# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Dalton Trans.' #TrackingRef '- 10317_0m_final.cif' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Christopher C. Cummins' _publ_contact_author_address ;Room: 6-435 Massachusetts Institute of Technology 77 Massachusetts Ave. Cambridge, MA 02139-4307 ; _publ_contact_author_email ccummins@mit.edu _publ_contact_author_phone ;(617) 253-5332 ; _publ_contact_author_fax ;(617) 253-7670 ; loop_ _publ_author_name _publ_author_address 'Christopher C. Cummins' ;Room: 6-435 Massachusetts Institute of Technology 77 Massachusetts Ave. Cambridge, MA 02139-4307 ; J.J.Curley '' A.F.Cozzolino '' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 805491' #TrackingRef '- 10317_0m_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic tris(3,5-dimethylphenyl(tertbutyl)amido)-(cyano)-molybdenum _chemical_name_common tris(3,5-dimethylphenyl(tertbutyl)amido)-(cyano)-molybdenum _chemical_formula_moiety 'C37 H54 Mo N4' _chemical_formula_sum 'C37 H54 Mo N4' _chemical_properties_physical 'moisture-sensitive, air-sensitive' _exptl_crystal_recrystallization_method THF _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour red _diffrn_ambient_temperature 100(2) _diffrn_ambient_pressure 101.3 _chemical_formula_weight 650.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? 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 30.186(2) _cell_length_b 10.5923(7) _cell_length_c 22.4853(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.4780(10) _cell_angle_gamma 90.00 _cell_volume 7176.3(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9051 _cell_measurement_theta_min 2.196 _cell_measurement_theta_max 31.490 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 0.394 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7978 _exptl_absorpt_correction_T_max 0.8909 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 95861 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 30.03 _reflns_number_total 10489 _reflns_number_gt 9081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 3.0 (Bruker-AXS, 2008)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2008)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WINGX (Farrugia, 1999)' _computing_publication_material 'WINGX (Farrugia, 1999)' _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^)+(0.0286P)^2^+12.3074P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10489 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.008 _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 C4 C 0.09706(5) 0.14193(15) -0.00519(7) 0.0224(3) Uani 1 1 d . . . C11 C 0.17067(5) 0.42666(13) 0.09442(6) 0.0172(3) Uani 1 1 d . . . C12 C 0.15861(5) 0.50524(14) 0.14081(7) 0.0193(3) Uani 1 1 d . . . H12 H 0.1287 0.5325 0.1422 0.023 Uiso 1 1 calc R . . C13 C 0.19024(5) 0.54400(15) 0.18517(7) 0.0221(3) Uani 1 1 d . . . C14 C 0.23366(5) 0.50068(15) 0.18307(7) 0.0227(3) Uani 1 1 d . . . H14 H 0.2551 0.5255 0.2135 0.027 Uiso 1 1 calc R . . C15 C 0.24653(5) 0.42170(15) 0.13752(7) 0.0210(3) Uani 1 1 d . . . C16 C 0.21469(5) 0.38654(14) 0.09297(7) 0.0195(3) Uani 1 1 d . . . H16 H 0.2231 0.3345 0.0611 0.023 Uiso 1 1 calc R . . C17 C 0.13244(5) 0.45798(15) -0.00733(7) 0.0219(3) Uani 1 1 d . . . C21 C 0.05012(5) 0.35064(13) 0.14321(6) 0.0159(3) Uani 1 1 d . . . C22 C 0.06512(5) 0.34782(14) 0.20344(6) 0.0185(3) Uani 1 1 d . . . H22 H 0.0763 0.2713 0.2205 0.022 Uiso 1 1 calc R . . C23 C 0.06384(5) 0.45631(16) 0.23851(7) 0.0218(3) Uani 1 1 d . . . C24 C 0.04793(5) 0.56785(15) 0.21244(7) 0.0233(3) Uani 1 1 d . . . H24 H 0.0473 0.6422 0.2360 0.028 Uiso 1 1 calc R . . C25 C 0.03286(5) 0.57358(14) 0.15265(7) 0.0219(3) Uani 1 1 d . . . C26 C 0.03393(5) 0.46408(14) 0.11840(7) 0.0181(3) Uani 1 1 d . . . H26 H 0.0235 0.4664 0.0777 0.022 Uiso 1 1 calc R . . C27 C 0.01132(5) 0.15886(14) 0.10103(7) 0.0196(3) Uani 1 1 d . . . C31 C 0.14695(5) 0.09642(13) 0.17696(6) 0.0161(3) Uani 1 1 d . . . C32 C 0.16816(5) 0.18679(14) 0.21411(7) 0.0182(3) Uani 1 1 d . . . H32 H 0.1866 0.2486 0.1975 0.022 Uiso 1 1 calc R . . C33 C 0.16246(5) 0.18696(15) 0.27535(7) 0.0203(3) Uani 1 1 d . . . C34 C 0.13509(5) 0.09672(15) 0.29908(7) 0.0205(3) Uani 1 1 d . . . H34 H 0.1307 0.0979 0.3405 0.025 Uiso 1 1 calc R . . C35 C 0.11395(5) 0.00420(14) 0.26310(7) 0.0189(3) Uani 1 1 d . . . C36 C 0.11990(5) 0.00549(14) 0.20209(6) 0.0176(3) Uani 1 1 d . . . H36 H 0.1054 -0.0562 0.1771 0.021 Uiso 1 1 calc R . . C37 C 0.18517(5) 0.00681(14) 0.09097(7) 0.0208(3) Uani 1 1 d . . . C131 C 0.17759(6) 0.63179(18) 0.23429(8) 0.0313(4) Uani 1 1 d . . . H13A H 0.1847 0.5919 0.2730 0.047 Uiso 1 1 calc R . . H13B H 0.1457 0.6495 0.2298 0.047 Uiso 1 1 calc R . . H13C H 0.1942 0.7109 0.2319 0.047 Uiso 1 1 calc R . . C151 C 0.29339(5) 0.37274(18) 0.13658(8) 0.0290(4) Uani 1 1 d . . . H15A H 0.3096 0.4218 0.1080 0.043 Uiso 1 1 calc R . . H15B H 0.2928 0.2837 0.1247 0.043 Uiso 1 1 calc R . . H15C H 0.3082 0.3809 0.1764 0.043 Uiso 1 1 calc R . . C171 C 0.16324(7) 0.4014(2) -0.05249(8) 0.0414(5) Uani 1 1 d . . . H17A H 0.1940 0.4053 -0.0361 0.062 Uiso 1 1 calc R . . H17B H 0.1603 0.4496 -0.0897 0.062 Uiso 1 1 calc R . . H17C H 0.1550 0.3132 -0.0604 0.062 Uiso 1 1 calc R . . C172 C 0.14381(11) 0.5961(2) 0.00347(10) 0.0600(8) Uani 1 1 d . . . H17D H 0.1236 0.6320 0.0315 0.090 Uiso 1 1 calc R . . H17E H 0.1407 0.6423 -0.0343 0.090 Uiso 1 1 calc R . . H17F H 0.1745 0.6031 0.0202 0.090 Uiso 1 1 calc R . . C173 C 0.08465(6) 0.4475(2) -0.03255(8) 0.0325(4) Uani 1 1 d . . . H17G H 0.0772 0.3585 -0.0397 0.049 Uiso 1 1 calc R . . H17H H 0.0812 0.4942 -0.0702 0.049 Uiso 1 1 calc R . . H17I H 0.0647 0.4831 -0.0041 0.049 Uiso 1 1 calc R . . C231 C 0.07826(6) 0.45280(19) 0.30402(7) 0.0313(4) Uani 1 1 d . . . H23A H 0.0992 0.5218 0.3133 0.047 Uiso 1 1 calc R . . H23B H 0.0927 0.3718 0.3136 0.047 Uiso 1 1 calc R . . H23C H 0.0523 0.4625 0.3277 0.047 Uiso 1 1 calc R . . C251 C 0.01607(7) 0.69633(16) 0.12575(9) 0.0345(4) Uani 1 1 d . . . H25A H 0.0314 0.7138 0.0894 0.052 Uiso 1 1 calc R . . H25B H 0.0219 0.7649 0.1544 0.052 Uiso 1 1 calc R . . H25C H -0.0159 0.6899 0.1159 0.052 Uiso 1 1 calc R . . C271 C 0.02330(5) 0.02723(15) 0.08032(8) 0.0250(3) Uani 1 1 d . . . H27A H 0.0344 0.0321 0.0403 0.038 Uiso 1 1 calc R . . H27B H -0.0031 -0.0267 0.0793 0.038 Uiso 1 1 calc R . . H27C H 0.0463 -0.0086 0.1080 0.038 Uiso 1 1 calc R . . C272 C -0.00805(8) 0.1442(2) 0.16253(10) 0.0470(6) Uani 1 1 d . . . H27D H 0.0140 0.1044 0.1902 0.070 Uiso 1 1 calc R . . H27E H -0.0347 0.0915 0.1587 0.070 Uiso 1 1 calc R . . H27F H -0.0158 0.2276 0.1777 0.070 Uiso 1 1 calc R . . C273 C -0.02228(7) 0.21797(18) 0.05672(12) 0.0461(6) Uani 1 1 d . . . H27G H -0.0309 0.3011 0.0713 0.069 Uiso 1 1 calc R . . H27H H -0.0485 0.1636 0.0520 0.069 Uiso 1 1 calc R . . H27I H -0.0091 0.2275 0.0182 0.069 Uiso 1 1 calc R . . C331 C 0.18744(6) 0.28141(16) 0.31526(8) 0.0287(3) Uani 1 1 d . . . H33A H 0.1719 0.2927 0.3519 0.043 Uiso 1 1 calc R . . H33B H 0.1890 0.3625 0.2945 0.043 Uiso 1 1 calc R . . H33C H 0.2175 0.2502 0.3252 0.043 Uiso 1 1 calc R . . C351 C 0.08612(6) -0.09793(16) 0.28917(7) 0.0254(3) Uani 1 1 d . . . H35A H 0.0559 -0.0942 0.2708 0.038 Uiso 1 1 calc R . . H35B H 0.0853 -0.0852 0.3323 0.038 Uiso 1 1 calc R . . H35C H 0.0991 -0.1807 0.2814 0.038 Uiso 1 1 calc R . . C371 C 0.22792(7) 0.0116(2) 0.13124(9) 0.0437(5) Uani 1 1 d . . . H37A H 0.2390 0.0986 0.1335 0.065 Uiso 1 1 calc R . . H37B H 0.2503 -0.0430 0.1148 0.065 Uiso 1 1 calc R . . H37C H 0.2218 -0.0177 0.1713 0.065 Uiso 1 1 calc R . . C372 C 0.19684(6) 0.04459(18) 0.02847(7) 0.0296(4) Uani 1 1 d . . . H37D H 0.1706 0.0356 0.0010 0.044 Uiso 1 1 calc R . . H37E H 0.2206 -0.0101 0.0155 0.044 Uiso 1 1 calc R . . H37F H 0.2068 0.1326 0.0287 0.044 Uiso 1 1 calc R . . C373 C 0.16636(9) -0.12646(19) 0.08934(13) 0.0569(7) Uani 1 1 d . . . H37G H 0.1599 -0.1525 0.1297 0.085 Uiso 1 1 calc R . . H37H H 0.1881 -0.1844 0.0736 0.085 Uiso 1 1 calc R . . H37I H 0.1389 -0.1283 0.0637 0.085 Uiso 1 1 calc R . . N1 N 0.13751(4) 0.38414(11) 0.04981(5) 0.0166(2) Uani 1 1 d . . . N2 N 0.05257(4) 0.23790(11) 0.10749(5) 0.0150(2) Uani 1 1 d . . . N3 N 0.15231(4) 0.09887(11) 0.11362(5) 0.0161(2) Uani 1 1 d . . . N41 N 0.08976(5) 0.09578(16) -0.04963(7) 0.0320(3) Uani 1 1 d . . . Mo1 Mo 0.111877(4) 0.226689(11) 0.077668(5) 0.01308(4) Uani 1 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 C4 0.0163(7) 0.0244(7) 0.0264(8) 0.0032(6) 0.0011(6) -0.0022(5) C11 0.0189(7) 0.0167(6) 0.0160(6) 0.0010(5) -0.0005(5) -0.0046(5) C12 0.0205(7) 0.0187(7) 0.0187(7) -0.0015(5) 0.0011(5) -0.0023(5) C13 0.0272(8) 0.0203(7) 0.0187(7) -0.0040(5) 0.0011(6) -0.0050(6) C14 0.0230(7) 0.0236(7) 0.0209(7) -0.0022(6) -0.0031(6) -0.0080(6) C15 0.0184(7) 0.0223(7) 0.0221(7) -0.0006(5) -0.0003(5) -0.0061(5) C16 0.0194(7) 0.0199(7) 0.0191(7) -0.0025(5) 0.0011(5) -0.0045(5) C17 0.0282(8) 0.0200(7) 0.0173(7) 0.0047(5) -0.0014(6) -0.0037(6) C21 0.0138(6) 0.0174(6) 0.0166(6) -0.0004(5) 0.0016(5) -0.0010(5) C22 0.0167(6) 0.0222(7) 0.0167(7) 0.0005(5) 0.0005(5) 0.0012(5) C23 0.0190(7) 0.0289(8) 0.0175(7) -0.0050(6) 0.0010(5) 0.0003(6) C24 0.0208(7) 0.0226(7) 0.0265(8) -0.0090(6) 0.0024(6) -0.0004(6) C25 0.0192(7) 0.0179(7) 0.0285(8) -0.0004(6) 0.0010(6) 0.0007(5) C26 0.0177(6) 0.0183(7) 0.0181(7) 0.0013(5) -0.0004(5) -0.0009(5) C27 0.0144(6) 0.0192(7) 0.0253(7) -0.0008(5) 0.0013(5) -0.0035(5) C31 0.0161(6) 0.0171(6) 0.0147(6) 0.0001(5) -0.0025(5) 0.0029(5) C32 0.0177(6) 0.0175(6) 0.0187(7) -0.0013(5) -0.0026(5) 0.0014(5) C33 0.0218(7) 0.0195(7) 0.0188(7) -0.0031(5) -0.0055(5) 0.0035(5) C34 0.0239(7) 0.0226(7) 0.0145(6) -0.0011(5) -0.0024(5) 0.0064(6) C35 0.0188(7) 0.0197(7) 0.0180(7) 0.0018(5) -0.0005(5) 0.0035(5) C36 0.0180(6) 0.0173(6) 0.0169(7) 0.0005(5) -0.0030(5) 0.0007(5) C37 0.0219(7) 0.0189(7) 0.0217(7) -0.0009(5) 0.0033(6) 0.0043(5) C131 0.0359(9) 0.0316(9) 0.0263(8) -0.0120(7) 0.0008(7) -0.0024(7) C151 0.0181(7) 0.0358(9) 0.0326(9) -0.0060(7) -0.0023(6) -0.0033(6) C171 0.0310(9) 0.0708(15) 0.0229(9) 0.0147(9) 0.0068(7) 0.0061(9) C172 0.115(2) 0.0258(10) 0.0362(11) 0.0120(8) -0.0234(13) -0.0203(12) C173 0.0275(8) 0.0458(11) 0.0236(8) 0.0134(7) -0.0031(7) 0.0055(7) C231 0.0335(9) 0.0409(10) 0.0191(8) -0.0081(7) -0.0022(7) 0.0032(7) C251 0.0421(10) 0.0189(8) 0.0415(10) 0.0004(7) -0.0056(8) 0.0047(7) C271 0.0204(7) 0.0180(7) 0.0360(9) -0.0024(6) -0.0043(6) -0.0025(5) C272 0.0483(12) 0.0478(12) 0.0479(12) -0.0157(10) 0.0278(10) -0.0273(10) C273 0.0293(9) 0.0244(9) 0.0805(17) 0.0095(9) -0.0312(10) -0.0047(7) C331 0.0336(9) 0.0272(8) 0.0242(8) -0.0088(6) -0.0067(7) -0.0010(7) C351 0.0291(8) 0.0245(8) 0.0231(8) 0.0029(6) 0.0054(6) -0.0016(6) C371 0.0319(10) 0.0705(15) 0.0280(10) -0.0013(9) -0.0030(8) 0.0296(10) C372 0.0302(9) 0.0368(9) 0.0223(8) 0.0004(7) 0.0064(6) 0.0122(7) C373 0.0687(16) 0.0201(9) 0.0871(19) -0.0147(10) 0.0483(14) -0.0060(9) N1 0.0182(6) 0.0174(6) 0.0140(5) 0.0007(4) -0.0013(4) -0.0027(4) N2 0.0141(5) 0.0155(5) 0.0154(5) -0.0007(4) -0.0001(4) -0.0015(4) N3 0.0173(6) 0.0168(6) 0.0141(5) -0.0007(4) -0.0007(4) 0.0016(4) N41 0.0283(7) 0.0405(9) 0.0272(8) -0.0019(6) 0.0019(6) -0.0082(6) Mo1 0.01246(6) 0.01427(6) 0.01227(6) 0.00019(4) -0.00118(4) -0.00083(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C4 N41 1.122(2) . ? C4 Mo1 2.0918(17) . ? C11 C16 1.398(2) . ? C11 C12 1.400(2) . ? C11 N1 1.4454(18) . ? C12 C13 1.400(2) . ? C12 H12 0.9500 . ? C13 C14 1.392(2) . ? C13 C131 1.510(2) . ? C14 C15 1.396(2) . ? C14 H14 0.9500 . ? C15 C16 1.396(2) . ? C15 C151 1.508(2) . ? C16 H16 0.9500 . ? C17 N1 1.5040(19) . ? C17 C172 1.519(3) . ? C17 C173 1.522(2) . ? C17 C171 1.539(3) . ? C21 C26 1.400(2) . ? C21 C22 1.402(2) . ? C21 N2 1.4435(18) . ? C22 C23 1.396(2) . ? C22 H22 0.9500 . ? C23 C24 1.391(2) . ? C23 C231 1.511(2) . ? C24 C25 1.394(2) . ? C24 H24 0.9500 . ? C25 C26 1.394(2) . ? C25 C251 1.509(2) . ? C26 H26 0.9500 . ? C27 N2 1.5003(18) . ? C27 C273 1.514(2) . ? C27 C271 1.521(2) . ? C27 C272 1.541(2) . ? C31 C32 1.3995(19) . ? C31 C36 1.403(2) . ? C31 N3 1.4434(18) . ? C32 C33 1.398(2) . ? C32 H32 0.9500 . ? C33 C34 1.391(2) . ? C33 C331 1.514(2) . ? C34 C35 1.400(2) . ? C34 H34 0.9500 . ? C35 C36 1.395(2) . ? C35 C351 1.510(2) . ? C36 H36 0.9500 . ? C37 N3 1.5020(19) . ? C37 C373 1.521(2) . ? C37 C372 1.523(2) . ? C37 C371 1.532(2) . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C173 H17G 0.9800 . ? C173 H17H 0.9800 . ? C173 H17I 0.9800 . ? C231 H23A 0.9800 . ? C231 H23B 0.9800 . ? C231 H23C 0.9800 . ? C251 H25A 0.9800 . ? C251 H25B 0.9800 . ? C251 H25C 0.9800 . ? C271 H27A 0.9800 . ? C271 H27B 0.9800 . ? C271 H27C 0.9800 . ? C272 H27D 0.9800 . ? C272 H27E 0.9800 . ? C272 H27F 0.9800 . ? C273 H27G 0.9800 . ? C273 H27H 0.9800 . ? C273 H27I 0.9800 . ? C331 H33A 0.9800 . ? C331 H33B 0.9800 . ? C331 H33C 0.9800 . ? C351 H35A 0.9800 . ? C351 H35B 0.9800 . ? C351 H35C 0.9800 . ? C371 H37A 0.9800 . ? C371 H37B 0.9800 . ? C371 H37C 0.9800 . ? C372 H37D 0.9800 . ? C372 H37E 0.9800 . ? C372 H37F 0.9800 . ? C373 H37G 0.9800 . ? C373 H37H 0.9800 . ? C373 H37I 0.9800 . ? N1 Mo1 1.9574(12) . ? N2 Mo1 1.9530(12) . ? N3 Mo1 1.9637(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 N41 C4 Mo1 178.95(15) . . ? C16 C11 C12 119.26(13) . . ? C16 C11 N1 120.56(13) . . ? C12 C11 N1 120.14(13) . . ? C13 C12 C11 120.57(14) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 118.82(14) . . ? C14 C13 C131 120.53(14) . . ? C12 C13 C131 120.66(15) . . ? C13 C14 C15 121.80(14) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C14 C15 C16 118.45(14) . . ? C14 C15 C151 121.29(14) . . ? C16 C15 C151 120.24(14) . . ? C15 C16 C11 121.08(14) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? N1 C17 C172 110.74(13) . . ? N1 C17 C173 109.00(13) . . ? C172 C17 C173 109.24(17) . . ? N1 C17 C171 109.06(13) . . ? C172 C17 C171 109.94(18) . . ? C173 C17 C171 108.83(15) . . ? C26 C21 C22 119.18(13) . . ? C26 C21 N2 121.10(13) . . ? C22 C21 N2 119.70(13) . . ? C23 C22 C21 120.66(14) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 118.80(14) . . ? C24 C23 C231 120.22(15) . . ? C22 C23 C231 120.96(15) . . ? C23 C24 C25 121.82(14) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C26 C25 C24 118.65(14) . . ? C26 C25 C251 120.95(15) . . ? C24 C25 C251 120.40(15) . . ? C25 C26 C21 120.88(14) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? N2 C27 C273 110.60(13) . . ? N2 C27 C271 109.25(12) . . ? C273 C27 C271 109.88(14) . . ? N2 C27 C272 109.09(13) . . ? C273 C27 C272 110.90(18) . . ? C271 C27 C272 107.03(15) . . ? C32 C31 C36 119.04(13) . . ? C32 C31 N3 120.13(13) . . ? C36 C31 N3 120.82(12) . . ? C33 C32 C31 120.63(14) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 119.24(14) . . ? C34 C33 C331 120.85(14) . . ? C32 C33 C331 119.87(15) . . ? C33 C34 C35 121.33(14) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C36 C35 C34 118.70(14) . . ? C36 C35 C351 119.80(14) . . ? C34 C35 C351 121.48(14) . . ? C35 C36 C31 121.04(13) . . ? C35 C36 H36 119.5 . . ? C31 C36 H36 119.5 . . ? N3 C37 C373 110.94(14) . . ? N3 C37 C372 109.68(12) . . ? C373 C37 C372 109.18(16) . . ? N3 C37 C371 109.15(13) . . ? C373 C37 C371 110.18(18) . . ? C372 C37 C371 107.64(14) . . ? C13 C131 H13A 109.5 . . ? C13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C15 C151 H15A 109.5 . . ? C15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C17 C172 H17D 109.5 . . ? C17 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C17 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C17 C173 H17G 109.5 . . ? C17 C173 H17H 109.5 . . ? H17G C173 H17H 109.5 . . ? C17 C173 H17I 109.5 . . ? H17G C173 H17I 109.5 . . ? H17H C173 H17I 109.5 . . ? C23 C231 H23A 109.5 . . ? C23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C25 C251 H25A 109.5 . . ? C25 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? C25 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? C27 C271 H27A 109.5 . . ? C27 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C27 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? C27 C272 H27D 109.5 . . ? C27 C272 H27E 109.5 . . ? H27D C272 H27E 109.5 . . ? C27 C272 H27F 109.5 . . ? H27D C272 H27F 109.5 . . ? H27E C272 H27F 109.5 . . ? C27 C273 H27G 109.5 . . ? C27 C273 H27H 109.5 . . ? H27G C273 H27H 109.5 . . ? C27 C273 H27I 109.5 . . ? H27G C273 H27I 109.5 . . ? H27H C273 H27I 109.5 . . ? C33 C331 H33A 109.5 . . ? C33 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C33 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C35 C351 H35A 109.5 . . ? C35 C351 H35B 109.5 . . ? H35A C351 H35B 109.5 . . ? C35 C351 H35C 109.5 . . ? H35A C351 H35C 109.5 . . ? H35B C351 H35C 109.5 . . ? C37 C371 H37A 109.5 . . ? C37 C371 H37B 109.5 . . ? H37A C371 H37B 109.5 . . ? C37 C371 H37C 109.5 . . ? H37A C371 H37C 109.5 . . ? H37B C371 H37C 109.5 . . ? C37 C372 H37D 109.5 . . ? C37 C372 H37E 109.5 . . ? H37D C372 H37E 109.5 . . ? C37 C372 H37F 109.5 . . ? H37D C372 H37F 109.5 . . ? H37E C372 H37F 109.5 . . ? C37 C373 H37G 109.5 . . ? C37 C373 H37H 109.5 . . ? H37G C373 H37H 109.5 . . ? C37 C373 H37I 109.5 . . ? H37G C373 H37I 109.5 . . ? H37H C373 H37I 109.5 . . ? C11 N1 C17 117.46(11) . . ? C11 N1 Mo1 108.30(9) . . ? C17 N1 Mo1 134.01(9) . . ? C21 N2 C27 116.44(11) . . ? C21 N2 Mo1 108.68(9) . . ? C27 N2 Mo1 134.88(9) . . ? C31 N3 C37 116.02(11) . . ? C31 N3 Mo1 108.34(9) . . ? C37 N3 Mo1 135.63(10) . . ? N2 Mo1 N1 116.51(5) . . ? N2 Mo1 N3 117.41(5) . . ? N1 Mo1 N3 118.12(5) . . ? N2 Mo1 C4 100.43(5) . . ? N1 Mo1 C4 98.51(6) . . ? N3 Mo1 C4 99.48(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.820 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.064 data_09039 _database_code_depnum_ccdc_archive 'CCDC 795137' #TrackingRef 'web_deposit_cif_file_0_JohnCurley_1285768058.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H60 Cl3 F3 Mo N4 O4 S' _chemical_formula_weight 952.27 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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 11.6455(8) _cell_length_b 25.1555(17) _cell_length_c 15.6470(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.9940(10) _cell_angle_gamma 90.00 _cell_volume 4583.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9102 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 30.51 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8279 _exptl_absorpt_correction_T_max 0.8961 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 121389 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 29.57 _reflns_number_total 12850 _reflns_number_gt 10830 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0279P)^2^+4.2663P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12850 _refine_ls_number_parameters 521 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.733806(11) 0.079556(5) 0.298342(8) 0.01083(4) Uani 1 1 d . . . N4 N 0.76513(12) 0.03286(6) 0.37485(8) 0.0142(3) Uani 1 1 d . . . C4 C 0.79301(16) -0.00103(7) 0.44839(11) 0.0197(3) Uani 1 1 d . . . H4A H 0.8754 -0.0107 0.4473 0.024 Uiso 1 1 calc R . . H4B H 0.7794 0.0189 0.5018 0.024 Uiso 1 1 calc R . . O1 O 0.72620(11) -0.04745(5) 0.44771(9) 0.0232(3) Uani 1 1 d . . . C41 C 0.78326(18) -0.09328(8) 0.41504(13) 0.0265(4) Uani 1 1 d . . . H41A H 0.8174 -0.0846 0.3600 0.040 Uiso 1 1 calc R . . H41B H 0.7277 -0.1222 0.4073 0.040 Uiso 1 1 calc R . . H41C H 0.8438 -0.1044 0.4555 0.040 Uiso 1 1 calc R . . N1 N 0.60640(12) 0.12034(5) 0.34221(8) 0.0127(3) Uani 1 1 d . . . C11 C 0.60954(14) 0.17573(6) 0.31635(10) 0.0142(3) Uani 1 1 d . . . C12 C 0.55538(14) 0.19172(7) 0.24025(10) 0.0156(3) Uani 1 1 d . . . H12 H 0.5176 0.1661 0.2051 0.019 Uiso 1 1 calc R . . C13 C 0.55640(15) 0.24504(7) 0.21542(11) 0.0173(3) Uani 1 1 d . . . C131 C 0.49792(17) 0.26223(7) 0.13300(11) 0.0226(4) Uani 1 1 d . . . H13A H 0.5504 0.2572 0.0854 0.034 Uiso 1 1 calc R . . H13B H 0.4768 0.2999 0.1369 0.034 Uiso 1 1 calc R . . H13C H 0.4286 0.2408 0.1232 0.034 Uiso 1 1 calc R . . C14 C 0.61270(16) 0.28207(7) 0.26741(12) 0.0208(4) Uani 1 1 d . . . H14 H 0.6134 0.3184 0.2510 0.025 Uiso 1 1 calc R . . C15 C 0.66827(16) 0.26656(7) 0.34346(11) 0.0198(3) Uani 1 1 d . . . C151 C 0.73146(19) 0.30676(8) 0.39812(14) 0.0293(4) Uani 1 1 d . . . H15A H 0.7584 0.2898 0.4511 0.044 Uiso 1 1 calc R . . H15B H 0.6796 0.3361 0.4118 0.044 Uiso 1 1 calc R . . H15C H 0.7974 0.3205 0.3669 0.044 Uiso 1 1 calc R . . C16 C 0.66607(15) 0.21336(7) 0.36766(11) 0.0171(3) Uani 1 1 d . . . H16 H 0.7032 0.2025 0.4193 0.020 Uiso 1 1 calc R . . C17 C 0.51540(14) 0.10554(7) 0.40611(10) 0.0157(3) Uani 1 1 d . . . C171 C 0.55334(17) 0.12223(8) 0.49621(11) 0.0235(4) Uani 1 1 d . . . H17A H 0.6289 0.1069 0.5096 0.035 Uiso 1 1 calc R . . H17B H 0.4975 0.1094 0.5375 0.035 Uiso 1 1 calc R . . H17C H 0.5580 0.1611 0.4992 0.035 Uiso 1 1 calc R . . C172 C 0.40265(15) 0.13307(8) 0.38063(12) 0.0220(4) Uani 1 1 d . . . H17D H 0.4134 0.1717 0.3821 0.033 Uiso 1 1 calc R . . H17E H 0.3427 0.1230 0.4207 0.033 Uiso 1 1 calc R . . H17F H 0.3797 0.1221 0.3227 0.033 Uiso 1 1 calc R . . C173 C 0.49582(16) 0.04550(7) 0.40431(11) 0.0200(3) Uani 1 1 d . . . H17G H 0.4800 0.0341 0.3454 0.030 Uiso 1 1 calc R . . H17H H 0.4302 0.0366 0.4400 0.030 Uiso 1 1 calc R . . H17I H 0.5646 0.0273 0.4264 0.030 Uiso 1 1 calc R . . N2 N 0.68519(12) 0.04065(5) 0.19681(8) 0.0130(3) Uani 1 1 d . . . C21 C 0.60271(14) 0.06930(6) 0.14394(10) 0.0142(3) Uani 1 1 d . . . C22 C 0.48503(15) 0.06537(7) 0.15892(10) 0.0153(3) Uani 1 1 d . . . H22 H 0.4585 0.0428 0.2031 0.018 Uiso 1 1 calc R . . C23 C 0.40629(15) 0.09426(7) 0.10962(11) 0.0170(3) Uani 1 1 d . . . C231 C 0.27980(16) 0.09218(9) 0.12810(12) 0.0253(4) Uani 1 1 d . . . H23A H 0.2464 0.0599 0.1028 0.038 Uiso 1 1 calc R . . H23B H 0.2418 0.1235 0.1034 0.038 Uiso 1 1 calc R . . H23C H 0.2690 0.0918 0.1901 0.038 Uiso 1 1 calc R . . C24 C 0.44778(15) 0.12605(7) 0.04346(11) 0.0180(3) Uani 1 1 d . . . H24 H 0.3948 0.1460 0.0096 0.022 Uiso 1 1 calc R . . C25 C 0.56382(16) 0.12931(7) 0.02599(11) 0.0183(3) Uani 1 1 d . . . C251 C 0.60550(18) 0.16241(8) -0.04762(12) 0.0266(4) Uani 1 1 d . . . H25A H 0.5413 0.1829 -0.0719 0.040 Uiso 1 1 calc R . . H25B H 0.6367 0.1390 -0.0916 0.040 Uiso 1 1 calc R . . H25C H 0.6656 0.1868 -0.0272 0.040 Uiso 1 1 calc R . . C26 C 0.64200(15) 0.10096(7) 0.07747(10) 0.0154(3) Uani 1 1 d . . . H26 H 0.7220 0.1033 0.0671 0.019 Uiso 1 1 calc R . . C27 C 0.70271(15) -0.01750(7) 0.17500(11) 0.0167(3) Uani 1 1 d . . . C271 C 0.68373(19) -0.02576(8) 0.07881(12) 0.0272(4) Uani 1 1 d . . . H27A H 0.6033 -0.0184 0.0637 0.041 Uiso 1 1 calc R . . H27B H 0.7022 -0.0626 0.0639 0.041 Uiso 1 1 calc R . . H27C H 0.7335 -0.0015 0.0473 0.041 Uiso 1 1 calc R . . C272 C 0.82726(15) -0.03233(7) 0.19684(11) 0.0197(3) Uani 1 1 d . . . H27D H 0.8790 -0.0119 0.1607 0.030 Uiso 1 1 calc R . . H27E H 0.8387 -0.0704 0.1867 0.030 Uiso 1 1 calc R . . H27F H 0.8438 -0.0242 0.2571 0.030 Uiso 1 1 calc R . . C273 C 0.61837(17) -0.05178(7) 0.22478(13) 0.0249(4) Uani 1 1 d . . . H27G H 0.6287 -0.0451 0.2861 0.037 Uiso 1 1 calc R . . H27H H 0.6328 -0.0894 0.2128 0.037 Uiso 1 1 calc R . . H27I H 0.5396 -0.0428 0.2072 0.037 Uiso 1 1 calc R . . N3 N 0.86969(12) 0.12336(5) 0.28397(9) 0.0135(3) Uani 1 1 d . . . C31 C 0.88535(14) 0.14055(7) 0.19631(10) 0.0152(3) Uani 1 1 d . . . C32 C 0.84466(14) 0.19018(7) 0.16982(11) 0.0167(3) Uani 1 1 d . . . H32 H 0.8064 0.2126 0.2091 0.020 Uiso 1 1 calc R . . C33 C 0.86001(15) 0.20696(7) 0.08602(11) 0.0200(3) Uani 1 1 d . . . C331 C 0.82185(19) 0.26203(8) 0.05883(13) 0.0279(4) Uani 1 1 d . . . H33A H 0.8859 0.2870 0.0663 0.042 Uiso 1 1 calc R . . H33B H 0.7575 0.2734 0.0940 0.042 Uiso 1 1 calc R . . H33C H 0.7975 0.2614 -0.0014 0.042 Uiso 1 1 calc R . . C34 C 0.91290(16) 0.17302(8) 0.02847(11) 0.0222(4) Uani 1 1 d . . . H34 H 0.9228 0.1844 -0.0288 0.027 Uiso 1 1 calc R . . C35 C 0.95169(15) 0.12269(8) 0.05305(11) 0.0200(3) Uani 1 1 d . . . C351 C 1.00192(18) 0.08479(9) -0.01157(12) 0.0291(4) Uani 1 1 d . . . H35A H 1.0779 0.0730 0.0085 0.044 Uiso 1 1 calc R . . H35B H 1.0091 0.1030 -0.0666 0.044 Uiso 1 1 calc R . . H35C H 0.9513 0.0539 -0.0184 0.044 Uiso 1 1 calc R . . C36 C 0.93964(14) 0.10698(7) 0.13817(11) 0.0168(3) Uani 1 1 d . . . H36 H 0.9683 0.0735 0.1566 0.020 Uiso 1 1 calc R . . C37 C 0.96629(14) 0.13746(7) 0.34604(11) 0.0167(3) Uani 1 1 d . . . C371 C 1.07491(17) 0.10763(10) 0.32268(14) 0.0317(5) Uani 1 1 d . . . H37A H 1.0598 0.0693 0.3231 0.048 Uiso 1 1 calc R . . H37B H 1.1361 0.1159 0.3644 0.048 Uiso 1 1 calc R . . H37C H 1.0989 0.1184 0.2655 0.048 Uiso 1 1 calc R . . C372 C 0.93165(17) 0.12269(8) 0.43648(11) 0.0241(4) Uani 1 1 d . . . H37D H 0.8530 0.1348 0.4463 0.036 Uiso 1 1 calc R . . H37E H 0.9841 0.1398 0.4778 0.036 Uiso 1 1 calc R . . H37F H 0.9356 0.0840 0.4435 0.036 Uiso 1 1 calc R . . C373 C 0.98687(19) 0.19772(8) 0.34261(13) 0.0277(4) Uani 1 1 d . . . H37G H 1.0119 0.2077 0.2853 0.042 Uiso 1 1 calc R . . H37H H 1.0464 0.2075 0.3847 0.042 Uiso 1 1 calc R . . H37I H 0.9155 0.2164 0.3556 0.042 Uiso 1 1 calc R . . F1 F 0.24557(14) -0.07692(6) 0.20173(9) 0.0519(4) Uani 1 1 d . . . F2 F 0.26618(12) -0.00744(6) 0.28068(10) 0.0469(4) Uani 1 1 d . . . F3 F 0.12000(11) -0.01433(5) 0.19525(8) 0.0322(3) Uani 1 1 d . . . S1 S 0.10853(4) -0.073930(17) 0.33315(3) 0.01896(9) Uani 1 1 d . . . C5 C 0.18936(17) -0.04178(8) 0.24854(13) 0.0264(4) Uani 1 1 d . . . O2 O 0.03216(14) -0.10881(6) 0.28703(10) 0.0342(3) Uani 1 1 d . . . O3 O 0.05416(13) -0.02990(6) 0.37534(9) 0.0297(3) Uani 1 1 d . . . O4 O 0.19768(12) -0.10007(6) 0.38295(9) 0.0289(3) Uani 1 1 d . . . C6 C 0.31592(17) -0.20208(8) 0.30972(12) 0.0248(4) Uani 1 1 d DU . . H6 H 0.2679 -0.1746 0.3383 0.030 Uiso 1 1 calc R . . Cl1 Cl 0.44727(5) -0.17276(2) 0.28053(3) 0.03212(11) Uani 1 1 d DU . . Cl2 Cl 0.24039(5) -0.22598(2) 0.21910(3) 0.03463(12) Uani 1 1 d DU . . Cl3 Cl 0.34283(5) -0.25435(2) 0.38281(3) 0.03466(12) Uani 1 1 d DU . . 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 0.01072(7) 0.01097(6) 0.01080(6) -0.00017(5) 0.00046(4) -0.00017(5) N4 0.0141(7) 0.0150(6) 0.0136(6) 0.0006(5) 0.0009(5) 0.0010(5) C4 0.0207(9) 0.0197(8) 0.0187(8) 0.0058(6) -0.0024(6) 0.0009(7) O1 0.0220(7) 0.0162(6) 0.0317(7) 0.0065(5) 0.0089(5) 0.0010(5) C41 0.0316(11) 0.0180(9) 0.0301(10) 0.0045(7) 0.0064(8) 0.0053(8) N1 0.0137(6) 0.0113(6) 0.0133(6) 0.0000(5) 0.0019(5) -0.0001(5) C11 0.0139(7) 0.0123(7) 0.0164(7) -0.0004(6) 0.0023(6) 0.0015(6) C12 0.0154(8) 0.0155(8) 0.0160(7) -0.0026(6) 0.0007(6) 0.0012(6) C13 0.0172(8) 0.0163(8) 0.0185(8) 0.0000(6) -0.0004(6) 0.0039(6) C131 0.0284(10) 0.0201(9) 0.0193(8) 0.0022(7) -0.0035(7) 0.0039(7) C14 0.0234(9) 0.0132(8) 0.0259(9) 0.0001(7) -0.0005(7) 0.0016(7) C15 0.0209(9) 0.0158(8) 0.0225(8) -0.0051(6) -0.0018(7) 0.0005(7) C151 0.0374(11) 0.0160(9) 0.0342(10) -0.0043(8) -0.0100(9) -0.0037(8) C16 0.0174(8) 0.0163(8) 0.0174(7) -0.0019(6) -0.0021(6) 0.0020(6) C17 0.0136(8) 0.0208(8) 0.0127(7) 0.0002(6) 0.0029(6) 0.0002(6) C171 0.0233(9) 0.0339(10) 0.0134(8) -0.0023(7) 0.0022(6) -0.0024(8) C172 0.0146(8) 0.0289(10) 0.0227(8) 0.0040(7) 0.0039(6) 0.0031(7) C173 0.0194(9) 0.0202(8) 0.0206(8) 0.0045(7) 0.0057(6) -0.0014(7) N2 0.0138(6) 0.0112(6) 0.0141(6) -0.0014(5) 0.0003(5) 0.0009(5) C21 0.0165(8) 0.0138(7) 0.0124(7) -0.0023(5) -0.0020(6) 0.0006(6) C22 0.0180(8) 0.0144(7) 0.0136(7) 0.0001(6) 0.0007(6) -0.0014(6) C23 0.0155(8) 0.0187(8) 0.0168(7) -0.0025(6) -0.0036(6) 0.0000(6) C231 0.0152(8) 0.0380(11) 0.0228(9) 0.0020(8) -0.0019(7) 0.0025(8) C24 0.0208(8) 0.0175(8) 0.0156(7) -0.0013(6) -0.0058(6) 0.0016(6) C25 0.0232(9) 0.0174(8) 0.0142(7) 0.0012(6) -0.0025(6) -0.0010(7) C251 0.0285(10) 0.0320(10) 0.0191(8) 0.0097(7) -0.0019(7) -0.0018(8) C26 0.0151(8) 0.0170(8) 0.0141(7) -0.0010(6) -0.0001(6) -0.0011(6) C27 0.0197(8) 0.0124(7) 0.0178(7) -0.0041(6) -0.0009(6) 0.0013(6) C271 0.0381(11) 0.0212(9) 0.0221(9) -0.0091(7) -0.0074(8) 0.0077(8) C272 0.0195(9) 0.0175(8) 0.0222(8) -0.0031(6) 0.0002(6) 0.0043(7) C273 0.0223(9) 0.0143(8) 0.0382(11) 0.0006(7) 0.0051(8) -0.0019(7) N3 0.0128(6) 0.0130(6) 0.0144(6) -0.0003(5) -0.0003(5) -0.0006(5) C31 0.0132(7) 0.0173(8) 0.0151(7) 0.0012(6) 0.0008(6) -0.0028(6) C32 0.0154(8) 0.0159(8) 0.0188(8) -0.0002(6) 0.0017(6) -0.0027(6) C33 0.0180(8) 0.0204(8) 0.0214(8) 0.0052(7) -0.0001(6) -0.0042(7) C331 0.0317(11) 0.0222(9) 0.0298(10) 0.0115(8) -0.0005(8) -0.0022(8) C34 0.0199(9) 0.0300(10) 0.0170(8) 0.0040(7) 0.0030(6) -0.0067(7) C35 0.0146(8) 0.0273(9) 0.0184(8) -0.0033(7) 0.0040(6) -0.0046(7) C351 0.0269(10) 0.0391(12) 0.0215(9) -0.0081(8) 0.0077(7) -0.0015(9) C36 0.0133(8) 0.0167(8) 0.0204(8) 0.0003(6) 0.0013(6) -0.0009(6) C37 0.0133(8) 0.0192(8) 0.0176(7) -0.0018(6) -0.0017(6) -0.0032(6) C371 0.0181(9) 0.0459(13) 0.0310(10) -0.0098(9) -0.0056(8) 0.0060(9) C372 0.0238(9) 0.0315(10) 0.0169(8) 0.0021(7) -0.0042(7) -0.0072(8) C373 0.0331(11) 0.0216(9) 0.0280(10) 0.0011(7) -0.0078(8) -0.0111(8) F1 0.0591(10) 0.0597(10) 0.0377(8) 0.0073(7) 0.0260(7) 0.0253(8) F2 0.0299(7) 0.0562(9) 0.0543(9) 0.0177(7) -0.0084(6) -0.0224(7) F3 0.0356(7) 0.0330(7) 0.0279(6) 0.0119(5) -0.0045(5) -0.0010(5) S1 0.0175(2) 0.0190(2) 0.0204(2) 0.00211(16) 0.00037(15) 0.00151(16) C5 0.0232(10) 0.0298(10) 0.0261(9) 0.0041(8) 0.0030(7) 0.0004(8) O2 0.0343(8) 0.0232(7) 0.0447(9) 0.0032(6) -0.0095(7) -0.0087(6) O3 0.0297(8) 0.0296(7) 0.0300(7) -0.0013(6) 0.0061(6) 0.0088(6) O4 0.0283(8) 0.0352(8) 0.0232(7) 0.0061(6) -0.0004(5) 0.0110(6) C6 0.0282(10) 0.0267(10) 0.0196(8) 0.0023(7) 0.0031(7) 0.0030(8) Cl1 0.0354(3) 0.0367(3) 0.0243(2) 0.00074(19) 0.00183(19) -0.0079(2) Cl2 0.0277(3) 0.0510(3) 0.0251(2) 0.0010(2) -0.00156(18) -0.0032(2) Cl3 0.0400(3) 0.0331(3) 0.0308(2) 0.0110(2) -0.0027(2) -0.0006(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 N4 1.7119(14) . ? Mo1 N1 1.9391(14) . ? Mo1 N2 1.9420(13) . ? Mo1 N3 1.9446(14) . ? N4 C4 1.464(2) . ? C4 O1 1.403(2) . ? O1 C41 1.430(2) . ? N1 C11 1.452(2) . ? N1 C17 1.516(2) . ? C11 C12 1.397(2) . ? C11 C16 1.399(2) . ? C12 C13 1.397(2) . ? C13 C14 1.393(2) . ? C13 C131 1.511(2) . ? C14 C15 1.400(2) . ? C15 C16 1.391(2) . ? C15 C151 1.508(2) . ? C17 C173 1.528(2) . ? C17 C171 1.529(2) . ? C17 C172 1.531(2) . ? N2 C21 1.449(2) . ? N2 C27 1.517(2) . ? C21 C26 1.393(2) . ? C21 C22 1.398(2) . ? C22 C23 1.393(2) . ? C23 C24 1.401(2) . ? C23 C231 1.507(2) . ? C24 C25 1.386(3) . ? C25 C26 1.400(2) . ? C25 C251 1.508(2) . ? C27 C273 1.530(3) . ? C27 C272 1.530(2) . ? C27 C271 1.532(2) . ? N3 C31 1.453(2) . ? N3 C37 1.515(2) . ? C31 C32 1.396(2) . ? C31 C36 1.400(2) . ? C32 C33 1.392(2) . ? C33 C34 1.392(3) . ? C33 C331 1.514(3) . ? C34 C35 1.396(3) . ? C35 C36 1.399(2) . ? C35 C351 1.515(3) . ? C37 C371 1.521(3) . ? C37 C372 1.524(2) . ? C37 C373 1.536(3) . ? F1 C5 1.328(2) . ? F2 C5 1.336(2) . ? F3 C5 1.342(2) . ? S1 O2 1.4352(15) . ? S1 O3 1.4417(14) . ? S1 O4 1.4454(14) . ? S1 C5 1.826(2) . ? C6 Cl2 1.761(2) . ? C6 Cl1 1.765(2) . ? C6 Cl3 1.7670(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Mo1 N1 105.70(6) . . ? N4 Mo1 N2 106.37(6) . . ? N1 Mo1 N2 110.01(6) . . ? N4 Mo1 N3 107.80(6) . . ? N1 Mo1 N3 111.73(6) . . ? N2 Mo1 N3 114.66(6) . . ? C4 N4 Mo1 172.24(12) . . ? O1 C4 N4 111.31(14) . . ? C4 O1 C41 114.37(15) . . ? C11 N1 C17 116.16(13) . . ? C11 N1 Mo1 112.71(10) . . ? C17 N1 Mo1 130.65(10) . . ? C12 C11 C16 119.71(15) . . ? C12 C11 N1 120.06(14) . . ? C16 C11 N1 120.24(14) . . ? C13 C12 C11 120.52(15) . . ? C14 C13 C12 119.07(16) . . ? C14 C13 C131 120.51(16) . . ? C12 C13 C131 120.42(16) . . ? C13 C14 C15 121.05(16) . . ? C16 C15 C14 119.28(16) . . ? C16 C15 C151 120.12(16) . . ? C14 C15 C151 120.59(16) . . ? C15 C16 C11 120.37(16) . . ? N1 C17 C173 109.67(13) . . ? N1 C17 C171 110.28(14) . . ? C173 C17 C171 109.22(14) . . ? N1 C17 C172 108.87(13) . . ? C173 C17 C172 108.38(15) . . ? C171 C17 C172 110.41(15) . . ? C21 N2 C27 116.22(12) . . ? C21 N2 Mo1 113.41(10) . . ? C27 N2 Mo1 129.18(10) . . ? C26 C21 C22 120.08(15) . . ? C26 C21 N2 119.18(15) . . ? C22 C21 N2 120.75(14) . . ? C23 C22 C21 120.54(15) . . ? C22 C23 C24 118.36(16) . . ? C22 C23 C231 120.80(16) . . ? C24 C23 C231 120.83(16) . . ? C25 C24 C23 121.98(16) . . ? C24 C25 C26 118.87(16) . . ? C24 C25 C251 120.74(16) . . ? C26 C25 C251 120.38(16) . . ? C21 C26 C25 120.12(16) . . ? N2 C27 C273 109.81(14) . . ? N2 C27 C272 108.39(13) . . ? C273 C27 C272 111.29(15) . . ? N2 C27 C271 109.53(14) . . ? C273 C27 C271 109.93(16) . . ? C272 C27 C271 107.85(15) . . ? C31 N3 C37 115.57(13) . . ? C31 N3 Mo1 113.18(10) . . ? C37 N3 Mo1 130.92(11) . . ? C32 C31 C36 120.09(15) . . ? C32 C31 N3 119.93(15) . . ? C36 C31 N3 119.97(15) . . ? C33 C32 C31 120.16(16) . . ? C32 C33 C34 119.26(17) . . ? C32 C33 C331 120.03(17) . . ? C34 C33 C331 120.70(16) . . ? C33 C34 C35 121.51(16) . . ? C34 C35 C36 118.77(16) . . ? C34 C35 C351 120.91(17) . . ? C36 C35 C351 120.28(17) . . ? C35 C36 C31 120.14(16) . . ? N3 C37 C371 109.98(14) . . ? N3 C37 C372 109.42(14) . . ? C371 C37 C372 109.72(16) . . ? N3 C37 C373 108.86(14) . . ? C371 C37 C373 110.34(16) . . ? C372 C37 C373 108.49(15) . . ? O2 S1 O3 115.26(10) . . ? O2 S1 O4 115.22(9) . . ? O3 S1 O4 114.82(9) . . ? O2 S1 C5 103.23(10) . . ? O3 S1 C5 103.17(9) . . ? O4 S1 C5 102.58(9) . . ? F1 C5 F2 107.75(18) . . ? F1 C5 F3 107.28(16) . . ? F2 C5 F3 107.04(17) . . ? F1 C5 S1 111.74(15) . . ? F2 C5 S1 111.32(14) . . ? F3 C5 S1 111.47(14) . . ? Cl2 C6 Cl1 110.93(10) . . ? Cl2 C6 Cl3 110.34(11) . . ? Cl1 C6 Cl3 109.49(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.521 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.072