0.011(9) Uiso 1 1 d . . . Cl1 Cl 0.38040(6) 0.97943(11) 0.73791(6) 0.0297(3) Uani 1 1 d . . . Cl2 Cl 0.33221(9) 1.00254(14) 1.01255(7) 0.0537(4) Uani 1 1 d . . . P1 P 0.41992(6) 0.68526(11) 0.78341(6) 0.0249(3) Uani 1 1 d . . . P2 P 0.22482(7) 0.76090(13) 0.68955(6) 0.0305(3) Uani 1 1 d . . . N1 N 0.2602(2) 0.9986(4) 0.8364(2) 0.0298(9) Uani 1 1 d . . . N2 N 0.2944(2) 0.6928(3) 0.86441(19) 0.0271(8) Uani 1 1 d . . . C1 C 0.1874(3) 1.0567(5) 0.8107(3) 0.0358(12) Uani 1 1 d . . . C2 C 0.1275(3) 1.0086(5) 0.8374(3) 0.0463(13) Uani 1 1 d . . . C3 C 0.0555(3) 1.0642(8) 0.8077(4) 0.0674(19) Uani 1 1 d . . . H3A H 0.0153 1.0324 0.8243 0.081 Uiso 1 1 calc R . . C4 C 0.0432(4) 1.1637(7) 0.7552(4) 0.0678(18) Uani 1 1 d . . . H4A H -0.0050 1.1989 0.7363 0.081 Uiso 1 1 calc R . . C5 C 0.1018(3) 1.2119(6) 0.7303(3) 0.0577(16) Uani 1 1 d . . . H5A H 0.0930 1.2807 0.6949 0.069 Uiso 1 1 calc R . . C6 C 0.1740(3) 1.1599(5) 0.7570(3) 0.0399(12) Uani 1 1 d . . . C7 C 0.1416(4) 0.9015(6) 0.8970(4) 0.0639(18) Uani 1 1 d . . . H7A H 0.1728 0.8320 0.8853 0.096 Uiso 1 1 calc R . . H7B H 0.0943 0.8633 0.8993 0.096 Uiso 1 1 calc R . . H7C H 0.1666 0.9407 0.9446 0.096 Uiso 1 1 calc R . . C8 C 0.2364(3) 1.2169(6) 0.7284(3) 0.0560(16) Uani 1 1 d . . . H8A H 0.2153 1.2704 0.6846 0.084 Uiso 1 1 calc R . . H8B H 0.2655 1.1446 0.7160 0.084 Uiso 1 1 calc R . . H8C H 0.2685 1.2723 0.7665 0.084 Uiso 1 1 calc R . . C9 C 0.3951(3) 1.1833(5) 0.9056(3) 0.0403(12) Uani 1 1 d . . . H9A H 0.3910 1.2397 0.9464 0.060 Uiso 1 1 calc R . . H9B H 0.3773 1.2317 0.8593 0.060 Uiso 1 1 calc R . . H9C H 0.4469 1.1583 0.9126 0.060 Uiso 1 1 calc R . . C10 C 0.2901(3) 0.5864(5) 0.9127(2) 0.0319(11) Uani 1 1 d . . . C11 C 0.3509(3) 0.5643(5) 0.9768(2) 0.0363(12) Uani 1 1 d . . . C12 C 0.3456(4) 0.4578(6) 1.0232(3) 0.0494(16) Uani 1 1 d . . . H12A H 0.3850 0.4427 1.0659 0.059 Uiso 1 1 calc R . . C13 C 0.2844(4) 0.3742(6) 1.0085(4) 0.0602(19) Uani 1 1 d . . . H13A H 0.2832 0.3018 1.0401 0.072 Uiso 1 1 calc R . . C14 C 0.2241(4) 0.3976(5) 0.9464(3) 0.0548(16) Uani 1 1 d . . . H14A H 0.1822 0.3410 0.9367 0.066 Uiso 1 1 calc R . . C15 C 0.2252(3) 0.5043(5) 0.8986(3) 0.0387(12) Uani 1 1 d . . . C16 C 0.4193(3) 0.6545(5) 0.9964(3) 0.0462(14) Uani 1 1 d . . . H16A H 0.4549 0.6212 1.0408 0.069 Uiso 1 1 calc R . . H16B H 0.4043 0.7443 1.0052 0.069 Uiso 1 1 calc R . . H16C H 0.4423 0.6554 0.9558 0.069 Uiso 1 1 calc R . . C17 C 0.1567(3) 0.5323(6) 0.8345(3) 0.0588(16) Uani 1 1 d . . . H17A H 0.1134 0.5431 0.8533 0.088 Uiso 1 1 calc R . . H17B H 0.1485 0.4582 0.7999 0.088 Uiso 1 1 calc R . . H17C H 0.1646 0.6133 0.8093 0.088 Uiso 1 1 calc R . . C18 C 0.4239(3) 0.5083(4) 0.8108(3) 0.0338(11) Uani 1 1 d . . . H18A H 0.4656 0.4654 0.7982 0.051 Uiso 1 1 calc R . . H18B H 0.3777 0.4644 0.7848 0.051 Uiso 1 1 calc R . . H18C H 0.4306 0.5019 0.8638 0.051 Uiso 1 1 calc R . . C19 C 0.5131(3) 0.7479(5) 0.8331(3) 0.0330(11) Uani 1 1 d . . . H19A H 0.5511 0.6925 0.8214 0.050 Uiso 1 1 calc R . . H19B H 0.5188 0.7453 0.8861 0.050 Uiso 1 1 calc R . . H19C H 0.5186 0.8391 0.8180 0.050 Uiso 1 1 calc R . . C20 C 0.4307(3) 0.6712(5) 0.6887(2) 0.0330(11) Uani 1 1 d . . . H20A H 0.4733 0.6149 0.6894 0.050 Uiso 1 1 calc R . . H20B H 0.4385 0.7592 0.6706 0.050 Uiso 1 1 calc R . . H20C H 0.3859 0.6321 0.6563 0.050 Uiso 1 1 calc R . . C21 C 0.2194(3) 0.5842(5) 0.6625(3) 0.0477(14) Uani 1 1 d . . . H21A H 0.1822 0.5732 0.6154 0.072 Uiso 1 1 calc R . . H21B H 0.2055 0.5313 0.7000 0.072 Uiso 1 1 calc R . . H21C H 0.2677 0.5549 0.6580 0.072 Uiso 1 1 calc R . . C22 C 0.1266(3) 0.8036(6) 0.6809(3) 0.0471(14) Uani 1 1 d . . . H22A H 0.0959 0.7758 0.6326 0.071 Uiso 1 1 calc R . . H22B H 0.1220 0.8993 0.6862 0.071 Uiso 1 1 calc R . . H22C H 0.1101 0.7583 0.7194 0.071 Uiso 1 1 calc R . . C23 C 0.2387(3) 0.8415(6) 0.6066(3) 0.0487(14) Uani 1 1 d . . . H23A H 0.2006 0.8111 0.5632 0.073 Uiso 1 1 calc R . . H23B H 0.2877 0.8185 0.6014 0.073 Uiso 1 1 calc R . . H23C H 0.2351 0.9375 0.6112 0.073 Uiso 1 1 calc R . . C31 C -0.0256(4) 0.9428(7) 0.5027(4) 0.082(2) Uiso 1 1 d . . . H31A H -0.0253 0.9326 0.5548 0.098 Uiso 1 1 calc R . . H31B H -0.0766 0.9669 0.4748 0.098 Uiso 1 1 calc R . . C30 C -0.0072(5) 0.8114(8) 0.4752(5) 0.089(2) Uiso 1 1 d . . . H30A H 0.0439 0.7875 0.5027 0.107 Uiso 1 1 calc R . . H30B H -0.0081 0.8210 0.4229 0.107 Uiso 1 1 calc R . . C32 C -0.0589(5) 0.6965(9) 0.4818(5) 0.109(3) Uiso 1 1 d . . . H32A H -0.0423 0.6154 0.4629 0.164 Uiso 1 1 calc R . . H32B H -0.1095 0.7170 0.4533 0.164 Uiso 1 1 calc R . . H32C H -0.0576 0.6840 0.5335 0.164 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 0.0277(2) 0.0225(2) 0.01739(19) 0.00327(16) 0.00750(14) 0.00075(17) Si1 0.0397(8) 0.0276(7) 0.0242(7) -0.0008(5) 0.0108(6) 0.0017(6) Cl1 0.0342(6) 0.0278(6) 0.0301(6) 0.0054(5) 0.0139(5) -0.0022(5) Cl2 0.0921(12) 0.0461(8) 0.0271(7) 0.0028(6) 0.0234(7) 0.0091(7) P1 0.0314(6) 0.0265(6) 0.0175(5) 0.0005(5) 0.0079(5) 0.0025(5) P2 0.0328(7) 0.0358(7) 0.0219(6) 0.0049(5) 0.0057(5) -0.0042(5) N1 0.036(2) 0.025(2) 0.032(2) 0.0055(16) 0.0142(18) 0.0035(16) N2 0.032(2) 0.029(2) 0.0199(18) 0.0014(15) 0.0075(16) 0.0008(16) C1 0.036(3) 0.041(3) 0.034(3) -0.011(2) 0.015(2) 0.001(2) C2 0.044(3) 0.050(3) 0.052(3) -0.004(3) 0.025(3) -0.001(3) C3 0.037(4) 0.096(5) 0.079(5) -0.024(4) 0.032(3) -0.003(3) C4 0.043(4) 0.092(5) 0.064(4) -0.002(4) 0.006(3) 0.021(4) C5 0.053(4) 0.063(4) 0.052(4) 0.002(3) 0.006(3) 0.022(3) C6 0.038(3) 0.036(3) 0.044(3) 0.004(2) 0.010(2) 0.012(2) C7 0.063(4) 0.069(4) 0.077(5) -0.001(4) 0.048(4) -0.013(3) C8 0.060(4) 0.043(3) 0.065(4) 0.027(3) 0.018(3) 0.016(3) C9 0.045(3) 0.042(3) 0.037(3) -0.010(2) 0.017(2) -0.006(2) C10 0.051(3) 0.027(3) 0.023(2) 0.0042(19) 0.018(2) 0.006(2) C11 0.065(4) 0.032(3) 0.017(2) 0.0057(19) 0.019(2) 0.018(2) C12 0.089(5) 0.043(3) 0.024(3) 0.013(2) 0.029(3) 0.030(3) C13 0.109(6) 0.037(3) 0.057(4) 0.022(3) 0.060(4) 0.026(4) C14 0.085(5) 0.038(3) 0.060(4) 0.003(3) 0.051(4) -0.001(3) C15 0.061(4) 0.031(3) 0.033(3) 0.004(2) 0.027(3) 0.002(2) C16 0.059(4) 0.052(3) 0.023(3) -0.001(2) 0.002(2) 0.017(3) C17 0.060(4) 0.060(4) 0.059(4) 0.006(3) 0.020(3) -0.024(3) C18 0.049(3) 0.026(3) 0.029(3) 0.0025(19) 0.015(2) 0.009(2) C19 0.037(3) 0.032(3) 0.029(3) 0.000(2) 0.009(2) 0.007(2) C20 0.041(3) 0.039(3) 0.021(2) 0.000(2) 0.011(2) 0.003(2) C21 0.051(4) 0.042(3) 0.043(3) -0.008(2) 0.001(3) -0.009(3) C22 0.034(3) 0.062(4) 0.042(3) 0.010(3) 0.005(2) -0.004(3) C23 0.050(3) 0.067(4) 0.027(3) 0.015(3) 0.006(2) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N2 1.752(3) . ? Mo1 N1 2.157(4) . ? Mo1 P2 2.4743(15) . ? Mo1 P1 2.4938(12) . ? Mo1 Cl1 2.5376(12) . ? Mo1 Si1 2.6571(13) . ? Mo1 H 1.93(3) . ? Si1 N1 1.643(4) . ? Si1 C9 1.839(5) . ? Si1 Cl2 2.0809(18) . ? Si1 H 1.51(3) . ? P1 C19 1.822(5) . ? P1 C18 1.823(4) . ? P1 C20 1.826(4) . ? P2 C23 1.813(5) . ? P2 C21 1.818(5) . ? P2 C22 1.821(5) . ? N1 C1 1.417(6) . ? N2 C10 1.400(5) . ? C1 C6 1.402(7) . ? C1 C2 1.409(7) . ? C2 C3 1.403(8) . ? C2 C7 1.505(8) . ? C3 C4 1.361(9) . ? C3 H3A 0.9300 . ? C4 C5 1.369(9) . ? C4 H4A 0.9300 . ? C5 C6 1.385(7) . ? C5 H5A 0.9300 . ? C6 C8 1.501(7) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C15 1.410(7) . ? C10 C11 1.411(7) . ? C11 C12 1.382(7) . ? C11 C16 1.506(7) . ? C12 C13 1.365(8) . ? C12 H12A 0.9300 . ? C13 C14 1.385(9) . ? C13 H13A 0.9300 . ? C14 C15 1.386(7) . ? C14 H14A 0.9300 . ? C15 C17 1.505(8) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C31 C30 1.473(9) . ? C31 C31 1.495(13) 3_576 ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C30 C32 1.510(10) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? 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 105.08(15) . . ? N2 Mo1 P2 97.72(12) . . ? N1 Mo1 P2 98.96(11) . . ? N2 Mo1 P1 91.28(12) . . ? N1 Mo1 P1 157.81(10) . . ? P2 Mo1 P1 93.45(4) . . ? N2 Mo1 Cl1 165.35(12) . . ? N1 Mo1 Cl1 86.70(10) . . ? P2 Mo1 Cl1 88.83(4) . . ? P1 Mo1 Cl1 75.18(4) . . ? N2 Mo1 Si1 102.01(12) . . ? N1 Mo1 Si1 38.15(11) . . ? P2 Mo1 Si1 136.19(4) . . ? P1 Mo1 Si1 124.46(5) . . ? Cl1 Mo1 Si1 81.73(4) . . ? N2 Mo1 H 92.8(10) . . ? N1 Mo1 H 72.0(10) . . ? P2 Mo1 H 167.7(10) . . ? P1 Mo1 H 92.7(10) . . ? Cl1 Mo1 H 82.5(10) . . ? Si1 Mo1 H 33.9(10) . . ? N1 Si1 C9 123.7(2) . . ? N1 Si1 Cl2 116.50(15) . . ? C9 Si1 Cl2 105.30(17) . . ? N1 Si1 Mo1 54.20(13) . . ? C9 Si1 Mo1 129.79(16) . . ? Cl2 Si1 Mo1 119.65(7) . . ? N1 Si1 H 99.6(13) . . ? C9 Si1 H 109.1(13) . . ? Cl2 Si1 H 99.7(13) . . ? Mo1 Si1 H 45.4(13) . . ? C19 P1 C18 103.1(2) . . ? C19 P1 C20 100.3(2) . . ? C18 P1 C20 100.8(2) . . ? C19 P1 Mo1 112.35(15) . . ? C18 P1 Mo1 116.47(16) . . ? C20 P1 Mo1 121.17(16) . . ? C23 P2 C21 101.6(3) . . ? C23 P2 C22 100.9(3) . . ? C21 P2 C22 102.8(3) . . ? C23 P2 Mo1 115.89(18) . . ? C21 P2 Mo1 117.25(18) . . ? C22 P2 Mo1 116.00(18) . . ? C1 N1 Si1 136.2(3) . . ? C1 N1 Mo1 136.1(3) . . ? Si1 N1 Mo1 87.65(16) . . ? C10 N2 Mo1 170.3(3) . . ? C6 C1 C2 119.5(5) . . ? C6 C1 N1 120.3(4) . . ? C2 C1 N1 120.2(5) . . ? C3 C2 C1 118.4(5) . . ? C3 C2 C7 121.4(5) . . ? C1 C2 C7 120.2(5) . . ? C4 C3 C2 121.3(6) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 121.0(6) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 119.5(5) . . ? C5 C6 C8 119.1(5) . . ? C1 C6 C8 121.4(4) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C15 120.6(4) . . ? N2 C10 C11 119.1(4) . . ? C15 C10 C11 120.2(4) . . ? C12 C11 C10 118.0(5) . . ? C12 C11 C16 120.0(5) . . ? C10 C11 C16 122.0(4) . . ? C13 C12 C11 122.4(5) . . ? C13 C12 H12A 118.8 . . ? C11 C12 H12A 118.8 . . ? C12 C13 C14 119.7(5) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C13 C14 C15 120.8(6) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C14 C15 C10 118.9(5) . . ? C14 C15 C17 119.4(5) . . ? C10 C15 C17 121.7(4) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P1 C18 H18A 109.5 . . ? P1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P1 C19 H19A 109.5 . . ? P1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P1 C20 H20A 109.5 . . ? P1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P2 C21 H21A 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P2 C22 H22A 109.5 . . ? P2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P2 C23 H23A 109.5 . . ? P2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? P2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C30 C31 C31 116.2(8) . 3_576 ? C30 C31 H31A 108.2 . . ? C31 C31 H31A 108.2 3_576 . ? C30 C31 H31B 108.2 . . ? C31 C31 H31B 108.2 3_576 . ? H31A C31 H31B 107.4 . . ? C31 C30 C32 115.5(7) . . ? C31 C30 H30A 108.4 . . ? C32 C30 H30A 108.4 . . ? C31 C30 H30B 108.4 . . ? C32 C30 H30B 108.4 . . ? H30A C30 H30B 107.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.386 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.108