Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bonanno, Jeffrey B.' 'Churchill, David G.' 'Murphy, Vincent J.' 'Parkin, G.' 'Savage, William' 'Shin, Jun Ho' _publ_contact_author_name 'Prof G Parkin' _publ_contact_author_address ; Prof G Parkin Department of Chemistry Columbia University New York New York 10027 UNITED STATES OF AMERICA ; data_moph10 _database_code_CSD 161663 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H32 Mo Te' _chemical_formula_weight 544.04 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.665(2) _cell_length_b 16.169(3) _cell_length_c 16.242(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.43(2) _cell_angle_gamma 90.00 _cell_volume 2271.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 5.18 _cell_measurement_theta_max 12.69 _exptl_crystal_description ? _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.2_mm _exptl_crystal_size_mid 0.5_mm _exptl_crystal_size_min 0.7_mm _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method ? _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.841 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2304 _exptl_absorpt_correction_T_max 0.2558 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.99 _diffrn_reflns_number 3731 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2950 _reflns_number_observed 2005 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2950 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_obs 0.0514 _refine_ls_wR_factor_all 0.1276 _refine_ls_wR_factor_obs 0.1094 _refine_ls_goodness_of_fit_all 1.020 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.020 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max -2.063 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.96025(9) 0.31604(5) 0.23478(5) 0.0372(3) Uani 1 d . . Te Te 0.91632(8) 0.14863(4) 0.19644(5) 0.0557(3) Uani 1 d . . C11 C 0.8298(10) 0.3041(6) 0.3561(5) 0.042(2) Uani 1 d . . C12 C 0.8807(11) 0.3871(6) 0.3434(5) 0.041(2) Uani 1 d . . H12A H 0.8138(11) 0.4360(6) 0.3401(5) 0.050 Uiso 1 calc R . C13 C 1.0431(12) 0.3884(7) 0.3486(5) 0.057(3) Uani 1 d . . H13A H 1.1071(12) 0.4384(7) 0.3487(5) 0.068 Uiso 1 calc R . C14 C 1.0982(12) 0.3081(8) 0.3623(6) 0.058(3) Uani 1 d . . H14A H 1.2063(12) 0.2913(8) 0.3725(6) 0.070 Uiso 1 calc R . C15 C 0.9654(13) 0.2572(6) 0.3669(6) 0.051(3) Uani 1 d . . H15A H 0.9683(13) 0.1977(6) 0.3781(6) 0.061 Uiso 1 calc R . C16 C 0.6655(12) 0.2788(7) 0.3711(6) 0.055(3) Uani 1 d . . C17 C 0.6244(14) 0.3203(7) 0.4521(7) 0.084(4) Uani 1 d . . H17A H 0.6957(14) 0.3025(7) 0.4961(7) 0.126 Uiso 1 calc R . H17B H 0.5212(14) 0.3050(7) 0.4645(7) 0.126 Uiso 1 calc R . H17C H 0.6304(14) 0.3793(7) 0.4464(7) 0.126 Uiso 1 calc R . C18 C 0.5567(13) 0.3052(10) 0.3015(7) 0.106(5) Uani 1 d . . H18A H 0.4536(13) 0.2885(10) 0.3124(7) 0.160 Uiso 1 calc R . H18B H 0.5861(13) 0.2798(10) 0.2514(7) 0.160 Uiso 1 calc R . H18C H 0.5604(13) 0.3643(10) 0.2959(7) 0.160 Uiso 1 calc R . C19 C 0.6528(13) 0.1858(7) 0.3844(7) 0.074(3) Uani 1 d . . H19A H 0.7233(13) 0.1693(7) 0.4293(7) 0.111 Uiso 1 calc R . H19B H 0.6781(13) 0.1572(7) 0.3351(7) 0.111 Uiso 1 calc R . H19C H 0.5491(13) 0.1722(7) 0.3972(7) 0.111 Uiso 1 calc R . C21 C 1.0543(10) 0.3833(6) 0.1170(5) 0.039(2) Uani 1 d . . C22 C 0.9695(12) 0.4396(6) 0.1623(5) 0.044(2) Uani 1 d . . H22A H 1.0092(12) 0.4921(6) 0.1850(5) 0.053 Uiso 1 calc R . C23 C 0.8130(11) 0.4122(6) 0.1636(6) 0.050(3) Uani 1 d . . H23A H 0.7280(11) 0.4437(6) 0.1856(6) 0.059 Uiso 1 calc R . C24 C 0.7975(12) 0.3374(7) 0.1205(6) 0.053(3) Uani 1 d . . H24A H 0.7013(12) 0.3077(7) 0.1055(6) 0.064 Uiso 1 calc R . C25 C 0.9513(11) 0.3187(6) 0.0931(5) 0.041(2) Uani 1 d . . H25A H 0.9762(11) 0.2719(6) 0.0579(5) 0.049 Uiso 1 calc R . C26 C 1.2163(10) 0.3949(6) 0.0905(6) 0.049(3) Uani 1 d . . C27 C 1.2043(12) 0.4466(8) 0.0114(6) 0.083(4) Uani 1 d . . H27A H 1.3059(12) 0.4554(8) -0.0076(6) 0.124 Uiso 1 calc R . H27B H 1.1576(12) 0.4989(8) 0.0224(6) 0.124 Uiso 1 calc R . H27C H 1.1421(12) 0.4177(8) -0.0302(6) 0.124 Uiso 1 calc R . C28 C 1.2960(12) 0.3116(7) 0.0739(7) 0.066(3) Uani 1 d . . H28A H 1.3987(12) 0.3216(7) 0.0572(7) 0.099 Uiso 1 calc R . H28B H 1.2378(12) 0.2825(7) 0.0309(7) 0.099 Uiso 1 calc R . H28C H 1.3010(12) 0.2788(7) 0.1233(7) 0.099 Uiso 1 calc R . C29 C 1.3147(12) 0.4428(7) 0.1556(7) 0.070(3) Uani 1 d . . H29A H 1.4174(12) 0.4495(7) 0.1374(7) 0.105 Uiso 1 calc R . H29B H 1.3191(12) 0.4129(7) 0.2067(7) 0.105 Uiso 1 calc R . H29C H 1.2695(12) 0.4962(7) 0.1636(7) 0.105 Uiso 1 calc R . C1 C 1.1379(12) 0.1119(6) 0.1566(6) 0.048(2) Uani 1 d . . C2 C 1.1507(13) 0.0902(6) 0.0761(6) 0.060(3) Uani 1 d . . H2A H 1.0637(13) 0.0912(6) 0.0397(6) 0.073 Uiso 1 calc R . C3 C 1.2927(17) 0.0665(7) 0.0478(8) 0.083(4) Uani 1 d . . H3A H 1.3020(17) 0.0527(7) -0.0072(8) 0.100 Uiso 1 calc R . C4 C 1.4165(16) 0.0640(7) 0.1024(11) 0.086(5) Uani 1 d . . H4A H 1.5117(16) 0.0482(7) 0.0840(11) 0.104 Uiso 1 calc R . C5 C 1.4065(14) 0.0841(8) 0.1840(9) 0.083(4) Uani 1 d . . H5A H 1.4938(14) 0.0818(8) 0.2201(9) 0.100 Uiso 1 calc R . C6 C 1.2659(14) 0.1078(6) 0.2123(7) 0.059(3) Uani 1 d . . H6A H 1.2570(14) 0.1209(6) 0.2676(7) 0.071 Uiso 1 calc R . H H 1.1604(115) 0.2795(56) 0.2207(53) 0.075(31) Uiso 1 d . . 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 0.0401(5) 0.0344(5) 0.0380(5) 0.0019(4) 0.0095(4) 0.0053(4) Te 0.0560(5) 0.0374(4) 0.0762(5) -0.0031(4) 0.0249(4) -0.0001(4) C11 0.034(6) 0.046(6) 0.045(6) 0.004(5) 0.008(5) 0.005(5) C12 0.042(6) 0.037(6) 0.046(6) -0.007(5) 0.009(5) 0.010(5) C13 0.064(8) 0.065(8) 0.042(6) -0.007(6) 0.009(5) -0.017(7) C14 0.040(7) 0.089(9) 0.046(6) 0.009(6) 0.006(5) 0.004(7) C15 0.062(8) 0.051(6) 0.041(6) 0.010(5) 0.010(5) 0.017(6) C16 0.039(6) 0.069(8) 0.059(7) 0.006(6) 0.018(6) 0.010(5) C17 0.087(9) 0.054(7) 0.118(10) 0.010(7) 0.066(8) 0.014(7) C18 0.049(8) 0.167(15) 0.104(11) 0.055(10) 0.014(8) -0.004(9) C19 0.065(8) 0.070(8) 0.090(9) 0.000(7) 0.032(7) -0.013(7) C21 0.047(6) 0.033(5) 0.037(5) 0.007(4) 0.005(5) 0.010(5) C22 0.062(7) 0.031(5) 0.041(6) 0.014(4) 0.010(5) 0.009(5) C23 0.051(7) 0.043(6) 0.056(6) 0.008(5) 0.013(5) 0.019(5) C24 0.042(6) 0.072(8) 0.046(6) 0.011(5) 0.003(5) 0.006(6) C25 0.048(6) 0.048(6) 0.028(5) 0.002(4) 0.012(4) -0.007(5) C26 0.038(6) 0.053(7) 0.056(6) 0.014(5) 0.011(5) -0.011(5) C27 0.054(7) 0.122(11) 0.074(8) 0.036(8) 0.016(6) 0.002(7) C28 0.047(7) 0.063(7) 0.091(9) -0.003(7) 0.028(6) 0.002(6) C29 0.039(7) 0.077(8) 0.093(9) 0.000(7) -0.001(6) 0.001(6) C1 0.060(7) 0.032(5) 0.054(6) 0.001(5) 0.023(6) 0.006(5) C2 0.071(8) 0.041(6) 0.072(7) 0.007(5) 0.029(6) 0.025(6) C3 0.107(11) 0.070(9) 0.078(9) 0.019(7) 0.048(9) 0.034(8) C4 0.063(9) 0.057(8) 0.146(14) 0.023(9) 0.054(10) 0.021(7) C5 0.064(9) 0.071(9) 0.114(11) 0.000(8) -0.001(8) 0.009(7) C6 0.072(8) 0.039(6) 0.069(7) -0.004(6) 0.015(7) 0.009(6) _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 C12 2.247(8) . ? Mo C13 2.268(9) . ? Mo C23 2.281(9) . ? Mo C24 2.289(10) . ? Mo C25 2.299(8) . ? Mo C22 2.324(8) . ? Mo C14 2.332(10) . ? Mo C11 2.337(9) . ? Mo C15 2.345(9) . ? Mo C21 2.386(8) . ? Mo Te 2.7985(11) . ? Te C1 2.146(10) . ? C11 C15 1.401(13) . ? C11 C12 1.431(13) . ? C11 C16 1.514(13) . ? C12 C13 1.405(13) . ? C13 C14 1.40(2) . ? C14 C15 1.420(14) . ? C16 C18 1.490(15) . ? C16 C19 1.53(2) . ? C16 C17 1.539(14) . ? C21 C22 1.406(12) . ? C21 C25 1.413(12) . ? C21 C26 1.504(12) . ? C22 C23 1.428(13) . ? C23 C24 1.401(13) . ? C24 C25 1.461(13) . ? C26 C27 1.531(12) . ? C26 C29 1.529(13) . ? C26 C28 1.545(14) . ? C1 C2 1.366(12) . ? C1 C6 1.389(14) . ? C2 C3 1.392(15) . ? C3 C4 1.35(2) . ? C4 C5 1.37(2) . ? C5 C6 1.382(15) . ? 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 C12 Mo C13 36.2(3) . . ? C12 Mo C23 82.0(3) . . ? C13 Mo C23 101.6(4) . . ? C12 Mo C24 110.9(3) . . ? C13 Mo C24 137.1(4) . . ? C23 Mo C24 35.7(3) . . ? C12 Mo C25 141.5(3) . . ? C13 Mo C25 142.8(4) . . ? C23 Mo C25 59.7(3) . . ? C24 Mo C25 37.1(3) . . ? C12 Mo C22 88.9(3) . . ? C13 Mo C22 87.2(4) . . ? C23 Mo C22 36.1(3) . . ? C24 Mo C22 59.8(4) . . ? C25 Mo C22 58.4(3) . . ? C12 Mo C14 59.7(3) . . ? C13 Mo C14 35.3(4) . . ? C23 Mo C14 136.8(4) . . ? C24 Mo C14 170.6(4) . . ? C25 Mo C14 151.1(3) . . ? C22 Mo C14 117.8(4) . . ? C12 Mo C11 36.3(3) . . ? C13 Mo C11 60.0(3) . . ? C23 Mo C11 101.5(3) . . ? C24 Mo C11 113.0(3) . . ? C25 Mo C11 148.9(3) . . ? C22 Mo C11 122.1(3) . . ? C14 Mo C11 59.7(3) . . ? C12 Mo C15 58.6(3) . . ? C13 Mo C15 58.4(4) . . ? C23 Mo C15 136.0(3) . . ? C24 Mo C15 141.3(4) . . ? C25 Mo C15 157.1(3) . . ? C22 Mo C15 144.4(3) . . ? C14 Mo C15 35.4(3) . . ? C11 Mo C15 34.8(3) . . ? C12 Mo C21 122.1(3) . . ? C13 Mo C21 108.2(3) . . ? C23 Mo C21 59.4(3) . . ? C24 Mo C21 60.3(3) . . ? C25 Mo C21 35.1(3) . . ? C22 Mo C21 34.7(3) . . ? C14 Mo C21 123.8(3) . . ? C11 Mo C21 156.8(3) . . ? C15 Mo C21 158.4(4) . . ? C12 Mo Te 128.7(2) . . ? C13 Mo Te 135.4(3) . . ? C23 Mo Te 118.8(3) . . ? C24 Mo Te 84.0(3) . . ? C25 Mo Te 78.4(2) . . ? C22 Mo Te 136.7(2) . . ? C14 Mo Te 101.5(3) . . ? C11 Mo Te 92.4(2) . . ? C15 Mo Te 78.8(2) . . ? C21 Mo Te 108.1(2) . . ? C1 Te Mo 102.9(3) . . ? C15 C11 C12 105.2(8) . . ? C15 C11 C16 128.5(9) . . ? C12 C11 C16 125.3(8) . . ? C15 C11 Mo 72.9(5) . . ? C12 C11 Mo 68.4(5) . . ? C16 C11 Mo 131.6(7) . . ? C13 C12 C11 108.8(9) . . ? C13 C12 Mo 72.7(5) . . ? C11 C12 Mo 75.3(5) . . ? C14 C13 C12 109.1(10) . . ? C14 C13 Mo 74.8(6) . . ? C12 C13 Mo 71.1(5) . . ? C13 C14 C15 106.1(9) . . ? C13 C14 Mo 69.8(6) . . ? C15 C14 Mo 72.8(6) . . ? C11 C15 C14 110.8(9) . . ? C11 C15 Mo 72.3(5) . . ? C14 C15 Mo 71.8(6) . . ? C18 C16 C11 111.0(9) . . ? C18 C16 C19 110.0(10) . . ? C11 C16 C19 111.5(8) . . ? C18 C16 C17 110.8(10) . . ? C11 C16 C17 106.8(9) . . ? C19 C16 C17 106.6(8) . . ? C22 C21 C25 106.3(8) . . ? C22 C21 C26 126.5(9) . . ? C25 C21 C26 126.8(8) . . ? C22 C21 Mo 70.2(5) . . ? C25 C21 Mo 69.1(5) . . ? C26 C21 Mo 131.0(6) . . ? C21 C22 C23 109.5(9) . . ? C21 C22 Mo 75.1(5) . . ? C23 C22 Mo 70.3(5) . . ? C24 C23 C22 108.8(8) . . ? C24 C23 Mo 72.5(5) . . ? C22 C23 Mo 73.6(5) . . ? C23 C24 C25 105.6(9) . . ? C23 C24 Mo 71.9(5) . . ? C25 C24 Mo 71.8(5) . . ? C21 C25 C24 109.6(8) . . ? C21 C25 Mo 75.8(5) . . ? C24 C25 Mo 71.1(5) . . ? C21 C26 C27 106.9(8) . . ? C21 C26 C29 110.9(8) . . ? C27 C26 C29 108.1(8) . . ? C21 C26 C28 112.0(8) . . ? C27 C26 C28 109.7(8) . . ? C29 C26 C28 109.0(8) . . ? C2 C1 C6 120.2(10) . . ? C2 C1 Te 119.1(8) . . ? C6 C1 Te 120.7(7) . . ? C1 C2 C3 120.7(12) . . ? C4 C3 C2 118.3(12) . . ? C3 C4 C5 122.2(12) . . ? C4 C5 C6 119.6(12) . . ? C5 C6 C1 118.9(10) . . ? _refine_diff_density_max 0.777 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.131 data_bum20 _database_code_CSD 161664 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Mo S2' _chemical_formula_weight 402.45 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' 'S' 'S' 0.1246 0.1234 '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 10.739(3) _cell_length_b 13.953(3) _cell_length_c 12.357(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.80(2) _cell_angle_gamma 90.00 _cell_volume 1850.7(7) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.84 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5099 _exptl_absorpt_correction_T_max 0.8969 _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 ? _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 2543 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 22.51 _reflns_number_total 2394 _reflns_number_gt 1739 _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^)+(0.0395P)^2^+5.5281P] 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 0.0006(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2394 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _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 0.27348(6) 1.08521(4) 0.21002(5) 0.0340(2) Uani 1 1 d . . . S1 S 0.4090(2) 0.95246(16) 0.27105(19) 0.0689(7) Uani 1 1 d . . . S2 S 0.3078(2) 0.92669(14) 0.13131(18) 0.0688(7) Uani 1 1 d . . . C11 C 0.3134(6) 1.1667(5) 0.0513(5) 0.0388(16) Uani 1 1 d . . . C12 C 0.4275(6) 1.1218(5) 0.0887(5) 0.0391(17) Uani 1 1 d . . . H12A H 0.4725 1.0749 0.0485 0.080 Uiso 1 1 d R . . C13 C 0.4683(6) 1.1609(5) 0.1889(6) 0.0457(19) Uani 1 1 d . . . H13A H 0.5444 1.1458 0.2281 0.080 Uiso 1 1 d R . . C14 C 0.3782(7) 1.2292(5) 0.2178(6) 0.051(2) Uani 1 1 d . . . H14A H 0.3846 1.2703 0.2799 0.080 Uiso 1 1 d R . . C15 C 0.2905(7) 1.2344(5) 0.1343(6) 0.0435(18) Uani 1 1 d . . . H15A H 0.2245 1.2808 0.1307 0.080 Uiso 1 1 d R . . C16 C 0.2577(7) 1.1606(5) -0.0617(6) 0.0494(19) Uani 1 1 d . . . C17 C 0.1242(8) 1.1927(8) -0.0649(7) 0.086(3) Uani 1 1 d . . . H17A H 0.1203 1.2568 -0.0368 0.080 Uiso 1 1 d R . . H17B H 0.0910 1.1918 -0.1378 0.080 Uiso 1 1 d R . . H17C H 0.0761 1.1507 -0.0209 0.080 Uiso 1 1 d R . . C18 C 0.3293(9) 1.2282(7) -0.1326(7) 0.086(3) Uani 1 1 d . . . H18A H 0.3247 1.2919 -0.1035 0.080 Uiso 1 1 d R . . H18B H 0.4149 1.2082 -0.1335 0.080 Uiso 1 1 d R . . H18C H 0.2945 1.2278 -0.2050 0.080 Uiso 1 1 d R . . C19 C 0.2638(9) 1.0602(6) -0.1079(7) 0.073(3) Uani 1 1 d . . . H19A H 0.3489 1.0389 -0.1070 0.080 Uiso 1 1 d R . . H19B H 0.2157 1.0183 -0.0640 0.080 Uiso 1 1 d R . . H19C H 0.2306 1.0593 -0.1809 0.080 Uiso 1 1 d R . . C21 C 0.1760(6) 1.0914(5) 0.3776(5) 0.0382(16) Uani 1 1 d . . . C22 C 0.1296(6) 1.1678(5) 0.3128(6) 0.0441(18) Uani 1 1 d . . . H22A H 0.1366 1.2342 0.3323 0.080 Uiso 1 1 d R . . C23 C 0.0642(7) 1.1324(7) 0.2213(7) 0.058(2) Uani 1 1 d . . . H23A H 0.0191 1.1702 0.1683 0.080 Uiso 1 1 d R . . C24 C 0.0670(7) 1.0338(8) 0.2246(7) 0.064(2) Uani 1 1 d . . . H24A H 0.0237 0.9907 0.1761 0.080 Uiso 1 1 d R . . C25 C 0.1378(7) 1.0071(5) 0.3190(6) 0.049(2) Uani 1 1 d . . . H25A H 0.1489 0.9427 0.3451 0.080 Uiso 1 1 d R . . C26 C 0.2294(7) 1.0982(6) 0.4930(6) 0.0519(19) Uani 1 1 d . . . C27 C 0.3402(10) 1.1627(9) 0.5009(7) 0.104(4) Uani 1 1 d . . . H27A H 0.4055 1.1373 0.4580 0.080 Uiso 1 1 d R . . H27B H 0.3168 1.2251 0.4744 0.080 Uiso 1 1 d R . . H27C H 0.3691 1.1677 0.5749 0.080 Uiso 1 1 d R . . C28 C 0.1234(9) 1.1366(9) 0.5612(7) 0.105(4) Uani 1 1 d . . . H28A H 0.0997 1.1989 0.5349 0.080 Uiso 1 1 d R . . H28B H 0.0528 1.0944 0.5563 0.080 Uiso 1 1 d R . . H28C H 0.1520 1.1415 0.6353 0.080 Uiso 1 1 d R . . C29 C 0.2663(12) 1.0013(8) 0.5365(8) 0.118(4) Uani 1 1 d . . . H29A H 0.3320 0.9754 0.4944 0.080 Uiso 1 1 d R . . H29B H 0.2945 1.0067 0.6106 0.080 Uiso 1 1 d R . . H29C H 0.1952 0.9596 0.5316 0.080 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0349(3) 0.0307(3) 0.0367(3) -0.0018(3) 0.0051(2) -0.0005(3) S1 0.0666(15) 0.0622(14) 0.0788(15) 0.0254(12) 0.0184(12) 0.0252(11) S2 0.1012(18) 0.0325(11) 0.0745(14) -0.0060(10) 0.0298(13) 0.0029(12) C11 0.048(4) 0.028(4) 0.040(4) 0.000(3) 0.003(3) -0.003(3) C12 0.026(4) 0.045(4) 0.047(4) 0.002(3) 0.019(3) 0.004(3) C13 0.011(3) 0.071(5) 0.055(5) 0.002(4) 0.004(3) -0.015(3) C14 0.069(6) 0.038(4) 0.045(5) -0.004(4) 0.015(4) -0.015(4) C15 0.042(4) 0.035(4) 0.054(5) 0.003(4) 0.023(4) 0.002(3) C16 0.055(5) 0.053(5) 0.040(4) 0.003(4) -0.006(4) 0.003(4) C17 0.061(6) 0.145(10) 0.050(5) -0.003(6) -0.017(4) 0.030(6) C18 0.100(8) 0.105(8) 0.052(5) 0.021(5) -0.001(5) -0.011(6) C19 0.086(7) 0.078(7) 0.053(5) -0.013(5) -0.018(5) 0.000(5) C21 0.032(4) 0.042(4) 0.041(4) 0.004(4) 0.010(3) -0.009(4) C22 0.043(4) 0.043(4) 0.048(4) -0.001(4) 0.016(4) 0.004(4) C23 0.031(4) 0.084(7) 0.060(6) 0.003(5) 0.012(4) 0.020(5) C24 0.020(4) 0.107(8) 0.066(6) -0.018(5) 0.007(4) -0.017(5) C25 0.045(5) 0.043(4) 0.062(5) 0.001(4) 0.026(4) -0.019(4) C26 0.054(5) 0.062(5) 0.041(4) 0.006(4) 0.010(3) 0.003(4) C27 0.110(9) 0.162(11) 0.040(5) 0.002(6) -0.011(5) -0.053(8) C28 0.084(7) 0.179(12) 0.053(6) -0.030(7) 0.011(5) 0.008(8) C29 0.187(13) 0.108(9) 0.058(6) 0.006(6) -0.016(7) 0.037(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C25 2.291(6) . ? Mo C15 2.292(7) . ? Mo C14 2.303(7) . ? Mo C11 2.319(6) . ? Mo C12 2.324(6) . ? Mo C22 2.334(7) . ? Mo C24 2.343(7) . ? Mo C23 2.351(7) . ? Mo C21 2.351(6) . ? Mo C13 2.366(6) . ? Mo S2 2.449(2) . ? Mo S1 2.459(2) . ? S1 S2 2.043(4) . ? C11 C15 1.422(9) . ? C11 C12 1.439(9) . ? C11 C16 1.504(9) . ? C12 C13 1.411(9) . ? C13 C14 1.412(10) . ? C14 C15 1.377(10) . ? C16 C17 1.501(10) . ? C16 C18 1.515(10) . ? C16 C19 1.515(10) . ? C21 C22 1.414(9) . ? C21 C25 1.434(9) . ? C21 C26 1.524(10) . ? C22 C23 1.402(11) . ? C23 C24 1.376(11) . ? C24 C25 1.422(11) . ? C26 C27 1.493(11) . ? C26 C29 1.504(12) . ? C26 C28 1.534(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 C25 Mo C15 137.1(3) . . ? C25 Mo C14 135.2(3) . . ? C15 Mo C14 34.9(2) . . ? C25 Mo C11 150.3(3) . . ? C15 Mo C11 35.9(2) . . ? C14 Mo C11 60.3(2) . . ? C25 Mo C12 164.3(2) . . ? C15 Mo C12 58.0(2) . . ? C14 Mo C12 58.6(2) . . ? C11 Mo C12 36.1(2) . . ? C25 Mo C22 58.1(2) . . ? C15 Mo C22 80.6(2) . . ? C14 Mo C22 83.0(3) . . ? C11 Mo C22 111.2(2) . . ? C12 Mo C22 137.7(3) . . ? C25 Mo C24 35.7(3) . . ? C15 Mo C24 113.4(3) . . ? C14 Mo C24 136.6(3) . . ? C11 Mo C24 114.6(3) . . ? C12 Mo C24 144.2(3) . . ? C22 Mo C24 57.7(3) . . ? C25 Mo C23 58.1(3) . . ? C15 Mo C23 81.9(3) . . ? C14 Mo C23 102.7(3) . . ? C11 Mo C23 96.6(3) . . ? C12 Mo C23 132.7(3) . . ? C22 Mo C23 34.8(3) . . ? C24 Mo C23 34.1(3) . . ? C25 Mo C21 36.0(2) . . ? C15 Mo C21 111.7(2) . . ? C14 Mo C21 99.3(2) . . ? C11 Mo C21 145.7(2) . . ? C12 Mo C21 155.0(2) . . ? C22 Mo C21 35.1(2) . . ? C24 Mo C21 59.6(3) . . ? C23 Mo C21 58.9(3) . . ? C25 Mo C13 149.1(3) . . ? C15 Mo C13 57.8(3) . . ? C14 Mo C13 35.2(2) . . ? C11 Mo C13 60.0(2) . . ? C12 Mo C13 35.0(2) . . ? C22 Mo C13 116.3(3) . . ? C24 Mo C13 171.0(3) . . ? C23 Mo C13 137.1(3) . . ? C21 Mo C13 120.1(2) . . ? C25 Mo S2 84.84(19) . . ? C15 Mo S2 130.04(17) . . ? C14 Mo S2 136.48(19) . . ? C11 Mo S2 94.16(17) . . ? C12 Mo S2 79.81(18) . . ? C22 Mo S2 140.55(19) . . ? C24 Mo S2 84.8(3) . . ? C23 Mo S2 115.6(3) . . ? C21 Mo S2 117.36(19) . . ? C13 Mo S2 102.41(19) . . ? C25 Mo S1 80.9(2) . . ? C15 Mo S1 139.06(18) . . ? C14 Mo S1 111.1(2) . . ? C11 Mo S1 120.35(18) . . ? C12 Mo S1 86.39(18) . . ? C22 Mo S1 126.87(19) . . ? C24 Mo S1 107.4(3) . . ? C23 Mo S1 138.6(2) . . ? C21 Mo S1 91.90(18) . . ? C13 Mo S1 81.6(2) . . ? S2 Mo S1 49.20(9) . . ? S2 S1 Mo 65.14(9) . . ? S1 S2 Mo 65.66(9) . . ? C15 C11 C12 102.9(6) . . ? C15 C11 C16 129.4(6) . . ? C12 C11 C16 125.7(6) . . ? C15 C11 Mo 71.0(4) . . ? C12 C11 Mo 72.1(4) . . ? C16 C11 Mo 132.8(5) . . ? C13 C12 C11 110.6(6) . . ? C13 C12 Mo 74.1(4) . . ? C11 C12 Mo 71.7(3) . . ? C12 C13 C14 106.7(6) . . ? C12 C13 Mo 70.9(4) . . ? C14 C13 Mo 70.0(4) . . ? C15 C14 C13 107.7(6) . . ? C15 C14 Mo 72.1(4) . . ? C13 C14 Mo 74.8(4) . . ? C14 C15 C11 112.1(6) . . ? C14 C15 Mo 73.0(4) . . ? C11 C15 Mo 73.1(4) . . ? C17 C16 C11 111.0(6) . . ? C17 C16 C18 107.5(7) . . ? C11 C16 C18 107.9(7) . . ? C17 C16 C19 108.6(7) . . ? C11 C16 C19 112.4(6) . . ? C18 C16 C19 109.2(7) . . ? C22 C21 C25 104.0(6) . . ? C22 C21 C26 126.7(7) . . ? C25 C21 C26 128.1(7) . . ? C22 C21 Mo 71.8(4) . . ? C25 C21 Mo 69.7(4) . . ? C26 C21 Mo 131.4(4) . . ? C23 C22 C21 110.5(7) . . ? C23 C22 Mo 73.2(4) . . ? C21 C22 Mo 73.1(4) . . ? C24 C23 C22 108.5(8) . . ? C24 C23 Mo 72.7(4) . . ? C22 C23 Mo 71.9(4) . . ? C23 C24 C25 107.3(8) . . ? C23 C24 Mo 73.2(5) . . ? C25 C24 Mo 70.1(4) . . ? C24 C25 C21 109.6(7) . . ? C24 C25 Mo 74.1(4) . . ? C21 C25 Mo 74.3(3) . . ? C27 C26 C29 108.6(9) . . ? C27 C26 C21 112.0(6) . . ? C29 C26 C21 111.4(7) . . ? C27 C26 C28 111.0(8) . . ? C29 C26 C28 108.0(8) . . ? C21 C26 C28 105.8(7) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.662 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.101 data_jun10 _database_code_CSD 161665 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H36 Cl6 I Mo N' _chemical_formula_weight 774.08 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9300(10) _cell_length_b 20.396(2) _cell_length_c 18.2470(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.110(10) _cell_angle_gamma 90.00 _cell_volume 3321.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 4.60 _cell_measurement_theta_max 15.04 _exptl_crystal_description ? _exptl_crystal_colour Orange _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method ? _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.821 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2048 _exptl_absorpt_correction_T_max 0.3657 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.36 _diffrn_reflns_number 5695 _diffrn_reflns_av_R_equivalents 0.0858 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4316 _reflns_number_observed 3369 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+8.1225P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4309 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_obs 0.0506 _refine_ls_wR_factor_all 0.1752 _refine_ls_wR_factor_obs 0.1287 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.275 _refine_ls_restrained_S_obs 1.061 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.19813(7) 0.30032(3) 0.69056(3) 0.0509(3) Uani 1 d . . I I 0.16702(7) 0.24470(3) 0.38592(3) 0.0727(3) Uani 1 d . . C1 C 0.1773(16) 0.2417(8) 0.8715(6) 0.149(6) Uani 1 d . . H1A H 0.1460(16) 0.1987(8) 0.8558(6) 0.223 Uiso 1 calc R . H1B H 0.1022(16) 0.2606(8) 0.9013(6) 0.223 Uiso 1 calc R . H1C H 0.2701(16) 0.2385(8) 0.8995(6) 0.223 Uiso 1 calc R . C2 C 0.1990(11) 0.2849(6) 0.8047(5) 0.075(2) Uani 1 d . . C3 C 0.2830(19) 0.3972(10) 0.8457(9) 0.165(8) Uani 1 d . . H3A H 0.1937(19) 0.4100(10) 0.8709(9) 0.198 Uiso 1 calc R . H3B H 0.3513(19) 0.3790(10) 0.8829(9) 0.198 Uiso 1 calc R . C4 C 0.3353(48) 0.4438(13) 0.8280(16) 0.416(34) Uani 1 d . . H4A H 0.3534(48) 0.4716(13) 0.8699(16) 0.624 Uiso 1 calc R . H4B H 0.2692(48) 0.4657(13) 0.7933(16) 0.624 Uiso 1 calc R . H4C H 0.4285(48) 0.4344(13) 0.8056(16) 0.624 Uiso 1 calc R . N N 0.2358(10) 0.3398(5) 0.7967(4) 0.092(3) Uani 1 d . . C11 C -0.0307(8) 0.2566(4) 0.6508(5) 0.061(2) Uani 1 d . . C12 C -0.0588(9) 0.2967(5) 0.7127(5) 0.072(2) Uani 1 d . . H12A H -0.1023(9) 0.2815(5) 0.7582(5) 0.086 Uiso 1 calc R . C13 C -0.0226(9) 0.3613(5) 0.6971(5) 0.074(2) Uani 1 d . . H13A H -0.0375(9) 0.3988(5) 0.7296(5) 0.088 Uiso 1 calc R . C14 C 0.0305(9) 0.3648(4) 0.6254(5) 0.067(2) Uani 1 d . . H14A H 0.0536(9) 0.4048(4) 0.5983(5) 0.081 Uiso 1 calc R . C15 C 0.0228(8) 0.3007(4) 0.5968(5) 0.063(2) Uani 1 d . . H15A H 0.0419(8) 0.2889(4) 0.5460(5) 0.076 Uiso 1 calc R . C21 C 0.4102(8) 0.3260(4) 0.6244(4) 0.056(2) Uani 1 d . . C22 C 0.4607(8) 0.3069(4) 0.6969(4) 0.062(2) Uani 1 d . . H22A H 0.5198(8) 0.3345(4) 0.7312(4) 0.075 Uiso 1 calc R . C23 C 0.4194(9) 0.2428(4) 0.7094(5) 0.065(2) Uani 1 d . . H23A H 0.4467(9) 0.2175(4) 0.7536(5) 0.078 Uiso 1 calc R . C24 C 0.3436(8) 0.2176(4) 0.6472(5) 0.062(2) Uani 1 d . . H24A H 0.3133(8) 0.1720(4) 0.6389(5) 0.074 Uiso 1 calc R . C25 C 0.3370(8) 0.2697(4) 0.5948(4) 0.059(2) Uani 1 d . . H25A H 0.2987(8) 0.2654(4) 0.5440(4) 0.071 Uiso 1 calc R . C31 C -0.0850(9) 0.1868(4) 0.6390(6) 0.081(3) Uani 1 d . . C32 C -0.2529(12) 0.1883(6) 0.6289(10) 0.166(7) Uani 1 d . . H32A H -0.2898(12) 0.1445(6) 0.6213(10) 0.249 Uiso 1 calc R . H32B H -0.2803(12) 0.2148(6) 0.5870(10) 0.249 Uiso 1 calc R . H32C H -0.2957(12) 0.2065(6) 0.6718(10) 0.249 Uiso 1 calc R . C33 C -0.0189(13) 0.1557(5) 0.5718(7) 0.121(4) Uani 1 d . . H33A H 0.0883(13) 0.1545(5) 0.5779(7) 0.181 Uiso 1 calc R . H33B H -0.0466(13) 0.1811(5) 0.5292(7) 0.181 Uiso 1 calc R . H33C H -0.0565(13) 0.1119(5) 0.5660(7) 0.181 Uiso 1 calc R . C34 C -0.0395(16) 0.1456(6) 0.7093(8) 0.141(5) Uani 1 d . . H34A H 0.0677(16) 0.1447(6) 0.7156(8) 0.212 Uiso 1 calc R . H34B H -0.0764(16) 0.1016(6) 0.7036(8) 0.212 Uiso 1 calc R . H34C H -0.0819(16) 0.1653(6) 0.7516(8) 0.212 Uiso 1 calc R . C41 C 0.4572(9) 0.3876(4) 0.5855(5) 0.073(2) Uani 1 d . . C42 C 0.6205(11) 0.3765(7) 0.5646(7) 0.125(5) Uani 1 d . . H42A H 0.6259(11) 0.3386(7) 0.5335(7) 0.188 Uiso 1 calc R . H42B H 0.6819(11) 0.3696(7) 0.6082(7) 0.188 Uiso 1 calc R . H42C H 0.6558(11) 0.4143(7) 0.5390(7) 0.188 Uiso 1 calc R . C43 C 0.4463(15) 0.4471(6) 0.6345(7) 0.121(4) Uani 1 d . . H43A H 0.4768(15) 0.4854(6) 0.6083(7) 0.181 Uiso 1 calc R . H43B H 0.5106(15) 0.4413(6) 0.6773(7) 0.181 Uiso 1 calc R . H43C H 0.3447(15) 0.4523(6) 0.6489(7) 0.181 Uiso 1 calc R . C44 C 0.3597(12) 0.3984(6) 0.5152(6) 0.111(4) Uani 1 d . . H44A H 0.3666(12) 0.3606(6) 0.4841(6) 0.166 Uiso 1 calc R . H44B H 0.3946(12) 0.4364(6) 0.4899(6) 0.166 Uiso 1 calc R . H44C H 0.2574(12) 0.4048(6) 0.5278(6) 0.166 Uiso 1 calc R . C51 C 0.0286(12) 0.4181(5) 0.3503(6) 0.096(3) Uani 1 d . . H51A H 0.0609(12) 0.3722(5) 0.3522(6) 0.115 Uiso 1 calc R . Cl11 Cl 0.1832(5) 0.4677(2) 0.3430(3) 0.166(2) Uani 1 d . . Cl12 Cl -0.0586(6) 0.4375(2) 0.4302(2) 0.171(2) Uani 1 d . . Cl13 Cl -0.0900(6) 0.4295(2) 0.2743(3) 0.184(2) Uani 1 d . . C61 C 0.2955(13) 0.0746(5) 0.4370(7) 0.106(3) Uani 1 d . . H61A H 0.2392(13) 0.1143(5) 0.4232(7) 0.128 Uiso 1 calc R . Cl21 Cl 0.3480(7) 0.0363(3) 0.3599(3) 0.212(3) Uani 1 d . . Cl22 Cl 0.1825(6) 0.0237(2) 0.4830(3) 0.201(2) Uani 1 d . . Cl23 Cl 0.4490(6) 0.0967(3) 0.4920(3) 0.200(2) Uani 1 d . . 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 0.0452(4) 0.0648(4) 0.0427(4) 0.0021(3) 0.0022(3) 0.0072(3) I 0.0898(5) 0.0741(4) 0.0533(4) -0.0001(3) -0.0096(3) 0.0078(3) C1 0.141(12) 0.250(18) 0.055(6) 0.052(9) 0.013(7) 0.006(11) C2 0.067(6) 0.108(7) 0.049(5) 0.004(5) 0.002(4) 0.005(6) C3 0.147(13) 0.236(20) 0.110(12) -0.100(14) -0.011(10) 0.003(13) C4 0.849(99) 0.210(27) 0.195(26) -0.033(22) 0.110(39) -0.174(41) N 0.079(6) 0.139(8) 0.059(5) -0.026(5) 0.002(4) 0.015(6) C11 0.039(4) 0.079(5) 0.065(5) -0.002(4) 0.008(4) 0.005(4) C12 0.049(5) 0.095(7) 0.072(6) -0.001(5) 0.017(4) 0.010(5) C13 0.053(5) 0.080(6) 0.088(7) -0.014(5) -0.002(4) 0.024(4) C14 0.051(5) 0.076(6) 0.074(6) 0.012(5) -0.001(4) 0.014(4) C15 0.044(4) 0.084(6) 0.061(5) 0.000(4) -0.008(4) 0.007(4) C21 0.041(4) 0.074(5) 0.052(4) 0.005(4) 0.002(3) -0.001(4) C22 0.042(4) 0.089(6) 0.057(5) 0.005(4) -0.003(3) 0.000(4) C23 0.043(4) 0.089(6) 0.063(5) 0.013(4) -0.002(4) 0.019(4) C24 0.047(5) 0.067(5) 0.072(6) 0.002(4) 0.012(4) 0.014(4) C25 0.041(4) 0.082(5) 0.054(5) -0.006(4) 0.003(4) 0.006(4) C31 0.052(5) 0.072(6) 0.119(8) 0.003(5) 0.019(5) -0.007(4) C32 0.061(7) 0.121(10) 0.317(22) -0.061(12) 0.019(10) -0.021(7) C33 0.106(9) 0.102(8) 0.156(11) -0.053(8) 0.040(8) -0.015(7) C34 0.148(12) 0.089(8) 0.189(15) 0.021(9) 0.030(11) -0.024(8) C41 0.054(5) 0.087(6) 0.076(6) 0.017(5) -0.008(4) -0.014(4) C42 0.068(7) 0.170(12) 0.138(10) 0.058(9) 0.011(7) -0.017(7) C43 0.146(11) 0.093(8) 0.123(10) 0.011(7) 0.010(8) -0.030(8) C44 0.105(8) 0.128(9) 0.097(8) 0.057(7) -0.024(6) -0.026(7) C51 0.106(8) 0.065(6) 0.116(8) -0.006(5) -0.021(7) 0.010(5) Cl11 0.143(3) 0.134(3) 0.220(5) 0.044(3) -0.029(3) -0.023(3) Cl12 0.191(4) 0.194(4) 0.128(3) 0.007(3) 0.024(3) 0.068(3) Cl13 0.239(5) 0.139(3) 0.167(4) -0.015(3) -0.109(4) 0.016(3) C61 0.108(9) 0.093(7) 0.120(9) 0.014(6) 0.029(7) 0.001(6) Cl21 0.293(7) 0.199(5) 0.151(4) -0.022(4) 0.103(4) -0.034(5) Cl22 0.213(5) 0.139(3) 0.262(6) 0.019(3) 0.145(4) -0.010(3) Cl23 0.161(4) 0.182(4) 0.254(6) -0.043(4) -0.043(4) 0.027(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 Mo C2 2.105(9) . ? Mo N 2.113(8) . ? Mo C25 2.267(7) . ? Mo C15 2.276(8) . ? Mo C24 2.287(7) . ? Mo C14 2.292(8) . ? Mo C23 2.313(7) . ? Mo C11 2.322(8) . ? Mo C13 2.337(8) . ? Mo C21 2.342(7) . ? Mo C12 2.345(8) . ? Mo C22 2.347(7) . ? C1 C2 1.523(14) . ? C2 N 1.177(12) . ? C3 C4 1.11(3) . ? C3 N 1.52(2) . ? C11 C12 1.424(11) . ? C11 C15 1.430(11) . ? C11 C31 1.517(12) . ? C12 C13 1.389(12) . ? C13 C14 1.410(12) . ? C14 C15 1.407(11) . ? C21 C25 1.418(11) . ? C21 C22 1.435(10) . ? C21 C41 1.510(11) . ? C22 C23 1.381(11) . ? C23 C24 1.397(11) . ? C24 C25 1.429(11) . ? C31 C32 1.504(13) . ? C31 C33 1.518(13) . ? C31 C34 1.57(2) . ? C41 C43 1.512(14) . ? C41 C44 1.539(12) . ? C41 C42 1.538(13) . ? C51 Cl11 1.720(11) . ? C51 Cl12 1.724(12) . ? C51 Cl13 1.728(11) . ? C61 Cl21 1.690(12) . ? C61 Cl22 1.692(11) . ? C61 Cl23 1.729(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo N 32.4(3) . . ? C2 Mo C25 137.6(3) . . ? N Mo C25 137.6(3) . . ? C2 Mo C15 136.2(3) . . ? N Mo C15 140.3(3) . . ? C25 Mo C15 78.6(3) . . ? C2 Mo C24 104.5(4) . . ? N Mo C24 121.7(3) . . ? C25 Mo C24 36.6(3) . . ? C15 Mo C24 97.3(3) . . ? C2 Mo C14 125.3(3) . . ? N Mo C14 109.6(3) . . ? C25 Mo C14 97.1(3) . . ? C15 Mo C14 35.9(3) . . ? C24 Mo C14 127.7(3) . . ? C2 Mo C23 78.8(3) . . ? N Mo C23 87.2(3) . . ? C25 Mo C23 59.1(3) . . ? C15 Mo C23 132.4(3) . . ? C24 Mo C23 35.4(3) . . ? C14 Mo C23 155.0(3) . . ? C2 Mo C11 102.9(4) . . ? N Mo C11 122.8(3) . . ? C25 Mo C11 98.8(3) . . ? C15 Mo C11 36.2(3) . . ? C24 Mo C11 96.5(3) . . ? C14 Mo C11 60.5(3) . . ? C23 Mo C11 126.1(3) . . ? C2 Mo C13 90.1(4) . . ? N Mo C13 81.7(3) . . ? C25 Mo C13 132.2(3) . . ? C15 Mo C13 58.6(3) . . ? C24 Mo C13 154.2(3) . . ? C14 Mo C13 35.5(3) . . ? C23 Mo C13 168.4(3) . . ? C11 Mo C13 59.1(3) . . ? C2 Mo C21 124.7(3) . . ? N Mo C21 106.4(3) . . ? C25 Mo C21 35.8(3) . . ? C15 Mo C21 99.1(3) . . ? C24 Mo C21 60.4(3) . . ? C14 Mo C21 97.4(3) . . ? C23 Mo C21 59.2(3) . . ? C11 Mo C21 130.1(3) . . ? C13 Mo C21 127.4(3) . . ? C2 Mo C12 78.1(3) . . ? N Mo C12 88.7(3) . . ? C25 Mo C12 133.7(3) . . ? C15 Mo C12 58.6(3) . . ? C24 Mo C12 127.4(3) . . ? C14 Mo C12 58.9(3) . . ? C23 Mo C12 142.6(3) . . ? C11 Mo C12 35.5(3) . . ? C13 Mo C12 34.5(3) . . ? C21 Mo C12 155.6(3) . . ? C2 Mo C22 89.6(3) . . ? N Mo C22 78.9(3) . . ? C25 Mo C22 58.7(3) . . ? C15 Mo C22 134.0(3) . . ? C24 Mo C22 58.7(3) . . ? C14 Mo C22 128.7(3) . . ? C23 Mo C22 34.5(3) . . ? C11 Mo C22 154.7(3) . . ? C13 Mo C22 144.1(3) . . ? C21 Mo C22 35.6(3) . . ? C12 Mo C22 167.2(3) . . ? N C2 C1 133.9(11) . . ? N C2 Mo 74.2(6) . . ? C1 C2 Mo 151.9(9) . . ? C4 C3 N 126.6(23) . . ? C2 N C3 137.0(12) . . ? C2 N Mo 73.4(6) . . ? C3 N Mo 149.6(10) . . ? C12 C11 C15 104.9(7) . . ? C12 C11 C31 126.0(8) . . ? C15 C11 C31 127.3(8) . . ? C12 C11 Mo 73.1(5) . . ? C15 C11 Mo 70.2(4) . . ? C31 C11 Mo 132.7(6) . . ? C13 C12 C11 109.5(8) . . ? C13 C12 Mo 72.4(5) . . ? C11 C12 Mo 71.3(4) . . ? C12 C13 C14 109.1(8) . . ? C12 C13 Mo 73.1(5) . . ? C14 C13 Mo 70.5(4) . . ? C15 C14 C13 106.5(8) . . ? C15 C14 Mo 71.5(4) . . ? C13 C14 Mo 74.0(5) . . ? C14 C15 C11 110.0(7) . . ? C14 C15 Mo 72.7(5) . . ? C11 C15 Mo 73.6(5) . . ? C25 C21 C22 104.9(7) . . ? C25 C21 C41 128.8(7) . . ? C22 C21 C41 125.1(7) . . ? C25 C21 Mo 69.2(4) . . ? C22 C21 Mo 72.4(4) . . ? C41 C21 Mo 132.2(6) . . ? C23 C22 C21 109.4(7) . . ? C23 C22 Mo 71.4(4) . . ? C21 C22 Mo 72.0(4) . . ? C22 C23 C24 109.7(7) . . ? C22 C23 Mo 74.1(4) . . ? C24 C23 Mo 71.3(4) . . ? C23 C24 C25 106.1(7) . . ? C23 C24 Mo 73.3(4) . . ? C25 C24 Mo 70.9(4) . . ? C21 C25 C24 109.9(7) . . ? C21 C25 Mo 75.0(4) . . ? C24 C25 Mo 72.5(4) . . ? C32 C31 C11 108.0(8) . . ? C32 C31 C33 109.0(10) . . ? C11 C31 C33 112.0(7) . . ? C32 C31 C34 109.7(10) . . ? C11 C31 C34 108.3(9) . . ? C33 C31 C34 109.8(9) . . ? C43 C41 C21 111.4(7) . . ? C43 C41 C44 109.4(9) . . ? C21 C41 C44 110.6(7) . . ? C43 C41 C42 110.3(9) . . ? C21 C41 C42 106.0(8) . . ? C44 C41 C42 109.0(9) . . ? Cl11 C51 Cl12 108.6(6) . . ? Cl11 C51 Cl13 109.2(6) . . ? Cl12 C51 Cl13 111.4(6) . . ? Cl21 C61 Cl22 108.6(7) . . ? Cl21 C61 Cl23 111.4(7) . . ? Cl22 C61 Cl23 110.2(7) . . ? _refine_diff_density_max 0.813 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.092 data_mcl10inv _database_code_CSD 161666 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Cl2 Mo' _chemical_formula_weight 409.23 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' '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 Orthorhombic _symmetry_space_group_name_H-M P22(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' _cell_length_a 6.7510(10) _cell_length_b 10.571(4) _cell_length_c 12.660(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 903.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 1.014 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5814 _exptl_absorpt_correction_T_max 0.6872 _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 ? _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 1535 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 29.99 _reflns_number_total 1535 _reflns_number_gt 1306 _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^)+(0.0414P)^2^+0.4901P] 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 0.033(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(12) _refine_ls_number_reflns 1535 _refine_ls_number_parameters 99 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _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 0.83247(5) 1.0000 1.0000 0.04445(17) Uani 1 2 d S . . Cl Cl 1.11415(19) 0.89058(19) 1.08872(18) 0.1041(7) Uani 1 1 d . . . C11 C 0.7297(8) 0.9457(4) 0.8313(4) 0.0547(12) Uani 1 1 d . . . C12 C 0.8727(10) 0.8576(5) 0.8674(5) 0.0772(19) Uani 1 1 d . . . H12A H 0.9951 0.8399 0.8316 0.080 Uiso 1 1 d R . . C13 C 0.7927(12) 0.7876(4) 0.9518(5) 0.084(2) Uani 1 1 d . . . H13A H 0.8556 0.7173 0.9862 0.080 Uiso 1 1 d R . . C14 C 0.6097(10) 0.8329(5) 0.9744(4) 0.0683(17) Uani 1 1 d . . . H14A H 0.5206 0.7997 1.0265 0.080 Uiso 1 1 d R . . C15 C 0.5672(7) 0.9308(5) 0.9014(4) 0.0553(12) Uani 1 1 d . . . H15A H 0.4431 0.9742 0.8938 0.080 Uiso 1 1 d R . . C21 C 0.7231(9) 1.0174(5) 0.7270(4) 0.0656(14) Uani 1 1 d . . . C22 C 0.9210(12) 1.0053(9) 0.6682(5) 0.110(2) Uani 1 1 d . . . H22A H 1.0206 1.0463 0.7101 0.080 Uiso 1 1 d R . . H22B H 0.9181 1.0426 0.5990 0.080 Uiso 1 1 d R . . H22C H 0.9513 0.9169 0.6623 0.080 Uiso 1 1 d R . . C23 C 0.6733(10) 1.1557(5) 0.7422(5) 0.0764(17) Uani 1 1 d . . . H23A H 0.5458 1.1625 0.7753 0.080 Uiso 1 1 d R . . H23B H 0.6710 1.1991 0.6756 0.080 Uiso 1 1 d R . . H23C H 0.7719 1.1931 0.7870 0.080 Uiso 1 1 d R . . C24 C 0.5626(16) 0.9553(7) 0.6591(5) 0.120(4) Uani 1 1 d . . . H24A H 0.4367 0.9663 0.6931 0.080 Uiso 1 1 d R . . H24B H 0.5915 0.8667 0.6532 0.080 Uiso 1 1 d R . . H24C H 0.5584 0.9924 0.5899 0.080 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.02252(18) 0.0347(2) 0.0761(3) 0.0110(3) 0.000 0.000 Cl 0.0339(5) 0.1132(13) 0.1650(17) 0.0788(13) 0.0038(9) 0.0182(7) C11 0.058(3) 0.0377(18) 0.068(3) -0.008(2) 0.026(2) -0.003(2) C12 0.094(4) 0.045(2) 0.092(4) 0.004(3) 0.047(4) 0.026(3) C13 0.135(6) 0.0306(19) 0.087(4) 0.005(2) 0.030(4) 0.001(3) C14 0.090(4) 0.050(2) 0.064(4) -0.015(2) 0.025(3) -0.036(3) C15 0.046(2) 0.058(3) 0.062(3) -0.025(2) 0.013(2) -0.015(2) C21 0.081(3) 0.050(3) 0.065(3) 0.003(3) 0.019(3) -0.008(3) C22 0.135(6) 0.099(5) 0.096(4) 0.029(5) 0.063(4) -0.001(8) C23 0.086(4) 0.052(3) 0.092(4) 0.016(3) -0.013(4) 0.001(3) C24 0.186(9) 0.105(6) 0.070(4) 0.000(4) 0.004(5) -0.064(6) _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 C12 2.271(5) . ? Mo C12 2.271(5) 2_577 ? Mo C15 2.302(5) . ? Mo C15 2.302(5) 2_577 ? Mo C11 2.318(5) . ? Mo C11 2.318(5) 2_577 ? Mo C13 2.342(5) . ? Mo C13 2.342(5) 2_577 ? Mo C14 2.342(5) . ? Mo C14 2.342(5) 2_577 ? Mo Cl 2.4931(14) 2_577 ? Mo Cl 2.4931(14) . ? C11 C12 1.417(8) . ? C11 C15 1.420(6) . ? C11 C21 1.523(7) . ? C12 C13 1.408(7) . ? C13 C14 1.355(9) . ? C14 C15 1.417(7) . ? C21 C23 1.513(8) . ? C21 C24 1.531(10) . ? C21 C22 1.535(9) . ? 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 C12 Mo C12 166.3(4) . 2_577 ? C12 Mo C15 58.8(2) . . ? C12 Mo C15 134.8(2) 2_577 . ? C12 Mo C15 134.8(2) . 2_577 ? C12 Mo C15 58.8(2) 2_577 2_577 ? C15 Mo C15 77.9(2) . 2_577 ? C12 Mo C11 36.0(2) . . ? C12 Mo C11 151.78(18) 2_577 . ? C15 Mo C11 35.79(16) . . ? C15 Mo C11 110.21(17) 2_577 . ? C12 Mo C11 151.78(18) . 2_577 ? C12 Mo C11 36.0(2) 2_577 2_577 ? C15 Mo C11 110.21(17) . 2_577 ? C15 Mo C11 35.79(16) 2_577 2_577 ? C11 Mo C11 145.2(2) . 2_577 ? C12 Mo C13 35.50(19) . . ? C12 Mo C13 147.30(19) 2_577 . ? C15 Mo C13 57.7(2) . . ? C15 Mo C13 110.9(2) 2_577 . ? C11 Mo C13 59.2(2) . . ? C11 Mo C13 116.29(19) 2_577 . ? C12 Mo C13 147.30(19) . 2_577 ? C12 Mo C13 35.50(19) 2_577 2_577 ? C15 Mo C13 110.9(2) . 2_577 ? C15 Mo C13 57.7(2) 2_577 2_577 ? C11 Mo C13 116.29(19) . 2_577 ? C11 Mo C13 59.2(2) 2_577 2_577 ? C13 Mo C13 166.8(4) . 2_577 ? C12 Mo C14 58.3(2) . . ? C12 Mo C14 132.8(2) 2_577 . ? C15 Mo C14 35.51(19) . . ? C15 Mo C14 79.36(19) 2_577 . ? C11 Mo C14 59.56(16) . . ? C11 Mo C14 97.02(17) 2_577 . ? C13 Mo C14 33.6(2) . . ? C13 Mo C14 133.3(3) 2_577 . ? C12 Mo C14 132.8(2) . 2_577 ? C12 Mo C14 58.3(2) 2_577 2_577 ? C15 Mo C14 79.35(19) . 2_577 ? C15 Mo C14 35.51(19) 2_577 2_577 ? C11 Mo C14 97.02(17) . 2_577 ? C11 Mo C14 59.56(16) 2_577 2_577 ? C13 Mo C14 133.3(3) . 2_577 ? C13 Mo C14 33.6(2) 2_577 2_577 ? C14 Mo C14 100.1(3) . 2_577 ? C12 Mo Cl 83.29(17) . 2_577 ? C12 Mo Cl 86.23(18) 2_577 2_577 ? C15 Mo Cl 119.77(14) . 2_577 ? C15 Mo Cl 133.65(15) 2_577 2_577 ? C11 Mo Cl 85.88(13) . 2_577 ? C11 Mo Cl 121.91(14) 2_577 2_577 ? C13 Mo Cl 114.51(18) . 2_577 ? C13 Mo Cl 76.1(2) 2_577 2_577 ? C14 Mo Cl 141.00(13) . 2_577 ? C14 Mo Cl 101.67(17) 2_577 2_577 ? C12 Mo Cl 86.23(18) . . ? C12 Mo Cl 83.29(17) 2_577 . ? C15 Mo Cl 133.65(15) . . ? C15 Mo Cl 119.77(14) 2_577 . ? C11 Mo Cl 121.91(14) . . ? C11 Mo Cl 85.88(13) 2_577 . ? C13 Mo Cl 76.1(2) . . ? C13 Mo Cl 114.51(18) 2_577 . ? C14 Mo Cl 101.67(17) . . ? C14 Mo Cl 141.00(13) 2_577 . ? Cl Mo Cl 80.58(7) 2_577 . ? C12 C11 C15 104.6(5) . . ? C12 C11 C21 128.8(5) . . ? C15 C11 C21 125.1(5) . . ? C12 C11 Mo 70.2(3) . . ? C15 C11 Mo 71.5(3) . . ? C21 C11 Mo 133.2(4) . . ? C13 C12 C11 109.2(5) . . ? C13 C12 Mo 75.0(3) . . ? C11 C12 Mo 73.8(3) . . ? C14 C13 C12 108.9(5) . . ? C14 C13 Mo 73.2(3) . . ? C12 C13 Mo 69.5(3) . . ? C13 C14 C15 107.8(5) . . ? C13 C14 Mo 73.2(3) . . ? C15 C14 Mo 70.7(3) . . ? C14 C15 C11 109.4(5) . . ? C14 C15 Mo 73.8(3) . . ? C11 C15 Mo 72.7(3) . . ? C23 C21 C11 112.2(5) . . ? C23 C21 C24 109.2(6) . . ? C11 C21 C24 107.1(5) . . ? C23 C21 C22 109.6(6) . . ? C11 C21 C22 110.7(5) . . ? C24 C21 C22 107.9(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.524 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.067 data_mob20 _database_code_CSD 161667 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Br2 Mo' _chemical_formula_weight 498.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'Br' 'Br' -0.2901 2.4595 '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 P22(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' _cell_length_a 7.0120(10) _cell_length_b 10.538(2) _cell_length_c 12.562(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 928.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 5.004 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.1275 _exptl_absorpt_correction_T_max 0.4344 _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 ? _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 976 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 976 _reflns_number_gt 869 _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^)+(0.0529P)^2^+1.8845P] 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 0.018(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 976 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 0.83204(13) 1.0000 1.0000 0.0295(3) Uani 1 2 d S . . Br Br 1.12007(16) 0.87827(12) 1.09061(11) 0.0673(5) Uani 1 1 d . . . C11 C 0.7296(16) 0.9560(9) 0.8261(8) 0.045(2) Uani 1 1 d . . . C12 C 0.8667(18) 0.8646(9) 0.8559(9) 0.058(3) Uani 1 1 d . . . H12A H 0.9847 0.8513 0.8188 0.080 Uiso 1 1 d R . . C13 C 0.7983(18) 0.7876(9) 0.9434(10) 0.061(3) Uani 1 1 d . . . H13A H 0.8636 0.7161 0.9735 0.080 Uiso 1 1 d R . . C14 C 0.6198(16) 0.8304(8) 0.9700(7) 0.042(2) Uani 1 1 d . . . H14A H 0.5353 0.7922 1.0209 0.080 Uiso 1 1 d R . . C15 C 0.5782(14) 0.9336(9) 0.9005(7) 0.039(2) Uani 1 1 d . . . H15A H 0.4578 0.9769 0.8979 0.080 Uiso 1 1 d R . . C21 C 0.7137(19) 1.0322(10) 0.7263(8) 0.058(3) Uani 1 1 d . . . C22 C 0.896(2) 1.0189(15) 0.6610(9) 0.092(5) Uani 1 1 d . . . H22A H 0.9188 0.9307 0.6466 0.080 Uiso 1 1 d R . . H22B H 0.9989 1.0521 0.7033 0.080 Uiso 1 1 d R . . H22C H 0.8890 1.0648 0.5951 0.080 Uiso 1 1 d R . . C23 C 0.6693(19) 1.1720(9) 0.7457(9) 0.062(3) Uani 1 1 d . . . H23A H 0.5508 1.1775 0.7836 0.080 Uiso 1 1 d R . . H23B H 0.6600 1.2193 0.6805 0.080 Uiso 1 1 d R . . H23C H 0.7699 1.2066 0.7887 0.080 Uiso 1 1 d R . . C24 C 0.549(3) 0.9747(15) 0.6627(10) 0.102(6) Uani 1 1 d . . . H24A H 0.4335 0.9852 0.7025 0.080 Uiso 1 1 d R . . H24B H 0.5726 0.8860 0.6512 0.080 Uiso 1 1 d R . . H24C H 0.5376 1.0170 0.5953 0.080 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0186(5) 0.0312(5) 0.0388(6) 0.0059(5) 0.000 0.000 Br 0.0305(6) 0.0790(8) 0.0923(10) 0.0355(7) -0.0038(6) 0.0108(5) C11 0.050(6) 0.041(5) 0.043(5) -0.010(4) -0.004(5) -0.008(4) C12 0.065(7) 0.043(5) 0.066(7) -0.013(5) 0.028(6) 0.008(6) C13 0.071(8) 0.032(5) 0.079(8) 0.007(5) -0.014(7) -0.002(5) C14 0.048(6) 0.043(5) 0.035(5) 0.002(4) 0.007(4) -0.018(5) C15 0.039(5) 0.045(5) 0.033(5) -0.015(4) 0.003(5) -0.003(4) C21 0.080(8) 0.055(7) 0.040(6) -0.003(5) 0.011(6) -0.009(6) C22 0.141(13) 0.081(10) 0.055(7) -0.002(7) 0.047(9) -0.004(11) C23 0.084(9) 0.059(6) 0.043(6) 0.018(5) -0.021(7) 0.004(7) C24 0.142(15) 0.094(12) 0.070(8) 0.019(8) -0.041(10) -0.030(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C15 2.285(10) . ? Mo C15 2.285(10) 2_577 ? Mo C12 2.317(10) 2_577 ? Mo C12 2.317(10) . ? Mo C11 2.346(10) . ? Mo C11 2.346(10) 2_577 ? Mo C14 2.356(9) . ? Mo C14 2.356(9) 2_577 ? Mo C13 2.360(10) 2_577 ? Mo C13 2.360(10) . ? Mo Br 2.6496(13) . ? Mo Br 2.6496(13) 2_577 ? C11 C12 1.412(15) . ? C11 C15 1.434(14) . ? C11 C21 1.493(14) . ? C12 C13 1.447(15) . ? C13 C14 1.372(16) . ? C14 C15 1.425(13) . ? C21 C23 1.526(14) . ? C21 C24 1.527(19) . ? C21 C22 1.527(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 C15 Mo C15 77.7(5) . 2_577 ? C15 Mo C12 134.2(4) . 2_577 ? C15 Mo C12 57.7(4) 2_577 2_577 ? C15 Mo C12 57.7(4) . . ? C15 Mo C12 134.2(4) 2_577 . ? C12 Mo C12 168.0(6) 2_577 . ? C15 Mo C11 36.0(4) . . ? C15 Mo C11 109.4(4) 2_577 . ? C12 Mo C11 151.8(4) 2_577 . ? C12 Mo C11 35.2(4) . . ? C15 Mo C11 109.4(4) . 2_577 ? C15 Mo C11 36.0(4) 2_577 2_577 ? C12 Mo C11 35.2(4) 2_577 2_577 ? C12 Mo C11 151.8(4) . 2_577 ? C11 Mo C11 144.3(6) . 2_577 ? C15 Mo C14 35.7(3) . . ? C15 Mo C14 80.1(4) 2_577 . ? C12 Mo C14 131.2(4) 2_577 . ? C12 Mo C14 58.3(4) . . ? C11 Mo C14 60.5(3) . . ? C11 Mo C14 96.0(3) 2_577 . ? C15 Mo C14 80.1(3) . 2_577 ? C15 Mo C14 35.7(3) 2_577 2_577 ? C12 Mo C14 58.3(4) 2_577 2_577 ? C12 Mo C14 131.2(4) . 2_577 ? C11 Mo C14 96.0(3) . 2_577 ? C11 Mo C14 60.5(3) 2_577 2_577 ? C14 Mo C14 101.7(5) . 2_577 ? C15 Mo C13 112.2(4) . 2_577 ? C15 Mo C13 57.8(4) 2_577 2_577 ? C12 Mo C13 36.0(4) 2_577 2_577 ? C12 Mo C13 146.1(4) . 2_577 ? C11 Mo C13 115.9(4) . 2_577 ? C11 Mo C13 60.1(4) 2_577 2_577 ? C14 Mo C13 134.8(4) . 2_577 ? C14 Mo C13 33.8(4) 2_577 2_577 ? C15 Mo C13 57.8(4) . . ? C15 Mo C13 112.2(4) 2_577 . ? C12 Mo C13 146.1(4) 2_577 . ? C12 Mo C13 36.0(4) . . ? C11 Mo C13 60.1(4) . . ? C11 Mo C13 115.9(4) 2_577 . ? C14 Mo C13 33.8(4) . . ? C14 Mo C13 134.8(4) 2_577 . ? C13 Mo C13 168.5(6) 2_577 . ? C15 Mo Br 132.9(2) . . ? C15 Mo Br 120.5(2) 2_577 . ? C12 Mo Br 83.3(3) 2_577 . ? C12 Mo Br 87.6(3) . . ? C11 Mo Br 122.5(3) . . ? C11 Mo Br 85.9(3) 2_577 . ? C14 Mo Br 100.5(3) . . ? C14 Mo Br 141.3(2) 2_577 . ? C13 Mo Br 114.0(3) 2_577 . ? C13 Mo Br 75.3(3) . . ? C15 Mo Br 120.5(2) . 2_577 ? C15 Mo Br 132.9(3) 2_577 2_577 ? C12 Mo Br 87.6(3) 2_577 2_577 ? C12 Mo Br 83.3(3) . 2_577 ? C11 Mo Br 85.9(3) . 2_577 ? C11 Mo Br 122.5(3) 2_577 2_577 ? C14 Mo Br 141.3(2) . 2_577 ? C14 Mo Br 100.5(3) 2_577 2_577 ? C13 Mo Br 75.3(3) 2_577 2_577 ? C13 Mo Br 114.0(3) . 2_577 ? Br Mo Br 80.67(6) . 2_577 ? C12 C11 C15 102.6(9) . . ? C12 C11 C21 129.9(11) . . ? C15 C11 C21 125.5(11) . . ? C12 C11 Mo 71.3(6) . . ? C15 C11 Mo 69.7(5) . . ? C21 C11 Mo 134.3(7) . . ? C11 C12 C13 111.0(10) . . ? C11 C12 Mo 73.5(6) . . ? C13 C12 Mo 73.6(6) . . ? C14 C13 C12 107.6(9) . . ? C14 C13 Mo 72.9(6) . . ? C12 C13 Mo 70.4(5) . . ? C13 C14 C15 106.8(9) . . ? C13 C14 Mo 73.3(6) . . ? C15 C14 Mo 69.4(5) . . ? C14 C15 C11 112.0(9) . . ? C14 C15 Mo 74.9(6) . . ? C11 C15 Mo 74.3(6) . . ? C11 C21 C23 113.6(9) . . ? C11 C21 C24 106.4(10) . . ? C23 C21 C24 108.2(12) . . ? C11 C21 C22 109.8(11) . . ? C23 C21 C22 110.2(11) . . ? C24 C21 C22 108.4(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.564 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.136 data_mobz10 _database_code_CSD 161668 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H40 Mo' _chemical_formula_weight 520.58 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7203(6) _cell_length_b 11.8270(7) _cell_length_c 23.325(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.519(5) _cell_angle_gamma 90.00 _cell_volume 2636.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 4.91 _cell_measurement_theta_max 15.02 _exptl_crystal_description Block _exptl_crystal_colour Dark_red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.6 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method ? _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.515 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3047 _exptl_absorpt_correction_T_max 0.3234 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.03 _diffrn_reflns_number 5182 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4610 _reflns_number_observed 3497 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+0.8129P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0078(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4609 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_obs 0.0332 _refine_ls_wR_factor_all 0.0893 _refine_ls_wR_factor_obs 0.0786 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.062 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.18627(3) 0.75509(2) 0.107254(10) 0.03343(11) Uani 1 d . . C11 C 0.2702(3) 0.8209(3) 0.20644(13) 0.0393(7) Uani 1 d . . C12 C 0.3746(3) 0.7601(3) 0.18345(14) 0.0458(8) Uani 1 d . . H12A H 0.4676(3) 0.7893(3) 0.18090(14) 0.055 Uiso 1 calc R . C13 C 0.3298(4) 0.6468(3) 0.17149(14) 0.0517(9) Uani 1 d . . H13A H 0.3873(4) 0.5836(3) 0.16223(14) 0.062 Uiso 1 calc R . C14 C 0.1941(4) 0.6395(3) 0.18538(13) 0.0481(8) Uani 1 d . . H14A H 0.1399(4) 0.5698(3) 0.18591(13) 0.058 Uiso 1 calc R . C15 C 0.1591(3) 0.7450(2) 0.20644(12) 0.0421(7) Uani 1 d . . H15A H 0.0727(3) 0.7619(2) 0.22084(12) 0.050 Uiso 1 calc R . C16 C 0.2867(3) 0.9353(3) 0.23712(14) 0.0448(8) Uani 1 d . . C17 C 0.1436(4) 0.9876(3) 0.2390(2) 0.0560(9) Uani 1 d . . H17A H 0.0883(4) 0.9351(3) 0.2565(2) 0.084 Uiso 1 calc R . H17B H 0.0968(4) 1.0047(3) 0.2001(2) 0.084 Uiso 1 calc R . H17C H 0.1559(4) 1.0558(3) 0.2617(2) 0.084 Uiso 1 calc R . C18 C 0.3621(4) 0.9100(4) 0.2998(2) 0.0707(11) Uani 1 d . . H18A H 0.3077(4) 0.8574(4) 0.3177(2) 0.106 Uiso 1 calc R . H18B H 0.3733(4) 0.9789(4) 0.3220(2) 0.106 Uiso 1 calc R . H18C H 0.4524(4) 0.8780(4) 0.2989(2) 0.106 Uiso 1 calc R . C19 C 0.3742(4) 1.0188(3) 0.2093(2) 0.0600(10) Uani 1 d . . H19A H 0.3809(4) 1.0889(3) 0.2304(2) 0.090 Uiso 1 calc R . H19B H 0.3306(4) 1.0318(3) 0.1695(2) 0.090 Uiso 1 calc R . H19C H 0.4662(4) 0.9883(3) 0.2106(2) 0.090 Uiso 1 calc R . C21 C 0.3234(3) 0.7950(3) 0.03581(13) 0.0411(7) Uani 1 d . . C22 C 0.3230(3) 0.8873(3) 0.07519(14) 0.0432(7) Uani 1 d . . H22A H 0.4069(3) 0.9207(3) 0.09883(14) 0.052 Uiso 1 calc R . C23 C 0.1850(4) 0.9338(3) 0.06911(14) 0.0446(8) Uani 1 d . . H23A H 0.1584(4) 1.0036(3) 0.08694(14) 0.054 Uiso 1 calc R . C24 C 0.1004(3) 0.8699(3) 0.02545(13) 0.0437(8) Uani 1 d . . H24A H 0.0014(3) 0.8845(3) 0.00970(13) 0.052 Uiso 1 calc R . C25 C 0.1823(3) 0.7860(3) 0.00594(13) 0.0404(7) Uani 1 d . . H25A H 0.1486(3) 0.7314(3) -0.02506(13) 0.048 Uiso 1 calc R . C26 C 0.4514(3) 0.7401(3) 0.01772(15) 0.0494(8) Uani 1 d . . C27 C 0.4071(4) 0.6535(4) -0.0301(2) 0.0821(14) Uani 1 d . . H27A H 0.3469(4) 0.6888(4) -0.0624(2) 0.123 Uiso 1 calc R . H27B H 0.3579(4) 0.5929(4) -0.0153(2) 0.123 Uiso 1 calc R . H27C H 0.4885(4) 0.6240(4) -0.0429(2) 0.123 Uiso 1 calc R . C28 C 0.5341(4) 0.8348(4) -0.0058(2) 0.0786(13) Uani 1 d . . H28A H 0.4751(4) 0.8720(4) -0.0377(2) 0.118 Uiso 1 calc R . H28B H 0.6137(4) 0.8030(4) -0.0190(2) 0.118 Uiso 1 calc R . H28C H 0.5653(4) 0.8885(4) 0.0247(2) 0.118 Uiso 1 calc R . C29 C 0.5462(4) 0.6823(4) 0.0680(2) 0.0781(13) Uani 1 d . . H29A H 0.5752(4) 0.7360(4) 0.0987(2) 0.117 Uiso 1 calc R . H29B H 0.6270(4) 0.6527(4) 0.0549(2) 0.117 Uiso 1 calc R . H29C H 0.4964(4) 0.6216(4) 0.0824(2) 0.117 Uiso 1 calc R . C1 C 0.1167(4) 0.5853(3) 0.05835(14) 0.0489(8) Uani 1 d . . H1A H 0.0233(4) 0.5979(3) 0.03625(14) 0.059 Uiso 1 calc R . H1B H 0.1774(4) 0.5745(3) 0.03009(14) 0.059 Uiso 1 calc R . C2 C -0.0531(3) 0.7543(2) 0.10247(13) 0.0417(7) Uani 1 d . . H2A H -0.0958(3) 0.7493(2) 0.06157(13) 0.050 Uiso 1 calc R . H2B H -0.0762(3) 0.6848(2) 0.12072(13) 0.050 Uiso 1 calc R . C31 C 0.1127(4) 0.4759(3) 0.08912(14) 0.0443(8) Uani 1 d . . C32 C 0.2296(4) 0.4052(3) 0.0997(2) 0.0608(10) Uani 1 d . . H32A H 0.3121(4) 0.4288(3) 0.0885(2) 0.073 Uiso 1 calc R . C33 C 0.2261(5) 0.3020(3) 0.1260(2) 0.0809(13) Uani 1 d . . H33A H 0.3056(5) 0.2566(3) 0.1318(2) 0.097 Uiso 1 calc R . C34 C 0.1076(6) 0.2643(3) 0.1441(2) 0.0769(13) Uani 1 d . . H34A H 0.1064(6) 0.1945(3) 0.1624(2) 0.092 Uiso 1 calc R . C35 C -0.0086(5) 0.3317(3) 0.1348(2) 0.0675(12) Uani 1 d . . H35A H -0.0895(5) 0.3074(3) 0.1470(2) 0.081 Uiso 1 calc R . C36 C -0.0079(4) 0.4358(3) 0.10714(15) 0.0537(9) Uani 1 d . . H36A H -0.0888(4) 0.4795(3) 0.10056(15) 0.064 Uiso 1 calc R . C41 C -0.1241(3) 0.8480(3) 0.12809(13) 0.0398(7) Uani 1 d . . C42 C -0.1477(3) 0.9540(3) 0.10211(15) 0.0473(8) Uani 1 d . . H42A H -0.1181(3) 0.9669(3) 0.06695(15) 0.057 Uiso 1 calc R . C43 C -0.2129(4) 1.0404(3) 0.1263(2) 0.0547(9) Uani 1 d . . H43A H -0.2257(4) 1.1101(3) 0.1077(2) 0.066 Uiso 1 calc R . C44 C -0.2595(4) 1.0238(3) 0.1783(2) 0.0557(9) Uani 1 d . . H44A H -0.3030(4) 1.0821(3) 0.1950(2) 0.067 Uiso 1 calc R . C45 C -0.2406(4) 0.9201(3) 0.2048(2) 0.0554(9) Uani 1 d . . H45A H -0.2716(4) 0.9079(3) 0.2397(2) 0.067 Uiso 1 calc R . C46 C -0.1757(3) 0.8335(3) 0.17998(14) 0.0482(8) Uani 1 d . . H46A H -0.1659(3) 0.7634(3) 0.19831(14) 0.058 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0387(2) 0.0298(2) 0.0302(2) 0.00236(11) 0.00197(10) 0.00220(12) C11 0.042(2) 0.041(2) 0.033(2) 0.0035(13) -0.0009(13) -0.0009(14) C12 0.043(2) 0.048(2) 0.042(2) 0.0020(15) -0.0041(14) 0.005(2) C13 0.060(2) 0.045(2) 0.044(2) 0.004(2) -0.007(2) 0.017(2) C14 0.071(2) 0.034(2) 0.034(2) 0.0072(13) -0.004(2) -0.005(2) C15 0.052(2) 0.043(2) 0.0288(15) 0.0040(14) -0.0002(13) -0.005(2) C16 0.050(2) 0.045(2) 0.037(2) -0.0053(14) 0.0018(15) -0.0058(15) C17 0.063(2) 0.046(2) 0.058(2) -0.012(2) 0.009(2) -0.002(2) C18 0.081(3) 0.075(3) 0.048(2) -0.011(2) -0.011(2) -0.009(2) C19 0.060(2) 0.050(2) 0.071(2) -0.013(2) 0.015(2) -0.015(2) C21 0.043(2) 0.039(2) 0.041(2) 0.0008(14) 0.0083(14) 0.0000(14) C22 0.046(2) 0.039(2) 0.044(2) 0.0036(14) 0.0072(15) -0.0015(15) C23 0.061(2) 0.033(2) 0.041(2) 0.0092(13) 0.015(2) 0.0082(15) C24 0.046(2) 0.050(2) 0.035(2) 0.0125(14) 0.0088(14) 0.009(2) C25 0.046(2) 0.042(2) 0.033(2) 0.0061(13) 0.0080(14) -0.0001(14) C26 0.042(2) 0.054(2) 0.052(2) -0.007(2) 0.0112(15) 0.005(2) C27 0.063(3) 0.097(3) 0.088(3) -0.041(3) 0.019(2) 0.009(2) C28 0.065(3) 0.078(3) 0.104(4) 0.006(3) 0.042(3) 0.002(2) C29 0.052(2) 0.098(3) 0.085(3) 0.000(3) 0.017(2) 0.026(2) C1 0.067(2) 0.038(2) 0.041(2) -0.0031(14) 0.006(2) -0.001(2) C2 0.044(2) 0.039(2) 0.040(2) -0.0007(14) 0.0034(13) -0.0044(15) C31 0.057(2) 0.035(2) 0.042(2) -0.0098(14) 0.010(2) -0.003(2) C32 0.066(2) 0.040(2) 0.082(3) -0.003(2) 0.027(2) 0.006(2) C33 0.095(4) 0.044(2) 0.102(4) 0.006(2) 0.015(3) 0.016(2) C34 0.121(4) 0.040(2) 0.070(3) 0.008(2) 0.020(3) -0.002(2) C35 0.094(3) 0.053(2) 0.062(2) -0.018(2) 0.030(2) -0.031(2) C36 0.058(2) 0.045(2) 0.058(2) -0.016(2) 0.011(2) -0.009(2) C41 0.031(2) 0.046(2) 0.042(2) -0.0001(14) 0.0038(13) -0.0058(14) C42 0.043(2) 0.053(2) 0.047(2) 0.009(2) 0.012(2) 0.002(2) C43 0.051(2) 0.050(2) 0.062(2) 0.004(2) 0.009(2) 0.009(2) C44 0.049(2) 0.058(2) 0.060(2) -0.011(2) 0.008(2) 0.005(2) C45 0.049(2) 0.074(3) 0.046(2) -0.004(2) 0.016(2) -0.003(2) C46 0.045(2) 0.047(2) 0.052(2) 0.007(2) 0.009(2) -0.005(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 C13 2.252(3) . ? Mo C22 2.266(3) . ? Mo C14 2.268(3) . ? Mo C23 2.292(3) . ? Mo C12 2.308(3) . ? Mo C2 2.309(3) . ? Mo C1 2.347(3) . ? Mo C21 2.364(3) . ? Mo C24 2.366(3) . ? Mo C15 2.379(3) . ? Mo C25 2.385(3) . ? Mo C11 2.436(3) . ? C11 C15 1.404(4) . ? C11 C12 1.426(4) . ? C11 C16 1.525(4) . ? C12 C13 1.421(4) . ? C13 C14 1.418(5) . ? C14 C15 1.405(4) . ? C16 C19 1.523(5) . ? C16 C17 1.531(5) . ? C16 C18 1.541(5) . ? C21 C25 1.424(4) . ? C21 C22 1.428(4) . ? C21 C26 1.530(4) . ? C22 C23 1.432(4) . ? C23 C24 1.407(5) . ? C24 C25 1.399(4) . ? C26 C29 1.516(5) . ? C26 C27 1.517(5) . ? C26 C28 1.537(5) . ? C1 C31 1.483(4) . ? C2 C41 1.488(4) . ? C31 C32 1.396(5) . ? C31 C36 1.398(5) . ? C32 C33 1.371(5) . ? C33 C34 1.372(6) . ? C34 C35 1.367(6) . ? C35 C36 1.391(5) . ? C41 C42 1.392(4) . ? C41 C46 1.403(4) . ? C42 C43 1.377(5) . ? C43 C44 1.384(5) . ? C44 C45 1.371(5) . ? C45 C46 1.385(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Mo C22 106.43(13) . . ? C13 Mo C14 36.56(13) . . ? C22 Mo C14 138.21(12) . . ? C13 Mo C23 137.88(13) . . ? C22 Mo C23 36.62(11) . . ? C14 Mo C23 149.83(11) . . ? C13 Mo C12 36.30(11) . . ? C22 Mo C12 78.81(12) . . ? C14 Mo C12 59.42(12) . . ? C23 Mo C12 102.87(12) . . ? C13 Mo C2 121.75(12) . . ? C22 Mo C2 129.31(11) . . ? C14 Mo C2 85.51(12) . . ? C23 Mo C2 92.93(11) . . ? C12 Mo C2 133.47(12) . . ? C13 Mo C1 85.71(12) . . ? C22 Mo C1 124.36(12) . . ? C14 Mo C1 80.76(11) . . ? C23 Mo C1 128.27(12) . . ? C12 Mo C1 120.93(11) . . ? C2 Mo C1 76.96(12) . . ? C13 Mo C21 102.83(12) . . ? C22 Mo C21 35.84(11) . . ? C14 Mo C21 138.27(12) . . ? C23 Mo C21 60.40(11) . . ? C12 Mo C21 93.89(12) . . ? C2 Mo C21 131.28(11) . . ? C1 Mo C21 88.73(11) . . ? C13 Mo C24 161.37(13) . . ? C22 Mo C24 58.65(11) . . ? C14 Mo C24 161.57(13) . . ? C23 Mo C24 35.11(11) . . ? C12 Mo C24 136.04(12) . . ? C2 Mo C24 76.07(11) . . ? C1 Mo C24 94.07(11) . . ? C21 Mo C24 58.56(11) . . ? C13 Mo C15 59.31(12) . . ? C22 Mo C15 122.10(11) . . ? C14 Mo C15 35.10(10) . . ? C23 Mo C15 115.46(11) . . ? C12 Mo C15 57.69(12) . . ? C2 Mo C15 75.94(11) . . ? C1 Mo C15 110.89(11) . . ? C21 Mo C15 150.76(11) . . ? C24 Mo C15 136.67(11) . . ? C13 Mo C25 129.98(12) . . ? C22 Mo C25 58.09(11) . . ? C14 Mo C25 151.73(11) . . ? C23 Mo C25 58.40(11) . . ? C12 Mo C25 128.77(12) . . ? C2 Mo C25 96.84(11) . . ? C1 Mo C25 72.45(11) . . ? C21 Mo C25 34.90(10) . . ? C24 Mo C25 34.26(10) . . ? C15 Mo C25 170.71(11) . . ? C13 Mo C11 59.37(11) . . ? C22 Mo C11 88.75(11) . . ? C14 Mo C11 58.21(11) . . ? C23 Mo C11 92.94(11) . . ? C12 Mo C11 34.86(11) . . ? C2 Mo C11 101.94(11) . . ? C1 Mo C11 138.74(11) . . ? C21 Mo C11 118.14(11) . . ? C24 Mo C11 126.17(11) . . ? C15 Mo C11 33.87(10) . . ? C25 Mo C11 146.53(11) . . ? C15 C11 C12 106.1(3) . . ? C15 C11 C16 125.6(3) . . ? C12 C11 C16 127.0(3) . . ? C15 C11 Mo 70.8(2) . . ? C12 C11 Mo 67.6(2) . . ? C16 C11 Mo 135.8(2) . . ? C13 C12 C11 109.6(3) . . ? C13 C12 Mo 69.7(2) . . ? C11 C12 Mo 77.5(2) . . ? C14 C13 C12 106.1(3) . . ? C14 C13 Mo 72.3(2) . . ? C12 C13 Mo 74.0(2) . . ? C15 C14 C13 108.7(3) . . ? C15 C14 Mo 76.8(2) . . ? C13 C14 Mo 71.1(2) . . ? C11 C15 C14 109.4(3) . . ? C11 C15 Mo 75.3(2) . . ? C14 C15 Mo 68.1(2) . . ? C19 C16 C11 113.3(3) . . ? C19 C16 C17 109.4(3) . . ? C11 C16 C17 110.7(3) . . ? C19 C16 C18 108.9(3) . . ? C11 C16 C18 105.3(3) . . ? C17 C16 C18 109.2(3) . . ? C25 C21 C22 104.9(3) . . ? C25 C21 C26 126.3(3) . . ? C22 C21 C26 126.9(3) . . ? C25 C21 Mo 73.4(2) . . ? C22 C21 Mo 68.3(2) . . ? C26 C21 Mo 134.5(2) . . ? C21 C22 C23 110.0(3) . . ? C21 C22 Mo 75.8(2) . . ? C23 C22 Mo 72.7(2) . . ? C24 C23 C22 106.2(3) . . ? C24 C23 Mo 75.3(2) . . ? C22 C23 Mo 70.7(2) . . ? C25 C24 C23 108.9(3) . . ? C25 C24 Mo 73.6(2) . . ? C23 C24 Mo 69.6(2) . . ? C24 C25 C21 110.0(3) . . ? C24 C25 Mo 72.2(2) . . ? C21 C25 Mo 71.8(2) . . ? C29 C26 C27 108.4(3) . . ? C29 C26 C21 112.8(3) . . ? C27 C26 C21 110.7(3) . . ? C29 C26 C28 108.7(3) . . ? C27 C26 C28 109.1(3) . . ? C21 C26 C28 107.1(3) . . ? C31 C1 Mo 122.8(2) . . ? C41 C2 Mo 121.0(2) . . ? C32 C31 C36 116.3(3) . . ? C32 C31 C1 121.0(3) . . ? C36 C31 C1 122.6(3) . . ? C33 C32 C31 121.8(4) . . ? C32 C33 C34 121.3(4) . . ? C35 C34 C33 118.5(4) . . ? C34 C35 C36 121.1(4) . . ? C35 C36 C31 121.0(4) . . ? C42 C41 C46 115.4(3) . . ? C42 C41 C2 123.2(3) . . ? C46 C41 C2 121.3(3) . . ? C43 C42 C41 122.8(3) . . ? C42 C43 C44 120.2(3) . . ? C45 C44 C43 118.9(3) . . ? C44 C45 C46 120.5(3) . . ? C45 C46 C41 122.1(3) . . ? _refine_diff_density_max 0.232 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.055 data_moo20 _database_code_CSD 161669 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Mo O' _chemical_formula_weight 354.33 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' 'O' 'O' 0.0106 0.0060 '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 C2/c 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' '-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 15.601(3) _cell_length_b 6.2830(10) _cell_length_c 17.732(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.21(2) _cell_angle_gamma 90.00 _cell_volume 1704.9(5) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6169 _exptl_absorpt_correction_T_max 0.9275 _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 ? _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 1547 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1490 _reflns_number_gt 1320 _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^)+(0.0380P)^2^+1.2461P] 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 0.0012(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1490 _refine_ls_number_parameters 94 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0725 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _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 0.0000 0.20671(6) 0.7500 0.04891(16) Uani 1 2 d S . . O O 0.0000 -0.0647(5) 0.7500 0.154(3) Uani 1 2 d S . . C11 C 0.04286(18) 0.2996(4) 0.63438(14) 0.0426(6) Uani 1 1 d . . . C12 C -0.0312(2) 0.1644(5) 0.61691(16) 0.0573(8) Uani 1 1 d . . . H12A H -0.0327 0.0312 0.5901 0.080 Uiso 1 1 d R . . C13 C -0.1034(2) 0.2682(6) 0.6371(2) 0.0726(10) Uani 1 1 d . . . H13A H -0.1625 0.2169 0.6272 0.080 Uiso 1 1 d R . . C14 C -0.0766(2) 0.4717(6) 0.66347(17) 0.0602(8) Uani 1 1 d . . . H14A H -0.1135 0.5815 0.6773 0.080 Uiso 1 1 d R . . C15 C 0.01171(19) 0.4932(4) 0.66086(15) 0.0472(7) Uani 1 1 d . . . H15A H 0.0462 0.6196 0.6731 0.080 Uiso 1 1 d R . . C21 C 0.1311(2) 0.2659(5) 0.61202(18) 0.0538(7) Uani 1 1 d . . . C22 C 0.1508(3) 0.0292(6) 0.6071(2) 0.0794(11) Uani 1 1 d . . . H22A H 0.1053 -0.0363 0.5701 0.080 Uiso 1 1 d R . . H22B H 0.2059 0.0100 0.5916 0.080 Uiso 1 1 d R . . H22C H 0.1529 -0.0355 0.6565 0.080 Uiso 1 1 d R . . C23 C 0.1270(3) 0.3681(8) 0.5331(2) 0.0851(12) Uani 1 1 d . . . H23A H 0.0817 0.3006 0.4964 0.080 Uiso 1 1 d R . . H23B H 0.1139 0.5168 0.5363 0.080 Uiso 1 1 d R . . H23C H 0.1819 0.3517 0.5170 0.080 Uiso 1 1 d R . . C24 C 0.2032(2) 0.3701(7) 0.6705(2) 0.0769(10) Uani 1 1 d . . . H24A H 0.1908 0.5193 0.6733 0.080 Uiso 1 1 d R . . H24B H 0.2055 0.3062 0.7200 0.080 Uiso 1 1 d R . . H24C H 0.2585 0.3517 0.6551 0.080 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0752(3) 0.0345(2) 0.0398(2) 0.000 0.01795(16) 0.000 O 0.376(9) 0.0321(19) 0.069(2) 0.000 0.085(4) 0.000 C11 0.0540(15) 0.0402(14) 0.0335(12) 0.0027(11) 0.0079(11) 0.0015(13) C12 0.069(2) 0.056(2) 0.0452(15) -0.0083(13) 0.0065(14) -0.0131(15) C13 0.0499(18) 0.094(3) 0.073(2) -0.0005(19) 0.0084(15) -0.0119(18) C14 0.0607(19) 0.069(2) 0.0517(17) 0.0124(15) 0.0139(14) 0.0205(17) C15 0.0641(18) 0.0366(14) 0.0414(14) 0.0070(11) 0.0114(12) 0.0061(13) C21 0.0586(18) 0.0489(18) 0.0574(17) 0.0058(13) 0.0199(14) 0.0071(13) C22 0.082(3) 0.061(2) 0.101(3) 0.001(2) 0.032(2) 0.0229(19) C23 0.093(3) 0.103(3) 0.072(2) 0.025(2) 0.045(2) 0.028(2) C24 0.0519(19) 0.082(3) 0.098(3) -0.001(2) 0.0167(18) -0.0059(18) _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 O 1.705(4) . ? Mo C12 2.330(3) . ? Mo C12 2.330(3) 2_556 ? Mo C13 2.346(4) 2_556 ? Mo C13 2.346(4) . ? Mo C11 2.350(2) 2_556 ? Mo C11 2.350(2) . ? Mo C14 2.417(3) 2_556 ? Mo C14 2.417(3) . ? Mo C15 2.426(3) . ? Mo C15 2.426(3) 2_556 ? C11 C12 1.419(4) . ? C11 C15 1.423(4) . ? C11 C21 1.520(4) . ? C12 C13 1.407(5) . ? C13 C14 1.397(5) . ? C14 C15 1.395(4) . ? C21 C24 1.522(5) . ? C21 C22 1.525(4) . ? C21 C23 1.530(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O Mo C12 83.45(8) . . ? O Mo C12 83.45(8) . 2_556 ? C12 Mo C12 166.89(16) . 2_556 ? O Mo C13 99.48(10) . 2_556 ? C12 Mo C13 148.94(12) . 2_556 ? C12 Mo C13 35.02(12) 2_556 2_556 ? O Mo C13 99.48(10) . . ? C12 Mo C13 35.02(12) . . ? C12 Mo C13 148.94(12) 2_556 . ? C13 Mo C13 161.0(2) 2_556 . ? O Mo C11 104.39(7) . 2_556 ? C12 Mo C11 150.81(11) . 2_556 ? C12 Mo C11 35.29(10) 2_556 2_556 ? C13 Mo C11 58.64(11) 2_556 2_556 ? C13 Mo C11 116.01(11) . 2_556 ? O Mo C11 104.39(7) . . ? C12 Mo C11 35.29(10) . . ? C12 Mo C11 150.81(11) 2_556 . ? C13 Mo C11 116.01(12) 2_556 . ? C13 Mo C11 58.64(11) . . ? C11 Mo C11 151.23(14) 2_556 . ? O Mo C14 133.53(9) . 2_556 ? C12 Mo C14 134.56(11) . 2_556 ? C12 Mo C14 57.02(12) 2_556 2_556 ? C13 Mo C14 34.06(12) 2_556 2_556 ? C13 Mo C14 126.98(15) . 2_556 ? C11 Mo C14 57.63(10) 2_556 2_556 ? C11 Mo C14 101.13(10) . 2_556 ? O Mo C14 133.53(9) . . ? C12 Mo C14 57.02(12) . . ? C12 Mo C14 134.56(11) 2_556 . ? C13 Mo C14 126.98(15) 2_556 . ? C13 Mo C14 34.06(12) . . ? C11 Mo C14 101.13(10) 2_556 . ? C11 Mo C14 57.63(10) . . ? C14 Mo C14 92.94(18) 2_556 . ? O Mo C15 137.90(7) . . ? C12 Mo C15 56.78(10) . . ? C12 Mo C15 135.83(11) 2_556 . ? C13 Mo C15 107.91(12) 2_556 . ? C13 Mo C15 56.49(12) . . ? C11 Mo C15 117.02(10) 2_556 . ? C11 Mo C15 34.61(9) . . ? C14 Mo C15 79.16(11) 2_556 . ? C14 Mo C15 33.48(10) . . ? O Mo C15 137.90(7) . 2_556 ? C12 Mo C15 135.83(11) . 2_556 ? C12 Mo C15 56.78(10) 2_556 2_556 ? C13 Mo C15 56.49(12) 2_556 2_556 ? C13 Mo C15 107.91(12) . 2_556 ? C11 Mo C15 34.61(9) 2_556 2_556 ? C11 Mo C15 117.02(10) . 2_556 ? C14 Mo C15 33.48(10) 2_556 2_556 ? C14 Mo C15 79.16(11) . 2_556 ? C15 Mo C15 84.19(13) . 2_556 ? C12 C11 C15 105.6(3) . . ? C12 C11 C21 126.9(3) . . ? C15 C11 C21 126.2(3) . . ? C12 C11 Mo 71.59(15) . . ? C15 C11 Mo 75.58(15) . . ? C21 C11 Mo 128.22(19) . . ? C13 C12 C11 108.9(3) . . ? C13 C12 Mo 73.1(2) . . ? C11 C12 Mo 73.13(15) . . ? C14 C13 C12 107.9(3) . . ? C14 C13 Mo 75.74(19) . . ? C12 C13 Mo 71.88(19) . . ? C15 C14 C13 108.1(3) . . ? C15 C14 Mo 73.60(16) . . ? C13 C14 Mo 70.19(19) . . ? C14 C15 C11 109.4(3) . . ? C14 C15 Mo 72.92(17) . . ? C11 C15 Mo 69.80(14) . . ? C11 C21 C24 110.5(3) . . ? C11 C21 C22 110.7(3) . . ? C24 C21 C22 109.2(3) . . ? C11 C21 C23 107.5(3) . . ? C24 C21 C23 109.7(3) . . ? C22 C21 C23 109.3(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.410 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.053 data_mop20 _database_code_CSD 161670 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H35 Mo P' _chemical_formula_weight 414.40 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' 'P' 'P' 0.1023 0.0942 '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/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 9.705(2) _cell_length_b 10.997(2) _cell_length_c 19.599(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.07(2) _cell_angle_gamma 90.00 _cell_volume 2090.4(7) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6778 _exptl_absorpt_correction_T_max 0.9330 _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 ? _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 3926 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3694 _reflns_number_gt 2493 _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^)+(0.0372P)^2^+0.3720P] 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 0.0051(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3694 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.021 _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 Mo Mo 0.45698(2) 0.25094(2) 0.181119(10) 0.02910(10) Uani 1 1 d . . . P P 0.20981(7) 0.25445(8) 0.14882(4) 0.03639(18) Uani 1 1 d . . . C1 C 0.0840(4) 0.2914(4) 0.21302(19) 0.0619(11) Uani 1 1 d . . . H1A H -0.0072 0.2889 0.1925 0.080 Uiso 1 1 d R . . H1B H 0.0909 0.2333 0.2495 0.080 Uiso 1 1 d R . . H1C H 0.1022 0.3714 0.2307 0.080 Uiso 1 1 d R . . C2 C 0.1634(3) 0.3653(3) 0.08156(17) 0.0504(9) Uani 1 1 d . . . H2A H 0.0659 0.3616 0.0716 0.080 Uiso 1 1 d R . . H2B H 0.1879 0.4456 0.0968 0.080 Uiso 1 1 d R . . H2C H 0.2120 0.3463 0.0411 0.080 Uiso 1 1 d R . . C3 C 0.1226(3) 0.1194(3) 0.11347(18) 0.0512(9) Uani 1 1 d . . . H3A H 0.0272 0.1377 0.1039 0.080 Uiso 1 1 d R . . H3B H 0.1651 0.0956 0.0720 0.080 Uiso 1 1 d R . . H3C H 0.1299 0.0542 0.1460 0.080 Uiso 1 1 d R . . C11 C 0.5797(3) 0.1924(3) 0.08820(14) 0.0357(7) Uani 1 1 d . . . C12 C 0.6494(3) 0.1520(3) 0.14942(15) 0.0409(7) Uani 1 1 d . . . H12A H 0.7418 0.1743 0.1633 0.080 Uiso 1 1 d R . . C13 C 0.5657(3) 0.0676(3) 0.18457(16) 0.0429(8) Uani 1 1 d . . . H13A H 0.5924 0.0226 0.2249 0.080 Uiso 1 1 d R . . C14 C 0.4425(3) 0.0532(3) 0.14511(15) 0.0411(8) Uani 1 1 d . . . H14A H 0.3694 -0.0027 0.1543 0.080 Uiso 1 1 d R . . C15 C 0.4511(3) 0.1296(3) 0.08605(14) 0.0386(7) Uani 1 1 d . . . H15A H 0.3831 0.1340 0.0493 0.080 Uiso 1 1 d R . . C16 C 0.6420(3) 0.2611(3) 0.02975(15) 0.0461(8) Uani 1 1 d . . . C17 C 0.7418(4) 0.3579(4) 0.05547(19) 0.0676(11) Uani 1 1 d . . . H17A H 0.6932 0.4172 0.0813 0.080 Uiso 1 1 d R . . H17B H 0.8126 0.3211 0.0840 0.080 Uiso 1 1 d R . . H17C H 0.7829 0.3969 0.0174 0.080 Uiso 1 1 d R . . C18 C 0.5315(4) 0.3189(5) -0.0154(2) 0.0927(16) Uani 1 1 d . . . H18A H 0.4819 0.3778 0.0102 0.080 Uiso 1 1 d R . . H18B H 0.5728 0.3582 -0.0534 0.080 Uiso 1 1 d R . . H18C H 0.4691 0.2570 -0.0320 0.080 Uiso 1 1 d R . . C19 C 0.7217(5) 0.1669(4) -0.0116(2) 0.0876(15) Uani 1 1 d . . . H19A H 0.7631 0.2064 -0.0495 0.080 Uiso 1 1 d R . . H19B H 0.7922 0.1303 0.0171 0.080 Uiso 1 1 d R . . H19C H 0.6591 0.1052 -0.0283 0.080 Uiso 1 1 d R . . C21 C 0.5386(3) 0.3183(3) 0.28599(14) 0.0352(7) Uani 1 1 d . . . C22 C 0.3960(3) 0.3482(3) 0.27930(15) 0.0395(7) Uani 1 1 d . . . H22A H 0.3252 0.3230 0.3092 0.080 Uiso 1 1 d R . . C23 C 0.3792(4) 0.4313(3) 0.22306(16) 0.0455(8) Uani 1 1 d . . . H23A H 0.2943 0.4703 0.2091 0.080 Uiso 1 1 d R . . C24 C 0.5076(4) 0.4534(3) 0.19461(17) 0.0490(9) Uani 1 1 d . . . H24A H 0.5268 0.5105 0.1591 0.080 Uiso 1 1 d R . . C25 C 0.6060(3) 0.3832(3) 0.23341(15) 0.0406(7) Uani 1 1 d . . . H25A H 0.7038 0.3846 0.2276 0.080 Uiso 1 1 d R . . C26 C 0.6084(3) 0.2549(3) 0.34707(14) 0.0427(7) Uani 1 1 d . . . C27 C 0.7514(4) 0.2088(4) 0.33046(19) 0.0611(10) Uani 1 1 d . . . H27A H 0.8066 0.2754 0.3155 0.080 Uiso 1 1 d R . . H27B H 0.7943 0.1729 0.3705 0.080 Uiso 1 1 d R . . H27D H 0.7435 0.1489 0.2949 0.080 Uiso 1 1 d R . . C28 C 0.5203(4) 0.1482(3) 0.37103(17) 0.0609(10) Uani 1 1 d . . . H28A H 0.5110 0.0890 0.3352 0.080 Uiso 1 1 d R . . H28D H 0.5640 0.1114 0.4106 0.080 Uiso 1 1 d R . . H28B H 0.4308 0.1775 0.3823 0.080 Uiso 1 1 d R . . C29 C 0.6245(4) 0.3505(3) 0.40399(16) 0.0599(10) Uani 1 1 d . . . H29D H 0.6798 0.4168 0.3886 0.080 Uiso 1 1 d R . . H29A H 0.5352 0.3802 0.4153 0.080 Uiso 1 1 d R . . H29B H 0.6685 0.3142 0.4436 0.080 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.03101(15) 0.02722(13) 0.02889(13) -0.00198(13) -0.00142(9) 0.00068(14) P 0.0330(4) 0.0389(4) 0.0371(4) 0.0004(4) -0.0017(3) 0.0008(4) C1 0.039(2) 0.088(3) 0.059(2) -0.003(2) 0.0067(17) 0.0116(19) C2 0.044(2) 0.050(2) 0.056(2) 0.0121(17) -0.0118(16) 0.0007(17) C3 0.042(2) 0.049(2) 0.062(2) 0.0023(17) -0.0075(17) -0.0110(17) C11 0.0341(17) 0.0395(16) 0.0337(15) -0.0073(13) 0.0045(13) 0.0002(14) C12 0.0334(17) 0.0445(18) 0.0450(17) -0.0089(15) 0.0031(14) 0.0092(15) C13 0.050(2) 0.0338(17) 0.0447(18) 0.0005(14) 0.0015(16) 0.0097(16) C14 0.050(2) 0.0304(15) 0.0430(18) -0.0026(14) 0.0055(15) -0.0013(15) C15 0.0415(18) 0.0367(17) 0.0375(16) -0.0112(13) 0.0007(13) 0.0000(14) C16 0.0416(18) 0.058(2) 0.0390(16) -0.0039(17) 0.0037(13) -0.0052(19) C17 0.070(3) 0.075(3) 0.059(2) 0.008(2) 0.0128(19) -0.027(2) C18 0.070(3) 0.133(4) 0.074(3) 0.056(3) -0.006(2) -0.015(3) C19 0.107(4) 0.086(3) 0.073(3) -0.015(2) 0.052(3) -0.018(3) C21 0.0423(19) 0.0296(16) 0.0334(15) -0.0042(13) -0.0037(13) -0.0011(14) C22 0.0411(19) 0.0387(17) 0.0382(16) -0.0129(14) -0.0045(13) 0.0045(15) C23 0.052(2) 0.0357(17) 0.0480(19) -0.0108(15) -0.0112(16) 0.0115(16) C24 0.070(3) 0.0295(17) 0.0463(19) -0.0004(14) -0.0114(18) -0.0085(17) C25 0.0457(19) 0.0360(16) 0.0394(16) -0.0051(14) -0.0075(14) -0.0089(15) C26 0.0500(18) 0.0422(16) 0.0354(14) -0.0016(17) -0.0067(13) 0.0040(19) C27 0.055(2) 0.073(3) 0.055(2) 0.0019(18) -0.0142(18) 0.0184(19) C28 0.085(3) 0.052(2) 0.0458(19) 0.0079(17) 0.0021(19) -0.002(2) C29 0.077(3) 0.061(2) 0.0401(18) -0.0059(17) -0.0178(18) 0.009(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 C12 2.268(3) . ? Mo C25 2.269(3) . ? Mo C13 2.276(3) . ? Mo C23 2.286(3) . ? Mo C14 2.289(3) . ? Mo C15 2.291(3) . ? Mo C24 2.293(3) . ? Mo C22 2.298(3) . ? Mo C21 2.298(3) . ? Mo C11 2.303(3) . ? Mo P 2.4589(9) . ? P C1 1.831(3) . ? P C3 1.833(3) . ? P C2 1.839(3) . ? C11 C15 1.425(4) . ? C11 C12 1.427(4) . ? C11 C16 1.516(4) . ? C12 C13 1.427(4) . ? C13 C14 1.409(4) . ? C14 C15 1.436(4) . ? C16 C18 1.507(5) . ? C16 C17 1.514(4) . ? C16 C19 1.540(5) . ? C21 C22 1.424(4) . ? C21 C25 1.431(4) . ? C21 C26 1.523(4) . ? C22 C23 1.437(4) . ? C23 C24 1.405(5) . ? C24 C25 1.426(4) . ? C26 C27 1.524(5) . ? C26 C28 1.535(5) . ? C26 C29 1.537(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Mo C25 85.04(12) . . ? C12 Mo C13 36.60(11) . . ? C25 Mo C13 105.49(12) . . ? C12 Mo C23 143.22(12) . . ? C25 Mo C23 59.65(11) . . ? C13 Mo C23 156.49(11) . . ? C12 Mo C14 60.10(11) . . ? C25 Mo C14 141.17(12) . . ? C13 Mo C14 35.97(11) . . ? C23 Mo C14 156.63(12) . . ? C12 Mo C15 59.62(11) . . ? C25 Mo C15 137.51(12) . . ? C13 Mo C15 60.41(11) . . ? C23 Mo C15 143.04(11) . . ? C14 Mo C15 36.54(10) . . ? C12 Mo C24 108.80(13) . . ? C25 Mo C24 36.42(11) . . ? C13 Mo C24 139.41(13) . . ? C23 Mo C24 35.73(12) . . ? C14 Mo C24 165.55(12) . . ? C15 Mo C24 131.15(12) . . ? C12 Mo C22 133.83(11) . . ? C25 Mo C22 60.18(11) . . ? C13 Mo C22 121.39(11) . . ? C23 Mo C22 36.53(10) . . ? C14 Mo C22 133.28(11) . . ? C15 Mo C22 162.31(11) . . ? C24 Mo C22 60.80(12) . . ? C12 Mo C21 97.99(11) . . ? C25 Mo C21 36.51(10) . . ? C13 Mo C21 96.57(11) . . ? C23 Mo C21 60.42(11) . . ? C14 Mo C21 126.66(11) . . ? C15 Mo C21 155.89(11) . . ? C24 Mo C21 61.22(11) . . ? C22 Mo C21 36.10(10) . . ? C12 Mo C11 36.37(10) . . ? C25 Mo C11 101.36(11) . . ? C13 Mo C11 61.53(11) . . ? C23 Mo C11 135.54(12) . . ? C14 Mo C11 61.21(11) . . ? C15 Mo C11 36.15(10) . . ? C24 Mo C11 104.34(12) . . ? C22 Mo C11 161.52(11) . . ? C21 Mo C11 128.74(11) . . ? C12 Mo P 137.94(8) . . ? C25 Mo P 134.91(9) . . ? C13 Mo P 117.95(9) . . ? C23 Mo P 75.36(9) . . ? C14 Mo P 83.52(8) . . ? C15 Mo P 78.71(8) . . ? C24 Mo P 102.56(9) . . ? C22 Mo P 85.98(8) . . ? C21 Mo P 121.77(8) . . ? C11 Mo P 109.16(8) . . ? C1 P C3 97.43(18) . . ? C1 P C2 101.14(17) . . ? C3 P C2 99.68(16) . . ? C1 P Mo 119.70(12) . . ? C3 P Mo 121.15(12) . . ? C2 P Mo 113.98(11) . . ? C15 C11 C12 105.2(3) . . ? C15 C11 C16 126.3(3) . . ? C12 C11 C16 126.9(3) . . ? C15 C11 Mo 71.44(16) . . ? C12 C11 Mo 70.45(16) . . ? C16 C11 Mo 133.6(2) . . ? C13 C12 C11 110.3(3) . . ? C13 C12 Mo 72.01(17) . . ? C11 C12 Mo 73.18(17) . . ? C14 C13 C12 107.1(3) . . ? C14 C13 Mo 72.53(17) . . ? C12 C13 Mo 71.39(17) . . ? C13 C14 C15 107.7(3) . . ? C13 C14 Mo 71.50(17) . . ? C15 C14 Mo 71.79(16) . . ? C11 C15 C14 109.6(3) . . ? C11 C15 Mo 72.41(16) . . ? C14 C15 Mo 71.67(16) . . ? C18 C16 C17 109.4(3) . . ? C18 C16 C11 111.1(3) . . ? C17 C16 C11 111.5(3) . . ? C18 C16 C19 109.5(3) . . ? C17 C16 C19 108.7(3) . . ? C11 C16 C19 106.5(3) . . ? C22 C21 C25 106.6(3) . . ? C22 C21 C26 125.5(3) . . ? C25 C21 C26 126.3(3) . . ? C22 C21 Mo 71.92(16) . . ? C25 C21 Mo 70.64(16) . . ? C26 C21 Mo 133.2(2) . . ? C21 C22 C23 107.5(3) . . ? C21 C22 Mo 71.98(17) . . ? C23 C22 Mo 71.29(17) . . ? C24 C23 C22 109.7(3) . . ? C24 C23 Mo 72.42(18) . . ? C22 C23 Mo 72.18(17) . . ? C23 C24 C25 106.3(3) . . ? C23 C24 Mo 71.85(18) . . ? C25 C24 Mo 70.88(17) . . ? C24 C25 C21 109.8(3) . . ? C24 C25 Mo 72.71(17) . . ? C21 C25 Mo 72.85(17) . . ? C21 C26 C27 111.5(3) . . ? C21 C26 C28 110.7(3) . . ? C27 C26 C28 109.4(3) . . ? C21 C26 C29 106.7(3) . . ? C27 C26 C29 108.2(3) . . ? C28 C26 C29 110.1(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.628 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.057 data_h2s10 _database_code_CSD 161671 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 Mo' _chemical_formula_weight 340.34 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1787(13) _cell_length_b 10.2650(16) _cell_length_c 11.3123(17) _cell_angle_alpha 79.229(3) _cell_angle_beta 73.725(3) _cell_angle_gamma 66.888(2) _cell_volume 835.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8609 _exptl_absorpt_correction_T_max 0.9268 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 '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 5668 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.22 _reflns_number_total 3619 _reflns_number_gt 3128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0399P)^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 0.0096(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3619 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0668 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _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 0.44606(3) 0.39451(2) 0.291516(17) 0.02870(9) Uani 1 1 d . . . H1 H 0.264(3) 0.396(3) 0.264(2) 0.037(7) Uiso 1 1 d . . . H2 H 0.305(4) 0.388(3) 0.424(3) 0.056(8) Uiso 1 1 d . . . C11 C 0.4737(3) 0.1620(2) 0.2713(2) 0.0323(5) Uani 1 1 d . . . C12 C 0.5052(4) 0.1647(3) 0.3877(2) 0.0372(6) Uani 1 1 d . . . H12A H 0.4343 0.1386 0.4686 0.045 Uiso 1 1 calc R . . C13 C 0.6586(4) 0.2046(3) 0.3706(3) 0.0417(6) Uani 1 1 d . . . H13A H 0.7180 0.2048 0.4357 0.050 Uiso 1 1 calc R . . C14 C 0.7239(4) 0.2266(3) 0.2406(3) 0.0409(6) Uani 1 1 d . . . H14A H 0.8380 0.2445 0.1998 0.049 Uiso 1 1 calc R . . C15 C 0.6097(4) 0.2023(3) 0.1789(2) 0.0368(6) Uani 1 1 d . . . H15A H 0.6295 0.2024 0.0884 0.044 Uiso 1 1 calc R . . C16 C 0.3413(4) 0.1032(3) 0.2493(2) 0.0379(6) Uani 1 1 d . . . C17 C 0.4435(4) -0.0579(3) 0.2430(3) 0.0535(8) Uani 1 1 d . . . H17A H 0.5503 -0.0753 0.1748 0.080 Uiso 1 1 calc R . . H17B H 0.3635 -0.1006 0.2305 0.080 Uiso 1 1 calc R . . H17C H 0.4813 -0.0995 0.3198 0.080 Uiso 1 1 calc R . . C18 C 0.1714(4) 0.1289(4) 0.3551(3) 0.0580(8) Uani 1 1 d . . . H18A H 0.2073 0.0859 0.4322 0.087 Uiso 1 1 calc R . . H18B H 0.0924 0.0867 0.3401 0.087 Uiso 1 1 calc R . . H18C H 0.1064 0.2303 0.3601 0.087 Uiso 1 1 calc R . . C19 C 0.2845(5) 0.1675(3) 0.1260(3) 0.0583(8) Uani 1 1 d . . . H19A H 0.2166 0.2688 0.1297 0.087 Uiso 1 1 calc R . . H19B H 0.2083 0.1223 0.1116 0.087 Uiso 1 1 calc R . . H19C H 0.3927 0.1519 0.0591 0.087 Uiso 1 1 calc R . . C21 C 0.2603(3) 0.6288(2) 0.2393(2) 0.0315(5) Uani 1 1 d . . . C22 C 0.2997(4) 0.6231(3) 0.3555(2) 0.0367(6) Uani 1 1 d . . . H22A H 0.2070 0.6490 0.4336 0.044 Uiso 1 1 calc R . . C23 C 0.4909(4) 0.5813(3) 0.3415(2) 0.0402(6) Uani 1 1 d . . . H23A H 0.5539 0.5787 0.4054 0.048 Uiso 1 1 calc R . . C24 C 0.5716(4) 0.5611(3) 0.2145(2) 0.0377(6) Uani 1 1 d . . . H24A H 0.7021 0.5419 0.1746 0.045 Uiso 1 1 calc R . . C25 C 0.4318(3) 0.5892(3) 0.1516(2) 0.0344(5) Uani 1 1 d . . . H25A H 0.4491 0.5906 0.0613 0.041 Uiso 1 1 calc R . . C26 C 0.0712(4) 0.6884(3) 0.2123(3) 0.0412(6) Uani 1 1 d . . . C27 C 0.0708(4) 0.6302(4) 0.0969(3) 0.0567(8) Uani 1 1 d . . . H27A H 0.1626 0.6488 0.0277 0.085 Uiso 1 1 calc R . . H27B H -0.0485 0.6764 0.0777 0.085 Uiso 1 1 calc R . . H27C H 0.0980 0.5285 0.1125 0.085 Uiso 1 1 calc R . . C28 C -0.0706(4) 0.6542(4) 0.3214(3) 0.0587(8) Uani 1 1 d . . . H28A H -0.0384 0.5520 0.3362 0.088 Uiso 1 1 calc R . . H28B H -0.1901 0.6972 0.3023 0.088 Uiso 1 1 calc R . . H28C H -0.0729 0.6919 0.3946 0.088 Uiso 1 1 calc R . . C29 C 0.0202(5) 0.8505(3) 0.1883(4) 0.0752(11) Uani 1 1 d . . . H29A H 0.0172 0.8885 0.2615 0.113 Uiso 1 1 calc R . . H29B H -0.0991 0.8933 0.1688 0.113 Uiso 1 1 calc R . . H29C H 0.1103 0.8720 0.1193 0.113 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 0.03109(13) 0.02441(12) 0.03251(12) -0.00081(7) -0.00970(8) -0.01110(9) C11 0.0353(14) 0.0199(11) 0.0402(12) -0.0006(9) -0.0132(11) -0.0061(10) C12 0.0456(16) 0.0279(13) 0.0402(13) 0.0055(10) -0.0162(12) -0.0148(12) C13 0.0446(16) 0.0330(14) 0.0545(15) 0.0042(11) -0.0283(13) -0.0132(12) C14 0.0306(14) 0.0310(14) 0.0570(16) -0.0021(12) -0.0085(12) -0.0085(11) C15 0.0395(15) 0.0268(13) 0.0389(12) -0.0034(10) -0.0060(11) -0.0083(11) C16 0.0443(15) 0.0262(13) 0.0494(14) -0.0030(11) -0.0207(12) -0.0125(11) C17 0.060(2) 0.0289(14) 0.081(2) -0.0055(14) -0.0311(17) -0.0150(14) C18 0.0474(18) 0.057(2) 0.078(2) -0.0091(16) -0.0137(16) -0.0267(16) C19 0.077(2) 0.0491(18) 0.0672(19) 0.0014(15) -0.0459(18) -0.0245(17) C21 0.0359(14) 0.0210(11) 0.0381(12) -0.0021(9) -0.0105(11) -0.0095(10) C22 0.0466(16) 0.0285(13) 0.0377(12) -0.0074(10) -0.0093(11) -0.0145(12) C23 0.0503(17) 0.0303(13) 0.0504(14) -0.0033(11) -0.0230(13) -0.0174(12) C24 0.0355(14) 0.0304(13) 0.0499(14) 0.0004(11) -0.0099(12) -0.0164(12) C25 0.0390(14) 0.0276(12) 0.0350(12) 0.0016(10) -0.0077(11) -0.0129(11) C26 0.0368(15) 0.0294(13) 0.0586(16) -0.0019(11) -0.0188(13) -0.0086(11) C27 0.056(2) 0.062(2) 0.0588(17) 0.0044(15) -0.0310(16) -0.0199(17) C28 0.0365(17) 0.071(2) 0.0674(19) -0.0133(16) -0.0077(15) -0.0173(16) C29 0.053(2) 0.0347(17) 0.137(3) -0.0007(19) -0.039(2) -0.0058(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo H1 1.60(2) . ? Mo H2 1.62(3) . ? Mo C14 2.242(3) . ? Mo C24 2.249(2) . ? Mo C13 2.277(3) . ? Mo C23 2.281(3) . ? Mo C15 2.285(3) . ? Mo C25 2.291(2) . ? Mo C22 2.325(2) . ? Mo C12 2.329(2) . ? Mo C21 2.355(2) . ? Mo C11 2.356(2) . ? C11 C12 1.418(3) . ? C11 C15 1.431(3) . ? C11 C16 1.524(3) . ? C12 C13 1.420(4) . ? C13 C14 1.425(4) . ? C14 C15 1.427(4) . ? C16 C18 1.526(4) . ? C16 C17 1.537(4) . ? C16 C19 1.541(4) . ? C21 C22 1.424(3) . ? C21 C25 1.428(3) . ? C21 C26 1.521(4) . ? C22 C23 1.419(4) . ? C23 C24 1.419(4) . ? C24 C25 1.420(3) . ? C26 C28 1.531(4) . ? C26 C27 1.535(4) . ? C26 C29 1.538(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H1 Mo H2 72.7(13) . . ? H1 Mo C14 125.3(9) . . ? H2 Mo C14 123.1(10) . . ? H1 Mo C24 124.8(9) . . ? H2 Mo C24 127.2(10) . . ? C14 Mo C24 88.93(10) . . ? H1 Mo C13 126.4(9) . . ? H2 Mo C13 87.2(10) . . ? C14 Mo C13 36.74(10) . . ? C24 Mo C13 107.17(10) . . ? H1 Mo C23 126.8(9) . . ? H2 Mo C23 91.3(10) . . ? C14 Mo C23 106.16(10) . . ? C24 Mo C23 36.52(9) . . ? C13 Mo C23 102.07(10) . . ? H1 Mo C15 89.1(9) . . ? H2 Mo C15 123.1(10) . . ? C14 Mo C15 36.73(10) . . ? C24 Mo C15 107.75(10) . . ? C13 Mo C15 61.12(10) . . ? C23 Mo C15 138.03(10) . . ? H1 Mo C25 88.7(9) . . ? H2 Mo C25 126.8(10) . . ? C14 Mo C25 108.51(9) . . ? C24 Mo C25 36.45(9) . . ? C13 Mo C25 139.25(10) . . ? C23 Mo C25 60.72(9) . . ? C15 Mo C25 105.36(9) . . ? H1 Mo C22 91.7(9) . . ? H2 Mo C22 71.6(10) . . ? C14 Mo C22 142.03(10) . . ? C24 Mo C22 59.63(10) . . ? C13 Mo C22 128.71(9) . . ? C23 Mo C22 35.88(10) . . ? C15 Mo C22 164.61(9) . . ? C25 Mo C22 59.30(9) . . ? H1 Mo C12 91.2(9) . . ? H2 Mo C12 67.3(10) . . ? C14 Mo C12 59.81(10) . . ? C24 Mo C12 143.03(10) . . ? C13 Mo C12 35.89(9) . . ? C23 Mo C12 129.47(9) . . ? C15 Mo C12 59.52(9) . . ? C25 Mo C12 164.88(9) . . ? C22 Mo C12 135.80(9) . . ? H1 Mo C21 69.6(9) . . ? H2 Mo C21 91.6(10) . . ? C14 Mo C21 144.23(9) . . ? C24 Mo C21 60.13(9) . . ? C13 Mo C21 162.27(9) . . ? C23 Mo C21 60.26(9) . . ? C15 Mo C21 132.30(9) . . ? C25 Mo C21 35.78(8) . . ? C22 Mo C21 35.43(8) . . ? C12 Mo C21 155.30(9) . . ? H1 Mo C11 69.8(9) . . ? H2 Mo C11 88.0(10) . . ? C14 Mo C11 60.19(9) . . ? C24 Mo C11 143.60(9) . . ? C13 Mo C11 60.15(9) . . ? C23 Mo C11 162.22(9) . . ? C15 Mo C11 35.87(9) . . ? C25 Mo C11 132.09(8) . . ? C22 Mo C11 156.07(9) . . ? C12 Mo C11 35.24(8) . . ? C21 Mo C11 137.52(8) . . ? C12 C11 C15 107.0(2) . . ? C12 C11 C16 125.8(2) . . ? C15 C11 C16 126.5(2) . . ? C12 C11 Mo 71.32(13) . . ? C15 C11 Mo 69.33(13) . . ? C16 C11 Mo 132.06(16) . . ? C11 C12 C13 109.9(2) . . ? C11 C12 Mo 73.45(13) . . ? C13 C12 Mo 70.06(14) . . ? C12 C13 C14 106.6(2) . . ? C12 C13 Mo 74.05(14) . . ? C14 C13 Mo 70.33(14) . . ? C13 C14 C15 108.8(2) . . ? C13 C14 Mo 72.93(15) . . ? C15 C14 Mo 73.24(15) . . ? C14 C15 C11 107.7(2) . . ? C14 C15 Mo 70.03(14) . . ? C11 C15 Mo 74.80(14) . . ? C11 C16 C18 111.5(2) . . ? C11 C16 C17 106.4(2) . . ? C18 C16 C17 108.9(2) . . ? C11 C16 C19 111.6(2) . . ? C18 C16 C19 109.6(2) . . ? C17 C16 C19 108.7(2) . . ? C22 C21 C25 106.4(2) . . ? C22 C21 C26 125.8(2) . . ? C25 C21 C26 127.1(2) . . ? C22 C21 Mo 71.16(14) . . ? C25 C21 Mo 69.68(13) . . ? C26 C21 Mo 131.18(17) . . ? C23 C22 C21 109.9(2) . . ? C23 C22 Mo 70.36(14) . . ? C21 C22 Mo 73.41(13) . . ? C22 C23 C24 106.5(2) . . ? C22 C23 Mo 73.77(14) . . ? C24 C23 Mo 70.50(14) . . ? C23 C24 C25 108.9(2) . . ? C23 C24 Mo 72.98(14) . . ? C25 C24 Mo 73.40(14) . . ? C24 C25 C21 108.2(2) . . ? C24 C25 Mo 70.15(13) . . ? C21 C25 Mo 74.54(13) . . ? C21 C26 C28 111.7(2) . . ? C21 C26 C27 111.4(2) . . ? C28 C26 C27 108.7(2) . . ? C21 C26 C29 106.5(2) . . ? C28 C26 C29 109.6(3) . . ? C27 C26 C29 108.9(3) . . ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 0.878 _refine_diff_density_max 0.371 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.066 data_mopme20 _database_code_CSD 161672 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H40 Cl2 I Mo P' _chemical_formula_weight 641.26 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'I' 'I' -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4901(7) _cell_length_b 16.0746(10) _cell_length_c 20.617(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.198(7) _cell_angle_gamma 90.00 _cell_volume 2760.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 52 _cell_measurement_theta_min 5.08 _cell_measurement_theta_max 12.47 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max .2 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method ? _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.853 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2872 _exptl_absorpt_correction_T_max 0.3297 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6033 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4852 _reflns_number_observed 2506 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+4.4813P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00001(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4852 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1304 _refine_ls_R_factor_obs 0.0539 _refine_ls_wR_factor_all 0.1189 _refine_ls_wR_factor_obs 0.0929 _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.131 _refine_ls_restrained_S_all 1.017 _refine_ls_restrained_S_obs 1.131 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.53449(8) 0.88391(5) 0.35800(3) 0.0344(2) Uani 1 d . . I I 0.03182(8) 0.61951(4) 0.35203(3) 0.0546(2) Uani 1 d . . C1 C 0.6229(10) 0.9202(5) 0.4662(4) 0.051(2) Uani 1 d . . H1A H 0.7192(10) 0.8900(5) 0.4838(4) 0.077 Uiso 1 calc R . H1B H 0.5418(10) 0.9071(5) 0.4912(4) 0.077 Uiso 1 calc R . H1C H 0.6447(10) 0.9788(5) 0.4690(4) 0.077 Uiso 1 calc R . P P 0.5593(3) 0.74670(15) 0.41526(11) 0.0459(6) Uani 1 d . . C11 C 0.7476(9) 0.9643(5) 0.3373(4) 0.042(2) Uani 1 d . . C12 C 0.8122(9) 0.8896(6) 0.3678(4) 0.046(2) Uani 1 d . . H12A H 0.8896(9) 0.8867(6) 0.4098(4) 0.055 Uiso 1 calc R . C13 C 0.7608(11) 0.8218(6) 0.3275(4) 0.050(2) Uani 1 d . . H13A H 0.7956(11) 0.7640(6) 0.3362(4) 0.061 Uiso 1 calc R . C14 C 0.6598(10) 0.8503(5) 0.2713(4) 0.046(2) Uani 1 d . . H14A H 0.6134(10) 0.8165(5) 0.2327(4) 0.055 Uiso 1 calc R . C15 C 0.6500(10) 0.9379(5) 0.2756(4) 0.044(2) Uani 1 d . . H15A H 0.5970(10) 0.9748(5) 0.2402(4) 0.053 Uiso 1 calc R . C16 C 0.8009(11) 1.0545(6) 0.3543(4) 0.053(2) Uani 1 d . . C17 C 0.8927(12) 1.0813(7) 0.3004(5) 0.085(4) Uani 1 d . . H17A H 0.8224(12) 1.0786(7) 0.2579(5) 0.128 Uiso 1 calc R . H17B H 0.9824(12) 1.0448(7) 0.3009(5) 0.128 Uiso 1 calc R . H17C H 0.9307(12) 1.1373(7) 0.3087(5) 0.128 Uiso 1 calc R . C18 C 0.9139(12) 1.0592(6) 0.4211(5) 0.080(3) Uani 1 d . . H18A H 1.0031(12) 1.0224(6) 0.4215(5) 0.121 Uiso 1 calc R . H18B H 0.8574(12) 1.0429(6) 0.4552(5) 0.121 Uiso 1 calc R . H18C H 0.9524(12) 1.1151(6) 0.4290(5) 0.121 Uiso 1 calc R . C19 C 0.6585(12) 1.1124(6) 0.3527(5) 0.074(3) Uani 1 d . . H19A H 0.5882(12) 1.1089(6) 0.3103(5) 0.111 Uiso 1 calc R . H19B H 0.6962(12) 1.1686(6) 0.3603(5) 0.111 Uiso 1 calc R . H19C H 0.6011(12) 1.0964(6) 0.3865(5) 0.111 Uiso 1 calc R . C21 C 0.2771(9) 0.8790(5) 0.2815(4) 0.039(2) Uani 1 d . . C22 C 0.2635(9) 0.8408(5) 0.3424(4) 0.041(2) Uani 1 d . . H22A H 0.2265(9) 0.7839(5) 0.3476(4) 0.049 Uiso 1 calc R . C23 C 0.2999(9) 0.9012(6) 0.3937(4) 0.047(2) Uani 1 d . . H23A H 0.2854(9) 0.8934(6) 0.4393(4) 0.056 Uiso 1 calc R . C24 C 0.3394(10) 0.9761(6) 0.3668(4) 0.049(2) Uani 1 d . . H24A H 0.3538(10) 1.0300(6) 0.3893(4) 0.059 Uiso 1 calc R . C25 C 0.3253(9) 0.9620(6) 0.2979(4) 0.048(2) Uani 1 d . . H25A H 0.3383(9) 1.0050(6) 0.2656(4) 0.057 Uiso 1 calc R . C26 C 0.2152(11) 0.8423(6) 0.2135(4) 0.047(2) Uani 1 d . . C27 C 0.2571(13) 0.7514(6) 0.2094(4) 0.071(3) Uani 1 d . . H27A H 0.2156(13) 0.7311(6) 0.1656(4) 0.106 Uiso 1 calc R . H27B H 0.2107(13) 0.7204(6) 0.2408(4) 0.106 Uiso 1 calc R . H27C H 0.3717(13) 0.7449(6) 0.2192(4) 0.106 Uiso 1 calc R . C28 C 0.0298(11) 0.8517(7) 0.2028(5) 0.086(4) Uani 1 d . . H28A H 0.0028(11) 0.9095(7) 0.2053(5) 0.128 Uiso 1 calc R . H28B H -0.0096(11) 0.8212(7) 0.2363(5) 0.128 Uiso 1 calc R . H28C H -0.0181(11) 0.8303(7) 0.1600(5) 0.128 Uiso 1 calc R . C29 C 0.2743(12) 0.8924(6) 0.1596(4) 0.069(3) Uani 1 d . . H29A H 0.2466(12) 0.9499(6) 0.1631(4) 0.103 Uiso 1 calc R . H29B H 0.2246(12) 0.8716(6) 0.1169(4) 0.103 Uiso 1 calc R . H29C H 0.3888(12) 0.8871(6) 0.1652(4) 0.103 Uiso 1 calc R . C31 C 0.4258(11) 0.7283(6) 0.4732(4) 0.068(3) Uani 1 d . . H31A H 0.3167(11) 0.7377(6) 0.4513(4) 0.102 Uiso 1 calc R . H31B H 0.4527(11) 0.7657(6) 0.5100(4) 0.102 Uiso 1 calc R . H31C H 0.4375(11) 0.6719(6) 0.4887(4) 0.102 Uiso 1 calc R . C32 C 0.7525(11) 0.7249(6) 0.4685(4) 0.062(3) Uani 1 d . . H32A H 0.7817(11) 0.7704(6) 0.4986(4) 0.092 Uiso 1 calc R . H32B H 0.8327(11) 0.7181(6) 0.4419(4) 0.092 Uiso 1 calc R . H32C H 0.7448(11) 0.6748(6) 0.4930(4) 0.092 Uiso 1 calc R . C33 C 0.5225(12) 0.6554(5) 0.3620(4) 0.068(3) Uani 1 d . . H33A H 0.4218(12) 0.6616(5) 0.3319(4) 0.101 Uiso 1 calc R . H33B H 0.5192(12) 0.6067(5) 0.3886(4) 0.101 Uiso 1 calc R . H33C H 0.6072(12) 0.6499(5) 0.3375(4) 0.101 Uiso 1 calc R . C41 C 1.1149(15) 0.5815(7) 0.5462(6) 0.097(4) Uani 1 d . . H41A H 1.0538(15) 0.5866(7) 0.5015(6) 0.116 Uiso 1 calc R . H41B H 1.0527(15) 0.5475(7) 0.5709(6) 0.116 Uiso 1 calc R . Cl41 Cl 1.2952(6) 0.5300(2) 0.5435(2) 0.143(2) Uani 1 d . . Cl42 Cl 1.1373(4) 0.6776(2) 0.58082(15) 0.0983(10) Uani 1 d . . 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 0.0323(4) 0.0365(4) 0.0354(4) -0.0027(4) 0.0089(3) 0.0032(4) I 0.0568(5) 0.0459(4) 0.0599(4) -0.0052(3) 0.0082(3) -0.0012(4) C1 0.050(6) 0.049(5) 0.055(5) -0.015(5) 0.011(5) 0.004(5) P 0.0488(14) 0.0473(14) 0.0420(12) 0.0058(11) 0.0097(11) 0.0031(13) C11 0.031(5) 0.045(5) 0.048(5) 0.010(4) 0.004(4) 0.001(4) C12 0.033(5) 0.061(6) 0.045(5) 0.010(5) 0.008(4) 0.003(5) C13 0.053(6) 0.047(6) 0.060(6) 0.010(5) 0.031(5) 0.014(5) C14 0.047(6) 0.048(5) 0.048(5) -0.005(4) 0.022(5) 0.004(5) C15 0.036(5) 0.051(6) 0.048(5) 0.009(4) 0.010(4) 0.000(4) C16 0.049(6) 0.045(6) 0.059(6) 0.008(5) -0.004(5) -0.014(5) C17 0.068(8) 0.085(8) 0.100(8) 0.020(7) 0.011(7) -0.041(7) C18 0.076(8) 0.063(7) 0.085(8) 0.000(6) -0.028(6) -0.019(6) C19 0.067(7) 0.045(6) 0.099(8) -0.004(6) -0.009(6) -0.004(6) C21 0.036(4) 0.040(5) 0.045(4) -0.006(4) 0.014(4) 0.007(4) C22 0.028(4) 0.052(5) 0.044(5) 0.003(4) 0.010(4) -0.008(4) C23 0.035(5) 0.067(7) 0.041(5) -0.006(5) 0.014(4) 0.010(5) C24 0.038(5) 0.047(6) 0.062(6) -0.022(5) 0.010(5) 0.002(5) C25 0.033(5) 0.054(6) 0.052(5) -0.003(5) -0.002(4) 0.013(5) C26 0.050(6) 0.055(6) 0.036(5) -0.007(4) 0.006(4) -0.003(5) C27 0.090(8) 0.069(7) 0.051(6) -0.018(5) 0.010(6) -0.010(7) C28 0.039(6) 0.128(10) 0.085(8) -0.031(7) 0.001(5) 0.002(7) C29 0.074(8) 0.085(8) 0.047(5) 0.000(6) 0.010(5) -0.012(7) C31 0.068(7) 0.075(7) 0.063(6) 0.018(6) 0.019(5) -0.011(6) C32 0.063(7) 0.067(7) 0.053(6) 0.010(5) 0.006(5) 0.018(6) C33 0.094(8) 0.040(5) 0.067(6) -0.002(5) 0.012(6) -0.007(6) C41 0.105(11) 0.090(9) 0.093(9) 0.022(7) 0.011(8) -0.023(9) Cl41 0.161(4) 0.069(2) 0.187(4) 0.031(2) 0.002(3) 0.005(3) Cl42 0.090(2) 0.115(3) 0.088(2) -0.011(2) 0.012(2) -0.028(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 C24 2.255(8) . ? Mo C23 2.270(8) . ? Mo C1 2.287(7) . ? Mo C15 2.291(8) . ? Mo C14 2.314(8) . ? Mo C25 2.326(8) . ? Mo C12 2.329(8) . ? Mo C11 2.329(8) . ? Mo C13 2.357(8) . ? Mo C22 2.365(7) . ? Mo C21 2.435(8) . ? Mo P 2.491(2) . ? P C32 1.821(8) . ? P C33 1.822(8) . ? P C31 1.824(8) . ? C11 C12 1.416(10) . ? C11 C15 1.440(10) . ? C11 C16 1.539(11) . ? C12 C13 1.390(11) . ? C13 C14 1.379(11) . ? C14 C15 1.414(11) . ? C16 C18 1.521(11) . ? C16 C19 1.522(12) . ? C16 C17 1.537(12) . ? C21 C25 1.417(11) . ? C21 C22 1.422(10) . ? C21 C26 1.519(10) . ? C22 C23 1.424(10) . ? C23 C24 1.393(11) . ? C24 C25 1.420(11) . ? C26 C27 1.510(12) . ? C26 C29 1.533(11) . ? C26 C28 1.554(12) . ? C41 Cl42 1.697(12) . ? C41 Cl41 1.751(12) . ? 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 C24 Mo C23 35.9(3) . . ? C24 Mo C1 82.0(3) . . ? C23 Mo C1 78.2(3) . . ? C24 Mo C15 103.7(3) . . ? C23 Mo C15 136.3(3) . . ? C1 Mo C15 121.3(3) . . ? C24 Mo C14 132.1(3) . . ? C23 Mo C14 147.4(3) . . ? C1 Mo C14 134.4(3) . . ? C15 Mo C14 35.8(3) . . ? C24 Mo C25 36.1(3) . . ? C23 Mo C25 58.6(3) . . ? C1 Mo C25 117.0(3) . . ? C15 Mo C25 78.1(3) . . ? C14 Mo C25 97.6(3) . . ? C24 Mo C12 135.6(3) . . ? C23 Mo C12 154.7(3) . . ? C1 Mo C12 76.7(3) . . ? C15 Mo C12 58.5(3) . . ? C14 Mo C12 57.8(3) . . ? C25 Mo C12 132.9(3) . . ? C24 Mo C11 105.0(3) . . ? C23 Mo C11 138.9(3) . . ? C1 Mo C11 85.3(3) . . ? C15 Mo C11 36.3(3) . . ? C14 Mo C11 59.9(3) . . ? C25 Mo C11 98.2(3) . . ? C12 Mo C11 35.4(3) . . ? C24 Mo C13 161.7(3) . . ? C23 Mo C13 161.9(3) . . ? C1 Mo C13 103.8(3) . . ? C15 Mo C13 58.2(3) . . ? C14 Mo C13 34.3(3) . . ? C25 Mo C13 131.6(3) . . ? C12 Mo C13 34.5(3) . . ? C11 Mo C13 58.9(3) . . ? C24 Mo C22 59.5(3) . . ? C23 Mo C22 35.7(3) . . ? C1 Mo C22 109.5(3) . . ? C15 Mo C22 123.7(3) . . ? C14 Mo C22 114.1(3) . . ? C25 Mo C22 57.6(3) . . ? C12 Mo C22 164.9(3) . . ? C11 Mo C22 155.2(3) . . ? C13 Mo C22 131.4(3) . . ? C24 Mo C21 59.5(3) . . ? C23 Mo C21 58.7(3) . . ? C1 Mo C21 136.3(3) . . ? C15 Mo C21 89.5(3) . . ? C14 Mo C21 88.9(3) . . ? C25 Mo C21 34.5(3) . . ? C12 Mo C21 145.5(3) . . ? C11 Mo C21 122.0(3) . . ? C13 Mo C21 119.3(3) . . ? C22 Mo C21 34.4(2) . . ? C24 Mo P 122.6(2) . . ? C23 Mo P 87.3(2) . . ? C1 Mo P 77.4(2) . . ? C15 Mo P 132.7(2) . . ? C14 Mo P 98.6(2) . . ? C25 Mo P 135.7(2) . . ? C12 Mo P 90.1(2) . . ? C11 Mo P 125.5(2) . . ? C13 Mo P 75.7(2) . . ? C22 Mo P 78.2(2) . . ? C21 Mo P 105.1(2) . . ? C32 P C33 103.7(4) . . ? C32 P C31 100.1(4) . . ? C33 P C31 102.0(5) . . ? C32 P Mo 116.1(3) . . ? C33 P Mo 116.0(3) . . ? C31 P Mo 116.6(3) . . ? C12 C11 C15 104.4(7) . . ? C12 C11 C16 128.7(7) . . ? C15 C11 C16 124.9(7) . . ? C12 C11 Mo 72.3(5) . . ? C15 C11 Mo 70.4(5) . . ? C16 C11 Mo 133.3(6) . . ? C13 C12 C11 110.4(7) . . ? C13 C12 Mo 73.9(5) . . ? C11 C12 Mo 72.3(5) . . ? C14 C13 C12 108.3(8) . . ? C14 C13 Mo 71.2(5) . . ? C12 C13 Mo 71.6(5) . . ? C13 C14 C15 108.2(8) . . ? C13 C14 Mo 74.5(5) . . ? C15 C14 Mo 71.2(5) . . ? C14 C15 C11 108.6(8) . . ? C14 C15 Mo 73.0(5) . . ? C11 C15 Mo 73.3(5) . . ? C18 C16 C19 110.3(8) . . ? C18 C16 C17 108.8(8) . . ? C19 C16 C17 109.0(8) . . ? C18 C16 C11 111.0(7) . . ? C19 C16 C11 112.0(7) . . ? C17 C16 C11 105.5(8) . . ? C25 C21 C22 105.4(7) . . ? C25 C21 C26 128.1(7) . . ? C22 C21 C26 125.1(8) . . ? C25 C21 Mo 68.5(4) . . ? C22 C21 Mo 70.1(4) . . ? C26 C21 Mo 135.8(5) . . ? C21 C22 C23 108.5(7) . . ? C21 C22 Mo 75.5(4) . . ? C23 C22 Mo 68.5(4) . . ? C24 C23 C22 109.1(7) . . ? C24 C23 Mo 71.5(5) . . ? C22 C23 Mo 75.8(4) . . ? C23 C24 C25 106.3(8) . . ? C23 C24 Mo 72.7(5) . . ? C25 C24 Mo 74.7(5) . . ? C21 C25 C24 110.6(8) . . ? C21 C25 Mo 76.9(5) . . ? C24 C25 Mo 69.3(5) . . ? C27 C26 C21 112.6(7) . . ? C27 C26 C29 110.7(8) . . ? C21 C26 C29 111.2(7) . . ? C27 C26 C28 109.2(8) . . ? C21 C26 C28 104.7(7) . . ? C29 C26 C28 108.1(8) . . ? Cl42 C41 Cl41 114.6(7) . . ? _refine_diff_density_max 0.480 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.100 data_mos20 _database_code_CSD 161673 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 Mo S2' _chemical_formula_weight 556.65 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' 'S' 'S' 0.1246 0.1234 '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 C2/c 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' '-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 21.214(7) _cell_length_b 7.0890(10) _cell_length_c 18.633(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.45(2) _cell_angle_gamma 90.00 _cell_volume 2736.2(11) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6598 _exptl_absorpt_correction_T_max 0.8294 _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 ? _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 1836 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 22.50 _reflns_number_total 1781 _reflns_number_gt 1590 _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^)+(0.0437P)^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_number_reflns 1781 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0712 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.009 _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 Mo Mo 0.0000 0.16088(5) 0.7500 0.02531(16) Uani 1 2 d S . . S S 0.04131(4) 0.44430(12) 0.69434(5) 0.0355(2) Uani 1 1 d . . . C11 C -0.07677(14) 0.1687(5) 0.62813(17) 0.0331(8) Uani 1 1 d . . . C12 C -0.10940(14) 0.1829(5) 0.68580(18) 0.0378(8) Uani 1 1 d . . . H12A H -0.1383 0.2836 0.6915 0.080 Uiso 1 1 d R . . C13 C -0.09795(15) 0.0215(5) 0.73066(19) 0.0414(9) Uani 1 1 d . . . H13A H -0.1204 -0.0134 0.7683 0.080 Uiso 1 1 d R . . C14 C -0.05685(16) -0.0954(5) 0.7009(2) 0.0430(9) Uani 1 1 d . . . H14A H -0.0461 -0.2239 0.7151 0.080 Uiso 1 1 d R . . C15 C -0.04012(16) 0.0000(5) 0.64028(19) 0.0406(9) Uani 1 1 d . . . H15A H -0.0145 -0.0508 0.6082 0.080 Uiso 1 1 d R . . C21 C -0.09193(18) 0.2852(5) 0.55851(19) 0.0483(10) Uani 1 1 d . . . C22 C -0.0385(2) 0.2752(7) 0.5154(2) 0.0688(13) Uani 1 1 d . . . H22A H -0.0005 0.3351 0.5435 0.080 Uiso 1 1 d R . . H22B H -0.0292 0.1453 0.5070 0.080 Uiso 1 1 d R . . H22C H -0.0519 0.3389 0.4692 0.080 Uiso 1 1 d R . . C23 C -0.1078(2) 0.4898(6) 0.5721(2) 0.0645(12) Uani 1 1 d . . . H23A H -0.1419 0.4936 0.5987 0.080 Uiso 1 1 d R . . H23B H -0.0700 0.5503 0.6005 0.080 Uiso 1 1 d R . . H23C H -0.1214 0.5546 0.5261 0.080 Uiso 1 1 d R . . C24 C -0.1526(2) 0.1911(7) 0.5129(2) 0.0905(18) Uani 1 1 d . . . H24A H -0.1868 0.1970 0.5393 0.080 Uiso 1 1 d R . . H24B H -0.1658 0.2550 0.4666 0.080 Uiso 1 1 d R . . H24C H -0.1431 0.0614 0.5044 0.080 Uiso 1 1 d R . . C1 C 0.11802(15) 0.4083(5) 0.67214(18) 0.0357(8) Uani 1 1 d . . . C2 C 0.13305(17) 0.2617(6) 0.63035(19) 0.0478(9) Uani 1 1 d . . . H2A H 0.1007 0.1683 0.6121 0.080 Uiso 1 1 d R . . C3 C 0.19505(18) 0.2464(7) 0.6156(2) 0.0580(11) Uani 1 1 d . . . H3A H 0.2053 0.1418 0.5874 0.080 Uiso 1 1 d R . . C4 C 0.24099(18) 0.3809(7) 0.6414(2) 0.0618(12) Uani 1 1 d . . . H4A H 0.2830 0.3727 0.6300 0.080 Uiso 1 1 d R . . C5 C 0.22623(18) 0.5272(7) 0.6822(3) 0.0655(12) Uani 1 1 d . . . H5A H 0.2584 0.6213 0.7003 0.080 Uiso 1 1 d R . . C6 C 0.16569(17) 0.5401(6) 0.6981(2) 0.0504(10) Uani 1 1 d . . . H6A H 0.1563 0.6424 0.7280 0.080 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0263(2) 0.0193(2) 0.0298(2) 0.000 0.00482(15) 0.000 S 0.0332(5) 0.0268(5) 0.0480(5) 0.0021(4) 0.0118(4) -0.0030(3) C11 0.0311(17) 0.0322(18) 0.0322(17) -0.0065(16) -0.0015(14) -0.0060(15) C12 0.0250(16) 0.047(2) 0.0380(18) -0.0041(17) -0.0008(14) -0.0025(15) C13 0.0336(19) 0.045(2) 0.045(2) 0.0011(18) 0.0063(16) -0.0157(17) C14 0.049(2) 0.0270(19) 0.047(2) 0.0014(17) -0.0021(18) -0.0108(17) C15 0.044(2) 0.035(2) 0.041(2) -0.0145(17) 0.0046(16) -0.0031(17) C21 0.058(2) 0.045(2) 0.037(2) 0.0037(17) -0.0017(17) -0.0040(18) C22 0.099(3) 0.071(3) 0.040(2) 0.013(2) 0.025(2) 0.006(3) C23 0.070(3) 0.053(3) 0.065(3) 0.019(2) 0.002(2) 0.014(2) C24 0.093(4) 0.102(4) 0.057(3) 0.012(3) -0.026(3) -0.021(3) C1 0.0339(18) 0.039(2) 0.0336(18) 0.0018(16) 0.0058(15) -0.0046(16) C2 0.041(2) 0.055(2) 0.047(2) -0.010(2) 0.0098(17) -0.0086(19) C3 0.053(2) 0.075(3) 0.049(2) -0.010(2) 0.0190(19) 0.004(2) C4 0.037(2) 0.090(3) 0.062(3) 0.001(3) 0.0179(19) -0.007(2) C5 0.040(2) 0.072(3) 0.087(3) -0.008(3) 0.019(2) -0.020(2) C6 0.040(2) 0.049(2) 0.064(3) -0.006(2) 0.0148(18) -0.0096(18) _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 C13 2.258(3) . ? Mo C13 2.258(3) 2_556 ? Mo C14 2.262(3) . ? Mo C14 2.262(3) 2_556 ? Mo C15 2.335(3) . ? Mo C15 2.335(3) 2_556 ? Mo C12 2.376(3) 2_556 ? Mo C12 2.376(3) . ? Mo C11 2.493(3) . ? Mo C11 2.493(3) 2_556 ? Mo S 2.5044(9) . ? Mo S 2.5044(9) 2_556 ? S C1 1.782(3) . ? C11 C12 1.402(4) . ? C11 C15 1.418(5) . ? C11 C21 1.513(5) . ? C12 C13 1.407(5) . ? C13 C14 1.401(5) . ? C14 C15 1.425(5) . ? C21 C23 1.523(6) . ? C21 C22 1.525(5) . ? C21 C24 1.533(5) . ? C1 C2 1.377(5) . ? C1 C6 1.385(5) . ? C2 C3 1.405(5) . ? C3 C4 1.374(6) . ? C4 C5 1.362(6) . ? C5 C6 1.381(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Mo C13 128.11(19) . 2_556 ? C13 Mo C14 36.12(13) . . ? C13 Mo C14 96.03(14) 2_556 . ? C13 Mo C14 96.03(14) . 2_556 ? C13 Mo C14 36.12(13) 2_556 2_556 ? C14 Mo C14 73.14(18) . 2_556 ? C13 Mo C15 59.84(13) . . ? C13 Mo C15 94.31(13) 2_556 . ? C14 Mo C15 36.07(12) . . ? C14 Mo C15 91.37(13) 2_556 . ? C13 Mo C15 94.31(13) . 2_556 ? C13 Mo C15 59.84(13) 2_556 2_556 ? C14 Mo C15 91.37(13) . 2_556 ? C14 Mo C15 36.07(12) 2_556 2_556 ? C15 Mo C15 121.55(18) . 2_556 ? C13 Mo C12 150.96(13) . 2_556 ? C13 Mo C12 35.23(12) 2_556 2_556 ? C14 Mo C12 129.36(13) . 2_556 ? C14 Mo C12 58.08(13) 2_556 2_556 ? C15 Mo C12 127.23(12) . 2_556 ? C15 Mo C12 57.26(12) 2_556 2_556 ? C13 Mo C12 35.23(12) . . ? C13 Mo C12 150.96(13) 2_556 . ? C14 Mo C12 58.08(13) . . ? C14 Mo C12 129.36(13) 2_556 . ? C15 Mo C12 57.26(12) . . ? C15 Mo C12 127.23(12) 2_556 . ? C12 Mo C12 172.46(18) 2_556 . ? C13 Mo C11 57.77(12) . . ? C13 Mo C11 123.56(12) 2_556 . ? C14 Mo C11 57.51(12) . . ? C14 Mo C11 124.96(12) 2_556 . ? C15 Mo C11 33.94(11) . . ? C15 Mo C11 148.36(12) 2_556 . ? C12 Mo C11 146.35(10) 2_556 . ? C12 Mo C11 33.35(10) . . ? C13 Mo C11 123.56(12) . 2_556 ? C13 Mo C11 57.77(12) 2_556 2_556 ? C14 Mo C11 124.96(12) . 2_556 ? C14 Mo C11 57.51(12) 2_556 2_556 ? C15 Mo C11 148.36(12) . 2_556 ? C15 Mo C11 33.94(11) 2_556 2_556 ? C12 Mo C11 33.35(10) 2_556 2_556 ? C12 Mo C11 146.35(10) . 2_556 ? C11 Mo C11 177.45(15) . 2_556 ? C13 Mo S 132.60(9) . . ? C13 Mo S 91.44(10) 2_556 . ? C14 Mo S 132.87(9) . . ? C14 Mo S 127.47(10) 2_556 . ? C15 Mo S 97.08(9) . . ? C15 Mo S 131.32(9) 2_556 . ? C12 Mo S 76.40(9) 2_556 . ? C12 Mo S 97.46(9) . . ? C11 Mo S 79.81(8) . . ? C11 Mo S 98.11(8) 2_556 . ? C13 Mo S 91.44(10) . 2_556 ? C13 Mo S 132.60(9) 2_556 2_556 ? C14 Mo S 127.47(10) . 2_556 ? C14 Mo S 132.87(9) 2_556 2_556 ? C15 Mo S 131.32(9) . 2_556 ? C15 Mo S 97.08(9) 2_556 2_556 ? C12 Mo S 97.45(9) 2_556 2_556 ? C12 Mo S 76.40(9) . 2_556 ? C11 Mo S 98.11(8) . 2_556 ? C11 Mo S 79.81(8) 2_556 2_556 ? S Mo S 73.31(4) . 2_556 ? C1 S Mo 113.57(12) . . ? C12 C11 C15 106.4(3) . . ? C12 C11 C21 124.7(3) . . ? C15 C11 C21 127.2(3) . . ? C12 C11 Mo 68.71(17) . . ? C15 C11 Mo 66.91(17) . . ? C21 C11 Mo 140.3(2) . . ? C11 C12 C13 110.3(3) . . ? C11 C12 Mo 77.94(17) . . ? C13 C12 Mo 67.83(18) . . ? C14 C13 C12 106.7(3) . . ? C14 C13 Mo 72.09(19) . . ? C12 C13 Mo 76.94(19) . . ? C13 C14 C15 108.4(3) . . ? C13 C14 Mo 71.79(19) . . ? C15 C14 Mo 74.76(19) . . ? C11 C15 C14 107.8(3) . . ? C11 C15 Mo 79.15(19) . . ? C14 C15 Mo 69.17(18) . . ? C11 C21 C23 113.0(3) . . ? C11 C21 C22 112.4(3) . . ? C23 C21 C22 110.4(4) . . ? C11 C21 C24 103.7(3) . . ? C23 C21 C24 108.5(4) . . ? C22 C21 C24 108.5(4) . . ? C2 C1 C6 117.8(3) . . ? C2 C1 S 125.0(3) . . ? C6 C1 S 117.2(3) . . ? C1 C2 C3 120.6(4) . . ? C4 C3 C2 120.1(4) . . ? C5 C4 C3 119.5(4) . . ? C4 C5 C6 120.4(4) . . ? C5 C6 C1 121.5(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.231 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.070 data_mose10 _database_code_CSD 161674 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H32 Mo Se' _chemical_formula_weight 495.40 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5880(10) _cell_length_b 15.9170(10) _cell_length_c 16.169(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.070(10) _cell_angle_gamma 90.00 _cell_volume 2207.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 4.39 _cell_measurement_theta_max 14.98 _exptl_crystal_description Block _exptl_crystal_colour Dark_Orange _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method ? _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 2.248 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1638 _exptl_absorpt_correction_T_max 0.3035 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3696 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 23.99 _reflns_number_total 3377 _reflns_number_observed 2166 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+9.1960P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3377 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_obs 0.0560 _refine_ls_wR_factor_all 0.1568 _refine_ls_wR_factor_obs 0.1247 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_goodness_of_fit_obs 1.068 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.068 _refine_ls_shift/esd_max -0.015 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.98223(10) 0.32051(4) 0.23808(5) 0.0438(3) Uani 1 d . . Se Se 0.94541(14) 0.16036(6) 0.20520(7) 0.0618(4) Uani 1 d . . H H 1.1306(71) 0.3086(36) 0.2100(36) 0.016(16) Uiso 1 d . . C11 C 0.8506(11) 0.3098(5) 0.3607(5) 0.047(2) Uani 1 d . . C12 C 0.9008(13) 0.3938(6) 0.3473(5) 0.054(3) Uani 1 d . . H12A H 0.8328(13) 0.4433(6) 0.3438(5) 0.065 Uiso 1 calc R . C13 C 1.0668(15) 0.3954(7) 0.3482(6) 0.067(3) Uani 1 d . . H13A H 1.1318(15) 0.4459(7) 0.3471(6) 0.081 Uiso 1 calc R . C14 C 1.1204(13) 0.3135(8) 0.3651(6) 0.069(3) Uani 1 d . . H14A H 1.2294(13) 0.2961(8) 0.3746(6) 0.083 Uiso 1 calc R . C15 C 0.9883(13) 0.2624(6) 0.3721(6) 0.058(3) Uani 1 d . . H15A H 0.9917(13) 0.2021(6) 0.3842(6) 0.069 Uiso 1 calc R . C16 C 0.6869(13) 0.2822(6) 0.3763(6) 0.060(3) Uani 1 d . . C17 C 0.5726(14) 0.3125(10) 0.3076(8) 0.107(5) Uani 1 d . . H17A H 0.4693(14) 0.2943(10) 0.3188(8) 0.160 Uiso 1 calc R . H17B H 0.6012(14) 0.2897(10) 0.2556(8) 0.160 Uiso 1 calc R . H17C H 0.5750(14) 0.3728(10) 0.3051(8) 0.160 Uiso 1 calc R . C18 C 0.6756(14) 0.1878(6) 0.3850(7) 0.081(4) Uani 1 d . . H18A H 0.5701(14) 0.1725(6) 0.3948(7) 0.121 Uiso 1 calc R . H18B H 0.7433(14) 0.1695(6) 0.4307(7) 0.121 Uiso 1 calc R . H18C H 0.7064(14) 0.1614(6) 0.3350(7) 0.121 Uiso 1 calc R . C19 C 0.6436(14) 0.3220(7) 0.4578(7) 0.087(4) Uani 1 d . . H19A H 0.5396(14) 0.3057(7) 0.4698(7) 0.130 Uiso 1 calc R . H19B H 0.6489(14) 0.3821(7) 0.4534(7) 0.130 Uiso 1 calc R . H19C H 0.7151(14) 0.3033(7) 0.5017(7) 0.130 Uiso 1 calc R . C21 C 1.0731(11) 0.3862(5) 0.1180(5) 0.043(2) Uani 1 d . . C22 C 0.9855(12) 0.4445(5) 0.1639(5) 0.048(2) Uani 1 d . . H22A H 1.0244(12) 0.4985(5) 0.1855(5) 0.058 Uiso 1 calc R . C23 C 0.8317(12) 0.4162(6) 0.1666(6) 0.056(3) Uani 1 d . . H23A H 0.7453(12) 0.4478(6) 0.1887(6) 0.067 Uiso 1 calc R . C24 C 0.8184(11) 0.3400(6) 0.1262(6) 0.050(2) Uani 1 d . . H24A H 0.7215(11) 0.3091(6) 0.1132(6) 0.061 Uiso 1 calc R . C25 C 0.9672(10) 0.3213(5) 0.0964(5) 0.046(2) Uani 1 d . . H25A H 0.9901(10) 0.2730(5) 0.0614(5) 0.055 Uiso 1 calc R . C26 C 1.2349(12) 0.4000(6) 0.0892(6) 0.055(3) Uani 1 d . . C27 C 1.2183(14) 0.4516(7) 0.0096(7) 0.081(4) Uani 1 d . . H27A H 1.3196(14) 0.4617(7) -0.0108(7) 0.122 Uiso 1 calc R . H27B H 1.1693(14) 0.5043(7) 0.0208(7) 0.122 Uiso 1 calc R . H27C H 1.1556(14) 0.4213(7) -0.0313(7) 0.122 Uiso 1 calc R . C28 C 1.3162(12) 0.3162(6) 0.0709(7) 0.070(3) Uani 1 d . . H28A H 1.4188(12) 0.3272(6) 0.0527(7) 0.105 Uiso 1 calc R . H28B H 1.2565(12) 0.2865(6) 0.0283(7) 0.105 Uiso 1 calc R . H28C H 1.3238(12) 0.2827(6) 0.1203(7) 0.105 Uiso 1 calc R . C29 C 1.3349(14) 0.4489(7) 0.1529(7) 0.077(3) Uani 1 d . . H29A H 1.4372(14) 0.4568(7) 0.1330(7) 0.116 Uiso 1 calc R . H29B H 1.3426(14) 0.4181(7) 0.2040(7) 0.116 Uiso 1 calc R . H29C H 1.2880(14) 0.5026(7) 0.1619(7) 0.116 Uiso 1 calc R . C1 C 1.1399(13) 0.1228(5) 0.1659(6) 0.057(3) Uani 1 d . . C2 C 1.2734(15) 0.1172(6) 0.2181(7) 0.070(3) Uani 1 d . . H2A H 1.2689(15) 0.1327(6) 0.2734(7) 0.083 Uiso 1 calc R . C3 C 1.4108(15) 0.0895(7) 0.1896(8) 0.080(3) Uani 1 d . . H3A H 1.4983(15) 0.0850(7) 0.2259(8) 0.095 Uiso 1 calc R . C4 C 1.4212(17) 0.0682(7) 0.1085(10) 0.086(4) Uani 1 d . . H4A H 1.5158(17) 0.0505(7) 0.0891(10) 0.103 Uiso 1 calc R . C5 C 1.2913(18) 0.0730(6) 0.0555(7) 0.080(4) Uani 1 d . . H5A H 1.2972(18) 0.0590(6) -0.0001(7) 0.096 Uiso 1 calc R . C6 C 1.1516(14) 0.0989(6) 0.0855(6) 0.063(3) Uani 1 d . . H6A H 1.0629(14) 0.1001(6) 0.0499(6) 0.076 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0589(6) 0.0388(4) 0.0350(4) 0.0011(3) 0.0149(4) 0.0058(4) Se 0.0768(8) 0.0425(5) 0.0689(7) -0.0032(4) 0.0288(6) -0.0002(5) C11 0.062(6) 0.043(5) 0.036(5) 0.001(4) 0.015(5) 0.013(5) C12 0.084(8) 0.043(5) 0.038(5) -0.008(4) 0.031(5) -0.001(5) C13 0.089(9) 0.072(7) 0.042(6) -0.009(5) 0.019(6) -0.019(7) C14 0.054(7) 0.115(10) 0.038(5) 0.012(6) -0.002(5) 0.008(7) C15 0.072(8) 0.061(6) 0.041(6) 0.004(4) 0.015(6) 0.008(6) C16 0.064(7) 0.056(6) 0.061(7) 0.009(5) 0.020(6) 0.005(5) C17 0.057(8) 0.154(14) 0.110(11) 0.051(10) 0.014(8) 0.001(9) C18 0.091(9) 0.066(7) 0.090(8) -0.002(6) 0.042(7) -0.016(6) C19 0.100(9) 0.072(7) 0.096(9) 0.010(6) 0.069(8) 0.012(7) C21 0.068(7) 0.034(4) 0.027(4) 0.010(3) 0.009(4) 0.006(4) C22 0.071(7) 0.035(5) 0.040(5) 0.010(4) 0.003(5) 0.015(5) C23 0.050(7) 0.065(6) 0.055(6) 0.013(5) 0.015(5) 0.014(5) C24 0.034(5) 0.068(6) 0.049(5) 0.000(5) 0.007(5) -0.006(5) C25 0.047(6) 0.052(5) 0.039(5) 0.003(4) 0.011(4) 0.002(5) C26 0.069(7) 0.042(5) 0.054(6) 0.014(4) 0.013(5) -0.007(5) C27 0.082(9) 0.089(8) 0.073(8) 0.037(6) 0.008(7) -0.012(7) C28 0.060(7) 0.072(7) 0.081(7) 0.003(6) 0.033(6) 0.010(6) C29 0.078(9) 0.065(7) 0.088(9) 0.000(6) -0.001(7) -0.008(6) C1 0.079(8) 0.038(5) 0.055(6) 0.008(4) 0.016(6) 0.003(5) C2 0.099(10) 0.053(6) 0.059(7) -0.002(5) 0.022(7) 0.014(6) C3 0.081(9) 0.067(7) 0.091(9) 0.003(6) 0.009(8) 0.012(6) C4 0.085(10) 0.065(7) 0.110(11) 0.020(7) 0.039(9) 0.020(7) C5 0.126(12) 0.064(7) 0.055(7) 0.007(5) 0.046(8) 0.014(7) C6 0.091(9) 0.051(6) 0.049(6) -0.001(5) 0.020(6) 0.015(6) _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 C13 2.232(10) . ? Mo C24 2.252(9) . ? Mo C12 2.259(8) . ? Mo C23 2.273(9) . ? Mo C25 2.288(8) . ? Mo C22 2.311(8) . ? Mo C14 2.318(10) . ? Mo C11 2.340(8) . ? Mo C15 2.355(9) . ? Mo C21 2.373(7) . ? Mo Se 2.6198(12) . ? Se C1 1.914(10) . ? C11 C15 1.407(13) . ? C11 C12 1.425(12) . ? C11 C16 1.507(13) . ? C12 C13 1.425(14) . ? C13 C14 1.405(15) . ? C14 C15 1.405(14) . ? C16 C18 1.514(13) . ? C16 C17 1.521(15) . ? C16 C19 1.527(13) . ? C21 C25 1.409(12) . ? C21 C22 1.427(12) . ? C21 C26 1.506(13) . ? C22 C23 1.399(13) . ? C23 C24 1.379(13) . ? C24 C25 1.422(12) . ? C26 C29 1.519(14) . ? C26 C27 1.526(12) . ? C26 C28 1.541(13) . ? C1 C6 1.363(13) . ? C1 C2 1.390(14) . ? C2 C3 1.363(15) . ? C3 C4 1.36(2) . ? C4 C5 1.37(2) . ? C5 C6 1.381(15) . ? 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 C13 Mo C24 136.9(4) . . ? C13 Mo C12 37.0(4) . . ? C24 Mo C12 110.5(4) . . ? C13 Mo C23 101.5(4) . . ? C24 Mo C23 35.5(3) . . ? C12 Mo C23 81.9(4) . . ? C13 Mo C25 142.6(4) . . ? C24 Mo C25 36.5(3) . . ? C12 Mo C25 141.0(3) . . ? C23 Mo C25 59.2(3) . . ? C13 Mo C22 86.9(4) . . ? C24 Mo C22 59.3(3) . . ? C12 Mo C22 88.7(3) . . ? C23 Mo C22 35.5(3) . . ? C25 Mo C22 58.5(3) . . ? C13 Mo C14 35.9(4) . . ? C24 Mo C14 170.3(4) . . ? C12 Mo C14 59.9(4) . . ? C23 Mo C14 137.1(4) . . ? C25 Mo C14 152.3(3) . . ? C22 Mo C14 118.8(4) . . ? C13 Mo C11 60.9(4) . . ? C24 Mo C11 112.4(3) . . ? C12 Mo C11 36.1(3) . . ? C23 Mo C11 101.1(3) . . ? C25 Mo C11 147.6(3) . . ? C22 Mo C11 121.5(3) . . ? C14 Mo C11 59.6(4) . . ? C13 Mo C15 59.0(4) . . ? C24 Mo C15 140.8(4) . . ? C12 Mo C15 58.4(3) . . ? C23 Mo C15 135.7(3) . . ? C25 Mo C15 157.1(3) . . ? C22 Mo C15 144.4(3) . . ? C14 Mo C15 35.0(3) . . ? C11 Mo C15 34.9(3) . . ? C13 Mo C21 108.1(3) . . ? C24 Mo C21 60.1(3) . . ? C12 Mo C21 122.7(3) . . ? C23 Mo C21 59.5(3) . . ? C25 Mo C21 35.1(3) . . ? C22 Mo C21 35.4(3) . . ? C14 Mo C21 124.8(4) . . ? C11 Mo C21 156.9(3) . . ? C15 Mo C21 159.1(4) . . ? C13 Mo Se 135.4(3) . . ? C24 Mo Se 84.7(2) . . ? C12 Mo Se 128.5(2) . . ? C23 Mo Se 119.3(3) . . ? C25 Mo Se 78.6(2) . . ? C22 Mo Se 136.9(2) . . ? C14 Mo Se 100.5(3) . . ? C11 Mo Se 92.4(2) . . ? C15 Mo Se 78.5(2) . . ? C21 Mo Se 107.7(2) . . ? C1 Se Mo 105.8(3) . . ? C15 C11 C12 105.3(9) . . ? C15 C11 C16 127.3(8) . . ? C12 C11 C16 126.3(8) . . ? C15 C11 Mo 73.1(5) . . ? C12 C11 Mo 68.9(4) . . ? C16 C11 Mo 131.3(7) . . ? C11 C12 C13 109.0(9) . . ? C11 C12 Mo 75.1(5) . . ? C13 C12 Mo 70.5(5) . . ? C14 C13 C12 107.7(9) . . ? C14 C13 Mo 75.4(6) . . ? C12 C13 Mo 72.5(6) . . ? C13 C14 C15 107.2(10) . . ? C13 C14 Mo 68.7(6) . . ? C15 C14 Mo 73.9(6) . . ? C14 C15 C11 110.8(9) . . ? C14 C15 Mo 71.1(6) . . ? C11 C15 Mo 72.0(5) . . ? C11 C16 C18 111.7(8) . . ? C11 C16 C17 110.9(8) . . ? C18 C16 C17 110.0(10) . . ? C11 C16 C19 107.2(9) . . ? C18 C16 C19 108.2(8) . . ? C17 C16 C19 108.7(10) . . ? C25 C21 C22 104.8(8) . . ? C25 C21 C26 128.6(8) . . ? C22 C21 C26 126.0(8) . . ? C25 C21 Mo 69.1(4) . . ? C22 C21 Mo 69.9(4) . . ? C26 C21 Mo 131.8(6) . . ? C23 C22 C21 109.4(8) . . ? C23 C22 Mo 70.8(5) . . ? C21 C22 Mo 74.7(4) . . ? C24 C23 C22 108.8(9) . . ? C24 C23 Mo 71.4(5) . . ? C22 C23 Mo 73.7(5) . . ? C23 C24 C25 107.0(8) . . ? C23 C24 Mo 73.1(6) . . ? C25 C24 Mo 73.1(5) . . ? C21 C25 C24 110.0(8) . . ? C21 C25 Mo 75.8(5) . . ? C24 C25 Mo 70.4(5) . . ? C21 C26 C29 111.2(8) . . ? C21 C26 C27 107.1(8) . . ? C29 C26 C27 108.7(9) . . ? C21 C26 C28 111.6(7) . . ? C29 C26 C28 109.1(9) . . ? C27 C26 C28 109.1(9) . . ? C6 C1 C2 117.5(10) . . ? C6 C1 Se 120.9(9) . . ? C2 C1 Se 121.6(8) . . ? C3 C2 C1 121.1(11) . . ? C4 C3 C2 120.5(13) . . ? C3 C4 C5 119.7(12) . . ? C4 C5 C6 119.3(11) . . ? C1 C6 C5 121.9(12) . . ? _refine_diff_density_max 1.187 _refine_diff_density_min -1.583 _refine_diff_density_rms 0.125 data_mose60 _database_code_CSD 161675 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H52 Mo2 Se2' _chemical_formula_weight 834.58 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.023(3) _cell_length_b 11.239(3) _cell_length_c 14.012(4) _cell_angle_alpha 92.13(2) _cell_angle_beta 92.25(2) _cell_angle_gamma 94.92(2) _cell_volume 1726.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 5.05 _cell_measurement_theta_max 13.97 _exptl_crystal_description Block _exptl_crystal_colour Dark_red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method ? _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 2.857 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2048 _exptl_absorpt_correction_T_max 0.3487 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 13.18 _diffrn_reflns_number 5263 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.1249 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4446 _reflns_number_observed 2570 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.9507P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4446 _refine_ls_number_parameters 359 _refine_ls_number_restraints 136 _refine_ls_R_factor_all 0.1366 _refine_ls_R_factor_obs 0.0678 _refine_ls_wR_factor_all 0.1785 _refine_ls_wR_factor_obs 0.1441 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.133 _refine_ls_restrained_S_all 1.033 _refine_ls_restrained_S_obs 1.116 _refine_ls_shift/esd_max -2.364 _refine_ls_shift/esd_mean 0.025 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.34574(11) 0.54086(11) 0.57101(8) 0.0456(4) Uani 1 d . . Se1 Se 0.44060(13) 0.36916(13) 0.47701(9) 0.0499(4) Uani 1 d . . C11 C 0.2431(13) 0.7055(14) 0.5202(9) 0.054(4) Uani 1 d . . C12 C 0.1615(13) 0.6103(14) 0.5467(10) 0.058(4) Uani 1 d . . H12A H 0.1014(13) 0.6168(14) 0.5960(10) 0.070 Uiso 1 calc R . C13 C 0.1654(13) 0.5086(14) 0.4818(10) 0.057(4) Uani 1 d . . H13A H 0.1096(13) 0.4357(14) 0.4790(10) 0.068 Uiso 1 calc R . C14 C 0.2505(15) 0.5412(15) 0.4158(9) 0.061(4) Uani 1 d . . H14A H 0.2702(15) 0.4924(15) 0.3600(9) 0.074 Uiso 1 calc R . C15 C 0.2979(14) 0.6611(16) 0.4385(9) 0.065(5) Uani 1 d . . H15A H 0.3582(14) 0.7069(16) 0.4016(9) 0.078 Uiso 1 calc R . C16 C 0.2530(17) 0.8355(14) 0.5557(11) 0.072(5) Uani 1 d . . C17 C 0.2159(20) 0.8487(15) 0.6581(12) 0.110(7) Uani 1 d . . H17A H 0.1362(20) 0.8087(15) 0.6642(12) 0.164 Uiso 1 calc R . H17B H 0.2145(20) 0.9320(15) 0.6756(12) 0.164 Uiso 1 calc R . H17C H 0.2734(20) 0.8139(15) 0.6995(12) 0.164 Uiso 1 calc R . C18 C 0.3774(20) 0.8982(17) 0.5465(17) 0.129(8) Uani 1 d . . H18A H 0.4012(20) 0.8900(17) 0.4816(17) 0.194 Uiso 1 calc R . H18B H 0.4348(20) 0.8634(17) 0.5880(17) 0.194 Uiso 1 calc R . H18C H 0.3759(20) 0.9814(17) 0.5641(17) 0.194 Uiso 1 calc R . C19 C 0.1586(23) 0.8929(16) 0.4933(13) 0.133(9) Uani 1 d . . H19A H 0.0795(23) 0.8518(16) 0.4999(13) 0.199 Uiso 1 calc R . H19B H 0.1801(23) 0.8874(16) 0.4276(13) 0.199 Uiso 1 calc R . H19C H 0.1570(23) 0.9754(16) 0.5132(13) 0.199 Uiso 1 calc R . C21 C 0.2781(14) 0.4233(13) 0.6979(9) 0.054(4) Uani 1 d . . C22 C 0.2707(14) 0.5475(13) 0.7203(8) 0.054(4) Uani 1 d . . H22A H 0.1957(14) 0.5831(13) 0.7366(8) 0.065 Uiso 1 calc R . C23 C 0.3886(15) 0.6086(15) 0.7273(9) 0.064(4) Uani 1 d . . H23A H 0.4099(15) 0.6915(15) 0.7501(9) 0.076 Uiso 1 calc R . C24 C 0.4702(15) 0.5204(17) 0.7101(9) 0.067(5) Uani 1 d . . H24A H 0.5594(15) 0.5332(17) 0.7148(9) 0.081 Uiso 1 calc R . C25 C 0.4034(14) 0.4122(15) 0.6942(10) 0.061(4) Uani 1 d . . H25A H 0.4390(14) 0.3363(15) 0.6825(10) 0.073 Uiso 1 calc R . C26 C 0.1784(15) 0.3227(13) 0.7052(10) 0.062(4) Uani 1 d . . C27 C 0.1867(20) 0.2721(17) 0.8033(11) 0.115(8) Uani 1 d . . H27A H 0.2668(20) 0.2470(17) 0.8151(11) 0.173 Uiso 1 calc R . H27B H 0.1273(20) 0.2048(17) 0.8066(11) 0.173 Uiso 1 calc R . H27C H 0.1711(20) 0.3323(17) 0.8506(11) 0.173 Uiso 1 calc R . C28 C 0.1939(17) 0.2216(14) 0.6299(13) 0.094(6) Uani 1 d . . H28A H 0.1888(17) 0.2524(14) 0.5671(13) 0.140 Uiso 1 calc R . H28B H 0.1306(17) 0.1583(14) 0.6355(13) 0.140 Uiso 1 calc R . H28C H 0.2718(17) 0.1912(14) 0.6405(13) 0.140 Uiso 1 calc R . C29 C 0.0512(15) 0.3610(16) 0.6897(11) 0.084(5) Uani 1 d . . H29A H 0.0433(15) 0.3936(16) 0.6276(11) 0.126 Uiso 1 calc R . H29B H 0.0366(15) 0.4205(16) 0.7378(11) 0.126 Uiso 1 calc R . H29C H -0.0072(15) 0.2931(16) 0.6938(11) 0.126 Uiso 1 calc R . Mo2 Mo 0.34764(12) 0.93862(11) 0.07366(8) 0.0503(4) Uani 0.484(3) d PD 1 Se2 Se 0.4378(3) 1.1179(3) -0.0183(2) 0.0574(11) Uani 0.484(3) d P 1 C31 C 0.2536(21) 0.7539(16) 0.0216(17) 0.063(3) Uiso 0.484(3) d PGD 1 C32 C 0.1626(18) 0.8271(21) 0.0524(21) 0.063(3) Uiso 0.484(3) d PGD 1 H32A H 0.1065(152) 0.8080(118) 0.1033(113) 0.075 Uiso 0.484(3) calc PR 1 C33 C 0.1566(24) 0.9168(34) -0.0037(23) 0.063(3) Uiso 0.484(3) d PGD 1 H33A H 0.0959(24) 0.9755(34) -0.0008(23) 0.075 Uiso 0.484(3) calc PR 1 C34 C 0.2516(28) 0.9114(27) -0.0774(16) 0.063(3) Uiso 0.484(3) d PGD 1 H34A H 0.2630(28) 0.9617(27) -0.1326(16) 0.075 Uiso 0.484(3) calc PR 1 C35 C 0.3017(30) 0.8066(23) -0.0600(16) 0.063(3) Uiso 0.484(3) d PGD 1 H35A H 0.3628(30) 0.7726(23) -0.0993(16) 0.075 Uiso 0.484(3) calc PR 1 C36 C 0.2597(23) 0.6240(23) 0.0474(17) 0.072(4) Uiso 0.484(3) d PD 1 C37 C 0.2205(32) 0.5986(28) 0.1465(17) 0.106(5) Uiso 0.484(3) d PD 1 H37A H 0.1415(32) 0.6261(28) 0.1551(17) 0.159 Uiso 0.484(3) calc PR 1 H37B H 0.2781(32) 0.6392(28) 0.1924(17) 0.159 Uiso 0.484(3) calc PR 1 H37C H 0.2169(32) 0.5141(28) 0.1554(17) 0.159 Uiso 0.484(3) calc PR 1 C38 C 0.3836(24) 0.5793(27) 0.0376(24) 0.106(5) Uiso 0.484(3) d PD 1 H38A H 0.4114(24) 0.5943(27) -0.0252(24) 0.159 Uiso 0.484(3) calc PR 1 H38B H 0.3786(24) 0.4949(27) 0.0474(24) 0.159 Uiso 0.484(3) calc PR 1 H38C H 0.4398(24) 0.6201(27) 0.0844(24) 0.159 Uiso 0.484(3) calc PR 1 C39 C 0.1737(29) 0.5447(23) -0.0208(21) 0.106(5) Uiso 0.484(3) d PD 1 H39A H 0.1953(29) 0.5579(23) -0.0855(21) 0.159 Uiso 0.484(3) calc PR 1 H39B H 0.0914(29) 0.5639(23) -0.0126(21) 0.159 Uiso 0.484(3) calc PR 1 H39C H 0.1801(29) 0.4624(23) -0.0071(21) 0.159 Uiso 0.484(3) calc PR 1 C41 C 0.2857(24) 1.0404(18) 0.2084(15) 0.061(3) Uiso 0.484(3) d PGD 1 C42 C 0.2872(31) 0.9173(20) 0.2275(16) 0.061(3) Uiso 0.484(3) d PGD 1 H42A H 0.2177(47) 0.8648(60) 0.2471(177) 0.074 Uiso 0.484(3) calc PR 1 C43 C 0.4075(33) 0.8884(46) 0.2254(18) 0.061(3) Uiso 0.484(3) d PGD 1 H43A H 0.4376(33) 0.8124(46) 0.2432(18) 0.074 Uiso 0.484(3) calc PR 1 C44 C 0.4732(27) 0.9851(26) 0.2099(16) 0.061(3) Uiso 0.484(3) d PGD 1 H44A H 0.5625(27) 0.9911(26) 0.2100(16) 0.074 Uiso 0.484(3) calc PR 1 C45 C 0.4077(28) 1.0769(24) 0.1996(17) 0.061(3) Uiso 0.484(3) d PGD 1 H45A H 0.4409(28) 1.1596(24) 0.1921(17) 0.074 Uiso 0.484(3) calc PR 1 C46 C 0.1812(24) 1.1182(22) 0.2208(16) 0.072(4) Uiso 0.484(3) d PD 1 C47 C 0.1812(35) 1.2106(27) 0.1473(22) 0.126(6) Uiso 0.484(3) d PD 1 H47A H 0.1747(35) 1.1723(27) 0.0847(22) 0.188 Uiso 0.484(3) calc PR 1 H47B H 0.2557(35) 1.2617(27) 0.1541(22) 0.188 Uiso 0.484(3) calc PR 1 H47C H 0.1133(35) 1.2574(27) 0.1557(22) 0.188 Uiso 0.484(3) calc PR 1 C48 C 0.0603(25) 1.0449(31) 0.2142(26) 0.126(6) Uiso 0.484(3) d PD 1 H48A H 0.0594(25) 0.9850(31) 0.2613(26) 0.188 Uiso 0.484(3) calc PR 1 H48B H 0.0480(25) 1.0069(31) 0.1516(26) 0.188 Uiso 0.484(3) calc PR 1 H48C H -0.0036(25) 1.0959(31) 0.2253(26) 0.188 Uiso 0.484(3) calc PR 1 C49 C 0.1914(35) 1.1792(29) 0.3184(19) 0.126(6) Uiso 0.484(3) d PD 1 H49A H 0.1914(35) 1.1202(29) 0.3662(19) 0.188 Uiso 0.484(3) calc PR 1 H49B H 0.1235(35) 1.2261(29) 0.3265(19) 0.188 Uiso 0.484(3) calc PR 1 H49C H 0.2659(35) 1.2303(29) 0.3249(19) 0.188 Uiso 0.484(3) calc PR 1 Mo2A Mo 0.34764(12) 0.93862(11) 0.07366(8) 0.0503(4) Uani 0.516(3) d PD 2 Se2A Se 0.5337(3) 1.1011(2) 0.0796(2) 0.0522(10) Uani 0.516(3) d P 2 C31A C 0.1973(20) 1.0740(17) 0.1081(16) 0.063(3) Uiso 0.516(3) d PGD 2 C32A C 0.1388(18) 0.9610(19) 0.0770(19) 0.063(3) Uiso 0.516(3) d PGD 2 H32B H 0.0775(162) 0.9120(97) 0.1104(73) 0.075 Uiso 0.516(3) calc PR 2 C33A C 0.1713(24) 0.9460(33) -0.0235(22) 0.063(3) Uiso 0.516(3) d PGD 2 H33B H 0.1365(24) 0.8821(33) -0.0685(22) 0.075 Uiso 0.516(3) calc PR 2 C34A C 0.2373(26) 1.0347(24) -0.0449(18) 0.063(3) Uiso 0.516(3) d PGD 2 H34B H 0.2658(26) 1.0469(24) -0.1094(18) 0.075 Uiso 0.516(3) calc PR 2 C35A C 0.2623(26) 1.1172(21) 0.0299(19) 0.063(3) Uiso 0.516(3) d PGD 2 H35B H 0.3064(26) 1.1963(21) 0.0266(19) 0.075 Uiso 0.516(3) calc PR 2 C36A C 0.1710(21) 1.1499(20) 0.1968(17) 0.072(4) Uiso 0.516(3) d PD 2 C37A C 0.0850(26) 1.2436(23) 0.1727(22) 0.106(5) Uiso 0.516(3) d PD 2 H37D H 0.1196(26) 1.2940(23) 0.1252(22) 0.159 Uiso 0.516(3) calc PR 2 H37E H 0.0726(26) 1.2911(23) 0.2293(22) 0.159 Uiso 0.516(3) calc PR 2 H37F H 0.0083(26) 1.2050(23) 0.1485(22) 0.159 Uiso 0.516(3) calc PR 2 C38A C 0.1134(29) 1.0725(27) 0.2717(19) 0.106(5) Uiso 0.516(3) d PD 2 H38D H 0.1664(29) 1.0122(27) 0.2882(19) 0.159 Uiso 0.516(3) calc PR 2 H38E H 0.0366(29) 1.0350(27) 0.2469(19) 0.159 Uiso 0.516(3) calc PR 2 H38F H 0.1009(29) 1.1212(27) 0.3276(19) 0.159 Uiso 0.516(3) calc PR 2 C39A C 0.2887(25) 1.2152(25) 0.2386(21) 0.106(5) Uiso 0.516(3) d PD 2 H39D H 0.3255(25) 1.2645(25) 0.1912(21) 0.159 Uiso 0.516(3) calc PR 2 H39E H 0.3437(25) 1.1581(25) 0.2580(21) 0.159 Uiso 0.516(3) calc PR 2 H39F H 0.2713(25) 1.2645(25) 0.2929(21) 0.159 Uiso 0.516(3) calc PR 2 C41A C 0.3316(23) 0.7423(15) 0.1120(16) 0.061(3) Uiso 0.516(3) d PGD 2 C42A C 0.2750(25) 0.8103(19) 0.1822(15) 0.061(3) Uiso 0.516(3) d PGD 2 H42B H 0.1907(32) 0.7977(159) 0.2018(93) 0.074 Uiso 0.516(3) calc PR 2 C43A C 0.3724(32) 0.8910(41) 0.2282(18) 0.061(3) Uiso 0.516(3) d PGD 2 H43B H 0.3651(32) 0.9443(41) 0.2843(18) 0.074 Uiso 0.516(3) calc PR 2 C44A C 0.4809(26) 0.8673(24) 0.1853(18) 0.061(3) Uiso 0.516(3) d PGD 2 H44B H 0.5620(26) 0.9054(24) 0.2044(18) 0.074 Uiso 0.516(3) calc PR 2 C45A C 0.4574(25) 0.7822(21) 0.1163(19) 0.061(3) Uiso 0.516(3) d PGD 2 H45B H 0.5190(25) 0.7484(21) 0.0774(19) 0.074 Uiso 0.516(3) calc PR 2 C46A C 0.2674(23) 0.6305(21) 0.0626(17) 0.072(4) Uiso 0.516(3) d PD 2 C47A C 0.1303(21) 0.6380(29) 0.0618(24) 0.126(6) Uiso 0.516(3) d PD 2 H47D H 0.1052(21) 0.6482(29) 0.1262(24) 0.188 Uiso 0.516(3) calc PR 2 H47E H 0.0897(21) 0.5657(29) 0.0331(24) 0.188 Uiso 0.516(3) calc PR 2 H47F H 0.1095(21) 0.7048(29) 0.0257(24) 0.188 Uiso 0.516(3) calc PR 2 C48A C 0.3045(32) 0.6146(29) -0.0383(17) 0.126(6) Uiso 0.516(3) d PD 2 H48D H 0.2879(32) 0.6838(29) -0.0730(17) 0.188 Uiso 0.516(3) calc PR 2 H48E H 0.2593(32) 0.5452(29) -0.0679(17) 0.188 Uiso 0.516(3) calc PR 2 H48F H 0.3901(32) 0.6044(29) -0.0387(17) 0.188 Uiso 0.516(3) calc PR 2 C49A C 0.2934(32) 0.5220(22) 0.1167(23) 0.126(6) Uiso 0.516(3) d PD 2 H49D H 0.2697(32) 0.5320(22) 0.1815(23) 0.188 Uiso 0.516(3) calc PR 2 H49E H 0.3790(32) 0.5119(22) 0.1163(23) 0.188 Uiso 0.516(3) calc PR 2 H49F H 0.2482(32) 0.4527(22) 0.0869(23) 0.188 Uiso 0.516(3) calc PR 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 0.0358(8) 0.0663(9) 0.0342(6) -0.0035(6) -0.0020(6) 0.0061(6) Se1 0.0404(9) 0.0616(10) 0.0458(8) -0.0096(7) -0.0023(7) 0.0012(7) C11 0.030(8) 0.098(12) 0.038(8) 0.009(8) 0.003(7) 0.017(9) C12 0.031(9) 0.082(11) 0.062(9) -0.005(9) 0.001(7) 0.016(8) C13 0.042(9) 0.072(10) 0.057(9) -0.005(8) -0.006(8) 0.014(8) C14 0.066(12) 0.085(12) 0.035(8) 0.001(8) -0.015(8) 0.025(10) C15 0.055(11) 0.107(14) 0.038(8) 0.025(9) 0.012(8) 0.022(10) C16 0.095(14) 0.060(10) 0.063(10) 0.001(8) 0.011(10) 0.021(11) C17 0.156(21) 0.084(13) 0.093(13) -0.023(10) 0.043(14) 0.029(14) C18 0.110(19) 0.079(13) 0.193(24) -0.004(14) 0.019(18) -0.024(14) C19 0.206(27) 0.096(15) 0.102(15) -0.008(12) -0.040(17) 0.070(17) C21 0.055(11) 0.062(10) 0.043(8) -0.001(7) -0.004(7) 0.009(9) C22 0.058(11) 0.065(10) 0.039(8) -0.003(7) 0.000(7) 0.000(9) C23 0.063(12) 0.090(12) 0.035(8) -0.002(8) 0.002(8) -0.014(11) C24 0.039(10) 0.129(15) 0.033(8) 0.008(9) 0.003(7) -0.003(11) C25 0.046(10) 0.084(12) 0.052(9) -0.008(8) -0.008(8) 0.014(10) C26 0.065(12) 0.063(10) 0.058(9) 0.008(8) 0.006(8) 0.002(9) C27 0.135(19) 0.127(16) 0.080(13) 0.055(12) -0.005(13) -0.023(15) C28 0.080(14) 0.074(12) 0.123(15) -0.006(11) 0.011(12) -0.014(11) C29 0.059(12) 0.114(14) 0.074(11) -0.017(10) -0.008(10) -0.004(11) Mo2 0.0474(9) 0.0701(9) 0.0324(6) 0.0035(6) -0.0058(6) 0.0015(7) Se2 0.049(2) 0.070(2) 0.054(2) 0.010(2) -0.007(2) 0.011(2) Mo2A 0.0474(9) 0.0701(9) 0.0324(6) 0.0035(6) -0.0058(6) 0.0015(7) Se2A 0.061(2) 0.062(2) 0.0318(14) 0.0017(13) -0.0040(14) -0.003(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 C12 2.256(13) . ? Mo1 C22 2.281(13) . ? Mo1 C13 2.300(14) . ? Mo1 C23 2.309(13) . ? Mo1 C21 2.361(14) . ? Mo1 C11 2.367(14) . ? Mo1 C24 2.369(14) . ? Mo1 C14 2.378(12) . ? Mo1 C25 2.395(14) . ? Mo1 C15 2.405(13) . ? Mo1 Se1 2.606(2) 2_666 ? Mo1 Se1 2.611(2) . ? Se1 Mo1 2.606(2) 2_666 ? C11 C12 1.41(2) . ? C11 C15 1.41(2) . ? C11 C16 1.52(2) . ? C12 C13 1.44(2) . ? C13 C14 1.38(2) . ? C14 C15 1.42(2) . ? C16 C18 1.50(2) . ? C16 C17 1.51(2) . ? C16 C19 1.53(2) . ? C21 C25 1.40(2) . ? C21 C22 1.43(2) . ? C21 C26 1.52(2) . ? C22 C23 1.42(2) . ? C23 C24 1.42(2) . ? C24 C25 1.37(2) . ? C26 C27 1.51(2) . ? C26 C29 1.51(2) . ? C26 C28 1.55(2) . ? Mo2 C42 2.30(2) . ? Mo2 C32 2.30(2) . ? Mo2 C33 2.32(2) . ? Mo2 C43 2.31(2) . ? Mo2 C41 2.33(2) . ? Mo2 C31 2.32(2) . ? Mo2 C34 2.33(2) . ? Mo2 C35 2.36(2) . ? Mo2 C44 2.33(2) . ? Mo2 C45 2.34(2) . ? Mo2 Se2 2.580(3) . ? Mo2 Se2 2.639(4) 2_675 ? Se2 Mo2 2.639(4) 2_675 ? C31 C32 1.42 . ? C31 C35 1.41(4) . ? C31 C36 1.52(2) . ? C32 C33 1.31(4) . ? C33 C34 1.50(5) . ? C34 C35 1.37(4) . ? C36 C37 1.50(2) . ? C36 C38 1.50(2) . ? C36 C39 1.53(2) . ? C41 C45 1.38(4) . ? C41 C42 1.42 . ? C41 C46 1.52(2) . ? C42 C43 1.39(5) . ? C43 C44 1.28(5) . ? C44 C45 1.32(4) . ? C46 C47 1.49(2) . ? C46 C49 1.50(2) . ? C46 C48 1.50(2) . ? Mo2A C42A 2.26(2) . ? Mo2A C43A 2.26(2) . ? Mo2A C41A 2.28(2) . ? Mo2A C44A 2.32(2) . ? Mo2A C45A 2.30(2) . ? Mo2A C32A 2.34(2) . ? Mo2A C33A 2.34(2) . ? Mo2A C31A 2.39(2) . ? Mo2A C34A 2.37(2) . ? Mo2A C35A 2.38(2) . ? Mo2A Se2A 2.602(3) 2_675 ? Mo2A Se2A 2.623(3) . ? Se2A Mo2A 2.602(3) 2_675 ? C31A C32A 1.42 . ? C31A C35A 1.41(3) . ? C31A C36A 1.53(2) . ? C32A C33A 1.47(4) . ? C33A C34A 1.24(4) . ? C34A C35A 1.38(3) . ? C36A C38A 1.51(2) . ? C36A C37A 1.51(2) . ? C36A C39A 1.52(2) . ? C41A C45A 1.42(4) . ? C41A C42A 1.42 . ? C41A C46A 1.52(2) . ? C42A C43A 1.46(5) . ? C43A C44A 1.40(4) . ? C44A C45A 1.34(4) . ? C46A C48A 1.50(2) . ? C46A C49A 1.50(2) . ? C46A C47A 1.52(2) . ? 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 C12 Mo1 C22 76.6(5) . . ? C12 Mo1 C13 36.8(5) . . ? C22 Mo1 C13 99.4(5) . . ? C12 Mo1 C23 99.7(6) . . ? C22 Mo1 C23 35.9(5) . . ? C13 Mo1 C23 131.9(6) . . ? C12 Mo1 C21 92.6(5) . . ? C22 Mo1 C21 35.8(4) . . ? C13 Mo1 C21 94.7(5) . . ? C23 Mo1 C21 60.0(5) . . ? C12 Mo1 C11 35.3(5) . . ? C22 Mo1 C11 93.7(5) . . ? C13 Mo1 C11 60.1(5) . . ? C23 Mo1 C11 97.4(5) . . ? C21 Mo1 C11 122.2(5) . . ? C12 Mo1 C24 133.0(5) . . ? C22 Mo1 C24 58.0(5) . . ? C13 Mo1 C24 152.7(5) . . ? C23 Mo1 C24 35.2(5) . . ? C21 Mo1 C24 58.1(5) . . ? C11 Mo1 C24 130.2(6) . . ? C12 Mo1 C14 58.3(5) . . ? C22 Mo1 C14 132.3(6) . . ? C13 Mo1 C14 34.3(5) . . ? C23 Mo1 C14 155.5(6) . . ? C21 Mo1 C14 126.1(6) . . ? C11 Mo1 C14 58.6(5) . . ? C24 Mo1 C14 168.6(5) . . ? C12 Mo1 C25 126.6(5) . . ? C22 Mo1 C25 56.9(5) . . ? C13 Mo1 C25 123.0(6) . . ? C23 Mo1 C25 57.4(5) . . ? C21 Mo1 C25 34.2(5) . . ? C11 Mo1 C25 150.4(5) . . ? C24 Mo1 C25 33.5(5) . . ? C14 Mo1 C25 143.0(6) . . ? C12 Mo1 C15 57.1(5) . . ? C22 Mo1 C15 127.9(5) . . ? C13 Mo1 C15 57.7(5) . . ? C23 Mo1 C15 126.3(6) . . ? C21 Mo1 C15 149.0(5) . . ? C11 Mo1 C15 34.4(4) . . ? C24 Mo1 C15 147.3(6) . . ? C14 Mo1 C15 34.6(5) . . ? C25 Mo1 C15 175.2(5) . . ? C12 Mo1 Se1 129.5(4) . 2_666 ? C22 Mo1 Se1 126.3(4) . 2_666 ? C13 Mo1 Se1 130.1(4) . 2_666 ? C23 Mo1 Se1 90.4(4) . 2_666 ? C21 Mo1 Se1 133.6(4) . 2_666 ? C11 Mo1 Se1 94.5(4) . 2_666 ? C24 Mo1 Se1 77.0(4) . 2_666 ? C14 Mo1 Se1 96.1(4) . 2_666 ? C25 Mo1 Se1 100.5(4) . 2_666 ? C15 Mo1 Se1 77.0(4) . 2_666 ? C12 Mo1 Se1 128.5(4) . . ? C22 Mo1 Se1 130.7(4) . . ? C13 Mo1 Se1 91.8(4) . . ? C23 Mo1 Se1 128.1(4) . . ? C21 Mo1 Se1 95.8(4) . . ? C11 Mo1 Se1 132.3(3) . . ? C24 Mo1 Se1 93.0(4) . . ? C14 Mo1 Se1 76.3(4) . . ? C25 Mo1 Se1 76.8(4) . . ? C15 Mo1 Se1 98.6(4) . . ? Se1 Mo1 Se1 74.24(6) 2_666 . ? Mo1 Se1 Mo1 105.76(6) 2_666 . ? C12 C11 C15 104.8(14) . . ? C12 C11 C16 128.7(13) . . ? C15 C11 C16 125.3(15) . . ? C12 C11 Mo1 68.0(8) . . ? C15 C11 Mo1 74.3(8) . . ? C16 C11 Mo1 131.4(10) . . ? C11 C12 C13 110.5(13) . . ? C11 C12 Mo1 76.6(8) . . ? C13 C12 Mo1 73.3(8) . . ? C14 C13 C12 106.5(14) . . ? C14 C13 Mo1 75.9(8) . . ? C12 C13 Mo1 69.9(8) . . ? C13 C14 C15 108.2(14) . . ? C13 C14 Mo1 69.8(8) . . ? C15 C14 Mo1 73.7(8) . . ? C11 C15 C14 110.1(14) . . ? C11 C15 Mo1 71.4(8) . . ? C14 C15 Mo1 71.7(8) . . ? C18 C16 C17 109.3(17) . . ? C18 C16 C11 113.4(15) . . ? C17 C16 C11 111.9(13) . . ? C18 C16 C19 110.5(16) . . ? C17 C16 C19 107.1(15) . . ? C11 C16 C19 104.4(14) . . ? C25 C21 C22 103.9(14) . . ? C25 C21 C26 126.7(14) . . ? C22 C21 C26 127.2(14) . . ? C25 C21 Mo1 74.2(9) . . ? C22 C21 Mo1 69.0(8) . . ? C26 C21 Mo1 133.3(9) . . ? C23 C22 C21 110.4(14) . . ? C23 C22 Mo1 73.1(8) . . ? C21 C22 Mo1 75.2(8) . . ? C24 C23 C22 105.7(14) . . ? C24 C23 Mo1 74.7(8) . . ? C22 C23 Mo1 71.0(8) . . ? C25 C24 C23 108.2(14) . . ? C25 C24 Mo1 74.3(9) . . ? C23 C24 Mo1 70.1(8) . . ? C24 C25 C21 111.7(15) . . ? C24 C25 Mo1 72.2(9) . . ? C21 C25 Mo1 71.6(8) . . ? C27 C26 C29 107.7(15) . . ? C27 C26 C21 109.3(14) . . ? C29 C26 C21 113.7(13) . . ? C27 C26 C28 108.5(14) . . ? C29 C26 C28 107.2(14) . . ? C21 C26 C28 110.3(13) . . ? C42 Mo2 C32 77.3(11) . . ? C42 Mo2 C33 98.3(12) . . ? C32 Mo2 C33 32.8(10) . . ? C42 Mo2 C43 35.3(12) . . ? C32 Mo2 C43 101.2(13) . . ? C33 Mo2 C43 130.1(13) . . ? C42 Mo2 C41 35.8(2) . . ? C32 Mo2 C41 92.5(9) . . ? C33 Mo2 C41 95.4(12) . . ? C43 Mo2 C41 58.8(12) . . ? C42 Mo2 C31 93.2(9) . . ? C32 Mo2 C31 35.8(2) . . ? C33 Mo2 C31 57.5(11) . . ? C43 Mo2 C31 98.0(14) . . ? C41 Mo2 C31 121.6(9) . . ? C42 Mo2 C34 135.1(12) . . ? C32 Mo2 C34 59.5(11) . . ? C33 Mo2 C34 37.7(12) . . ? C43 Mo2 C34 157.0(15) . . ? C41 Mo2 C34 128.9(10) . . ? C31 Mo2 C34 59.1(10) . . ? C42 Mo2 C35 128.2(10) . . ? C32 Mo2 C35 58.0(10) . . ? C33 Mo2 C35 57.6(13) . . ? C43 Mo2 C35 126.7(15) . . ? C41 Mo2 C35 150.1(11) . . ? C31 Mo2 C35 35.0(9) . . ? C34 Mo2 C35 34.0(9) . . ? C42 Mo2 C44 55.5(11) . . ? C32 Mo2 C44 131.3(11) . . ? C33 Mo2 C44 151.1(13) . . ? C43 Mo2 C44 32.1(13) . . ? C41 Mo2 C44 56.6(10) . . ? C31 Mo2 C44 128.2(9) . . ? C34 Mo2 C44 169.2(11) . . ? C35 Mo2 C44 146.3(11) . . ? C42 Mo2 C45 56.5(10) . . ? C32 Mo2 C45 126.8(10) . . ? C33 Mo2 C45 125.3(13) . . ? C43 Mo2 C45 55.4(15) . . ? C41 Mo2 C45 34.5(9) . . ? C31 Mo2 C45 149.3(10) . . ? C34 Mo2 C45 145.3(10) . . ? C35 Mo2 C45 175.1(11) . . ? C44 Mo2 C45 32.8(9) . . ? C42 Mo2 Se2 133.5(6) . . ? C32 Mo2 Se2 130.2(7) . . ? C33 Mo2 Se2 97.7(8) . . ? C43 Mo2 Se2 126.3(12) . . ? C41 Mo2 Se2 99.4(6) . . ? C31 Mo2 Se2 131.8(6) . . ? C34 Mo2 Se2 76.1(8) . . ? C35 Mo2 Se2 97.1(7) . . ? C44 Mo2 Se2 94.2(7) . . ? C45 Mo2 Se2 78.8(7) . . ? C42 Mo2 Se2 122.6(8) . 2_675 ? C32 Mo2 Se2 127.9(6) . 2_675 ? C33 Mo2 Se2 131.4(10) . 2_675 ? C43 Mo2 Se2 87.4(9) . 2_675 ? C41 Mo2 Se2 133.1(7) . 2_675 ? C31 Mo2 Se2 92.3(6) . 2_675 ? C34 Mo2 Se2 95.2(8) . 2_675 ? C35 Mo2 Se2 75.6(8) . 2_675 ? C44 Mo2 Se2 77.3(8) . 2_675 ? C45 Mo2 Se2 100.5(8) . 2_675 ? Se2 Mo2 Se2 73.84(11) . 2_675 ? Mo2 Se2 Mo2 106.16(11) . 2_675 ? C32 C31 C35 106.1(22) . . ? C32 C31 C36 124.2(19) . . ? C35 C31 C36 125.8(19) . . ? C32 C31 Mo2 71.5(10) . . ? C35 C31 Mo2 74.0(11) . . ? C36 C31 Mo2 137.0(15) . . ? C33 C32 C31 109.7(26) . . ? C33 C32 Mo2 74.3(12) . . ? C31 C32 Mo2 72.7(10) . . ? C34 C33 C32 109.6(30) . . ? C34 C33 Mo2 71.4(11) . . ? C32 C33 Mo2 72.9(12) . . ? C35 C34 C33 103.3(26) . . ? C35 C34 Mo2 74.2(11) . . ? C33 C34 Mo2 70.8(11) . . ? C34 C35 C31 111.1(26) . . ? C34 C35 Mo2 71.8(11) . . ? C31 C35 Mo2 71.0(10) . . ? C37 C36 C38 107.4(18) . . ? C37 C36 C31 113.7(18) . . ? C38 C36 C31 114.0(18) . . ? C37 C36 C39 106.4(18) . . ? C38 C36 C39 105.9(18) . . ? C31 C36 C39 108.9(17) . . ? C45 C41 C42 103.1(23) . . ? C45 C41 C46 127.8(20) . . ? C42 C41 C46 127.4(22) . . ? C45 C41 Mo2 73.5(11) . . ? C42 C41 Mo2 70.9(10) . . ? C46 C41 Mo2 130.7(15) . . ? C43 C42 C41 107.9(27) . . ? C43 C42 Mo2 72.8(12) . . ? C41 C42 Mo2 73.3(10) . . ? C44 C43 C42 107.0(34) . . ? C44 C43 Mo2 74.9(13) . . ? C42 C43 Mo2 72.0(12) . . ? C43 C44 C45 112.4(32) . . ? C43 C44 Mo2 72.9(13) . . ? C45 C44 Mo2 74.2(12) . . ? C41 C45 C44 109.6(25) . . ? C41 C45 Mo2 72.1(11) . . ? C44 C45 Mo2 73.0(11) . . ? C47 C46 C49 109.0(18) . . ? C47 C46 C48 108.8(19) . . ? C49 C46 C48 106.5(18) . . ? C47 C46 C41 111.0(18) . . ? C49 C46 C41 110.0(18) . . ? C48 C46 C41 111.4(18) . . ? C42A Mo2A C43A 37.6(13) . . ? C42A Mo2A C41A 36.4(2) . . ? C43A Mo2A C41A 60.6(13) . . ? C42A Mo2A C44A 60.5(10) . . ? C43A Mo2A C44A 35.6(11) . . ? C41A Mo2A C44A 58.8(9) . . ? C42A Mo2A C45A 60.2(10) . . ? C43A Mo2A C45A 58.7(12) . . ? C41A Mo2A C45A 36.0(9) . . ? C44A Mo2A C45A 33.6(9) . . ? C42A Mo2A C32A 74.5(10) . . ? C43A Mo2A C32A 96.5(11) . . ? C41A Mo2A C32A 95.4(8) . . ? C44A Mo2A C32A 131.3(10) . . ? C45A Mo2A C32A 130.9(9) . . ? C42A Mo2A C33A 99.5(11) . . ? C43A Mo2A C33A 131.0(12) . . ? C41A Mo2A C33A 101.0(11) . . ? C44A Mo2A C33A 158.7(11) . . ? C45A Mo2A C33A 131.9(12) . . ? C32A Mo2A C33A 36.7(11) . . ? C42A Mo2A C31A 91.9(8) . . ? C43A Mo2A C31A 93.3(11) . . ? C41A Mo2A C31A 123.9(8) . . ? C44A Mo2A C31A 125.3(9) . . ? C45A Mo2A C31A 150.3(9) . . ? C32A Mo2A C31A 34.9(2) . . ? C33A Mo2A C31A 57.8(11) . . ? C42A Mo2A C34A 128.3(11) . . ? C43A Mo2A C34A 148.9(12) . . ? C41A Mo2A C34A 129.2(9) . . ? C44A Mo2A C34A 170.8(11) . . ? C45A Mo2A C34A 149.3(10) . . ? C32A Mo2A C34A 56.0(10) . . ? C33A Mo2A C34A 30.4(9) . . ? C31A Mo2A C34A 56.1(9) . . ? C42A Mo2A C35A 126.1(9) . . ? C43A Mo2A C35A 121.8(13) . . ? C41A Mo2A C35A 152.4(10) . . ? C44A Mo2A C35A 141.5(10) . . ? C45A Mo2A C35A 171.6(10) . . ? C32A Mo2A C35A 57.3(9) . . ? C33A Mo2A C35A 55.1(11) . . ? C31A Mo2A C35A 34.4(8) . . ? C34A Mo2A C35A 33.7(8) . . ? C42A Mo2A Se2A 130.0(5) . 2_675 ? C43A Mo2A Se2A 133.9(9) . 2_675 ? C41A Mo2A Se2A 93.6(5) . 2_675 ? C44A Mo2A Se2A 98.9(8) . 2_675 ? C45A Mo2A Se2A 77.8(7) . 2_675 ? C32A Mo2A Se2A 125.3(6) . 2_675 ? C33A Mo2A Se2A 88.6(9) . 2_675 ? C31A Mo2A Se2A 131.8(6) . 2_675 ? C34A Mo2A Se2A 77.2(7) . 2_675 ? C35A Mo2A Se2A 99.0(7) . 2_675 ? C42A Mo2A Se2A 132.4(7) . . ? C43A Mo2A Se2A 94.9(11) . . ? C41A Mo2A Se2A 131.9(6) . . ? C44A Mo2A Se2A 77.1(7) . . ? C45A Mo2A Se2A 96.1(7) . . ? C32A Mo2A Se2A 130.0(5) . . ? C33A Mo2A Se2A 124.2(8) . . ? C31A Mo2A Se2A 96.0(5) . . ? C34A Mo2A Se2A 93.8(7) . . ? C35A Mo2A Se2A 75.5(7) . . ? Se2A Mo2A Se2A 74.01(10) 2_675 . ? Mo2A Se2A Mo2A 105.99(10) 2_675 . ? C32A C31A C35A 106.1(20) . . ? C32A C31A C36A 127.4(19) . . ? C35A C31A C36A 124.7(18) . . ? C32A C31A Mo2A 70.4(10) . . ? C35A C31A Mo2A 72.2(10) . . ? C36A C31A Mo2A 133.8(14) . . ? C31A C32A C33A 104.6(21) . . ? C31A C32A Mo2A 74.7(10) . . ? C33A C32A Mo2A 71.6(11) . . ? C34A C33A C32A 108.9(30) . . ? C34A C33A Mo2A 76.1(13) . . ? C32A C33A Mo2A 71.7(11) . . ? C35A C34A C33A 113.3(30) . . ? C35A C34A Mo2A 73.6(11) . . ? C33A C34A Mo2A 73.4(12) . . ? C34A C35A C31A 107.0(24) . . ? C34A C35A Mo2A 72.7(11) . . ? C31A C35A Mo2A 73.4(10) . . ? C38A C36A C37A 107.9(17) . . ? C38A C36A C39A 109.3(17) . . ? C37A C36A C39A 107.3(17) . . ? C38A C36A C31A 110.8(17) . . ? C37A C36A C31A 111.6(17) . . ? C39A C36A C31A 109.9(17) . . ? C45A C41A C42A 107.3(21) . . ? C45A C41A C46A 129.1(18) . . ? C42A C41A C46A 122.1(20) . . ? C45A C41A Mo2A 72.7(10) . . ? C42A C41A Mo2A 70.8(9) . . ? C46A C41A Mo2A 132.7(15) . . ? C43A C42A C41A 105.6(23) . . ? C43A C42A Mo2A 71.3(11) . . ? C41A C42A Mo2A 72.8(9) . . ? C42A C43A C44A 107.3(29) . . ? C42A C43A Mo2A 71.0(11) . . ? C44A C43A Mo2A 74.3(12) . . ? C45A C44A C43A 109.6(28) . . ? C45A C44A Mo2A 72.6(11) . . ? C43A C44A Mo2A 70.1(11) . . ? C44A C45A C41A 110.1(24) . . ? C44A C45A Mo2A 73.8(11) . . ? C41A C45A Mo2A 71.3(10) . . ? C48A C46A C49A 109.3(18) . . ? C48A C46A C41A 111.9(18) . . ? C49A C46A C41A 110.4(18) . . ? C48A C46A C47A 108.6(18) . . ? C49A C46A C47A 106.8(18) . . ? C41A C46A C47A 109.6(18) . . ? _refine_diff_density_max 0.945 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.134 data_mosily10 _database_code_CSD 161676 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H48 Mo Si2' _chemical_formula_weight 512.76 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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' '-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 17.528(2) _cell_length_b 19.8608(15) _cell_length_c 9.0166(11) _cell_angle_alpha 90.00 _cell_angle_beta 119.619(7) _cell_angle_gamma 90.00 _cell_volume 2728.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 8.44 _cell_measurement_theta_max 12.54 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method ? _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2933 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2301 _reflns_number_observed 2105 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+4.1970P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00024(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2301 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_obs 0.0315 _refine_ls_wR_factor_all 0.0816 _refine_ls_wR_factor_obs 0.0789 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.074 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.074 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.0000 0.28783(2) 0.7500 0.03213(13) Uani 1 d S . C11 C 0.0417(2) 0.34838(14) 0.5748(3) 0.0399(6) Uani 1 d . . C12 C -0.0331(2) 0.37822(15) 0.5735(4) 0.0424(7) Uani 1 d . . H12A H -0.0363(2) 0.42490(15) 0.6052(4) 0.051 Uiso 1 calc R . C13 C -0.1050(2) 0.3323(2) 0.5005(4) 0.0458(7) Uani 1 d . . H13A H -0.1659(2) 0.3421(2) 0.4699(4) 0.055 Uiso 1 calc R . C14 C -0.0750(2) 0.2750(2) 0.4534(3) 0.0456(7) Uani 1 d . . H14A H -0.1111(2) 0.2361(2) 0.3912(3) 0.055 Uiso 1 calc R . C15 C 0.0131(2) 0.28477(14) 0.4976(3) 0.0425(7) Uani 1 d . . H15A H 0.0489(2) 0.25261(14) 0.4761(3) 0.051 Uiso 1 calc R . C16 C 0.1259(2) 0.3842(2) 0.6103(4) 0.0472(7) Uani 1 d . . C17 C 0.2064(2) 0.3386(2) 0.7056(5) 0.0635(9) Uani 1 d . . H17A H 0.2581(2) 0.3628(2) 0.7257(5) 0.095 Uiso 1 calc R . H17B H 0.1997(2) 0.2994(2) 0.6380(5) 0.095 Uiso 1 calc R . H17C H 0.2118(2) 0.3252(2) 0.8127(5) 0.095 Uiso 1 calc R . C18 C 0.1168(3) 0.4041(2) 0.4383(5) 0.0695(11) Uani 1 d . . H18A H 0.1691(3) 0.4268(2) 0.4568(5) 0.104 Uiso 1 calc R . H18B H 0.0673(3) 0.4335(2) 0.3792(5) 0.104 Uiso 1 calc R . H18C H 0.1082(3) 0.3644(2) 0.3711(5) 0.104 Uiso 1 calc R . C19 C 0.1408(3) 0.4487(2) 0.7147(5) 0.0683(10) Uani 1 d . . H19A H 0.1943(3) 0.4698(2) 0.7344(5) 0.102 Uiso 1 calc R . H19B H 0.1449(3) 0.4377(2) 0.8220(5) 0.102 Uiso 1 calc R . H19C H 0.0926(3) 0.4790(2) 0.6528(5) 0.102 Uiso 1 calc R . Si Si 0.09688(6) 0.13112(5) 0.65405(11) 0.0501(2) Uani 1 d . . C21 C 0.0919(2) 0.19792(14) 0.7940(4) 0.0409(6) Uani 1 d . . H21A H 0.1497(2) 0.21824(14) 0.8460(4) 0.049 Uiso 1 calc R . H21B H 0.0903(2) 0.17281(14) 0.8848(4) 0.049 Uiso 1 calc R . C22 C 0.1709(3) 0.1521(2) 0.5645(5) 0.0773(12) Uani 1 d . . H22A H 0.1703(3) 0.1156(2) 0.4940(5) 0.116 Uiso 1 calc R . H22B H 0.2297(3) 0.1588(2) 0.6564(5) 0.116 Uiso 1 calc R . H22C H 0.1505(3) 0.1924(2) 0.4975(5) 0.116 Uiso 1 calc R . C23 C 0.1456(3) 0.0538(2) 0.7885(5) 0.0842(13) Uani 1 d . . H23A H 0.1490(3) 0.0184(2) 0.7194(5) 0.126 Uiso 1 calc R . H23B H 0.1093(3) 0.0395(2) 0.8348(5) 0.126 Uiso 1 calc R . H23C H 0.2035(3) 0.0639(2) 0.8800(5) 0.126 Uiso 1 calc R . C24 C -0.0090(3) 0.1028(2) 0.4639(5) 0.0674(10) Uani 1 d . . H24A H 0.0032(3) 0.0684(2) 0.4035(5) 0.101 Uiso 1 calc R . H24B H -0.0366(3) 0.1404(2) 0.3895(5) 0.101 Uiso 1 calc R . H24C H -0.0474(3) 0.0851(2) 0.5019(5) 0.101 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0320(2) 0.0379(2) 0.0277(2) 0.000 0.01566(15) 0.000 C11 0.043(2) 0.045(2) 0.0362(14) 0.0067(12) 0.0232(13) -0.0002(12) C12 0.044(2) 0.043(2) 0.0405(14) 0.0092(12) 0.0213(14) 0.0037(13) C13 0.037(2) 0.059(2) 0.0380(15) 0.0105(13) 0.0158(13) 0.0047(14) C14 0.049(2) 0.055(2) 0.0265(13) 0.0002(12) 0.0139(13) -0.0097(14) C15 0.051(2) 0.050(2) 0.0305(14) 0.0013(12) 0.0233(13) 0.0013(13) C16 0.045(2) 0.053(2) 0.050(2) 0.0065(14) 0.0287(15) -0.0029(14) C17 0.043(2) 0.073(2) 0.075(2) 0.013(2) 0.029(2) 0.000(2) C18 0.067(3) 0.088(3) 0.064(2) 0.016(2) 0.041(2) -0.010(2) C19 0.065(3) 0.061(2) 0.087(3) -0.010(2) 0.043(2) -0.019(2) Si 0.0457(5) 0.0536(5) 0.0497(5) -0.0104(4) 0.0226(4) 0.0056(4) C21 0.037(2) 0.047(2) 0.0388(15) 0.0011(12) 0.0186(13) 0.0047(12) C22 0.071(3) 0.095(3) 0.081(3) -0.023(2) 0.050(2) 0.006(2) C23 0.098(3) 0.059(2) 0.080(3) -0.006(2) 0.031(3) 0.024(2) C24 0.069(2) 0.067(2) 0.063(2) -0.027(2) 0.030(2) -0.003(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 C13 2.266(3) 2_556 ? Mo C13 2.266(3) . ? Mo C12 2.276(3) 2_556 ? Mo C12 2.276(3) . ? Mo C21 2.304(3) 2_556 ? Mo C21 2.304(3) . ? Mo C14 2.339(3) . ? Mo C14 2.339(3) 2_556 ? Mo C11 2.370(3) . ? Mo C11 2.370(3) 2_556 ? Mo C15 2.398(3) . ? Mo C15 2.398(3) 2_556 ? C11 C15 1.409(4) . ? C11 C12 1.433(4) . ? C11 C16 1.522(4) . ? C12 C13 1.427(4) . ? C13 C14 1.405(4) . ? C14 C15 1.405(4) . ? C16 C18 1.530(4) . ? C16 C17 1.532(4) . ? C16 C19 1.534(5) . ? Si C21 1.863(3) . ? Si C23 1.881(4) . ? Si C22 1.883(4) . ? Si C24 1.885(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Mo C13 134.1(2) 2_556 . ? C13 Mo C12 36.61(10) 2_556 2_556 ? C13 Mo C12 100.84(11) . 2_556 ? C13 Mo C12 100.84(11) 2_556 . ? C13 Mo C12 36.61(10) . . ? C12 Mo C12 75.85(15) 2_556 . ? C13 Mo C21 128.95(11) 2_556 2_556 ? C13 Mo C21 88.59(11) . 2_556 ? C12 Mo C21 130.29(10) 2_556 2_556 ? C12 Mo C21 125.19(10) . 2_556 ? C13 Mo C21 88.59(11) 2_556 . ? C13 Mo C21 128.94(11) . . ? C12 Mo C21 125.19(10) 2_556 . ? C12 Mo C21 130.29(10) . . ? C21 Mo C21 78.4(2) 2_556 . ? C13 Mo C14 154.08(11) 2_556 . ? C13 Mo C14 35.49(11) . . ? C12 Mo C14 133.69(11) 2_556 . ? C12 Mo C14 58.78(10) . . ? C21 Mo C14 76.61(10) 2_556 . ? C21 Mo C14 93.57(11) . . ? C13 Mo C14 35.49(11) 2_556 2_556 ? C13 Mo C14 154.08(11) . 2_556 ? C12 Mo C14 58.78(10) 2_556 2_556 ? C12 Mo C14 133.69(11) . 2_556 ? C21 Mo C14 93.57(11) 2_556 2_556 ? C21 Mo C14 76.61(10) . 2_556 ? C14 Mo C14 167.46(15) . 2_556 ? C13 Mo C11 95.58(11) 2_556 . ? C13 Mo C11 60.49(10) . . ? C12 Mo C11 90.57(10) 2_556 . ? C12 Mo C11 35.87(10) . . ? C21 Mo C11 134.27(10) 2_556 . ? C21 Mo C11 95.07(10) . . ? C14 Mo C11 58.50(10) . . ? C14 Mo C11 129.30(11) 2_556 . ? C13 Mo C11 60.49(10) 2_556 2_556 ? C13 Mo C11 95.58(10) . 2_556 ? C12 Mo C11 35.87(10) 2_556 2_556 ? C12 Mo C11 90.57(10) . 2_556 ? C21 Mo C11 95.07(10) 2_556 2_556 ? C21 Mo C11 134.27(10) . 2_556 ? C14 Mo C11 129.30(11) . 2_556 ? C14 Mo C11 58.50(10) 2_556 2_556 ? C11 Mo C11 119.03(14) . 2_556 ? C13 Mo C15 122.69(11) 2_556 . ? C13 Mo C15 58.65(11) . . ? C12 Mo C15 124.94(10) 2_556 . ? C12 Mo C15 57.81(10) . . ? C21 Mo C15 101.75(10) 2_556 . ? C21 Mo C15 75.94(10) . . ? C14 Mo C15 34.47(10) . . ? C14 Mo C15 144.97(10) 2_556 . ? C11 Mo C15 34.38(9) . . ? C11 Mo C15 148.33(10) 2_556 . ? C13 Mo C15 58.65(11) 2_556 2_556 ? C13 Mo C15 122.69(11) . 2_556 ? C12 Mo C15 57.81(10) 2_556 2_556 ? C12 Mo C15 124.94(10) . 2_556 ? C21 Mo C15 75.94(10) 2_556 2_556 ? C21 Mo C15 101.75(10) . 2_556 ? C14 Mo C15 144.97(10) . 2_556 ? C14 Mo C15 34.47(10) 2_556 2_556 ? C11 Mo C15 148.33(10) . 2_556 ? C11 Mo C15 34.38(9) 2_556 2_556 ? C15 Mo C15 177.09(14) . 2_556 ? C15 C11 C12 105.4(3) . . ? C15 C11 C16 126.4(3) . . ? C12 C11 C16 126.6(3) . . ? C15 C11 Mo 73.9(2) . . ? C12 C11 Mo 68.48(15) . . ? C16 C11 Mo 133.1(2) . . ? C13 C12 C11 109.6(3) . . ? C13 C12 Mo 71.3(2) . . ? C11 C12 Mo 75.7(2) . . ? C14 C13 C12 106.2(3) . . ? C14 C13 Mo 75.1(2) . . ? C12 C13 Mo 72.1(2) . . ? C15 C14 C13 109.0(3) . . ? C15 C14 Mo 75.1(2) . . ? C13 C14 Mo 69.5(2) . . ? C14 C15 C11 109.7(3) . . ? C14 C15 Mo 70.4(2) . . ? C11 C15 Mo 71.72(15) . . ? C11 C16 C18 107.6(3) . . ? C11 C16 C17 111.8(3) . . ? C18 C16 C17 109.1(3) . . ? C11 C16 C19 111.9(3) . . ? C18 C16 C19 107.8(3) . . ? C17 C16 C19 108.6(3) . . ? C21 Si C23 107.7(2) . . ? C21 Si C22 114.0(2) . . ? C23 Si C22 105.5(2) . . ? C21 Si C24 118.3(2) . . ? C23 Si C24 105.8(2) . . ? C22 Si C24 104.7(2) . . ? Si C21 Mo 134.30(15) . . ? _refine_diff_density_max 0.281 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.055 data_mosulf _database_code_CSD 161677 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H32 Mo O6 S2' _chemical_formula_weight 528.52 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 8.6263(6) _cell_length_b 17.0614(12) _cell_length_c 15.7394(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.674(6) _cell_angle_gamma 90.00 _cell_volume 2316.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 9.18 _cell_measurement_theta_max 14.99 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method ? _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2499 _exptl_absorpt_correction_T_max 0.2765 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4181 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 22.49 _reflns_number_total 3024 _reflns_number_observed 2596 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0220P)^2^+1.7788P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3024 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_obs 0.0288 _refine_ls_wR_factor_all 0.0699 _refine_ls_wR_factor_obs 0.0655 _refine_ls_goodness_of_fit_all 1.050 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.050 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.06277(3) 0.34082(2) 0.15041(2) 0.03036(13) Uani 1 d . . S1 S 0.41472(11) 0.25834(6) 0.19292(6) 0.0397(3) Uani 1 d . . C1 C 0.4540(5) 0.1863(3) 0.2707(3) 0.0677(14) Uani 1 d . . H1A H 0.4206(5) 0.2047(3) 0.3251(3) 0.102 Uiso 1 calc R . H1B H 0.5634(5) 0.1760(3) 0.2729(3) 0.102 Uiso 1 calc R . H1C H 0.3995(5) 0.1390(3) 0.2564(3) 0.102 Uiso 1 calc R . O11 O 0.2415(3) 0.26396(13) 0.19739(14) 0.0337(6) Uani 1 d . . O12 O 0.4671(3) 0.2274(2) 0.1136(2) 0.0549(8) Uani 1 d . . O13 O 0.4895(3) 0.3296(2) 0.2204(2) 0.0584(8) Uani 1 d . . S2 S 0.27273(11) 0.40532(6) -0.01364(6) 0.0385(3) Uani 1 d . . C2 C 0.4730(4) 0.3943(2) -0.0269(3) 0.0520(11) Uani 1 d . . H2A H 0.5270(4) 0.4187(2) 0.0197(3) 0.078 Uiso 1 calc R . H2B H 0.5031(4) 0.4187(2) -0.0791(3) 0.078 Uiso 1 calc R . H2C H 0.4984(4) 0.3396(2) -0.0286(3) 0.078 Uiso 1 calc R . O21 O 0.2502(3) 0.36122(14) 0.06760(14) 0.0378(6) Uani 1 d . . O22 O 0.1943(3) 0.3683(2) -0.0844(2) 0.0538(7) Uani 1 d . . O23 O 0.2389(3) 0.48799(14) -0.0041(2) 0.0482(7) Uani 1 d . . C11 C 0.0341(4) 0.3889(2) 0.2864(2) 0.0388(9) Uani 1 d . . C12 C 0.1766(5) 0.4197(2) 0.2542(2) 0.0427(10) Uani 1 d . . H12B H 0.2795(5) 0.4115(2) 0.2798(2) 0.051 Uiso 1 calc R . C13 C 0.1433(6) 0.4696(2) 0.1852(3) 0.0582(13) Uani 1 d . . H13B H 0.2191(6) 0.5009(2) 0.1540(3) 0.070 Uiso 1 calc R . C14 C -0.0147(6) 0.4683(2) 0.1700(3) 0.0626(14) Uani 1 d . . H14A H -0.0706(6) 0.5006(2) 0.1283(3) 0.075 Uiso 1 calc R . C15 C -0.0834(5) 0.4211(2) 0.2334(2) 0.0494(11) Uani 1 d . . H15A H -0.1951(5) 0.4156(2) 0.2424(2) 0.059 Uiso 1 calc R . C16 C 0.0133(5) 0.3535(2) 0.3744(2) 0.0412(10) Uani 1 d . . C17 C -0.1347(5) 0.3064(3) 0.3809(3) 0.0620(12) Uani 1 d . . H17A H -0.1429(5) 0.2852(3) 0.4372(3) 0.093 Uiso 1 calc R . H17B H -0.1330(5) 0.2643(3) 0.3405(3) 0.093 Uiso 1 calc R . H17C H -0.2220(5) 0.3397(3) 0.3692(3) 0.093 Uiso 1 calc R . C18 C 0.0038(5) 0.4235(2) 0.4359(2) 0.0586(12) Uani 1 d . . H18A H 0.0971(5) 0.4539(2) 0.4324(2) 0.088 Uiso 1 calc R . H18B H -0.0080(5) 0.4045(2) 0.4929(2) 0.088 Uiso 1 calc R . H18C H -0.0836(5) 0.4556(2) 0.4207(2) 0.088 Uiso 1 calc R . C19 C 0.1515(5) 0.3024(2) 0.4000(2) 0.0537(11) Uani 1 d . . H19A H 0.2453(5) 0.3324(2) 0.3959(2) 0.081 Uiso 1 calc R . H19B H 0.1568(5) 0.2579(2) 0.3628(2) 0.081 Uiso 1 calc R . H19C H 0.1393(5) 0.2848(2) 0.4575(2) 0.081 Uiso 1 calc R . C21 C -0.0468(4) 0.2123(2) 0.1121(2) 0.0369(9) Uani 1 d . . C22 C 0.0011(4) 0.2566(2) 0.0412(2) 0.0369(9) Uani 1 d . . H22B H 0.0742(4) 0.2383(2) -0.0016(2) 0.044 Uiso 1 calc R . C23 C -0.0880(4) 0.3267(2) 0.0347(2) 0.0409(10) Uani 1 d . . H23B H -0.0938(4) 0.3621(2) -0.0142(2) 0.049 Uiso 1 calc R . C24 C -0.1868(4) 0.3263(2) 0.1050(3) 0.0458(10) Uani 1 d . . H24A H -0.2707(4) 0.3638(2) 0.1149(3) 0.055 Uiso 1 calc R . C25 C -0.1571(4) 0.2585(2) 0.1543(2) 0.0415(10) Uani 1 d . . H25A H -0.2129(4) 0.2433(2) 0.2056(2) 0.050 Uiso 1 calc R . C26 C -0.0060(5) 0.1280(2) 0.1342(2) 0.0445(10) Uani 1 d . . C27 C 0.0107(5) 0.1161(2) 0.2304(2) 0.0569(12) Uani 1 d . . H27A H 0.0365(5) 0.0623(2) 0.2420(2) 0.085 Uiso 1 calc R . H27B H -0.0853(5) 0.1289(2) 0.2573(2) 0.085 Uiso 1 calc R . H27C H 0.0915(5) 0.1494(2) 0.2522(2) 0.085 Uiso 1 calc R . C28 C -0.1450(6) 0.0786(3) 0.1016(3) 0.0719(14) Uani 1 d . . H28A H -0.1264(6) 0.0242(3) 0.1137(3) 0.108 Uiso 1 calc R . H28B H -0.1571(6) 0.0857(3) 0.0414(3) 0.108 Uiso 1 calc R . H28C H -0.2377(6) 0.0952(3) 0.1295(3) 0.108 Uiso 1 calc R . C29 C 0.1402(5) 0.1013(2) 0.0893(3) 0.0611(12) Uani 1 d . . H29A H 0.1627(5) 0.0480(2) 0.1045(3) 0.092 Uiso 1 calc R . H29B H 0.2255(5) 0.1342(2) 0.1061(3) 0.092 Uiso 1 calc R . H29C H 0.1246(5) 0.1049(2) 0.0289(3) 0.092 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0294(2) 0.0286(2) 0.0329(2) 0.00001(13) -0.00777(14) 0.00130(14) S1 0.0275(5) 0.0474(6) 0.0442(6) 0.0079(5) -0.0047(4) 0.0022(5) C1 0.046(3) 0.088(4) 0.068(3) 0.035(3) -0.004(2) 0.018(3) O11 0.0264(13) 0.0359(14) 0.0387(14) 0.0090(11) -0.0062(11) 0.0005(11) O12 0.046(2) 0.068(2) 0.051(2) -0.0019(15) 0.0085(14) 0.009(2) O13 0.037(2) 0.062(2) 0.076(2) -0.003(2) -0.0087(15) -0.0096(15) S2 0.0385(6) 0.0384(5) 0.0384(5) 0.0076(4) -0.0071(4) -0.0060(5) C2 0.041(2) 0.056(3) 0.059(3) 0.005(2) 0.002(2) -0.007(2) O21 0.0354(14) 0.0393(14) 0.0385(14) 0.0101(12) -0.0048(11) -0.0048(12) O22 0.061(2) 0.061(2) 0.0396(15) 0.0016(14) -0.0152(14) -0.012(2) O23 0.051(2) 0.0349(15) 0.059(2) 0.0116(13) -0.0038(14) 0.0021(13) C11 0.048(2) 0.030(2) 0.038(2) -0.007(2) -0.005(2) 0.004(2) C12 0.059(3) 0.035(2) 0.035(2) -0.008(2) -0.009(2) -0.010(2) C13 0.098(4) 0.028(2) 0.049(3) -0.008(2) -0.003(3) -0.016(2) C14 0.108(4) 0.032(2) 0.048(3) -0.005(2) -0.021(3) 0.021(3) C15 0.054(3) 0.043(2) 0.051(3) -0.012(2) -0.007(2) 0.020(2) C16 0.047(2) 0.039(2) 0.037(2) -0.005(2) 0.001(2) 0.001(2) C17 0.060(3) 0.073(3) 0.054(3) 0.001(2) 0.005(2) -0.009(3) C18 0.074(3) 0.056(3) 0.046(2) -0.013(2) 0.005(2) 0.001(2) C19 0.061(3) 0.061(3) 0.039(2) 0.007(2) 0.000(2) 0.012(2) C21 0.031(2) 0.039(2) 0.041(2) -0.004(2) -0.005(2) -0.007(2) C22 0.034(2) 0.041(2) 0.035(2) -0.012(2) -0.005(2) -0.005(2) C23 0.036(2) 0.048(2) 0.038(2) 0.002(2) -0.018(2) -0.001(2) C24 0.023(2) 0.055(3) 0.059(3) -0.004(2) -0.017(2) 0.005(2) C25 0.027(2) 0.051(2) 0.046(2) -0.003(2) 0.000(2) -0.008(2) C26 0.043(2) 0.036(2) 0.054(2) -0.007(2) -0.002(2) -0.010(2) C27 0.067(3) 0.046(3) 0.058(3) 0.009(2) 0.003(2) -0.009(2) C28 0.073(3) 0.052(3) 0.090(4) -0.009(3) -0.009(3) -0.024(3) C29 0.072(3) 0.040(2) 0.071(3) -0.009(2) 0.002(3) 0.005(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 O21 2.117(2) . ? Mo O11 2.148(2) . ? Mo C23 2.238(3) . ? Mo C24 2.274(4) . ? Mo C15 2.283(4) . ? Mo C14 2.297(4) . ? Mo C22 2.297(3) . ? Mo C11 2.309(4) . ? Mo C12 2.325(3) . ? Mo C25 2.362(4) . ? Mo C13 2.367(4) . ? Mo C21 2.460(3) . ? S1 O12 1.433(3) . ? S1 O13 1.440(3) . ? S1 O11 1.500(2) . ? S1 C1 1.765(4) . ? S2 O22 1.443(3) . ? S2 O23 1.448(3) . ? S2 O21 1.498(2) . ? S2 C2 1.752(4) . ? C11 C15 1.416(5) . ? C11 C12 1.435(5) . ? C11 C16 1.523(5) . ? C12 C13 1.408(5) . ? C13 C14 1.381(7) . ? C14 C15 1.418(6) . ? C16 C17 1.514(5) . ? C16 C19 1.527(5) . ? C16 C18 1.539(5) . ? C21 C25 1.408(5) . ? C21 C22 1.414(5) . ? C21 C26 1.520(5) . ? C22 C23 1.424(5) . ? C23 C24 1.405(5) . ? C24 C25 1.414(5) . ? C26 C29 1.522(5) . ? C26 C27 1.533(5) . ? C26 C28 1.549(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O21 Mo O11 76.24(9) . . ? O21 Mo C23 87.56(12) . . ? O11 Mo C23 128.46(12) . . ? O21 Mo C24 123.47(12) . . ? O11 Mo C24 135.59(12) . . ? C23 Mo C24 36.27(13) . . ? O21 Mo C15 133.20(13) . . ? O11 Mo C15 124.62(12) . . ? C23 Mo C15 102.15(14) . . ? C24 Mo C15 73.62(15) . . ? O21 Mo C14 98.76(15) . . ? O11 Mo C14 137.77(13) . . ? C23 Mo C14 92.51(15) . . ? C24 Mo C14 82.5(2) . . ? C15 Mo C14 36.07(15) . . ? O21 Mo C22 79.30(11) . . ? O11 Mo C22 92.00(11) . . ? C23 Mo C22 36.57(13) . . ? C24 Mo C22 59.11(14) . . ? C15 Mo C22 132.72(14) . . ? C14 Mo C22 128.84(14) . . ? O21 Mo C11 127.11(12) . . ? O11 Mo C11 88.97(11) . . ? C23 Mo C11 136.48(14) . . ? C24 Mo C11 102.63(14) . . ? C15 Mo C11 35.92(13) . . ? C14 Mo C11 60.31(14) . . ? C22 Mo C11 152.79(13) . . ? O21 Mo C12 91.05(12) . . ? O11 Mo C12 79.39(12) . . ? C23 Mo C12 150.53(14) . . ? C24 Mo C12 132.41(15) . . ? C15 Mo C12 58.82(15) . . ? C14 Mo C12 58.61(15) . . ? C22 Mo C12 168.41(14) . . ? C11 Mo C12 36.07(13) . . ? O21 Mo C25 137.14(11) . . ? O11 Mo C25 101.61(11) . . ? C23 Mo C25 59.86(14) . . ? C24 Mo C25 35.46(13) . . ? C15 Mo C25 83.85(15) . . ? C14 Mo C25 109.0(2) . . ? C22 Mo C25 57.88(13) . . ? C11 Mo C25 95.31(13) . . ? C12 Mo C25 131.20(13) . . ? O21 Mo C13 76.45(13) . . ? O11 Mo C13 106.23(14) . . ? C23 Mo C13 117.03(15) . . ? C24 Mo C13 116.6(2) . . ? C15 Mo C13 58.2(2) . . ? C14 Mo C13 34.4(2) . . ? C22 Mo C13 144.93(14) . . ? C11 Mo C13 59.32(14) . . ? C12 Mo C13 34.90(13) . . ? C25 Mo C13 141.2(2) . . ? O21 Mo C21 106.83(11) . . ? O11 Mo C21 79.18(10) . . ? C23 Mo C21 59.13(13) . . ? C24 Mo C21 57.74(13) . . ? C15 Mo C21 117.51(14) . . ? C14 Mo C21 139.9(2) . . ? C22 Mo C21 34.36(12) . . ? C11 Mo C21 119.93(12) . . ? C12 Mo C21 147.75(12) . . ? C25 Mo C21 33.88(12) . . ? C13 Mo C21 174.3(2) . . ? O12 S1 O13 115.3(2) . . ? O12 S1 O11 112.9(2) . . ? O13 S1 O11 112.0(2) . . ? O12 S1 C1 106.7(2) . . ? O13 S1 C1 107.3(2) . . ? O11 S1 C1 101.3(2) . . ? S1 O11 Mo 137.23(14) . . ? O22 S2 O23 114.4(2) . . ? O22 S2 O21 112.0(2) . . ? O23 S2 O21 111.8(2) . . ? O22 S2 C2 108.4(2) . . ? O23 S2 C2 108.4(2) . . ? O21 S2 C2 100.7(2) . . ? S2 O21 Mo 135.68(15) . . ? C15 C11 C12 105.1(3) . . ? C15 C11 C16 126.8(4) . . ? C12 C11 C16 125.2(3) . . ? C15 C11 Mo 71.1(2) . . ? C12 C11 Mo 72.6(2) . . ? C16 C11 Mo 135.8(2) . . ? C13 C12 C11 109.0(4) . . ? C13 C12 Mo 74.2(2) . . ? C11 C12 Mo 71.3(2) . . ? C14 C13 C12 108.4(4) . . ? C14 C13 Mo 70.0(2) . . ? C12 C13 Mo 70.9(2) . . ? C13 C14 C15 107.9(4) . . ? C13 C14 Mo 75.6(2) . . ? C15 C14 Mo 71.4(2) . . ? C11 C15 C14 109.4(4) . . ? C11 C15 Mo 73.0(2) . . ? C14 C15 Mo 72.5(2) . . ? C17 C16 C11 112.4(3) . . ? C17 C16 C19 109.6(3) . . ? C11 C16 C19 111.5(3) . . ? C17 C16 C18 108.6(3) . . ? C11 C16 C18 105.8(3) . . ? C19 C16 C18 108.9(3) . . ? C25 C21 C22 106.1(3) . . ? C25 C21 C26 125.3(3) . . ? C22 C21 C26 128.1(3) . . ? C25 C21 Mo 69.2(2) . . ? C22 C21 Mo 66.5(2) . . ? C26 C21 Mo 134.5(2) . . ? C21 C22 C23 110.1(3) . . ? C21 C22 Mo 79.1(2) . . ? C23 C22 Mo 69.5(2) . . ? C24 C23 C22 105.7(3) . . ? C24 C23 Mo 73.2(2) . . ? C22 C23 Mo 74.0(2) . . ? C23 C24 C25 109.2(3) . . ? C23 C24 Mo 70.5(2) . . ? C25 C24 Mo 75.7(2) . . ? C21 C25 C24 108.6(3) . . ? C21 C25 Mo 76.9(2) . . ? C24 C25 Mo 68.9(2) . . ? C21 C26 C29 111.6(3) . . ? C21 C26 C27 111.7(3) . . ? C29 C26 C27 110.5(4) . . ? C21 C26 C28 105.3(3) . . ? C29 C26 C28 109.0(3) . . ? C27 C26 C28 108.6(3) . . ? _refine_diff_density_max 0.236 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.055 data_sem50 _database_code_CSD 161678 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Mo Se2' _chemical_formula_weight 496.25 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' 'Se' 'Se' -0.0929 2.2259 '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 10.814(6) _cell_length_b 14.229(8) _cell_length_c 12.368(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.45(4) _cell_angle_gamma 90.00 _cell_volume 1902.5(18) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 4.508 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.1445 _exptl_absorpt_correction_T_max 0.4658 _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 ? _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 2134 _diffrn_reflns_av_R_equivalents 0.1404 _diffrn_reflns_av_sigmaI/netI 0.1484 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 21.04 _reflns_number_total 2011 _reflns_number_gt 1042 _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^)+(0.1724P)^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 0.0000(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2011 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1753 _refine_ls_R_factor_gt 0.0946 _refine_ls_wR_factor_ref 0.2980 _refine_ls_wR_factor_gt 0.2287 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 1.684 _refine_ls_shift/su_mean 0.017 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 0.2694(2) 1.08677(14) 0.20615(18) 0.0555(9) Uani 1 1 d . . . Se1 Se 0.4140(3) 0.9525(2) 0.2749(3) 0.0960(14) Uani 1 1 d . . . Se2 Se 0.2985(3) 0.92393(19) 0.1175(3) 0.0940(13) Uani 1 1 d . . . C11 C 0.310(2) 1.1676(17) 0.051(2) 0.065(7) Uiso 1 1 d . . . C12 C 0.425(2) 1.1218(17) 0.078(2) 0.066(7) Uiso 1 1 d . . . H12A H 0.4631 1.0747 0.0341 0.080 Uiso 1 1 d R . . C13 C 0.462(3) 1.1618(17) 0.182(2) 0.073(7) Uiso 1 1 d . . . H13A H 0.5402 1.1453 0.2151 0.080 Uiso 1 1 d R . . C14 C 0.377(2) 1.2245(18) 0.215(2) 0.073(7) Uiso 1 1 d . . . H14A H 0.3870 1.2595 0.2808 0.080 Uiso 1 1 d R . . C15 C 0.281(3) 1.2329(18) 0.134(2) 0.071(7) Uiso 1 1 d . . . H15A H 0.2194 1.2816 0.1378 0.080 Uiso 1 1 d R . . C16 C 0.248(2) 1.1658(17) -0.066(2) 0.069(7) Uiso 1 1 d . . . C17 C 0.120(3) 1.195(2) -0.065(3) 0.111(11) Uiso 1 1 d . . . H17A H 0.0710 1.1516 -0.0253 0.080 Uiso 1 1 d R . . H17B H 0.1211 1.2549 -0.0288 0.080 Uiso 1 1 d R . . H17C H 0.0854 1.2025 -0.1367 0.080 Uiso 1 1 d R . . C18 C 0.324(3) 1.229(2) -0.136(3) 0.103(10) Uiso 1 1 d . . . H18A H 0.2957 1.2286 -0.2104 0.080 Uiso 1 1 d R . . H18B H 0.3128 1.2900 -0.1058 0.080 Uiso 1 1 d R . . H18C H 0.4106 1.2127 -0.1326 0.080 Uiso 1 1 d R . . C19 C 0.252(4) 1.067(2) -0.112(3) 0.121(12) Uiso 1 1 d . . . H19A H 0.2035 1.0268 -0.0681 0.080 Uiso 1 1 d R . . H19B H 0.2203 1.0650 -0.1857 0.080 Uiso 1 1 d R . . H19C H 0.3364 1.0467 -0.1102 0.080 Uiso 1 1 d R . . C21 C 0.168(2) 1.0908(17) 0.372(2) 0.063(7) Uiso 1 1 d . . . C22 C 0.131(2) 1.1681(18) 0.309(2) 0.064(7) Uiso 1 1 d . . . H22A H 0.1348 1.2331 0.3292 0.080 Uiso 1 1 d R . . C23 C 0.063(3) 1.132(2) 0.221(2) 0.085(8) Uiso 1 1 d . . . H23A H 0.0194 1.1683 0.1674 0.080 Uiso 1 1 d R . . C24 C 0.067(3) 1.0319(19) 0.226(2) 0.075(7) Uiso 1 1 d . . . H24A H 0.0254 0.9871 0.1805 0.080 Uiso 1 1 d R . . C25 C 0.135(3) 1.011(2) 0.317(2) 0.087(8) Uiso 1 1 d . . . H25A H 0.1516 0.9484 0.3432 0.080 Uiso 1 1 d R . . C26 C 0.223(3) 1.0998(18) 0.491(2) 0.076(8) Uiso 1 1 d . . . C27 C 0.336(3) 1.156(2) 0.497(3) 0.115(11) Uiso 1 1 d . . . H27A H 0.4000 1.1280 0.4558 0.080 Uiso 1 1 d R . . H27B H 0.3188 1.2181 0.4708 0.080 Uiso 1 1 d R . . H27C H 0.3624 1.1594 0.5720 0.080 Uiso 1 1 d R . . C28 C 0.124(3) 1.144(2) 0.559(2) 0.100(10) Uiso 1 1 d . . . H28A H 0.1537 1.1536 0.6324 0.080 Uiso 1 1 d R . . H28B H 0.1005 1.2030 0.5279 0.080 Uiso 1 1 d R . . H28C H 0.0543 1.1024 0.5591 0.080 Uiso 1 1 d R . . C29 C 0.252(3) 1.005(2) 0.535(3) 0.113(11) Uiso 1 1 d . . . H29A H 0.3160 0.9732 0.4974 0.080 Uiso 1 1 d R . . H29B H 0.2758 1.0114 0.6102 0.080 Uiso 1 1 d R . . H29C H 0.1765 0.9698 0.5290 0.080 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0538(15) 0.0561(13) 0.0566(15) -0.0015(11) -0.0003(10) -0.0024(11) Se1 0.086(2) 0.096(2) 0.106(3) 0.0355(19) 0.013(2) 0.0287(18) Se2 0.129(3) 0.0577(17) 0.097(2) -0.0093(16) 0.030(2) -0.0035(17) _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 C15 2.26(3) . ? Mo C14 2.28(3) . ? Mo C11 2.29(2) . ? Mo C25 2.29(3) . ? Mo C22 2.30(2) . ? Mo C23 2.33(3) . ? Mo C24 2.34(3) . ? Mo C21 2.35(2) . ? Mo C13 2.36(3) . ? Mo C12 2.39(2) . ? Mo Se2 2.586(4) . ? Mo Se1 2.598(4) . ? Se1 Se2 2.322(6) . ? C11 C15 1.43(3) . ? C11 C12 1.43(3) . ? C11 C16 1.59(4) . ? C12 C13 1.46(3) . ? C13 C14 1.35(3) . ? C14 C15 1.43(4) . ? C16 C17 1.45(4) . ? C16 C18 1.50(4) . ? C16 C19 1.51(4) . ? C21 C25 1.37(4) . ? C21 C22 1.40(3) . ? C21 C26 1.58(4) . ? C22 C23 1.39(4) . ? C23 C24 1.43(4) . ? C24 C25 1.36(4) . ? C26 C27 1.46(4) . ? C26 C29 1.48(4) . ? C26 C28 1.51(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Mo C14 36.6(9) . . ? C15 Mo C11 36.5(8) . . ? C14 Mo C11 59.9(9) . . ? C15 Mo C25 135.1(10) . . ? C14 Mo C25 135.0(10) . . ? C11 Mo C25 151.1(11) . . ? C15 Mo C22 78.2(9) . . ? C14 Mo C22 83.1(9) . . ? C11 Mo C22 110.4(9) . . ? C25 Mo C22 58.4(9) . . ? C15 Mo C23 80.7(10) . . ? C14 Mo C23 104.2(10) . . ? C11 Mo C23 97.5(10) . . ? C25 Mo C23 57.4(11) . . ? C22 Mo C23 34.9(9) . . ? C15 Mo C24 114.1(10) . . ? C14 Mo C24 139.3(9) . . ? C11 Mo C24 117.1(10) . . ? C25 Mo C24 34.1(9) . . ? C22 Mo C24 59.1(9) . . ? C23 Mo C24 35.6(9) . . ? C15 Mo C21 110.5(9) . . ? C14 Mo C21 100.7(9) . . ? C11 Mo C21 145.3(9) . . ? C25 Mo C21 34.2(9) . . ? C22 Mo C21 35.1(8) . . ? C23 Mo C21 57.0(10) . . ? C24 Mo C21 57.2(9) . . ? C15 Mo C13 58.7(10) . . ? C14 Mo C13 33.8(8) . . ? C11 Mo C13 58.7(9) . . ? C25 Mo C13 149.4(11) . . ? C22 Mo C13 115.5(9) . . ? C23 Mo C13 137.0(10) . . ? C24 Mo C13 172.5(9) . . ? C21 Mo C13 122.0(9) . . ? C15 Mo C12 60.2(9) . . ? C14 Mo C12 59.2(9) . . ? C11 Mo C12 35.6(8) . . ? C25 Mo C12 163.9(9) . . ? C22 Mo C12 137.6(9) . . ? C23 Mo C12 133.1(10) . . ? C24 Mo C12 144.4(10) . . ? C21 Mo C12 157.7(9) . . ? C13 Mo C12 35.8(8) . . ? C15 Mo Se2 130.4(6) . . ? C14 Mo Se2 136.3(6) . . ? C11 Mo Se2 93.9(6) . . ? C25 Mo Se2 85.2(7) . . ? C22 Mo Se2 140.6(6) . . ? C23 Mo Se2 114.1(7) . . ? C24 Mo Se2 82.5(7) . . ? C21 Mo Se2 117.2(6) . . ? C13 Mo Se2 103.6(6) . . ? C12 Mo Se2 79.0(6) . . ? C15 Mo Se1 140.0(7) . . ? C14 Mo Se1 108.4(7) . . ? C11 Mo Se1 121.3(6) . . ? C25 Mo Se1 80.9(8) . . ? C22 Mo Se1 125.8(6) . . ? C23 Mo Se1 138.2(7) . . ? C24 Mo Se1 106.0(7) . . ? C21 Mo Se1 91.3(6) . . ? C13 Mo Se1 81.3(7) . . ? C12 Mo Se1 86.8(6) . . ? Se2 Mo Se1 53.22(14) . . ? Se2 Se1 Mo 63.13(13) . . ? Se1 Se2 Mo 63.65(12) . . ? C15 C11 C12 110(2) . . ? C15 C11 C16 125(2) . . ? C12 C11 C16 123(2) . . ? C15 C11 Mo 71.0(14) . . ? C12 C11 Mo 76.3(15) . . ? C16 C11 Mo 132.7(17) . . ? C11 C12 C13 104(2) . . ? C11 C12 Mo 68.1(14) . . ? C13 C12 Mo 71.0(13) . . ? C14 C13 C12 110(3) . . ? C14 C13 Mo 69.6(16) . . ? C12 C13 Mo 73.2(15) . . ? C13 C14 C15 110(3) . . ? C13 C14 Mo 76.6(16) . . ? C15 C14 Mo 71.2(15) . . ? C11 C15 C14 106(2) . . ? C11 C15 Mo 72.5(15) . . ? C14 C15 Mo 72.2(15) . . ? C17 C16 C18 112(3) . . ? C17 C16 C19 108(3) . . ? C18 C16 C19 108(2) . . ? C17 C16 C11 111(2) . . ? C18 C16 C11 107(2) . . ? C19 C16 C11 110(2) . . ? C25 C21 C22 108(2) . . ? C25 C21 C26 128(2) . . ? C22 C21 C26 124(2) . . ? C25 C21 Mo 70.8(15) . . ? C22 C21 Mo 70.6(13) . . ? C26 C21 Mo 130.2(17) . . ? C23 C22 C21 106(2) . . ? C23 C22 Mo 73.8(15) . . ? C21 C22 Mo 74.3(14) . . ? C22 C23 C24 109(3) . . ? C22 C23 Mo 71.3(16) . . ? C24 C23 Mo 72.5(16) . . ? C25 C24 C23 106(3) . . ? C25 C24 Mo 71.1(17) . . ? C23 C24 Mo 71.9(16) . . ? C24 C25 C21 111(3) . . ? C24 C25 Mo 74.8(16) . . ? C21 C25 Mo 75.0(16) . . ? C27 C26 C29 108(3) . . ? C27 C26 C28 110(3) . . ? C29 C26 C28 108(2) . . ? C27 C26 C21 113(2) . . ? C29 C26 C21 110(2) . . ? C28 C26 C21 108(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 21.04 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.905 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.198