Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Alice Sullivan' 'Nikolas Kaltsoyannis' 'Majid Motevalli' 'A. Duro Oduwole' 'Bernardetta C. Parkin' 'Ramkrishna Ramnauth' _publ_contact_author_name 'Prof Alice Sullivan' _publ_contact_author_address ; Department of Chemistry Queen Mary, University of London Mile End Road London E14 NS UNITED KINGDOM ; _publ_contact_author_email A.C.SULLIVAN@QMUL.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The structural and electrochemical properties of new bis-imido transition metal salen complexes ; data_2rr50b _database_code_CSD 209224 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H66 Mo N4 O2' _chemical_formula_weight 730.91 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' 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7723(3) _cell_length_b 14.2968(3) _cell_length_c 14.0076(4) _cell_angle_alpha 65.2730(10) _cell_angle_beta 84.6770(10) _cell_angle_gamma 81.9760(10) _cell_volume 1938.90(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8828 _exptl_absorpt_correction_T_max 0.9634 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 29831 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 29.74 _reflns_number_total 9363 _reflns_number_gt 7819 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0665P)^2^+1.3728P] 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 9363 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.002 _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 0.14922(2) 0.240440(15) 0.159076(15) 0.01866(8) Uani 1 1 d . . . N1 N 0.1817(2) 0.14172(16) 0.27592(16) 0.0224(4) Uani 1 1 d . . . N2 N 0.1938(2) 0.18183(16) 0.07708(16) 0.0234(4) Uani 1 1 d . . . N3 N 0.1287(2) 0.39094(16) 0.01539(16) 0.0232(4) Uani 1 1 d . . . N4 N 0.3156(2) 0.31696(17) 0.13533(16) 0.0220(4) Uani 1 1 d . . . O1 O 0.09877(16) 0.34635(13) 0.22999(12) 0.0191(3) Uani 1 1 d . . . O2 O -0.03693(16) 0.25550(13) 0.14746(12) 0.0210(4) Uani 1 1 d . . . C1 C 0.2340(3) 0.0438(2) 0.3506(2) 0.0281(6) Uani 1 1 d . . . C2 C 0.1836(5) 0.0351(3) 0.4517(3) 0.0712(14) Uani 1 1 d . . . H2A H 0.2085 0.0910 0.4663 0.107 Uiso 1 1 calc R . . H2B H 0.2158 -0.0320 0.5056 0.107 Uiso 1 1 calc R . . H2C H 0.0918 0.0402 0.4525 0.107 Uiso 1 1 calc R . . C3 C 0.3721(4) 0.0429(4) 0.3460(4) 0.093(2) Uani 1 1 d . . . H3A H 0.4066 0.0424 0.2790 0.140 Uiso 1 1 calc R . . H3B H 0.4083 -0.0192 0.4042 0.140 Uiso 1 1 calc R . . H3C H 0.3928 0.1048 0.3519 0.140 Uiso 1 1 calc R . . C4 C 0.1952(5) -0.0449(3) 0.3323(3) 0.0717(14) Uani 1 1 d . . . H4A H 0.1037 -0.0369 0.3283 0.108 Uiso 1 1 calc R . . H4B H 0.2221 -0.1106 0.3907 0.108 Uiso 1 1 calc R . . H4C H 0.2345 -0.0446 0.2663 0.108 Uiso 1 1 calc R . . C5 C 0.2265(3) 0.1304(2) 0.0114(2) 0.0304(6) Uani 1 1 d . . . C6 C 0.3578(3) 0.0707(3) 0.0351(3) 0.0459(8) Uani 1 1 d . . . H6A H 0.4196 0.1194 0.0216 0.069 Uiso 1 1 calc R . . H6B H 0.3782 0.0333 -0.0102 0.069 Uiso 1 1 calc R . . H6C H 0.3595 0.0211 0.1090 0.069 Uiso 1 1 calc R . . C7 C 0.1293(3) 0.0548(3) 0.0306(3) 0.0416(8) Uani 1 1 d . . . H7A H 0.1317 0.0033 0.1038 0.062 Uiso 1 1 calc R . . H7B H 0.1487 0.0195 -0.0167 0.062 Uiso 1 1 calc R . . H7C H 0.0454 0.0931 0.0170 0.062 Uiso 1 1 calc R . . C8 C 0.2239(4) 0.2096(3) -0.0958(2) 0.0453(8) Uani 1 1 d . . . H8A H 0.1399 0.2477 -0.1092 0.068 Uiso 1 1 calc R . . H8B H 0.2447 0.1767 -0.1451 0.068 Uiso 1 1 calc R . . H8C H 0.2853 0.2576 -0.1055 0.068 Uiso 1 1 calc R . . C9 C 0.2403(3) 0.4470(2) -0.0160(2) 0.0301(6) Uani 1 1 d . . . H9A H 0.2313 0.5023 0.0100 0.036 Uiso 1 1 calc R . . H9B H 0.2509 0.4794 -0.0936 0.036 Uiso 1 1 calc R . . C10 C 0.3531(3) 0.3696(2) 0.0313(2) 0.0288(6) Uani 1 1 d . . . H10A H 0.3732 0.3218 -0.0040 0.035 Uiso 1 1 calc R . . H10B H 0.4276 0.4054 0.0256 0.035 Uiso 1 1 calc R . . C11 C 0.0421(3) 0.4102(2) -0.04441(19) 0.0263(6) Uani 1 1 d . . . H11A H 0.0826 0.4140 -0.1121 0.032 Uiso 1 1 calc R . . H11B H 0.0045 0.4815 -0.0573 0.032 Uiso 1 1 calc R . . C12 C -0.0631(3) 0.3503(2) -0.02603(19) 0.0237(5) Uani 1 1 d . . . C13 C -0.1309(3) 0.3694(2) -0.10923(19) 0.0256(5) Uani 1 1 d . . . H13 H -0.1099 0.4226 -0.1750 0.031 Uiso 1 1 calc R . . C14 C -0.2300(3) 0.3152(2) -0.10341(19) 0.0248(5) Uani 1 1 d . . . C15 C -0.2648(3) 0.2433(2) -0.00953(19) 0.0254(5) Uani 1 1 d . . . H15 H -0.3349 0.2077 -0.0046 0.030 Uiso 1 1 calc R . . C16 C -0.2029(2) 0.2214(2) 0.07601(18) 0.0229(5) Uani 1 1 d . . . C17 C -0.0979(2) 0.27509(19) 0.06696(18) 0.0207(5) Uani 1 1 d . . . C18 C -0.3012(3) 0.3300(2) -0.19334(19) 0.0281(6) Uani 1 1 d . . . C19 C -0.2387(3) 0.3997(2) -0.2895(2) 0.0350(7) Uani 1 1 d . . . H19A H -0.2388 0.4673 -0.2871 0.052 Uiso 1 1 calc R . . H19B H -0.2836 0.4084 -0.3509 0.052 Uiso 1 1 calc R . . H19C H -0.1520 0.3700 -0.2946 0.052 Uiso 1 1 calc R . . C20 C -0.4347(3) 0.3798(3) -0.1867(2) 0.0508(9) Uani 1 1 d . . . H20A H -0.4793 0.3334 -0.1243 0.076 Uiso 1 1 calc R . . H20B H -0.4786 0.3921 -0.2499 0.076 Uiso 1 1 calc R . . H20C H -0.4320 0.4459 -0.1818 0.076 Uiso 1 1 calc R . . C21 C -0.3049(5) 0.2248(3) -0.1962(3) 0.0624(13) Uani 1 1 d . . . H21A H -0.3476 0.2344 -0.2590 0.094 Uiso 1 1 calc R . . H21B H -0.3505 0.1804 -0.1332 0.094 Uiso 1 1 calc R . . H21C H -0.2191 0.1921 -0.1983 0.094 Uiso 1 1 calc R . . C22 C -0.2478(3) 0.1427(2) 0.17615(19) 0.0286(6) Uani 1 1 d . . . C23 C -0.2917(3) 0.1990(3) 0.2431(2) 0.0416(8) Uani 1 1 d . . . H23A H -0.2234 0.2342 0.2498 0.062 Uiso 1 1 calc R . . H23B H -0.3178 0.1497 0.3129 0.062 Uiso 1 1 calc R . . H23C H -0.3629 0.2503 0.2109 0.062 Uiso 1 1 calc R . . C24 C -0.1417(3) 0.0559(2) 0.2248(2) 0.0396(7) Uani 1 1 d . . . H24A H -0.1141 0.0229 0.1764 0.059 Uiso 1 1 calc R . . H24B H -0.1722 0.0042 0.2915 0.059 Uiso 1 1 calc R . . H24C H -0.0711 0.0851 0.2375 0.059 Uiso 1 1 calc R . . C25 C -0.3585(3) 0.0909(3) 0.1672(2) 0.0409(8) Uani 1 1 d . . . H25A H -0.4293 0.1438 0.1375 0.061 Uiso 1 1 calc R . . H25B H -0.3833 0.0411 0.2372 0.061 Uiso 1 1 calc R . . H25C H -0.3338 0.0548 0.1213 0.061 Uiso 1 1 calc R . . C26 C 0.3598(2) 0.3409(2) 0.19917(19) 0.0235(5) Uani 1 1 d . . . H26A H 0.3715 0.4154 0.1627 0.028 Uiso 1 1 calc R . . H26B H 0.4446 0.3024 0.2145 0.028 Uiso 1 1 calc R . . C27 C 0.3002(2) 0.32679(19) 0.29291(19) 0.0218(5) Uani 1 1 d . . . C28 C 0.3749(3) 0.3198(2) 0.3685(2) 0.0245(5) Uani 1 1 d . . . H28 H 0.4635 0.3169 0.3577 0.029 Uiso 1 1 calc R . . C29 C 0.3218(3) 0.3173(2) 0.45568(19) 0.0249(5) Uani 1 1 d . . . C30 C 0.1896(3) 0.32586(19) 0.46479(19) 0.0245(5) Uani 1 1 d . . . H30 H 0.1529 0.3233 0.5301 0.029 Uiso 1 1 calc R . . C31 C 0.1103(2) 0.33711(19) 0.39210(18) 0.0217(5) Uani 1 1 d . . . C32 C 0.1669(2) 0.33575(18) 0.30201(18) 0.0197(5) Uani 1 1 d . . . C33 C 0.3982(3) 0.3050(2) 0.5424(2) 0.0321(6) Uani 1 1 d . . . C34 C 0.5398(3) 0.2986(3) 0.5174(2) 0.0380(7) Uani 1 1 d . . . H34A H 0.5595 0.3620 0.4570 0.057 Uiso 1 1 calc R . . H34B H 0.5662 0.2386 0.5006 0.057 Uiso 1 1 calc R . . H34C H 0.5843 0.2912 0.5785 0.057 Uiso 1 1 calc R . . C35 C 0.3592(4) 0.3976(3) 0.5692(3) 0.0514(9) Uani 1 1 d . . . H35A H 0.3779 0.4611 0.5085 0.077 Uiso 1 1 calc R . . H35B H 0.4056 0.3899 0.6295 0.077 Uiso 1 1 calc R . . H35C H 0.2690 0.4016 0.5868 0.077 Uiso 1 1 calc R . . C36 C 0.3726(4) 0.2038(3) 0.6305(2) 0.0493(9) Uani 1 1 d . . . H36A H 0.2837 0.2070 0.6527 0.074 Uiso 1 1 calc R . . H36B H 0.4242 0.1901 0.6900 0.074 Uiso 1 1 calc R . . H36C H 0.3932 0.1480 0.6065 0.074 Uiso 1 1 calc R . . C37 C -0.0327(3) 0.3461(2) 0.40894(19) 0.0252(5) Uani 1 1 d . . . C38 C -0.0731(3) 0.3476(3) 0.5091(2) 0.0373(7) Uani 1 1 d . . . H38A H -0.0395 0.4047 0.5159 0.056 Uiso 1 1 calc R . . H38B H -0.0422 0.2818 0.5655 0.056 Uiso 1 1 calc R . . H38C H -0.1649 0.3574 0.5140 0.056 Uiso 1 1 calc R . . C39 C -0.0830(3) 0.2525(3) 0.4053(2) 0.0367(7) Uani 1 1 d . . . H39A H -0.0504 0.1891 0.4639 0.055 Uiso 1 1 calc R . . H39B H -0.0559 0.2478 0.3386 0.055 Uiso 1 1 calc R . . H39C H -0.1749 0.2609 0.4112 0.055 Uiso 1 1 calc R . . C40 C -0.0934(3) 0.4465(3) 0.3302(2) 0.0416(8) Uani 1 1 d . . . H40A H -0.1836 0.4531 0.3473 0.062 Uiso 1 1 calc R . . H40B H -0.0801 0.4475 0.2597 0.062 Uiso 1 1 calc R . . H40C H -0.0562 0.5043 0.3323 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02466(13) 0.01690(12) 0.01407(11) -0.00539(8) -0.00356(8) -0.00250(8) N1 0.0290(11) 0.0183(10) 0.0165(9) -0.0028(8) -0.0061(8) -0.0022(9) N2 0.0279(11) 0.0251(11) 0.0193(10) -0.0104(9) -0.0014(9) -0.0049(9) N3 0.0304(12) 0.0228(11) 0.0173(10) -0.0080(9) -0.0012(9) -0.0069(9) N4 0.0234(11) 0.0248(11) 0.0186(10) -0.0091(9) 0.0005(8) -0.0053(9) O1 0.0245(9) 0.0209(8) 0.0129(7) -0.0072(7) -0.0049(6) -0.0020(7) O2 0.0253(9) 0.0243(9) 0.0109(7) -0.0042(7) -0.0052(7) -0.0023(7) C1 0.0347(15) 0.0206(13) 0.0230(12) -0.0031(10) -0.0077(11) 0.0007(11) C2 0.115(4) 0.047(2) 0.0245(16) 0.0025(16) 0.003(2) 0.018(2) C3 0.038(2) 0.054(3) 0.118(4) 0.035(3) -0.022(2) 0.0004(19) C4 0.131(4) 0.0255(18) 0.056(2) -0.0098(17) -0.042(3) 0.004(2) C5 0.0311(15) 0.0405(16) 0.0297(14) -0.0235(13) -0.0017(11) -0.0063(12) C6 0.0332(17) 0.064(2) 0.062(2) -0.049(2) -0.0057(15) 0.0028(15) C7 0.0405(18) 0.052(2) 0.0521(19) -0.0389(17) -0.0016(15) -0.0122(15) C8 0.054(2) 0.065(2) 0.0274(15) -0.0272(16) 0.0036(14) -0.0142(17) C9 0.0404(16) 0.0296(14) 0.0184(12) -0.0044(11) -0.0010(11) -0.0160(12) C10 0.0312(14) 0.0385(16) 0.0200(12) -0.0135(11) 0.0060(11) -0.0148(12) C11 0.0393(15) 0.0220(13) 0.0149(11) -0.0040(10) -0.0031(11) -0.0055(11) C12 0.0320(14) 0.0218(12) 0.0151(11) -0.0045(10) -0.0050(10) -0.0034(10) C13 0.0351(15) 0.0232(13) 0.0153(11) -0.0037(10) -0.0056(10) -0.0041(11) C14 0.0339(14) 0.0253(13) 0.0168(11) -0.0096(10) -0.0070(10) -0.0011(11) C15 0.0289(14) 0.0288(14) 0.0193(12) -0.0089(11) -0.0045(10) -0.0065(11) C16 0.0282(13) 0.0258(13) 0.0143(11) -0.0070(10) -0.0018(10) -0.0048(10) C17 0.0253(13) 0.0211(12) 0.0147(10) -0.0066(9) -0.0061(9) 0.0015(10) C18 0.0407(16) 0.0278(14) 0.0163(11) -0.0075(10) -0.0073(11) -0.0065(12) C19 0.0464(18) 0.0421(17) 0.0167(12) -0.0102(12) -0.0073(12) -0.0081(14) C20 0.0398(18) 0.083(3) 0.0267(15) -0.0182(17) -0.0090(13) -0.0067(18) C21 0.124(4) 0.0369(19) 0.0338(17) -0.0140(15) -0.029(2) -0.018(2) C22 0.0303(14) 0.0360(15) 0.0152(11) -0.0040(11) -0.0012(10) -0.0109(12) C23 0.0355(17) 0.066(2) 0.0220(13) -0.0160(14) 0.0041(12) -0.0121(16) C24 0.0406(17) 0.0342(16) 0.0271(14) 0.0070(12) -0.0057(13) -0.0105(13) C25 0.0424(18) 0.054(2) 0.0217(13) -0.0049(13) -0.0019(12) -0.0249(15) C26 0.0242(13) 0.0244(13) 0.0229(12) -0.0106(10) -0.0041(10) -0.0011(10) C27 0.0256(13) 0.0220(12) 0.0196(11) -0.0102(10) -0.0036(10) -0.0015(10) C28 0.0272(13) 0.0241(13) 0.0238(12) -0.0103(11) -0.0070(10) -0.0026(10) C29 0.0344(14) 0.0203(12) 0.0202(12) -0.0073(10) -0.0087(11) -0.0024(11) C30 0.0348(14) 0.0221(13) 0.0155(11) -0.0063(10) -0.0039(10) -0.0024(11) C31 0.0298(13) 0.0190(12) 0.0165(11) -0.0067(9) -0.0020(10) -0.0048(10) C32 0.0280(13) 0.0140(11) 0.0168(11) -0.0052(9) -0.0035(10) -0.0031(9) C33 0.0405(16) 0.0350(15) 0.0217(12) -0.0112(12) -0.0152(12) 0.0011(13) C34 0.0369(16) 0.054(2) 0.0224(13) -0.0123(13) -0.0146(12) -0.0066(14) C35 0.058(2) 0.064(2) 0.0483(19) -0.0392(18) -0.0290(17) 0.0104(18) C36 0.053(2) 0.058(2) 0.0233(14) -0.0029(15) -0.0139(14) -0.0021(17) C37 0.0278(14) 0.0298(14) 0.0178(11) -0.0093(11) -0.0005(10) -0.0046(11) C38 0.0349(16) 0.058(2) 0.0241(13) -0.0224(14) 0.0049(12) -0.0074(14) C39 0.0353(16) 0.0482(18) 0.0350(15) -0.0228(14) 0.0086(13) -0.0193(14) C40 0.0358(17) 0.0442(18) 0.0302(15) -0.0062(14) 0.0039(13) 0.0092(14) _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 N1 1.682(2) . ? Mo1 N2 1.686(2) . ? Mo1 O2 2.0012(17) . ? Mo1 O1 2.1220(17) . ? Mo1 N4 2.157(2) . ? Mo1 N3 2.249(2) . ? N1 C1 1.427(3) . ? N2 C5 1.394(3) . ? N3 C11 1.236(3) . ? N3 C9 1.468(3) . ? N4 C26 1.235(3) . ? N4 C10 1.382(3) . ? O1 C32 1.248(3) . ? O2 C17 1.266(3) . ? C1 C2 1.431(4) . ? C1 C3 1.481(5) . ? C1 C4 1.512(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.454(4) . ? C5 C6 1.534(4) . ? C5 C7 1.537(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.517(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.455(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.342(3) . ? C12 C17 1.358(3) . ? C13 C14 1.381(4) . ? C13 H13 0.9500 . ? C14 C15 1.346(4) . ? C14 C18 1.460(3) . ? C15 C16 1.324(3) . ? C15 H15 0.9500 . ? C16 C17 1.421(4) . ? C16 C22 1.474(3) . ? C18 C19 1.468(4) . ? C18 C21 1.527(4) . ? C18 C20 1.526(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.481(4) . ? C22 C25 1.529(4) . ? C22 C24 1.533(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.355(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.352(3) . ? C27 C32 1.423(4) . ? C28 C29 1.288(4) . ? C28 H28 0.9500 . ? C29 C30 1.411(4) . ? C29 C33 1.466(3) . ? C30 C31 1.333(4) . ? C30 H30 0.9500 . ? C31 C32 1.356(3) . ? C31 C37 1.533(4) . ? C33 C36 1.500(4) . ? C33 C35 1.517(4) . ? C33 C34 1.532(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.437(4) . ? C37 C40 1.500(4) . ? C37 C39 1.533(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 N2 100.66(10) . . ? N1 Mo1 O2 106.08(9) . . ? N2 Mo1 O2 99.33(9) . . ? N1 Mo1 O1 91.94(9) . . ? N2 Mo1 O1 166.52(8) . . ? O2 Mo1 O1 81.55(7) . . ? N1 Mo1 N4 98.79(9) . . ? N2 Mo1 N4 96.72(9) . . ? O2 Mo1 N4 147.15(8) . . ? O1 Mo1 N4 76.43(7) . . ? N1 Mo1 N3 167.84(9) . . ? N2 Mo1 N3 87.30(9) . . ? O2 Mo1 N3 81.38(7) . . ? O1 Mo1 N3 79.50(7) . . ? N4 Mo1 N3 70.93(8) . . ? C1 N1 Mo1 159.6(2) . . ? C5 N2 Mo1 177.5(2) . . ? C11 N3 C9 122.6(2) . . ? C11 N3 Mo1 120.28(18) . . ? C9 N3 Mo1 114.97(16) . . ? C26 N4 C10 115.7(2) . . ? C26 N4 Mo1 126.53(18) . . ? C10 N4 Mo1 114.94(17) . . ? C32 O1 Mo1 115.34(16) . . ? C17 O2 Mo1 128.06(16) . . ? N1 C1 C2 106.6(3) . . ? N1 C1 C3 108.5(2) . . ? C2 C1 C3 110.1(4) . . ? N1 C1 C4 111.6(2) . . ? C2 C1 C4 107.6(3) . . ? C3 C1 C4 112.3(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C8 106.6(3) . . ? N2 C5 C6 110.6(2) . . ? C8 C5 C6 110.5(3) . . ? N2 C5 C7 108.1(2) . . ? C8 C5 C7 111.1(3) . . ? C6 C5 C7 109.8(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 107.9(2) . . ? N3 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? N3 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? N4 C10 C9 103.7(2) . . ? N4 C10 H10A 111.0 . . ? C9 C10 H10A 111.0 . . ? N4 C10 H10B 111.0 . . ? C9 C10 H10B 111.0 . . ? H10A C10 H10B 109.0 . . ? N3 C11 C12 126.5(2) . . ? N3 C11 H11A 105.7 . . ? C12 C11 H11A 105.7 . . ? N3 C11 H11B 105.7 . . ? C12 C11 H11B 105.7 . . ? H11A C11 H11B 106.1 . . ? C13 C12 C17 116.7(2) . . ? C13 C12 C11 117.1(2) . . ? C17 C12 C11 126.2(2) . . ? C12 C13 C14 122.9(2) . . ? C12 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C15 C14 C13 119.1(2) . . ? C15 C14 C18 116.6(2) . . ? C13 C14 C18 124.4(2) . . ? C16 C15 C14 121.1(3) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 118.7(2) . . ? C15 C16 C22 117.9(2) . . ? C17 C16 C22 123.5(2) . . ? O2 C17 C12 118.5(2) . . ? O2 C17 C16 120.0(2) . . ? C12 C17 C16 121.5(2) . . ? C14 C18 C19 108.4(2) . . ? C14 C18 C21 108.9(2) . . ? C19 C18 C21 110.5(3) . . ? C14 C18 C20 111.4(2) . . ? C19 C18 C20 108.0(3) . . ? C21 C18 C20 109.7(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 C23 105.6(2) . . ? C16 C22 C25 114.8(2) . . ? C23 C22 C25 107.1(3) . . ? C16 C22 C24 110.0(2) . . ? C23 C22 C24 112.7(2) . . ? C25 C22 C24 106.7(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N4 C26 C27 121.4(2) . . ? N4 C26 H26A 107.0 . . ? C27 C26 H26A 107.0 . . ? N4 C26 H26B 107.0 . . ? C27 C26 H26B 107.0 . . ? H26A C26 H26B 106.7 . . ? C28 C27 C26 114.9(2) . . ? C28 C27 C32 124.2(2) . . ? C26 C27 C32 120.2(2) . . ? C29 C28 C27 117.7(3) . . ? C29 C28 H28 121.2 . . ? C27 C28 H28 121.2 . . ? C28 C29 C30 118.1(2) . . ? C28 C29 C33 120.2(3) . . ? C30 C29 C33 121.7(2) . . ? C31 C30 C29 127.3(2) . . ? C31 C30 H30 116.3 . . ? C29 C30 H30 116.3 . . ? C30 C31 C32 114.3(2) . . ? C30 C31 C37 123.7(2) . . ? C32 C31 C37 121.9(2) . . ? O1 C32 C31 118.1(2) . . ? O1 C32 C27 123.5(2) . . ? C31 C32 C27 118.4(2) . . ? C29 C33 C36 106.0(3) . . ? C29 C33 C35 107.5(2) . . ? C36 C33 C35 113.5(3) . . ? C29 C33 C34 114.2(2) . . ? C36 C33 C34 107.1(3) . . ? C35 C33 C34 108.7(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C40 104.2(3) . . ? C38 C37 C39 106.8(2) . . ? C40 C37 C39 111.7(3) . . ? C38 C37 C31 112.9(2) . . ? C40 C37 C31 111.4(2) . . ? C39 C37 C31 109.6(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.848 _diffrn_reflns_theta_full 29.74 _diffrn_measured_fraction_theta_full 0.848 _refine_diff_density_max 0.913 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.102