Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Odom, Aaron' 'Katayev, Evgeny' 'Li, Yahong' _publ_contact_author_name 'Prof Aaron Odom' _publ_contact_author_address ; Chemistry Michigan State University Department of Chemistry East Lansing 48824 UNITED STATES OF AMERICA ; _publ_contact_author_email 'ODOM@CEM.MSU.EDU' _publ_section_title ; Insertion of an electron-rich alkyne into a molybdenum amido bond ; data_Mo(NMe2)2(NHMe2)(dpma) _database_code_CSD 179378 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H32 Mo N6' _chemical_formula_weight 416.43 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.12(2) _cell_length_b 15.30(3) _cell_length_c 17.118(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3958(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelpiped _exptl_crystal_colour brown _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type emperical _exptl_absorpt_correction_T_min 0.1442 _exptl_absorpt_correction_T_max 0.3652 _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 CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16751 _diffrn_reflns_av_R_equivalents 0.2544 _diffrn_reflns_av_sigmaI/netI 0.1314 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 23.32 _reflns_number_total 2853 _reflns_number_gt 1628 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^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 0.00000(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2853 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1419 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.631 _refine_ls_shift/su_mean 0.009 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 0.09876(4) 0.23415(4) 0.61503(4) 0.0231(3) Uani 1 1 d . . . N1 N 0.1510(4) 0.1536(4) 0.7047(4) 0.0290(16) Uani 1 1 d . . . N2 N -0.0050(4) 0.2990(4) 0.5517(4) 0.0337(16) Uani 1 1 d . . . N3 N -0.0240(4) 0.1913(4) 0.6759(3) 0.0265(15) Uani 1 1 d . . . N4 N 0.1086(4) 0.3382(4) 0.6845(3) 0.0333(16) Uani 1 1 d . . . N5 N 0.1020(4) 0.1315(4) 0.5413(4) 0.0357(16) Uani 1 1 d . . . N6 N 0.2264(4) 0.2773(5) 0.5590(4) 0.0367(18) Uani 1 1 d . . . H6A H 0.243(4) 0.224(4) 0.542(4) 0.02(2) Uiso 1 1 d . . . C11 C 0.2268(5) 0.1099(5) 0.7224(5) 0.034(2) Uani 1 1 d . . . H11A H 0.2802 0.1169 0.6963 0.041 Uiso 1 1 calc R . . C12 C 0.2135(5) 0.0546(5) 0.7839(5) 0.042(2) Uani 1 1 d . . . H12A H 0.2554 0.0178 0.8063 0.050 Uiso 1 1 calc R . . C13 C 0.1252(5) 0.0634(5) 0.8068(5) 0.033(2) Uani 1 1 d . . . H13A H 0.0966 0.0332 0.8466 0.040 Uiso 1 1 calc R . . C14 C 0.0899(5) 0.1252(5) 0.7590(5) 0.033(2) Uani 1 1 d . . . C21 C -0.0183(6) 0.3467(5) 0.4848(5) 0.042(2) Uani 1 1 d . . . H21A H 0.0238 0.3544 0.4458 0.051 Uiso 1 1 calc R . . C22 C -0.1010(6) 0.3811(5) 0.4831(5) 0.046(2) Uani 1 1 d . . . H22A H -0.1248 0.4159 0.4437 0.055 Uiso 1 1 calc R . . C23 C -0.1441(6) 0.3545(6) 0.5518(5) 0.047(2) Uani 1 1 d . . . H23A H -0.2013 0.3685 0.5676 0.056 Uiso 1 1 calc R . . C24 C -0.0843(5) 0.3036(5) 0.5906(4) 0.0294(19) Uani 1 1 d . . . C31 C 0.0006(5) 0.1690(5) 0.7569(4) 0.038(2) Uani 1 1 d . . . H31A H -0.0436 0.1301 0.7790 0.046 Uiso 1 1 calc R . . H31B H 0.0022 0.2217 0.7883 0.046 Uiso 1 1 calc R . . C32 C -0.0885(5) 0.2652(6) 0.6720(5) 0.041(2) Uani 1 1 d . . . H32A H -0.0735 0.3093 0.7105 0.050 Uiso 1 1 calc R . . H32B H -0.1478 0.2442 0.6829 0.050 Uiso 1 1 calc R . . C33 C -0.0627(5) 0.1115(5) 0.6386(5) 0.044(2) Uani 1 1 d . . . H33A H -0.1155 0.0948 0.6660 0.066 Uiso 1 1 calc R . . H33B H -0.0205 0.0646 0.6407 0.066 Uiso 1 1 calc R . . H33C H -0.0769 0.1240 0.5850 0.066 Uiso 1 1 calc R . . C41 C 0.1471(6) 0.3422(6) 0.7633(5) 0.059(3) Uani 1 1 d . . . H41A H 0.1422 0.4007 0.7831 0.088 Uiso 1 1 calc R . . H41B H 0.2084 0.3258 0.7609 0.088 Uiso 1 1 calc R . . H41C H 0.1160 0.3028 0.7972 0.088 Uiso 1 1 calc R . . C42 C 0.0861(6) 0.4280(5) 0.6613(5) 0.054(3) Uani 1 1 d . . . H42A H 0.0955 0.4666 0.7047 0.081 Uiso 1 1 calc R . . H42B H 0.0252 0.4304 0.6457 0.081 Uiso 1 1 calc R . . H42C H 0.1230 0.4455 0.6185 0.081 Uiso 1 1 calc R . . C51 C 0.1355(5) 0.0445(5) 0.5564(5) 0.050(3) Uani 1 1 d . . . H51A H 0.1290 0.0093 0.5104 0.075 Uiso 1 1 calc R . . H51B H 0.1028 0.0186 0.5986 0.075 Uiso 1 1 calc R . . H51C H 0.1969 0.0479 0.5704 0.075 Uiso 1 1 calc R . . C52 C 0.0828(6) 0.1392(6) 0.4591(5) 0.050(2) Uani 1 1 d . . . H52A H 0.0881 0.0828 0.4348 0.074 Uiso 1 1 calc R . . H52B H 0.1239 0.1790 0.4354 0.074 Uiso 1 1 calc R . . H52C H 0.0237 0.1607 0.4523 0.074 Uiso 1 1 calc R . . C61 C 0.2162(5) 0.3358(5) 0.4910(5) 0.052(3) Uani 1 1 d . . . H61A H 0.2734 0.3498 0.4702 0.077 Uiso 1 1 calc R . . H61B H 0.1869 0.3886 0.5069 0.077 Uiso 1 1 calc R . . H61C H 0.1816 0.3071 0.4516 0.077 Uiso 1 1 calc R . . C62 C 0.2953(5) 0.3131(6) 0.6120(6) 0.061(3) Uani 1 1 d . . . H62A H 0.3470 0.3281 0.5822 0.091 Uiso 1 1 calc R . . H62B H 0.3106 0.2700 0.6505 0.091 Uiso 1 1 calc R . . H62C H 0.2730 0.3645 0.6376 0.091 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 0.0262(4) 0.0176(4) 0.0256(4) 0.0001(3) 0.0001(3) -0.0024(3) N1 0.027(4) 0.024(4) 0.036(4) -0.006(3) 0.004(3) -0.002(3) N2 0.042(4) 0.029(4) 0.030(4) 0.006(3) 0.000(4) -0.002(3) N3 0.030(4) 0.018(4) 0.032(4) 0.005(3) -0.001(3) 0.002(3) N4 0.059(4) 0.012(3) 0.029(4) -0.005(3) -0.006(4) 0.005(3) N5 0.040(4) 0.033(4) 0.034(4) -0.003(3) 0.001(4) -0.007(3) N6 0.036(4) 0.022(5) 0.052(5) -0.002(4) 0.007(4) -0.006(3) C11 0.025(5) 0.023(5) 0.053(6) 0.003(4) 0.000(4) -0.002(4) C12 0.048(6) 0.023(5) 0.055(6) 0.001(4) -0.022(5) 0.003(4) C13 0.034(5) 0.028(5) 0.037(5) 0.014(4) -0.003(4) 0.002(3) C14 0.041(5) 0.025(5) 0.034(5) 0.002(4) 0.002(5) 0.002(4) C21 0.050(6) 0.039(6) 0.037(5) 0.014(4) -0.001(5) -0.011(4) C22 0.048(6) 0.043(6) 0.046(6) 0.023(4) -0.021(6) -0.006(5) C23 0.035(5) 0.044(6) 0.060(6) 0.004(5) -0.003(5) 0.006(4) C24 0.027(5) 0.027(4) 0.034(5) 0.002(4) -0.002(4) 0.002(3) C31 0.044(5) 0.037(5) 0.033(5) 0.009(4) 0.006(4) 0.008(4) C32 0.030(5) 0.050(5) 0.043(5) 0.006(4) 0.009(4) 0.018(4) C33 0.032(5) 0.038(6) 0.062(6) 0.008(5) 0.001(4) -0.007(4) C41 0.098(8) 0.038(6) 0.040(6) -0.009(4) -0.019(6) 0.004(5) C42 0.085(7) 0.026(5) 0.051(6) -0.002(4) -0.014(6) 0.004(5) C51 0.054(6) 0.025(5) 0.071(7) -0.014(5) -0.001(5) -0.005(4) C52 0.059(7) 0.054(6) 0.036(5) -0.015(4) 0.001(5) -0.017(5) C61 0.048(6) 0.046(6) 0.061(6) 0.014(5) 0.010(5) -0.008(4) C62 0.032(5) 0.056(6) 0.095(8) 0.004(6) -0.008(6) -0.015(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 Mo N4 1.992(6) . ? Mo N5 2.015(7) . ? Mo N1 2.122(6) . ? Mo N2 2.149(6) . ? Mo N3 2.227(6) . ? Mo N6 2.253(7) . ? N1 C11 1.359(9) . ? N1 C14 1.380(9) . ? N2 C24 1.373(9) . ? N2 C21 1.373(9) . ? N3 C31 1.477(9) . ? N3 C32 1.494(9) . ? N3 C33 1.496(9) . ? N4 C42 1.469(9) . ? N4 C41 1.470(9) . ? N5 C52 1.441(10) . ? N5 C51 1.448(10) . ? N6 C61 1.476(10) . ? N6 C62 1.486(10) . ? C11 C12 1.365(10) . ? C12 C13 1.397(10) . ? C13 C14 1.361(10) . ? C14 C31 1.507(10) . ? C21 C22 1.358(11) . ? C22 C23 1.406(11) . ? C23 C24 1.365(11) . ? C24 C32 1.515(11) . ? 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 N4 Mo N5 174.0(3) . . ? N4 Mo N1 90.2(3) . . ? N5 Mo N1 89.5(3) . . ? N4 Mo N2 89.2(2) . . ? N5 Mo N2 93.5(3) . . ? N1 Mo N2 154.8(2) . . ? N4 Mo N3 91.0(2) . . ? N5 Mo N3 94.8(2) . . ? N1 Mo N3 78.5(2) . . ? N2 Mo N3 76.3(2) . . ? N4 Mo N6 87.5(3) . . ? N5 Mo N6 86.6(3) . . ? N1 Mo N6 99.2(2) . . ? N2 Mo N6 105.9(3) . . ? N3 Mo N6 177.3(2) . . ? C11 N1 C14 105.1(7) . . ? C11 N1 Mo 139.5(5) . . ? C14 N1 Mo 114.8(5) . . ? C24 N2 C21 104.4(6) . . ? C24 N2 Mo 114.6(5) . . ? C21 N2 Mo 140.6(6) . . ? C31 N3 C32 112.3(6) . . ? C31 N3 C33 108.2(6) . . ? C32 N3 C33 110.1(6) . . ? C31 N3 Mo 107.3(4) . . ? C32 N3 Mo 107.5(4) . . ? C33 N3 Mo 111.5(4) . . ? C42 N4 C41 107.4(6) . . ? C42 N4 Mo 124.6(5) . . ? C41 N4 Mo 127.6(5) . . ? C52 N5 C51 108.6(7) . . ? C52 N5 Mo 122.9(5) . . ? C51 N5 Mo 127.8(5) . . ? C61 N6 C62 109.3(7) . . ? C61 N6 Mo 115.1(5) . . ? C62 N6 Mo 116.7(5) . . ? C12 C11 N1 110.7(7) . . ? C11 C12 C13 107.3(7) . . ? C14 C13 C12 105.8(7) . . ? C13 C14 N1 111.1(7) . . ? C13 C14 C31 132.4(8) . . ? N1 C14 C31 116.4(7) . . ? C22 C21 N2 111.0(8) . . ? C21 C22 C23 107.3(8) . . ? C24 C23 C22 105.4(8) . . ? C23 C24 N2 111.9(7) . . ? C23 C24 C32 129.9(7) . . ? N2 C24 C32 117.6(6) . . ? N3 C31 C14 110.5(6) . . ? N3 C32 C24 107.9(6) . . ? 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 N4 Mo N1 C11 -107.3(8) . . . . ? N5 Mo N1 C11 66.7(8) . . . . ? N2 Mo N1 C11 163.9(7) . . . . ? N3 Mo N1 C11 161.7(8) . . . . ? N6 Mo N1 C11 -19.8(8) . . . . ? N4 Mo N1 C14 83.5(5) . . . . ? N5 Mo N1 C14 -102.5(5) . . . . ? N2 Mo N1 C14 -5.2(9) . . . . ? N3 Mo N1 C14 -7.5(5) . . . . ? N6 Mo N1 C14 171.0(5) . . . . ? N4 Mo N2 C24 -73.3(5) . . . . ? N5 Mo N2 C24 112.0(5) . . . . ? N1 Mo N2 C24 15.6(9) . . . . ? N3 Mo N2 C24 17.9(5) . . . . ? N6 Mo N2 C24 -160.5(5) . . . . ? N4 Mo N2 C21 98.6(8) . . . . ? N5 Mo N2 C21 -76.1(8) . . . . ? N1 Mo N2 C21 -172.5(7) . . . . ? N3 Mo N2 C21 -170.2(9) . . . . ? N6 Mo N2 C21 11.4(9) . . . . ? N4 Mo N3 C31 -65.2(5) . . . . ? N5 Mo N3 C31 113.4(5) . . . . ? N1 Mo N3 C31 24.9(4) . . . . ? N2 Mo N3 C31 -154.1(5) . . . . ? N6 Mo N3 C31 -8(5) . . . . ? N4 Mo N3 C32 55.9(5) . . . . ? N5 Mo N3 C32 -125.6(5) . . . . ? N1 Mo N3 C32 145.9(5) . . . . ? N2 Mo N3 C32 -33.1(5) . . . . ? N6 Mo N3 C32 113(5) . . . . ? N4 Mo N3 C33 176.6(5) . . . . ? N5 Mo N3 C33 -4.8(5) . . . . ? N1 Mo N3 C33 -93.4(5) . . . . ? N2 Mo N3 C33 87.6(5) . . . . ? N6 Mo N3 C33 -126(5) . . . . ? N5 Mo N4 C42 90(2) . . . . ? N1 Mo N4 C42 177.5(6) . . . . ? N2 Mo N4 C42 -27.7(6) . . . . ? N3 Mo N4 C42 -104.0(6) . . . . ? N6 Mo N4 C42 78.3(6) . . . . ? N5 Mo N4 C41 -83(2) . . . . ? N1 Mo N4 C41 4.5(7) . . . . ? N2 Mo N4 C41 159.3(7) . . . . ? N3 Mo N4 C41 83.0(7) . . . . ? N6 Mo N4 C41 -94.7(7) . . . . ? N4 Mo N5 C52 -85(2) . . . . ? N1 Mo N5 C52 -172.9(6) . . . . ? N2 Mo N5 C52 32.1(7) . . . . ? N3 Mo N5 C52 108.7(6) . . . . ? N6 Mo N5 C52 -73.7(6) . . . . ? N4 Mo N5 C51 85(2) . . . . ? N1 Mo N5 C51 -3.2(7) . . . . ? N2 Mo N5 C51 -158.2(7) . . . . ? N3 Mo N5 C51 -81.7(7) . . . . ? N6 Mo N5 C51 96.0(7) . . . . ? N4 Mo N6 C61 -90.8(6) . . . . ? N5 Mo N6 C61 90.3(6) . . . . ? N1 Mo N6 C61 179.3(6) . . . . ? N2 Mo N6 C61 -2.3(6) . . . . ? N3 Mo N6 C61 -148(5) . . . . ? N4 Mo N6 C62 39.3(6) . . . . ? N5 Mo N6 C62 -139.5(6) . . . . ? N1 Mo N6 C62 -50.5(6) . . . . ? N2 Mo N6 C62 127.8(6) . . . . ? N3 Mo N6 C62 -18(5) . . . . ? C14 N1 C11 C12 1.6(9) . . . . ? Mo N1 C11 C12 -168.2(5) . . . . ? N1 C11 C12 C13 -0.2(9) . . . . ? C11 C12 C13 C14 -1.3(9) . . . . ? C12 C13 C14 N1 2.3(9) . . . . ? C12 C13 C14 C31 -174.9(8) . . . . ? C11 N1 C14 C13 -2.4(9) . . . . ? Mo N1 C14 C13 170.3(5) . . . . ? C11 N1 C14 C31 175.3(7) . . . . ? Mo N1 C14 C31 -12.0(8) . . . . ? C24 N2 C21 C22 1.5(9) . . . . ? Mo N2 C21 C22 -170.9(6) . . . . ? N2 C21 C22 C23 -0.3(10) . . . . ? C21 C22 C23 C24 -1.1(10) . . . . ? C22 C23 C24 N2 2.1(10) . . . . ? C22 C23 C24 C32 172.0(8) . . . . ? C21 N2 C24 C23 -2.2(9) . . . . ? Mo N2 C24 C23 172.5(6) . . . . ? C21 N2 C24 C32 -173.5(7) . . . . ? Mo N2 C24 C32 1.2(8) . . . . ? C32 N3 C31 C14 -155.5(6) . . . . ? C33 N3 C31 C14 82.8(7) . . . . ? Mo N3 C31 C14 -37.6(7) . . . . ? C13 C14 C31 N3 -148.4(9) . . . . ? N1 C14 C31 N3 34.5(9) . . . . ? C31 N3 C32 C24 160.1(6) . . . . ? C33 N3 C32 C24 -79.3(8) . . . . ? Mo N3 C32 C24 42.2(7) . . . . ? C23 C24 C32 N3 160.4(8) . . . . ? N2 C24 C32 N3 -30.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.161 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.138 data_Mo[C(Et)=CEtNMe2](NMe2))dpma _database_code_CSD 179379 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H35 Mo N5' _chemical_formula_weight 453.48 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.9289(13) _cell_length_b 31.762(4) _cell_length_c 8.9905(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.546(13) _cell_angle_gamma 90.00 _cell_volume 2218.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelpiped _exptl_crystal_colour brown _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type emperical _exptl_absorpt_correction_T_min 0.7382 _exptl_absorpt_correction_T_max 0.8147 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9920 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3180 _reflns_number_gt 2842 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+5.9835P] 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 3180 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _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 Mo Mo 0.05330(5) 0.634982(11) 0.96125(4) 0.02243(15) Uani 1 1 d . . . N1 N 0.2265(4) 0.67991(12) 1.0786(4) 0.0289(9) Uani 1 1 d . . . N2 N -0.1285(4) 0.61502(12) 0.7693(4) 0.0276(8) Uani 1 1 d . . . N3 N -0.0335(5) 0.69657(11) 0.8376(4) 0.0301(9) Uani 1 1 d . . . N4 N 0.2654(4) 0.62144(12) 0.8137(4) 0.0264(8) Uani 1 1 d . . . N5 N -0.0773(4) 0.62898(11) 1.1186(4) 0.0270(8) Uani 1 1 d . . . C1 C 0.3028(9) 0.51260(18) 0.7460(8) 0.0629(18) Uani 1 1 d . . . H1A H 0.3829 0.4926 0.7198 0.094 Uiso 1 1 calc R . . H1B H 0.2377 0.5251 0.6552 0.094 Uiso 1 1 calc R . . H1C H 0.2261 0.4986 0.7998 0.094 Uiso 1 1 calc R . . C2 C 0.4000(7) 0.54652(16) 0.8455(6) 0.0441(13) Uani 1 1 d . . . H2A H 0.4674 0.5335 0.9357 0.053 Uiso 1 1 calc R . . H2B H 0.4796 0.5599 0.7912 0.053 Uiso 1 1 calc R . . C3 C 0.2870(6) 0.57971(14) 0.8932(5) 0.0289(10) Uani 1 1 d . . . C4 C 0.1908(5) 0.57827(13) 0.9988(5) 0.0255(10) Uani 1 1 d . . . C5 C 0.1896(7) 0.54199(15) 1.1061(5) 0.0364(11) Uani 1 1 d . . . H5A H 0.2640 0.5199 1.0816 0.044 Uiso 1 1 calc R . . H5B H 0.0738 0.5307 1.0921 0.044 Uiso 1 1 calc R . . C6 C 0.2496(9) 0.55456(19) 1.2716(6) 0.0574(16) Uani 1 1 d . . . H6A H 0.2479 0.5304 1.3352 0.086 Uiso 1 1 calc R . . H6B H 0.1741 0.5758 1.2975 0.086 Uiso 1 1 calc R . . H6C H 0.3646 0.5655 1.2865 0.086 Uiso 1 1 calc R . . C11 C 0.3519(6) 0.68117(17) 1.2067(6) 0.0397(12) Uani 1 1 d . . . H11A H 0.3746 0.6597 1.2784 0.048 Uiso 1 1 calc R . . C12 C 0.4393(7) 0.71838(18) 1.2148(7) 0.0493(15) Uani 1 1 d . . . H12A H 0.5308 0.7265 1.2912 0.059 Uiso 1 1 calc R . . C13 C 0.3665(6) 0.74197(17) 1.0881(7) 0.0442(14) Uani 1 1 d . . . H13A H 0.3999 0.7687 1.0633 0.053 Uiso 1 1 calc R . . C14 C 0.2346(6) 0.71792(14) 1.0059(6) 0.0324(11) Uani 1 1 d . . . C21 C -0.2001(6) 0.57734(16) 0.7153(5) 0.0341(11) Uani 1 1 d . . . H21A H -0.1786 0.5517 0.7653 0.041 Uiso 1 1 calc R . . C22 C -0.3073(6) 0.58282(19) 0.5779(6) 0.0441(14) Uani 1 1 d . . . H22A H -0.3709 0.5621 0.5186 0.053 Uiso 1 1 calc R . . C23 C -0.3032(6) 0.6255(2) 0.5434(6) 0.0449(14) Uani 1 1 d . . . H23A H -0.3645 0.6386 0.4567 0.054 Uiso 1 1 calc R . . C24 C -0.1920(6) 0.64485(16) 0.6609(5) 0.0327(11) Uani 1 1 d . . . C31 C 0.1221(6) 0.72409(15) 0.8534(6) 0.0377(12) Uani 1 1 d . . . H31A H 0.1856 0.7172 0.7750 0.045 Uiso 1 1 calc R . . H31B H 0.0870 0.7533 0.8410 0.045 Uiso 1 1 calc R . . C32 C -0.1171(6) 0.68803(16) 0.6767(6) 0.0392(12) Uani 1 1 d . . . H32A H -0.2073 0.7086 0.6433 0.047 Uiso 1 1 calc R . . H32B H -0.0327 0.6907 0.6126 0.047 Uiso 1 1 calc R . . C33 C -0.1594(6) 0.71567(15) 0.9183(6) 0.0409(12) Uani 1 1 d . . . H33A H -0.2004 0.7417 0.8700 0.061 Uiso 1 1 calc R . . H33B H -0.1051 0.7210 1.0220 0.061 Uiso 1 1 calc R . . H33C H -0.2544 0.6968 0.9153 0.061 Uiso 1 1 calc R . . C41 C 0.4303(6) 0.64481(15) 0.8485(6) 0.0348(11) Uani 1 1 d . . . H41A H 0.5022 0.6361 0.7800 0.052 Uiso 1 1 calc R . . H41B H 0.4874 0.6390 0.9510 0.052 Uiso 1 1 calc R . . H41C H 0.4080 0.6745 0.8371 0.052 Uiso 1 1 calc R . . C42 C 0.2172(6) 0.61624(17) 0.6468(5) 0.0381(12) Uani 1 1 d . . . H42A H 0.3188 0.6111 0.6067 0.057 Uiso 1 1 calc R . . H42B H 0.1618 0.6414 0.6022 0.057 Uiso 1 1 calc R . . H42C H 0.1398 0.5928 0.6232 0.057 Uiso 1 1 calc R . . C51 C -0.0703(7) 0.65547(17) 1.2533(6) 0.0444(13) Uani 1 1 d . . . H51A H -0.1484 0.6446 1.3129 0.067 Uiso 1 1 calc R . . H51B H -0.1026 0.6837 1.2223 0.067 Uiso 1 1 calc R . . H51C H 0.0446 0.6554 1.3129 0.067 Uiso 1 1 calc R . . C52 C -0.2021(6) 0.59512(16) 1.1208(6) 0.0388(12) Uani 1 1 d . . . H52A H -0.2514 0.5979 1.2096 0.058 Uiso 1 1 calc R . . H52B H -0.1452 0.5684 1.1228 0.058 Uiso 1 1 calc R . . H52C H -0.2915 0.5969 1.0316 0.058 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 0.0211(2) 0.0235(2) 0.0215(2) 0.00256(16) 0.00156(15) -0.00135(16) N1 0.0224(19) 0.033(2) 0.031(2) -0.0020(17) 0.0031(17) -0.0025(16) N2 0.0218(19) 0.035(2) 0.025(2) 0.0002(17) 0.0022(16) -0.0020(16) N3 0.023(2) 0.026(2) 0.040(2) 0.0077(17) 0.0048(17) 0.0013(16) N4 0.0223(19) 0.036(2) 0.0214(19) 0.0023(16) 0.0053(15) -0.0001(16) N5 0.0174(18) 0.033(2) 0.030(2) 0.0020(17) 0.0047(15) 0.0038(16) C1 0.085(5) 0.038(3) 0.075(5) -0.013(3) 0.038(4) 0.003(3) C2 0.047(3) 0.037(3) 0.054(3) 0.004(3) 0.025(3) 0.009(2) C3 0.026(2) 0.026(2) 0.035(3) 0.000(2) 0.006(2) 0.0024(19) C4 0.026(2) 0.023(2) 0.025(2) 0.0017(18) 0.001(2) 0.0022(18) C5 0.041(3) 0.032(3) 0.037(3) 0.008(2) 0.009(2) 0.007(2) C6 0.081(4) 0.053(4) 0.035(3) 0.013(3) 0.003(3) 0.009(3) C11 0.031(3) 0.055(3) 0.031(3) -0.005(2) 0.002(2) -0.006(2) C12 0.035(3) 0.064(4) 0.049(4) -0.023(3) 0.009(3) -0.020(3) C13 0.034(3) 0.041(3) 0.064(4) -0.017(3) 0.025(3) -0.014(2) C14 0.026(2) 0.027(2) 0.047(3) -0.008(2) 0.014(2) -0.006(2) C21 0.029(3) 0.041(3) 0.034(3) -0.008(2) 0.009(2) -0.011(2) C22 0.034(3) 0.069(4) 0.028(3) -0.014(3) 0.005(2) -0.014(3) C23 0.024(3) 0.085(4) 0.023(3) 0.006(3) -0.001(2) -0.004(3) C24 0.022(2) 0.052(3) 0.024(3) 0.007(2) 0.005(2) 0.003(2) C31 0.030(3) 0.025(3) 0.058(3) 0.011(2) 0.010(2) -0.001(2) C32 0.026(3) 0.053(3) 0.037(3) 0.018(2) 0.003(2) 0.006(2) C33 0.034(3) 0.033(3) 0.057(3) 0.004(2) 0.013(2) 0.008(2) C41 0.022(2) 0.038(3) 0.045(3) 0.003(2) 0.009(2) 0.001(2) C42 0.036(3) 0.051(3) 0.028(3) 0.002(2) 0.007(2) 0.004(2) C51 0.055(3) 0.048(3) 0.036(3) -0.009(2) 0.022(3) -0.005(3) C52 0.038(3) 0.044(3) 0.038(3) 0.001(2) 0.016(2) -0.010(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 Mo N5 1.923(4) . ? Mo C4 2.098(4) . ? Mo N1 2.111(4) . ? Mo N2 2.112(4) . ? Mo N3 2.287(4) . ? Mo N4 2.380(4) . ? Mo C3 2.710(4) . ? N1 C11 1.363(6) . ? N1 C14 1.380(6) . ? N2 C21 1.371(6) . ? N2 C24 1.380(6) . ? N3 C33 1.476(6) . ? N3 C32 1.491(6) . ? N3 C31 1.495(6) . ? N4 C41 1.481(6) . ? N4 C42 1.482(6) . ? N4 C3 1.499(6) . ? N5 C52 1.464(6) . ? N5 C51 1.466(6) . ? C1 C2 1.509(8) . ? C2 C3 1.501(6) . ? C3 C4 1.332(6) . ? C4 C5 1.504(6) . ? C5 C6 1.522(7) . ? C11 C12 1.364(7) . ? C12 C13 1.389(8) . ? C13 C14 1.383(7) . ? C14 C31 1.491(7) . ? C21 C22 1.364(7) . ? C22 C23 1.393(8) . ? C23 C24 1.378(7) . ? C24 C32 1.490(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Mo C4 97.79(16) . . ? N5 Mo N1 95.25(15) . . ? C4 Mo N1 103.59(16) . . ? N5 Mo N2 101.04(15) . . ? C4 Mo N2 96.97(16) . . ? N1 Mo N2 151.71(15) . . ? N5 Mo N3 106.77(14) . . ? C4 Mo N3 155.36(16) . . ? N1 Mo N3 76.52(14) . . ? N2 Mo N3 76.70(14) . . ? N5 Mo N4 159.51(14) . . ? C4 Mo N4 62.10(15) . . ? N1 Mo N4 86.51(13) . . ? N2 Mo N4 86.17(13) . . ? N3 Mo N4 93.51(13) . . ? N5 Mo C3 126.52(14) . . ? C4 Mo C3 28.74(15) . . ? N1 Mo C3 98.34(14) . . ? N2 Mo C3 90.38(14) . . ? N3 Mo C3 126.67(14) . . ? N4 Mo C3 33.47(13) . . ? C11 N1 C14 106.2(4) . . ? C11 N1 Mo 137.2(3) . . ? C14 N1 Mo 116.2(3) . . ? C21 N2 C24 106.4(4) . . ? C21 N2 Mo 135.9(3) . . ? C24 N2 Mo 117.6(3) . . ? C33 N3 C32 109.8(4) . . ? C33 N3 C31 109.8(4) . . ? C32 N3 C31 113.4(4) . . ? C33 N3 Mo 106.3(3) . . ? C32 N3 Mo 110.4(3) . . ? C31 N3 Mo 106.9(3) . . ? C41 N4 C42 107.9(4) . . ? C41 N4 C3 109.3(3) . . ? C42 N4 C3 111.4(4) . . ? C41 N4 Mo 118.9(3) . . ? C42 N4 Mo 121.1(3) . . ? C3 N4 Mo 85.4(2) . . ? C52 N5 C51 108.9(4) . . ? C52 N5 Mo 123.2(3) . . ? C51 N5 Mo 127.9(3) . . ? C3 C2 C1 114.0(5) . . ? C4 C3 N4 110.1(4) . . ? C4 C3 C2 129.7(4) . . ? N4 C3 C2 120.2(4) . . ? C4 C3 Mo 49.2(2) . . ? N4 C3 Mo 61.1(2) . . ? C2 C3 Mo 173.7(3) . . ? C3 C4 C5 124.2(4) . . ? C3 C4 Mo 102.1(3) . . ? C5 C4 Mo 133.7(3) . . ? C4 C5 C6 112.7(4) . . ? N1 C11 C12 110.3(5) . . ? C11 C12 C13 107.5(5) . . ? C14 C13 C12 106.6(5) . . ? N1 C14 C13 109.4(5) . . ? N1 C14 C31 118.3(4) . . ? C13 C14 C31 131.9(5) . . ? C22 C21 N2 110.4(5) . . ? C21 C22 C23 106.7(5) . . ? C24 C23 C22 107.6(4) . . ? C23 C24 N2 108.8(5) . . ? C23 C24 C32 131.7(5) . . ? N2 C24 C32 118.9(4) . . ? C14 C31 N3 109.9(4) . . ? C24 C32 N3 110.5(4) . . ? 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 N5 Mo N1 C11 65.8(5) . . . . ? C4 Mo N1 C11 -33.5(5) . . . . ? N2 Mo N1 C11 -169.0(4) . . . . ? N3 Mo N1 C11 171.8(5) . . . . ? N4 Mo N1 C11 -93.7(5) . . . . ? C3 Mo N1 C11 -62.3(5) . . . . ? N5 Mo N1 C14 -122.3(3) . . . . ? C4 Mo N1 C14 138.4(3) . . . . ? N2 Mo N1 C14 2.9(5) . . . . ? N3 Mo N1 C14 -16.3(3) . . . . ? N4 Mo N1 C14 78.2(3) . . . . ? C3 Mo N1 C14 109.6(3) . . . . ? N5 Mo N2 C21 -72.2(4) . . . . ? C4 Mo N2 C21 27.2(4) . . . . ? N1 Mo N2 C21 163.8(4) . . . . ? N3 Mo N2 C21 -177.0(4) . . . . ? N4 Mo N2 C21 88.5(4) . . . . ? C3 Mo N2 C21 55.2(4) . . . . ? N5 Mo N2 C24 112.0(3) . . . . ? C4 Mo N2 C24 -148.7(3) . . . . ? N1 Mo N2 C24 -12.1(5) . . . . ? N3 Mo N2 C24 7.1(3) . . . . ? N4 Mo N2 C24 -87.4(3) . . . . ? C3 Mo N2 C24 -120.6(3) . . . . ? N5 Mo N3 C33 2.8(3) . . . . ? C4 Mo N3 C33 178.1(4) . . . . ? N1 Mo N3 C33 -88.7(3) . . . . ? N2 Mo N3 C33 100.6(3) . . . . ? N4 Mo N3 C33 -174.2(3) . . . . ? C3 Mo N3 C33 -179.1(3) . . . . ? N5 Mo N3 C32 -116.1(3) . . . . ? C4 Mo N3 C32 59.1(5) . . . . ? N1 Mo N3 C32 152.4(3) . . . . ? N2 Mo N3 C32 -18.4(3) . . . . ? N4 Mo N3 C32 66.8(3) . . . . ? C3 Mo N3 C32 61.9(3) . . . . ? N5 Mo N3 C31 120.1(3) . . . . ? C4 Mo N3 C31 -64.6(5) . . . . ? N1 Mo N3 C31 28.6(3) . . . . ? N2 Mo N3 C31 -142.2(3) . . . . ? N4 Mo N3 C31 -56.9(3) . . . . ? C3 Mo N3 C31 -61.8(3) . . . . ? N5 Mo N4 C41 -94.4(5) . . . . ? C4 Mo N4 C41 -106.1(3) . . . . ? N1 Mo N4 C41 1.3(3) . . . . ? N2 Mo N4 C41 153.9(3) . . . . ? N3 Mo N4 C41 77.5(3) . . . . ? C3 Mo N4 C41 -109.6(4) . . . . ? N5 Mo N4 C42 127.5(4) . . . . ? C4 Mo N4 C42 115.8(4) . . . . ? N1 Mo N4 C42 -136.8(3) . . . . ? N2 Mo N4 C42 15.8(3) . . . . ? N3 Mo N4 C42 -60.6(3) . . . . ? C3 Mo N4 C42 112.3(4) . . . . ? N5 Mo N4 C3 15.2(5) . . . . ? C4 Mo N4 C3 3.5(2) . . . . ? N1 Mo N4 C3 110.8(2) . . . . ? N2 Mo N4 C3 -96.5(2) . . . . ? N3 Mo N4 C3 -172.9(2) . . . . ? C4 Mo N5 C52 -63.0(4) . . . . ? N1 Mo N5 C52 -167.5(3) . . . . ? N2 Mo N5 C52 35.7(4) . . . . ? N3 Mo N5 C52 115.0(3) . . . . ? N4 Mo N5 C52 -73.4(5) . . . . ? C3 Mo N5 C52 -63.1(4) . . . . ? C4 Mo N5 C51 116.1(4) . . . . ? N1 Mo N5 C51 11.6(4) . . . . ? N2 Mo N5 C51 -145.2(4) . . . . ? N3 Mo N5 C51 -65.9(4) . . . . ? N4 Mo N5 C51 105.7(5) . . . . ? C3 Mo N5 C51 116.0(4) . . . . ? C41 N4 C3 C4 113.9(4) . . . . ? C42 N4 C3 C4 -126.8(4) . . . . ? Mo N4 C3 C4 -5.1(3) . . . . ? C41 N4 C3 C2 -68.0(5) . . . . ? C42 N4 C3 C2 51.3(5) . . . . ? Mo N4 C3 C2 173.0(4) . . . . ? C41 N4 C3 Mo 119.1(3) . . . . ? C42 N4 C3 Mo -121.7(3) . . . . ? C1 C2 C3 C4 76.9(7) . . . . ? C1 C2 C3 N4 -100.8(5) . . . . ? C1 C2 C3 Mo -1(3) . . . . ? N5 Mo C3 C4 0.2(4) . . . . ? N1 Mo C3 C4 103.1(3) . . . . ? N2 Mo C3 C4 -103.9(3) . . . . ? N3 Mo C3 C4 -177.5(3) . . . . ? N4 Mo C3 C4 173.6(4) . . . . ? N5 Mo C3 N4 -173.5(2) . . . . ? C4 Mo C3 N4 -173.6(4) . . . . ? N1 Mo C3 N4 -70.5(2) . . . . ? N2 Mo C3 N4 82.5(2) . . . . ? N3 Mo C3 N4 8.8(3) . . . . ? N5 Mo C3 C2 83(3) . . . . ? C4 Mo C3 C2 83(3) . . . . ? N1 Mo C3 C2 -174(3) . . . . ? N2 Mo C3 C2 -21(3) . . . . ? N3 Mo C3 C2 -95(3) . . . . ? N4 Mo C3 C2 -104(3) . . . . ? N4 C3 C4 C5 -176.2(4) . . . . ? C2 C3 C4 C5 5.9(8) . . . . ? Mo C3 C4 C5 177.8(6) . . . . ? N4 C3 C4 Mo 6.0(4) . . . . ? C2 C3 C4 Mo -171.9(4) . . . . ? N5 Mo C4 C3 -179.9(3) . . . . ? N1 Mo C4 C3 -82.5(3) . . . . ? N2 Mo C4 C3 77.9(3) . . . . ? N3 Mo C4 C3 4.7(5) . . . . ? N4 Mo C4 C3 -4.0(3) . . . . ? N5 Mo C4 C5 2.6(5) . . . . ? N1 Mo C4 C5 100.0(4) . . . . ? N2 Mo C4 C5 -99.6(4) . . . . ? N3 Mo C4 C5 -172.8(4) . . . . ? N4 Mo C4 C5 178.5(5) . . . . ? C3 Mo C4 C5 -177.5(6) . . . . ? C3 C4 C5 C6 118.1(5) . . . . ? Mo C4 C5 C6 -64.8(6) . . . . ? C14 N1 C11 C12 -1.0(5) . . . . ? Mo N1 C11 C12 171.4(4) . . . . ? N1 C11 C12 C13 0.5(6) . . . . ? C11 C12 C13 C14 0.2(6) . . . . ? C11 N1 C14 C13 1.1(5) . . . . ? Mo N1 C14 C13 -173.2(3) . . . . ? C11 N1 C14 C31 174.4(4) . . . . ? Mo N1 C14 C31 0.1(5) . . . . ? C12 C13 C14 N1 -0.8(6) . . . . ? C12 C13 C14 C31 -172.9(5) . . . . ? C24 N2 C21 C22 -0.7(5) . . . . ? Mo N2 C21 C22 -176.9(3) . . . . ? N2 C21 C22 C23 0.1(6) . . . . ? C21 C22 C23 C24 0.4(6) . . . . ? C22 C23 C24 N2 -0.9(6) . . . . ? C22 C23 C24 C32 169.6(5) . . . . ? C21 N2 C24 C23 1.0(5) . . . . ? Mo N2 C24 C23 178.0(3) . . . . ? C21 N2 C24 C32 -170.9(4) . . . . ? Mo N2 C24 C32 6.1(5) . . . . ? N1 C14 C31 N3 26.1(6) . . . . ? C13 C14 C31 N3 -162.4(5) . . . . ? C33 N3 C31 C14 78.6(5) . . . . ? C32 N3 C31 C14 -158.2(4) . . . . ? Mo N3 C31 C14 -36.3(4) . . . . ? C23 C24 C32 N3 167.9(5) . . . . ? N2 C24 C32 N3 -22.4(6) . . . . ? C33 N3 C32 C24 -90.7(5) . . . . ? C31 N3 C32 C24 146.1(4) . . . . ? Mo N3 C32 C24 26.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.977 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.080