Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name C.Carrano 'Justin Hoffman' 'Ba Tran' _publ_contact_author_name 'Prof Carl Carrano' _publ_contact_author_address ; Department of Chemistry and Biochemistry San Diego State University 5500 Campanile Dr. San Diego CA 92182-1030 UNITED STATES OF AMERICA ; _publ_contact_author_email CARRANO@SCIENCES.SDSU.EDU _publ_section_title ; Oxidation State and Metal Ion Dependent Stereoisomerization in Oxo Molybdenum and Tungsten Complexes of a Bulky Alkoxy Heteroscorpionate Ligand ; data_ltgreen_Compound_6 _database_code_depnum_ccdc_archive 'CCDC 246847' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H25 Cl2 Mo N4 O2' _chemical_formula_weight 568.32 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 19.1477(10) _cell_length_b 15.6625(8) _cell_length_c 17.5373(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.015(5) _cell_angle_gamma 90.00 _cell_volume 4726.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 32013 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 20.85 _reflns_number_total 4961 _reflns_number_gt 3892 _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^)+(0.0400P)^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 4961 _refine_ls_number_parameters 591 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.500 _refine_ls_restrained_S_all 1.500 _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 Mo1 Mo 0.36634(4) 1.18299(4) 0.37525(3) 0.0336(2) Uani 1 1 d . . . Cl2 Cl 0.45398(10) 1.10327(12) 0.48405(10) 0.0426(5) Uani 1 1 d . . . Cl1 Cl 0.39048(10) 1.30397(11) 0.46462(10) 0.0378(5) Uani 1 1 d . . . O2 O 0.2775(2) 1.1490(3) 0.3773(2) 0.0218(7) Uani 1 1 d . . . O1 O 0.3700(2) 1.1051(3) 0.2918(2) 0.0238(8) Uani 1 1 d . . . N2 N 0.3055(3) 1.2682(3) 0.2663(3) 0.0270(14) Uani 1 1 d . . . N1 N 0.3270(3) 1.2725(3) 0.2014(3) 0.0252(13) Uani 1 1 d . . . N4 N 0.4684(3) 1.2374(3) 0.3498(3) 0.0249(13) Uani 1 1 d . . . N3 N 0.4605(3) 1.2332(3) 0.2676(3) 0.0237(13) Uani 1 1 d . . . C1 C 0.2945(4) 1.3535(4) 0.0664(4) 0.0379(19) Uani 1 1 d . . . H1B H 0.2829 1.4126 0.0520 0.057 Uiso 1 1 calc R . . H1C H 0.2594 1.3186 0.0206 0.057 Uiso 1 1 calc R . . H1D H 0.3469 1.3418 0.0759 0.057 Uiso 1 1 calc R . . C2 C 0.2857(4) 1.3338(4) 0.1451(4) 0.0271(17) Uani 1 1 d . . . C3 C 0.2370(4) 1.3678(4) 0.1749(4) 0.0308(18) Uani 1 1 d . . . H3A H 0.2008 1.4111 0.1497 0.037 Uiso 1 1 calc R . . C4 C 0.2513(4) 1.3259(4) 0.2497(4) 0.0291(17) Uani 1 1 d . . . C5 C 0.2104(4) 1.3400(4) 0.3059(4) 0.040(2) Uani 1 1 d . . . H5A H 0.2175 1.2907 0.3411 0.060 Uiso 1 1 calc R . . H5B H 0.1560 1.3489 0.2711 0.060 Uiso 1 1 calc R . . H5C H 0.2320 1.3892 0.3410 0.060 Uiso 1 1 calc R . . C6 C 0.5329(4) 1.2573(4) 0.1802(4) 0.0363(19) Uani 1 1 d . . . H6A H 0.4974 1.2989 0.1431 0.054 Uiso 1 1 calc R . . H6B H 0.5204 1.2021 0.1538 0.054 Uiso 1 1 calc R . . H6C H 0.5850 1.2723 0.1909 0.054 Uiso 1 1 calc R . . C7 C 0.5264(4) 1.2550(4) 0.2628(4) 0.0255(17) Uani 1 1 d . . . C8 C 0.5801(4) 1.2709(4) 0.3447(4) 0.0279(17) Uani 1 1 d . . . H8A H 0.6319 1.2858 0.3623 0.033 Uiso 1 1 calc R . . C9 C 0.5425(4) 1.2607(4) 0.3962(4) 0.0269(17) Uani 1 1 d . . . C10 C 0.5754(4) 1.2744(4) 0.4896(3) 0.0320(17) Uani 1 1 d . . . H10A H 0.5610 1.2277 0.5151 0.048 Uiso 1 1 calc R . . H10B H 0.5555 1.3268 0.5008 0.048 Uiso 1 1 calc R . . H10C H 0.6311 1.2777 0.5130 0.048 Uiso 1 1 calc R . . C11 C 0.3839(3) 1.2114(4) 0.2004(4) 0.0238(17) Uani 1 1 d . . . H11A H 0.3861 1.2165 0.1458 0.029 Uiso 1 1 calc R . . C12 C 0.3614(3) 1.1188(4) 0.2093(3) 0.0215(16) Uani 1 1 d . . . C13 C 0.4194(3) 1.0591(4) 0.1969(4) 0.0236(16) Uani 1 1 d . . . C14 C 0.4799(4) 1.0222(4) 0.2659(4) 0.0335(18) Uani 1 1 d . . . H14A H 0.4843 1.0322 0.3201 0.040 Uiso 1 1 calc R . . C15 C 0.5331(4) 0.9716(5) 0.2561(5) 0.042(2) Uani 1 1 d . . . H15A H 0.5735 0.9481 0.3037 0.050 Uiso 1 1 calc R . . C16 C 0.5282(4) 0.9547(4) 0.1768(5) 0.043(2) Uani 1 1 d . . . H16A H 0.5644 0.9193 0.1705 0.051 Uiso 1 1 calc R . . C17 C 0.4697(4) 0.9907(4) 0.1079(5) 0.0377(19) Uani 1 1 d . . . H17A H 0.4662 0.9806 0.0540 0.045 Uiso 1 1 calc R . . C18 C 0.4149(4) 1.0428(4) 0.1172(4) 0.0370(19) Uani 1 1 d . . . H18A H 0.3750 1.0667 0.0694 0.044 Uiso 1 1 calc R . . C19 C 0.2761(3) 1.1007(4) 0.1457(4) 0.0238(16) Uani 1 1 d . . . C20 C 0.2432(4) 1.1345(4) 0.0645(4) 0.0292(17) Uani 1 1 d . . . H20A H 0.2732 1.1678 0.0461 0.035 Uiso 1 1 calc R . . C21 C 0.1653(4) 1.1188(4) 0.0102(4) 0.0364(19) Uani 1 1 d . . . H21A H 0.1432 1.1426 -0.0439 0.044 Uiso 1 1 calc R . . C22 C 0.1210(4) 1.0684(4) 0.0363(4) 0.0340(18) Uani 1 1 d . . . H22A H 0.0690 1.0582 0.0004 0.041 Uiso 1 1 calc R . . C23 C 0.1551(4) 1.0329(4) 0.1173(4) 0.0339(18) Uani 1 1 d . . . H23A H 0.1259 0.9979 0.1352 0.041 Uiso 1 1 calc R . . C24 C 0.2320(3) 1.0496(4) 0.1710(4) 0.0250(16) Uani 1 1 d . . . H24A H 0.2541 1.0258 0.2251 0.030 Uiso 1 1 calc R . . Mo2 Mo 0.14604(3) 0.72808(4) 0.15667(3) 0.0306(2) Uani 1 1 d . . . Cl3 Cl 0.13265(9) 0.59341(11) 0.08976(10) 0.0365(5) Uani 1 1 d . . . Cl4 Cl 0.06171(11) 0.79372(13) 0.03374(11) 0.0494(6) Uani 1 1 d . . . O4 O 0.2393(2) 0.7580(3) 0.1598(2) 0.0218(7) Uani 1 1 d . . . O3 O 0.1330(2) 0.8183(3) 0.2230(2) 0.0238(8) Uani 1 1 d . . . N6 N 0.2008(3) 0.6616(3) 0.2775(3) 0.0238(13) Uani 1 1 d . . . N5 N 0.1721(3) 0.6700(3) 0.3373(3) 0.0215(13) Uani 1 1 d . . . N8 N 0.0366(3) 0.6848(3) 0.1731(3) 0.0229(13) Uani 1 1 d . . . N7 N 0.0374(3) 0.6973(3) 0.2510(3) 0.0221(13) Uani 1 1 d . . . C25 C 0.1979(4) 0.6170(4) 0.4816(4) 0.0318(18) Uani 1 1 d . . . H25A H 0.2287 0.5726 0.5189 0.048 Uiso 1 1 calc R . . H25B H 0.1439 0.6058 0.4648 0.048 Uiso 1 1 calc R . . H25C H 0.2117 0.6709 0.5106 0.048 Uiso 1 1 calc R . . C26 C 0.2126(3) 0.6200(4) 0.4051(4) 0.0216(16) Uani 1 1 d . . . C27 C 0.2679(3) 0.5798(4) 0.3895(4) 0.0257(16) Uani 1 1 d . . . H27A H 0.3045 0.5412 0.4254 0.031 Uiso 1 1 calc R . . C28 C 0.2601(3) 0.6065(4) 0.3104(4) 0.0251(16) Uani 1 1 d . . . C29 C 0.3080(3) 0.5836(4) 0.2666(4) 0.0349(18) Uani 1 1 d . . . H29A H 0.3146 0.6329 0.2378 0.052 Uiso 1 1 calc R . . H29B H 0.2826 0.5392 0.2260 0.052 Uiso 1 1 calc R . . H29C H 0.3579 0.5638 0.3074 0.052 Uiso 1 1 calc R . . C30 C -0.0483(3) 0.6859(4) 0.3246(4) 0.0349(18) Uani 1 1 d . . . H30A H -0.0371 0.7427 0.3471 0.052 Uiso 1 1 calc R . . H30B H -0.0158 0.6460 0.3669 0.052 Uiso 1 1 calc R . . H30C H -0.1019 0.6729 0.3087 0.052 Uiso 1 1 calc R . . C31 C -0.0328(4) 0.6796(4) 0.2483(4) 0.0242(16) Uani 1 1 d . . . C32 C -0.0799(4) 0.6561(4) 0.1675(4) 0.0299(17) Uani 1 1 d . . . H32A H -0.1319 0.6401 0.1463 0.036 Uiso 1 1 calc R . . C33 C -0.0365(4) 0.6602(4) 0.1233(4) 0.0285(17) Uani 1 1 d . . . C34 C -0.0650(4) 0.6397(5) 0.0290(4) 0.0402(19) Uani 1 1 d . . . H34A H -0.0215 0.6246 0.0184 0.060 Uiso 1 1 calc R . . H34B H -0.0905 0.6889 -0.0042 0.060 Uiso 1 1 calc R . . H34C H -0.1009 0.5928 0.0138 0.060 Uiso 1 1 calc R . . C35 C 0.1088(3) 0.7298(4) 0.3208(4) 0.0226(16) Uani 1 1 d . . . H35A H 0.1002 0.7332 0.3719 0.027 Uiso 1 1 calc R . . C36 C 0.1272(3) 0.8203(4) 0.3002(3) 0.0203(16) Uani 1 1 d . . . C37 C 0.2054(4) 0.8514(4) 0.3706(4) 0.0258(17) Uani 1 1 d . . . C38 C 0.2223(4) 0.8479(4) 0.4558(4) 0.0264(17) Uani 1 1 d . . . H38A H 0.1875 0.8218 0.4723 0.032 Uiso 1 1 calc R . . C39 C 0.2904(4) 0.8829(4) 0.5170(4) 0.0306(17) Uani 1 1 d . . . H39A H 0.3011 0.8798 0.5740 0.037 Uiso 1 1 calc R . . C40 C 0.3413(4) 0.9217(4) 0.4936(4) 0.0320(18) Uani 1 1 d . . . H40A H 0.3865 0.9460 0.5346 0.038 Uiso 1 1 calc R . . C41 C 0.3263(4) 0.9252(4) 0.4096(4) 0.0337(18) Uani 1 1 d . . . H41A H 0.3619 0.9509 0.3940 0.040 Uiso 1 1 calc R . . C42 C 0.2581(4) 0.8904(4) 0.3479(4) 0.0280(17) Uani 1 1 d . . . H42A H 0.2480 0.8935 0.2911 0.034 Uiso 1 1 calc R . . C43 C 0.0605(3) 0.8790(4) 0.2892(4) 0.0233(16) Uani 1 1 d . . . C44 C 0.0133(3) 0.9156(4) 0.2099(3) 0.0228(16) Uani 1 1 d . . . H44A H 0.0225 0.9030 0.1633 0.027 Uiso 1 1 calc R . . C45 C -0.0455(3) 0.9693(4) 0.2008(4) 0.0270(17) Uani 1 1 d . . . H45A H -0.0750 0.9942 0.1482 0.032 Uiso 1 1 calc R . . C46 C -0.0623(3) 0.9876(4) 0.2673(4) 0.0243(16) Uani 1 1 d . . . H46A H -0.1034 1.0238 0.2596 0.029 Uiso 1 1 calc R . . C47 C -0.0181(4) 0.9520(4) 0.3454(4) 0.0310(17) Uani 1 1 d . . . H47A H -0.0288 0.9645 0.3910 0.037 Uiso 1 1 calc R . . C48 C 0.0421(4) 0.8981(4) 0.3562(4) 0.0286(17) Uani 1 1 d . . . H48A H 0.0713 0.8737 0.4091 0.034 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 0.0440(4) 0.0367(4) 0.0169(3) -0.0021(3) 0.0105(3) -0.0003(3) Cl2 0.0359(11) 0.0484(12) 0.0340(10) -0.0043(9) 0.0066(9) -0.0034(9) Cl1 0.0383(11) 0.0421(12) 0.0259(10) -0.0050(8) 0.0077(8) 0.0033(9) O2 0.0166(16) 0.044(2) 0.0040(14) 0.0008(13) 0.0036(12) 0.0123(14) O1 0.0204(17) 0.034(2) 0.0151(17) -0.0006(14) 0.0065(14) 0.0001(15) N2 0.025(3) 0.036(4) 0.015(3) -0.001(3) 0.005(3) 0.011(3) N1 0.025(3) 0.025(3) 0.017(3) 0.003(3) 0.002(3) -0.001(3) N4 0.020(3) 0.027(3) 0.019(3) -0.001(3) 0.000(3) -0.004(3) N3 0.030(4) 0.023(3) 0.013(3) 0.002(2) 0.004(3) -0.003(3) C1 0.028(4) 0.043(5) 0.028(4) 0.007(4) -0.002(3) 0.001(4) C2 0.023(4) 0.028(4) 0.016(4) -0.001(3) -0.004(3) -0.001(3) C3 0.025(4) 0.022(4) 0.033(4) 0.000(4) 0.001(4) 0.005(3) C4 0.027(4) 0.036(5) 0.016(4) -0.003(3) 0.001(3) 0.000(4) C5 0.032(4) 0.049(5) 0.027(4) -0.003(4) 0.002(4) 0.016(4) C6 0.028(4) 0.050(5) 0.026(4) -0.001(3) 0.007(3) -0.002(4) C7 0.026(4) 0.023(4) 0.027(4) 0.001(3) 0.012(4) -0.002(3) C8 0.019(4) 0.032(4) 0.020(4) 0.001(3) -0.002(3) 0.000(3) C9 0.029(4) 0.020(4) 0.027(4) 0.003(3) 0.008(4) 0.000(3) C10 0.034(4) 0.031(4) 0.024(4) 0.000(3) 0.007(3) -0.003(4) C11 0.022(4) 0.027(4) 0.016(4) -0.002(3) 0.002(3) -0.003(3) C12 0.021(4) 0.023(4) 0.014(4) -0.004(3) 0.002(3) -0.003(3) C13 0.023(4) 0.026(4) 0.020(4) -0.004(3) 0.007(3) -0.005(3) C14 0.028(4) 0.037(5) 0.036(4) -0.003(4) 0.014(4) 0.008(4) C15 0.028(4) 0.042(5) 0.049(5) 0.000(4) 0.012(4) 0.002(4) C16 0.031(5) 0.033(5) 0.071(6) -0.012(5) 0.028(5) -0.010(4) C17 0.045(5) 0.039(5) 0.042(5) -0.013(4) 0.031(4) -0.009(4) C18 0.035(5) 0.038(5) 0.032(4) -0.004(4) 0.010(4) -0.007(4) C19 0.023(4) 0.028(4) 0.017(4) -0.006(3) 0.006(3) 0.003(3) C20 0.026(4) 0.032(4) 0.026(4) -0.004(3) 0.008(4) -0.011(3) C21 0.037(5) 0.041(5) 0.021(4) -0.005(3) 0.005(4) -0.002(4) C22 0.025(4) 0.039(5) 0.027(4) -0.012(4) 0.001(4) 0.003(4) C23 0.030(4) 0.041(5) 0.035(5) -0.013(4) 0.018(4) -0.011(4) C24 0.022(4) 0.035(4) 0.013(3) -0.002(3) 0.003(3) -0.005(3) Mo2 0.0351(4) 0.0382(4) 0.0194(3) -0.0024(3) 0.0128(3) -0.0030(3) Cl3 0.0358(10) 0.0468(12) 0.0266(10) -0.0044(8) 0.0133(8) -0.0043(9) Cl4 0.0427(12) 0.0705(15) 0.0327(11) 0.0048(10) 0.0144(9) -0.0035(10) O4 0.0166(16) 0.044(2) 0.0040(14) 0.0008(13) 0.0036(12) 0.0123(14) O3 0.0204(17) 0.034(2) 0.0151(17) -0.0006(14) 0.0065(14) 0.0001(15) N6 0.019(3) 0.032(4) 0.017(3) -0.003(3) 0.006(3) -0.001(3) N5 0.019(3) 0.029(4) 0.013(3) 0.002(3) 0.004(3) 0.002(3) N8 0.017(3) 0.035(3) 0.015(3) 0.000(3) 0.005(3) 0.000(3) N7 0.020(3) 0.032(4) 0.010(3) 0.002(2) 0.003(2) 0.003(3) C25 0.035(4) 0.029(4) 0.024(4) 0.005(3) 0.005(3) 0.001(3) C26 0.015(4) 0.024(4) 0.019(4) -0.001(3) 0.002(3) -0.003(3) C27 0.018(4) 0.028(4) 0.021(4) 0.000(3) 0.000(3) 0.000(3) C28 0.016(4) 0.026(4) 0.023(4) -0.012(3) 0.001(3) -0.003(3) C29 0.024(4) 0.044(5) 0.032(4) -0.002(3) 0.008(3) 0.003(4) C30 0.018(4) 0.056(5) 0.029(4) 0.006(4) 0.009(3) -0.001(4) C31 0.016(4) 0.033(4) 0.024(4) 0.001(3) 0.009(3) 0.002(3) C32 0.016(4) 0.047(5) 0.019(4) 0.002(3) 0.001(3) -0.001(3) C33 0.025(4) 0.034(5) 0.022(4) 0.000(3) 0.006(4) 0.003(3) C34 0.025(4) 0.067(5) 0.021(4) -0.008(4) 0.003(3) -0.005(4) C35 0.019(4) 0.033(4) 0.015(4) 0.001(3) 0.007(3) 0.005(4) C36 0.016(4) 0.026(4) 0.016(4) 0.001(3) 0.005(3) -0.003(3) C37 0.027(4) 0.025(4) 0.020(4) 0.003(3) 0.005(3) 0.007(3) C38 0.024(4) 0.030(4) 0.023(4) 0.000(3) 0.009(3) 0.002(3) C39 0.030(4) 0.035(5) 0.022(4) 0.001(3) 0.007(4) 0.001(4) C40 0.025(4) 0.031(4) 0.027(4) -0.009(3) -0.001(3) 0.000(4) C41 0.026(4) 0.038(5) 0.034(5) 0.007(4) 0.011(4) -0.003(4) C42 0.028(4) 0.031(4) 0.025(4) 0.003(3) 0.011(4) 0.002(4) C43 0.018(4) 0.026(4) 0.023(4) -0.002(3) 0.008(3) -0.007(3) C44 0.025(4) 0.031(4) 0.009(4) 0.003(3) 0.003(3) 0.001(4) C45 0.019(4) 0.028(4) 0.019(4) 0.011(3) -0.006(3) 0.003(4) C46 0.016(4) 0.026(4) 0.024(4) 0.002(3) 0.003(3) 0.002(3) C47 0.030(4) 0.040(5) 0.025(4) -0.003(4) 0.014(4) 0.001(4) C48 0.028(4) 0.034(4) 0.018(4) 0.002(3) 0.005(3) 0.001(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 Mo1 O2 1.798(4) . ? Mo1 O1 1.931(4) . ? Mo1 N2 2.199(5) . ? Mo1 Cl2 2.2819(18) . ? Mo1 N4 2.348(5) . ? Mo1 Cl1 2.3717(17) . ? O1 C12 1.399(6) . ? N2 C4 1.308(8) . ? N2 N1 1.373(6) . ? N1 C2 1.355(8) . ? N1 C11 1.455(8) . ? N4 C9 1.341(7) . ? N4 N3 1.383(6) . ? N3 C7 1.345(7) . ? N3 C11 1.463(7) . ? C1 C2 1.495(9) . ? C2 C3 1.362(8) . ? C3 C4 1.382(8) . ? C4 C5 1.521(9) . ? C6 C7 1.509(8) . ? C7 C8 1.374(8) . ? C8 C9 1.390(8) . ? C9 C10 1.490(8) . ? C11 C12 1.540(8) . ? C12 C13 1.537(8) . ? C12 C19 1.547(8) . ? C13 C14 1.383(8) . ? C13 C18 1.387(8) . ? C14 C15 1.361(9) . ? C15 C16 1.378(9) . ? C16 C17 1.359(9) . ? C17 C18 1.393(9) . ? C19 C24 1.371(8) . ? C19 C20 1.386(8) . ? C20 C21 1.396(8) . ? C21 C22 1.375(9) . ? C22 C23 1.391(9) . ? C23 C24 1.381(8) . ? Mo2 O4 1.825(4) . ? Mo2 O3 1.914(4) . ? Mo2 N6 2.174(5) . ? Mo2 Cl4 2.2931(19) . ? Mo2 N8 2.338(5) . ? Mo2 Cl3 2.3723(18) . ? O3 C36 1.407(6) . ? N6 C28 1.339(7) . ? N6 N5 1.388(6) . ? N5 C26 1.350(7) . ? N5 C35 1.455(7) . ? N8 C33 1.340(7) . ? N8 N7 1.374(6) . ? N7 C31 1.353(7) . ? N7 C35 1.470(7) . ? C25 C26 1.487(8) . ? C26 C27 1.359(8) . ? C27 C28 1.394(8) . ? C28 C29 1.475(8) . ? C30 C31 1.495(8) . ? C31 C32 1.354(8) . ? C32 C33 1.366(8) . ? C33 C34 1.530(8) . ? C35 C36 1.542(8) . ? C36 C43 1.517(8) . ? C36 C37 1.543(8) . ? C37 C42 1.378(8) . ? C37 C38 1.386(8) . ? C38 C39 1.387(8) . ? C39 C40 1.355(8) . ? C40 C41 1.373(8) . ? C41 C42 1.391(8) . ? C43 C48 1.398(8) . ? C43 C44 1.406(8) . ? C44 C45 1.357(8) . ? C45 C46 1.371(8) . ? C46 C47 1.374(8) . ? C47 C48 1.374(8) . ? 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 O2 Mo1 O1 100.24(16) . . ? O2 Mo1 N2 92.95(18) . . ? O1 Mo1 N2 84.61(18) . . ? O2 Mo1 Cl2 100.16(12) . . ? O1 Mo1 Cl2 91.74(12) . . ? N2 Mo1 Cl2 166.82(15) . . ? O2 Mo1 N4 170.17(16) . . ? O1 Mo1 N4 76.97(17) . . ? N2 Mo1 N4 77.46(18) . . ? Cl2 Mo1 N4 89.39(13) . . ? O2 Mo1 Cl1 97.76(13) . . ? O1 Mo1 Cl1 160.84(13) . . ? N2 Mo1 Cl1 87.98(14) . . ? Cl2 Mo1 Cl1 91.49(6) . . ? N4 Mo1 Cl1 84.18(13) . . ? C12 O1 Mo1 131.4(4) . . ? C4 N2 N1 106.1(5) . . ? C4 N2 Mo1 132.8(4) . . ? N1 N2 Mo1 120.9(4) . . ? C2 N1 N2 110.3(5) . . ? C2 N1 C11 131.2(6) . . ? N2 N1 C11 118.4(5) . . ? C9 N4 N3 104.5(5) . . ? C9 N4 Mo1 137.0(4) . . ? N3 N4 Mo1 117.4(4) . . ? C7 N3 N4 112.1(5) . . ? C7 N3 C11 130.2(5) . . ? N4 N3 C11 117.7(5) . . ? N1 C2 C3 106.1(6) . . ? N1 C2 C1 123.5(6) . . ? C3 C2 C1 130.4(6) . . ? C2 C3 C4 107.0(6) . . ? N2 C4 C3 110.4(6) . . ? N2 C4 C5 122.6(6) . . ? C3 C4 C5 127.0(6) . . ? N3 C7 C8 105.9(5) . . ? N3 C7 C6 122.8(5) . . ? C8 C7 C6 131.3(6) . . ? C7 C8 C9 107.1(6) . . ? N4 C9 C8 110.4(5) . . ? N4 C9 C10 122.1(6) . . ? C8 C9 C10 127.5(6) . . ? N1 C11 N3 109.1(5) . . ? N1 C11 C12 112.1(5) . . ? N3 C11 C12 111.3(5) . . ? O1 C12 C13 106.8(5) . . ? O1 C12 C11 109.7(5) . . ? C13 C12 C11 107.9(5) . . ? O1 C12 C19 108.9(5) . . ? C13 C12 C19 112.8(5) . . ? C11 C12 C19 110.6(5) . . ? C14 C13 C18 117.6(6) . . ? C14 C13 C12 120.7(6) . . ? C18 C13 C12 121.7(6) . . ? C15 C14 C13 121.3(6) . . ? C14 C15 C16 121.1(7) . . ? C17 C16 C15 118.8(7) . . ? C16 C17 C18 120.5(7) . . ? C13 C18 C17 120.6(6) . . ? C24 C19 C20 119.3(6) . . ? C24 C19 C12 118.7(5) . . ? C20 C19 C12 122.0(6) . . ? C19 C20 C21 120.1(6) . . ? C22 C21 C20 120.3(6) . . ? C21 C22 C23 119.2(6) . . ? C24 C23 C22 120.2(6) . . ? C19 C24 C23 120.9(6) . . ? O4 Mo2 O3 100.27(16) . . ? O4 Mo2 N6 92.69(17) . . ? O3 Mo2 N6 84.11(17) . . ? O4 Mo2 Cl4 100.91(12) . . ? O3 Mo2 Cl4 90.82(12) . . ? N6 Mo2 Cl4 166.15(14) . . ? O4 Mo2 N8 171.85(15) . . ? O3 Mo2 N8 77.12(17) . . ? N6 Mo2 N8 79.40(17) . . ? Cl4 Mo2 N8 86.91(13) . . ? O4 Mo2 Cl3 97.79(13) . . ? O3 Mo2 Cl3 160.42(13) . . ? N6 Mo2 Cl3 87.56(14) . . ? Cl4 Mo2 Cl3 93.14(7) . . ? N8 Mo2 Cl3 83.95(13) . . ? C36 O3 Mo2 133.4(4) . . ? C28 N6 N5 106.2(5) . . ? C28 N6 Mo2 133.1(4) . . ? N5 N6 Mo2 120.6(4) . . ? C26 N5 N6 110.2(5) . . ? C26 N5 C35 131.0(5) . . ? N6 N5 C35 118.8(5) . . ? C33 N8 N7 104.1(5) . . ? C33 N8 Mo2 137.7(4) . . ? N7 N8 Mo2 117.4(3) . . ? C31 N7 N8 110.9(4) . . ? C31 N7 C35 130.4(5) . . ? N8 N7 C35 118.6(5) . . ? N5 C26 C27 106.8(5) . . ? N5 C26 C25 123.3(6) . . ? C27 C26 C25 129.8(6) . . ? C26 C27 C28 108.0(6) . . ? N6 C28 C27 108.7(5) . . ? N6 C28 C29 122.5(6) . . ? C27 C28 C29 128.8(6) . . ? N7 C31 C32 106.8(5) . . ? N7 C31 C30 122.6(5) . . ? C32 C31 C30 130.6(6) . . ? C31 C32 C33 106.8(6) . . ? N8 C33 C32 111.4(5) . . ? N8 C33 C34 122.7(6) . . ? C32 C33 C34 125.9(6) . . ? N5 C35 N7 109.4(5) . . ? N5 C35 C36 112.5(5) . . ? N7 C35 C36 110.3(5) . . ? O3 C36 C43 108.0(5) . . ? O3 C36 C35 109.2(5) . . ? C43 C36 C35 108.7(5) . . ? O3 C36 C37 108.6(5) . . ? C43 C36 C37 112.2(5) . . ? C35 C36 C37 110.1(5) . . ? C42 C37 C38 118.3(6) . . ? C42 C37 C36 119.0(5) . . ? C38 C37 C36 122.4(6) . . ? C37 C38 C39 120.9(6) . . ? C40 C39 C38 120.0(6) . . ? C39 C40 C41 120.2(6) . . ? C40 C41 C42 120.1(6) . . ? C37 C42 C41 120.4(6) . . ? C48 C43 C44 117.0(6) . . ? C48 C43 C36 122.1(5) . . ? C44 C43 C36 120.8(5) . . ? C45 C44 C43 120.6(6) . . ? C44 C45 C46 121.5(5) . . ? C45 C46 C47 119.5(6) . . ? C46 C47 C48 120.0(6) . . ? C47 C48 C43 121.4(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.85 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.884 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.088 data_sdsu5_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 246848' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H25 Cl Mo N4 O3' _chemical_formula_weight 548.87 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' 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 9.7589(6) _cell_length_b 15.5178(10) _cell_length_c 15.4080(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.1710(10) _cell_angle_gamma 90.00 _cell_volume 2327.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 5408 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.16 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 16668 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.19 _reflns_number_total 5482 _reflns_number_gt 4935 _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^)+(0.0464P)^2^+1.8860P] 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 5482 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 0.71897(2) 0.294603(15) 0.994349(12) 0.02843(8) Uani 1 1 d . . . Cl1 Cl 0.81323(8) 0.15979(5) 1.04263(4) 0.04356(18) Uani 1 1 d . . . O1 O 0.62639(18) 0.37297(11) 0.91519(10) 0.0288(4) Uani 1 1 d . . . O2 O 0.6290(2) 0.31030(14) 1.08317(11) 0.0394(5) Uani 1 1 d . . . O3 O 0.87047(19) 0.34937(14) 1.01601(12) 0.0390(4) Uani 1 1 d . . . N1 N 0.7003(2) 0.25174(14) 0.78741(12) 0.0259(4) Uani 1 1 d . . . N2 N 0.7905(2) 0.24912(14) 0.85971(12) 0.0277(4) Uani 1 1 d . . . N3 N 0.4945(2) 0.21362(13) 0.85061(12) 0.0251(4) Uani 1 1 d . . . N4 N 0.5379(2) 0.20781(14) 0.93707(12) 0.0278(4) Uani 1 1 d . . . C1 C 0.5504(2) 0.36944(15) 0.83449(14) 0.0247(5) Uani 1 1 d . . . C2 C 0.5588(2) 0.27645(16) 0.79710(15) 0.0246(5) Uani 1 1 d . . . C3 C 0.6892(4) 0.2281(3) 0.62629(18) 0.0440(7) Uani 1 1 d . . . C4 C 0.7628(3) 0.23109(18) 0.71417(16) 0.0322(5) Uani 1 1 d . . . C5 C 0.8975(3) 0.21525(19) 0.74073(18) 0.0359(6) Uani 1 1 d . . . C6 C 0.9112(3) 0.22616(18) 0.83090(17) 0.0319(5) Uani 1 1 d . . . C7 C 1.0367(3) 0.2150(3) 0.8906(2) 0.0441(7) Uani 1 1 d . . . C8 C 0.3256(3) 0.1484(2) 0.73956(19) 0.0373(6) Uani 1 1 d . . . C9 C 0.3938(2) 0.15605(16) 0.82845(16) 0.0283(5) Uani 1 1 d . . . C10 C 0.3705(3) 0.11212(18) 0.90334(18) 0.0330(5) Uani 1 1 d . . . C11 C 0.4608(3) 0.14640(17) 0.96922(16) 0.0312(5) Uani 1 1 d . . . C12 C 0.4746(4) 0.1210(3) 1.0630(2) 0.0439(7) Uani 1 1 d . . . C13 C 0.4007(2) 0.39269(16) 0.84821(15) 0.0268(5) Uani 1 1 d . . . C14 C 0.3698(3) 0.42648(19) 0.92812(18) 0.0354(6) Uani 1 1 d . . . C15 C 0.2359(3) 0.4495(2) 0.9422(2) 0.0428(7) Uani 1 1 d . . . C16 C 0.1319(3) 0.4385(2) 0.8788(2) 0.0439(7) Uani 1 1 d . . . C17 C 0.1611(3) 0.4045(2) 0.7997(2) 0.0414(7) Uani 1 1 d . . . C18 C 0.2942(3) 0.38113(18) 0.78424(18) 0.0331(5) Uani 1 1 d . . . C19 C 0.6194(2) 0.43046(16) 0.77203(15) 0.0279(5) Uani 1 1 d . . . C20 C 0.5598(3) 0.4495(2) 0.68982(18) 0.0409(7) Uani 1 1 d . . . C21 C 0.6289(4) 0.5008(2) 0.6332(2) 0.0455(7) Uani 1 1 d . . . C22 C 0.7553(3) 0.53357(18) 0.6571(2) 0.0400(6) Uani 1 1 d . . . C23 C 0.8156(3) 0.5152(2) 0.7385(2) 0.0424(7) Uani 1 1 d . . . C24 C 0.7478(3) 0.46413(19) 0.79561(19) 0.0362(6) Uani 1 1 d . . . H2 H 0.516(3) 0.2744(16) 0.7447(17) 0.017(6) Uiso 1 1 d . . . H3A H 0.649(4) 0.280(3) 0.610(3) 0.056(11) Uiso 1 1 d . . . H3B H 0.634(5) 0.185(3) 0.622(3) 0.062(12) Uiso 1 1 d . . . H3C H 0.741(4) 0.214(2) 0.584(3) 0.065(12) Uiso 1 1 d . . . H5 H 0.959(4) 0.195(2) 0.704(2) 0.057(11) Uiso 1 1 d . . . H7A H 1.103(5) 0.227(3) 0.863(3) 0.074(13) Uiso 1 1 d . . . H7B H 1.043(4) 0.161(3) 0.913(3) 0.067(12) Uiso 1 1 d . . . H7C H 1.041(4) 0.248(3) 0.936(3) 0.061(12) Uiso 1 1 d . . . H8A H 0.284(4) 0.201(3) 0.729(3) 0.060(11) Uiso 1 1 d . . . H8B H 0.268(4) 0.104(2) 0.738(2) 0.043(9) Uiso 1 1 d . . . H8C H 0.387(4) 0.145(2) 0.697(2) 0.044(9) Uiso 1 1 d . . . H10 H 0.300(3) 0.0646(19) 0.9085(18) 0.030(7) Uiso 1 1 d . . . H12A H 0.509(5) 0.163(3) 1.096(3) 0.081(15) Uiso 1 1 d . . . H12B H 0.389(5) 0.109(3) 1.076(3) 0.086(15) Uiso 1 1 d . . . H12C H 0.534(5) 0.080(3) 1.071(3) 0.071(13) Uiso 1 1 d . . . H14 H 0.436(3) 0.4336(19) 0.970(2) 0.036(8) Uiso 1 1 d . . . H15 H 0.215(3) 0.464(2) 0.991(2) 0.050(10) Uiso 1 1 d . . . H16 H 0.041(4) 0.452(2) 0.892(2) 0.052(10) Uiso 1 1 d . . . H17 H 0.098(4) 0.394(2) 0.762(2) 0.041(9) Uiso 1 1 d . . . H18 H 0.307(3) 0.356(2) 0.735(2) 0.035(8) Uiso 1 1 d . . . H20 H 0.468(4) 0.428(2) 0.674(2) 0.055(10) Uiso 1 1 d . . . H21 H 0.589(4) 0.509(3) 0.581(3) 0.064(11) Uiso 1 1 d . . . H22 H 0.796(4) 0.566(2) 0.622(2) 0.051(10) Uiso 1 1 d . . . H23 H 0.898(4) 0.537(2) 0.756(2) 0.048(9) Uiso 1 1 d . . . H24 H 0.787(4) 0.452(2) 0.848(2) 0.056(10) Uiso 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 Mo1 0.02462(12) 0.04185(14) 0.01817(11) -0.00081(8) -0.00285(8) 0.00389(9) Cl1 0.0440(4) 0.0549(5) 0.0310(3) 0.0105(3) -0.0025(3) 0.0146(3) O1 0.0283(9) 0.0342(9) 0.0229(8) -0.0020(7) -0.0050(6) 0.0023(7) O2 0.0341(10) 0.0622(13) 0.0219(8) -0.0038(8) 0.0011(7) 0.0031(9) O3 0.0302(10) 0.0539(12) 0.0316(9) -0.0035(8) -0.0064(7) 0.0014(9) N1 0.0263(10) 0.0319(11) 0.0194(9) -0.0003(8) 0.0003(7) 0.0020(8) N2 0.0235(10) 0.0366(12) 0.0229(9) 0.0022(8) 0.0008(7) 0.0037(9) N3 0.0250(10) 0.0296(11) 0.0201(9) 0.0006(7) -0.0016(7) 0.0012(8) N4 0.0294(11) 0.0350(11) 0.0186(9) 0.0020(8) -0.0002(8) 0.0034(8) C1 0.0229(11) 0.0291(12) 0.0216(10) -0.0004(9) -0.0019(8) 0.0001(9) C2 0.0248(11) 0.0303(12) 0.0181(10) 0.0004(8) -0.0030(8) 0.0015(9) C3 0.0460(18) 0.061(2) 0.0247(13) -0.0044(13) 0.0045(12) -0.0003(17) C4 0.0358(14) 0.0358(14) 0.0258(12) -0.0007(10) 0.0085(10) -0.0006(11) C5 0.0319(14) 0.0466(16) 0.0303(13) 0.0022(11) 0.0106(11) 0.0021(12) C6 0.0269(12) 0.0368(14) 0.0326(13) 0.0049(10) 0.0053(10) 0.0013(10) C7 0.0274(14) 0.062(2) 0.0429(17) 0.0060(15) 0.0048(12) 0.0062(14) C8 0.0377(15) 0.0378(16) 0.0352(14) -0.0011(11) -0.0064(12) -0.0066(13) C9 0.0227(11) 0.0301(13) 0.0319(12) -0.0007(10) -0.0006(9) 0.0036(10) C10 0.0261(12) 0.0329(14) 0.0402(14) 0.0064(11) 0.0031(10) 0.0008(10) C11 0.0273(12) 0.0358(14) 0.0311(12) 0.0070(10) 0.0066(10) 0.0045(10) C12 0.0471(19) 0.053(2) 0.0325(15) 0.0141(14) 0.0074(13) -0.0019(16) C13 0.0261(12) 0.0252(12) 0.0290(11) 0.0022(9) 0.0007(9) 0.0013(9) C14 0.0333(14) 0.0394(15) 0.0331(13) -0.0056(11) -0.0003(11) 0.0000(11) C15 0.0421(16) 0.0465(17) 0.0412(16) -0.0080(13) 0.0125(13) 0.0046(13) C16 0.0283(14) 0.0477(18) 0.0565(18) 0.0000(14) 0.0073(13) 0.0069(12) C17 0.0265(13) 0.0482(17) 0.0480(17) -0.0002(13) -0.0081(12) 0.0015(12) C18 0.0308(13) 0.0362(14) 0.0320(13) -0.0029(11) 0.0003(10) -0.0004(11) C19 0.0274(12) 0.0285(12) 0.0275(11) -0.0006(9) 0.0006(9) -0.0003(10) C20 0.0405(16) 0.0457(17) 0.0351(14) 0.0083(12) -0.0067(12) -0.0145(13) C21 0.0538(19) 0.0484(18) 0.0335(15) 0.0115(13) -0.0022(13) -0.0099(14) C22 0.0443(16) 0.0304(14) 0.0471(16) 0.0040(12) 0.0155(13) -0.0038(12) C23 0.0279(14) 0.0422(16) 0.0573(18) 0.0020(13) 0.0057(12) -0.0055(12) C24 0.0289(13) 0.0413(16) 0.0377(14) 0.0038(11) -0.0031(11) -0.0035(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 Mo1 O2 1.6965(18) . ? Mo1 O3 1.717(2) . ? Mo1 O1 1.9033(17) . ? Mo1 N4 2.343(2) . ? Mo1 N2 2.3451(19) . ? Mo1 Cl1 2.3825(8) . ? O1 C1 1.402(3) . ? N1 C4 1.360(3) . ? N1 N2 1.369(3) . ? N1 C2 1.451(3) . ? N2 C6 1.337(3) . ? N3 C9 1.353(3) . ? N3 N4 1.371(3) . ? N3 C2 1.449(3) . ? N4 C11 1.332(3) . ? C1 C13 1.534(3) . ? C1 C19 1.539(3) . ? C1 C2 1.558(3) . ? C2 H2 0.88(3) . ? C3 C4 1.487(4) . ? C3 H3A 0.92(4) . ? C3 H3B 0.85(4) . ? C3 H3C 0.89(4) . ? C4 C5 1.370(4) . ? C5 C6 1.396(4) . ? C5 H5 0.91(4) . ? C6 C7 1.487(4) . ? C7 H7A 0.83(5) . ? C7 H7B 0.91(5) . ? C7 H7C 0.87(4) . ? C8 C9 1.484(4) . ? C8 H8A 0.92(4) . ? C8 H8B 0.89(4) . ? C8 H8C 0.92(3) . ? C9 C10 1.373(4) . ? C10 C11 1.400(4) . ? C10 H10 1.01(3) . ? C11 C12 1.494(4) . ? C12 H12A 0.88(5) . ? C12 H12B 0.90(5) . ? C12 H12C 0.87(5) . ? C13 C18 1.391(4) . ? C13 C14 1.391(4) . ? C14 C15 1.387(4) . ? C14 H14 0.88(3) . ? C15 C16 1.366(5) . ? C15 H15 0.82(3) . ? C16 C17 1.376(4) . ? C16 H16 0.94(4) . ? C17 C18 1.386(4) . ? C17 H17 0.83(3) . ? C18 H18 0.88(3) . ? C19 C24 1.382(4) . ? C19 C20 1.387(4) . ? C20 C21 1.390(4) . ? C20 H20 0.97(4) . ? C21 C22 1.361(5) . ? C21 H21 0.88(4) . ? C22 C23 1.376(5) . ? C22 H22 0.86(4) . ? C23 C24 1.388(4) . ? C23 H23 0.90(4) . ? C24 H24 0.89(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 O2 Mo1 O3 105.13(10) . . ? O2 Mo1 O1 100.13(9) . . ? O3 Mo1 O1 99.80(9) . . ? O2 Mo1 N4 88.05(9) . . ? O3 Mo1 N4 166.67(8) . . ? O1 Mo1 N4 79.40(7) . . ? O2 Mo1 N2 164.08(9) . . ? O3 Mo1 N2 90.77(8) . . ? O1 Mo1 N2 77.49(7) . . ? N4 Mo1 N2 76.03(7) . . ? O2 Mo1 Cl1 94.87(7) . . ? O3 Mo1 Cl1 93.81(7) . . ? O1 Mo1 Cl1 156.29(5) . . ? N4 Mo1 Cl1 82.89(5) . . ? N2 Mo1 Cl1 83.04(5) . . ? C1 O1 Mo1 137.68(15) . . ? C4 N1 N2 111.6(2) . . ? C4 N1 C2 129.5(2) . . ? N2 N1 C2 118.98(18) . . ? C6 N2 N1 105.52(19) . . ? C6 N2 Mo1 134.44(17) . . ? N1 N2 Mo1 119.70(14) . . ? C9 N3 N4 111.67(19) . . ? C9 N3 C2 129.6(2) . . ? N4 N3 C2 118.7(2) . . ? C11 N4 N3 105.4(2) . . ? C11 N4 Mo1 134.61(17) . . ? N3 N4 Mo1 119.98(15) . . ? O1 C1 C13 108.43(18) . . ? O1 C1 C19 107.67(19) . . ? C13 C1 C19 113.9(2) . . ? O1 C1 C2 108.99(19) . . ? C13 C1 C2 110.18(19) . . ? C19 C1 C2 107.53(18) . . ? N3 C2 N1 109.62(19) . . ? N3 C2 C1 112.08(18) . . ? N1 C2 C1 111.0(2) . . ? N3 C2 H2 107.6(17) . . ? N1 C2 H2 106.5(16) . . ? C1 C2 H2 109.8(16) . . ? C4 C3 H3A 113(2) . . ? C4 C3 H3B 111(3) . . ? H3A C3 H3B 113(4) . . ? C4 C3 H3C 115(3) . . ? H3A C3 H3C 106(3) . . ? H3B C3 H3C 98(3) . . ? N1 C4 C5 105.8(2) . . ? N1 C4 C3 123.2(2) . . ? C5 C4 C3 131.0(2) . . ? C4 C5 C6 107.2(2) . . ? C4 C5 H5 123(2) . . ? C6 C5 H5 129(2) . . ? N2 C6 C5 109.8(2) . . ? N2 C6 C7 122.1(2) . . ? C5 C6 C7 128.1(3) . . ? C6 C7 H7A 107(3) . . ? C6 C7 H7B 112(3) . . ? H7A C7 H7B 112(4) . . ? C6 C7 H7C 115(3) . . ? H7A C7 H7C 107(4) . . ? H7B C7 H7C 105(4) . . ? C9 C8 H8A 105(2) . . ? C9 C8 H8B 109(2) . . ? H8A C8 H8B 115(3) . . ? C9 C8 H8C 112(2) . . ? H8A C8 H8C 103(3) . . ? H8B C8 H8C 113(3) . . ? N3 C9 C10 106.1(2) . . ? N3 C9 C8 123.7(2) . . ? C10 C9 C8 130.2(3) . . ? C9 C10 C11 106.7(2) . . ? C9 C10 H10 125.6(16) . . ? C11 C10 H10 127.8(16) . . ? N4 C11 C10 110.2(2) . . ? N4 C11 C12 122.3(3) . . ? C10 C11 C12 127.5(3) . . ? C11 C12 H12A 111(3) . . ? C11 C12 H12B 105(3) . . ? H12A C12 H12B 110(4) . . ? C11 C12 H12C 110(3) . . ? H12A C12 H12C 104(4) . . ? H12B C12 H12C 116(4) . . ? C18 C13 C14 118.5(2) . . ? C18 C13 C1 122.8(2) . . ? C14 C13 C1 118.7(2) . . ? C15 C14 C13 120.2(3) . . ? C15 C14 H14 120(2) . . ? C13 C14 H14 120(2) . . ? C16 C15 C14 121.0(3) . . ? C16 C15 H15 118(2) . . ? C14 C15 H15 121(2) . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16 119(2) . . ? C17 C16 H16 122(2) . . ? C16 C17 C18 120.6(3) . . ? C16 C17 H17 120(2) . . ? C18 C17 H17 120(2) . . ? C17 C18 C13 120.4(3) . . ? C17 C18 H18 117(2) . . ? C13 C18 H18 122(2) . . ? C24 C19 C20 118.1(2) . . ? C24 C19 C1 119.8(2) . . ? C20 C19 C1 121.9(2) . . ? C19 C20 C21 120.3(3) . . ? C19 C20 H20 118(2) . . ? C21 C20 H20 121(2) . . ? C22 C21 C20 121.1(3) . . ? C22 C21 H21 122(3) . . ? C20 C21 H21 117(3) . . ? C21 C22 C23 119.2(3) . . ? C21 C22 H22 120(2) . . ? C23 C22 H22 121(2) . . ? C22 C23 C24 120.3(3) . . ? C22 C23 H23 121(2) . . ? C24 C23 H23 119(2) . . ? C19 C24 C23 121.0(3) . . ? C19 C24 H24 119(2) . . ? C23 C24 H24 120(2) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.19 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.199 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.075 data_sdsu8_Compound_5 _database_code_depnum_ccdc_archive 'CCDC 246849' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H39 Cl2 Mo N6 O4' _chemical_formula_weight 714.51 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7513(6) _cell_length_b 13.6366(9) _cell_length_c 14.8639(10) _cell_angle_alpha 72.0210(10) _cell_angle_beta 73.2200(10) _cell_angle_gamma 80.7560(10) _cell_volume 1610.38(19) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8606 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.20 _exptl_crystal_description Block _exptl_crystal_colour Blue/Purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.629 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 11908 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.20 _reflns_number_total 7285 _reflns_number_gt 6762 _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^)+(0.0723P)^2^+7.2001P] 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 7285 _refine_ls_number_parameters 396 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.1968 _refine_ls_wR_factor_gt 0.1935 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 Mo1 Mo 0.60605(5) 0.89056(3) 0.26657(4) 0.03853(16) Uani 1 1 d . . . Cl1 Cl 0.49834(18) 0.99028(12) 0.13850(11) 0.0504(3) Uani 1 1 d . . . Cl2 Cl 0.36585(18) 0.83172(13) 0.36468(13) 0.0578(4) Uani 1 1 d . . . O1 O 0.6564(4) 0.7703(2) 0.2172(2) 0.0298(7) Uani 1 1 d . . . O2 O 0.6022(5) 1.0070(4) 0.3199(3) 0.0569(13) Uani 1 1 d . . . N1 N 0.9676(4) 0.8335(3) 0.1761(3) 0.0272(7) Uani 1 1 d . . . N2 N 0.8554(4) 0.9166(3) 0.1782(3) 0.0286(8) Uani 1 1 d . . . N3 N 0.8736(4) 0.7285(3) 0.3374(3) 0.0294(8) Uani 1 1 d . . . N4 N 0.7395(4) 0.7882(3) 0.3706(3) 0.0300(8) Uani 1 1 d . . . C1 C 0.9232(5) 0.7308(3) 0.2344(3) 0.0260(8) Uani 1 1 d . . . H1A H 1.0181 0.6812 0.2242 0.031 Uiso 1 1 calc R . . C2 C 0.7860(5) 0.6978(3) 0.2045(3) 0.0253(8) Uani 1 1 d . . . C3 C 0.8374(5) 0.6974(3) 0.0971(3) 0.0275(9) Uani 1 1 d . . . C4 C 0.9708(6) 0.6371(4) 0.0594(4) 0.0354(10) Uani 1 1 d . . . H4A H 1.0377 0.5986 0.0996 0.042 Uiso 1 1 calc R . . C5 C 1.0053(7) 0.6335(4) -0.0360(4) 0.0417(12) Uani 1 1 d . . . H5A H 1.0951 0.5921 -0.0599 0.050 Uiso 1 1 calc R . . C6 C 0.9103(7) 0.6896(4) -0.0968(4) 0.0430(12) Uani 1 1 d . . . H6A H 0.9341 0.6861 -0.1616 0.052 Uiso 1 1 calc R . . C7 C 0.7796(7) 0.7511(4) -0.0613(4) 0.0424(12) Uani 1 1 d . . . H7A H 0.7148 0.7904 -0.1024 0.051 Uiso 1 1 calc R . . C8 C 0.7433(6) 0.7553(4) 0.0348(4) 0.0346(10) Uani 1 1 d . . . H8A H 0.6543 0.7977 0.0580 0.041 Uiso 1 1 calc R . . C9 C 0.7388(5) 0.5913(3) 0.2730(3) 0.0286(9) Uani 1 1 d . . . C10 C 0.8525(6) 0.5078(4) 0.2875(4) 0.0380(11) Uani 1 1 d . . . H10A H 0.9608 0.5160 0.2544 0.046 Uiso 1 1 calc R . . C11 C 0.8064(7) 0.4126(4) 0.3507(5) 0.0484(14) Uani 1 1 d . . . H11A H 0.8838 0.3568 0.3610 0.058 Uiso 1 1 calc R . . C12 C 0.6477(8) 0.3997(5) 0.3984(5) 0.0550(16) Uani 1 1 d . . . H12A H 0.6167 0.3355 0.4418 0.066 Uiso 1 1 calc R . . C13 C 0.5344(8) 0.4814(5) 0.3824(5) 0.0584(17) Uani 1 1 d . . . H13A H 0.4257 0.4722 0.4137 0.070 Uiso 1 1 calc R . . C14 C 0.5794(6) 0.5771(4) 0.3204(4) 0.0438(12) Uani 1 1 d . . . H14A H 0.5014 0.6326 0.3105 0.053 Uiso 1 1 calc R . . C15 C 1.2637(6) 0.7942(4) 0.1180(4) 0.0434(12) Uani 1 1 d . . . H15A H 1.2354 0.7234 0.1490 0.065 Uiso 1 1 calc R . . H15B H 1.3375 0.8095 0.1487 0.065 Uiso 1 1 calc R . . H15C H 1.3142 0.8027 0.0490 0.065 Uiso 1 1 calc R . . C16 C 1.1163(5) 0.8661(4) 0.1293(4) 0.0332(10) Uani 1 1 d . . . C17 C 1.0981(6) 0.9717(4) 0.0978(4) 0.0390(11) Uani 1 1 d . . . H17A H 1.1797 1.0162 0.0615 0.047 Uiso 1 1 calc R . . C18 C 0.9370(6) 1.0009(4) 0.1294(4) 0.0330(10) Uani 1 1 d . . . C19 C 0.8563(7) 1.1065(4) 0.1171(5) 0.0452(13) Uani 1 1 d . . . H19A H 0.7425 1.1023 0.1472 0.068 Uiso 1 1 calc R . . H19B H 0.8733 1.1421 0.0480 0.068 Uiso 1 1 calc R . . H19C H 0.9004 1.1443 0.1482 0.068 Uiso 1 1 calc R . . C20 C 1.0997(7) 0.6128(5) 0.3949(4) 0.0444(12) Uani 1 1 d . . . H20A H 1.1337 0.6095 0.3277 0.067 Uiso 1 1 calc R . . H20B H 1.0836 0.5437 0.4385 0.067 Uiso 1 1 calc R . . H20C H 1.1813 0.6420 0.4089 0.067 Uiso 1 1 calc R . . C21 C 0.9472(6) 0.6789(4) 0.4096(4) 0.0338(10) Uani 1 1 d . . . C22 C 0.8557(6) 0.7058(4) 0.4918(4) 0.0400(11) Uani 1 1 d . . . H22A H 0.8746 0.6825 0.5544 0.048 Uiso 1 1 calc R . . C23 C 0.7293(6) 0.7740(4) 0.4649(4) 0.0353(10) Uani 1 1 d . . . C24 C 0.6027(7) 0.8299(5) 0.5268(4) 0.0487(14) Uani 1 1 d . . . H24A H 0.5301 0.8718 0.4887 0.073 Uiso 1 1 calc R . . H24B H 0.6520 0.8740 0.5487 0.073 Uiso 1 1 calc R . . H24C H 0.5435 0.7801 0.5830 0.073 Uiso 1 1 calc R . . O1S O 0.2450(5) 0.5331(4) 0.1897(4) 0.0592(11) Uani 1 1 d . . . N1S N 0.4677(5) 0.4263(3) 0.1589(4) 0.0417(10) Uani 1 1 d . . . C1S C 0.3130(6) 0.4469(5) 0.1986(4) 0.0426(12) Uani 1 1 d . . . C2S C 0.5412(9) 0.3209(5) 0.1749(6) 0.0650(18) Uani 1 1 d . . . H2SA H 0.4603 0.2730 0.2138 0.097 Uiso 1 1 calc R . . H2SB H 0.6234 0.3130 0.2092 0.097 Uiso 1 1 calc R . . H2SC H 0.5890 0.3063 0.1124 0.097 Uiso 1 1 calc R . . C3S C 0.5696(7) 0.5099(5) 0.1024(6) 0.0604(17) Uani 1 1 d . . . H3SA H 0.5057 0.5755 0.0968 0.091 Uiso 1 1 calc R . . H3SB H 0.6196 0.5014 0.0376 0.091 Uiso 1 1 calc R . . H3SC H 0.6518 0.5086 0.1348 0.091 Uiso 1 1 calc R . . O2S O 0.8514(6) 0.7893(3) -0.3204(3) 0.0570(11) Uani 1 1 d . . . N2S N 0.9943(6) 0.9274(4) -0.3601(4) 0.0442(10) Uani 1 1 d . . . C4S C 0.8616(7) 0.8790(5) -0.3247(5) 0.0473(13) Uani 1 1 d . . . C5S C 1.1441(9) 0.8761(7) -0.4016(7) 0.079(2) Uani 1 1 d . . . H5SA H 1.1276 0.8056 -0.3960 0.119 Uiso 1 1 calc R . . H5SB H 1.2224 0.8755 -0.3666 0.119 Uiso 1 1 calc R . . H5SC H 1.1828 0.9128 -0.4700 0.119 Uiso 1 1 calc R . . C6S C 1.0013(9) 1.0332(5) -0.3639(6) 0.0638(18) Uani 1 1 d . . . H6SA H 0.8958 1.0611 -0.3349 0.096 Uiso 1 1 calc R . . H6SB H 1.0368 1.0734 -0.4315 0.096 Uiso 1 1 calc R . . H6SC H 1.0759 1.0367 -0.3280 0.096 Uiso 1 1 calc R . . H1SA H 0.260(9) 0.392(6) 0.235(5) 0.06(2) Uiso 1 1 d . . . H1SB H 0.782(9) 0.925(6) -0.306(5) 0.06(2) Uiso 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 Mo1 0.0326(2) 0.0347(2) 0.0457(3) -0.01249(19) -0.01052(18) 0.00814(17) Cl1 0.0484(8) 0.0504(8) 0.0533(8) -0.0101(6) -0.0230(6) 0.0040(6) Cl2 0.0402(7) 0.0617(9) 0.0601(9) -0.0113(7) -0.0032(6) -0.0012(6) O1 0.0222(14) 0.0305(16) 0.0344(17) -0.0067(13) -0.0065(12) -0.0014(12) O2 0.057(2) 0.095(3) 0.0258(17) 0.0040(19) -0.0170(17) -0.057(2) N1 0.0242(17) 0.0247(17) 0.0309(19) -0.0057(14) -0.0060(14) -0.0032(14) N2 0.0253(18) 0.0244(17) 0.036(2) -0.0075(15) -0.0104(15) 0.0017(14) N3 0.0244(18) 0.0323(19) 0.032(2) -0.0076(15) -0.0084(15) -0.0039(15) N4 0.0219(17) 0.0336(19) 0.033(2) -0.0095(16) -0.0039(15) -0.0023(15) C1 0.0210(19) 0.025(2) 0.029(2) -0.0044(16) -0.0050(16) -0.0031(15) C2 0.0210(19) 0.025(2) 0.028(2) -0.0047(16) -0.0054(16) -0.0042(15) C3 0.026(2) 0.024(2) 0.031(2) -0.0051(17) -0.0060(17) -0.0069(16) C4 0.034(2) 0.031(2) 0.037(3) -0.0080(19) -0.007(2) -0.0010(19) C5 0.042(3) 0.035(3) 0.044(3) -0.015(2) 0.000(2) -0.005(2) C6 0.050(3) 0.048(3) 0.033(3) -0.013(2) -0.006(2) -0.014(2) C7 0.041(3) 0.050(3) 0.037(3) -0.006(2) -0.015(2) -0.008(2) C8 0.028(2) 0.038(2) 0.036(2) -0.007(2) -0.0103(19) -0.0027(19) C9 0.027(2) 0.028(2) 0.030(2) -0.0046(17) -0.0069(17) -0.0076(17) C10 0.032(2) 0.030(2) 0.049(3) -0.002(2) -0.014(2) -0.0061(19) C11 0.051(3) 0.032(3) 0.060(4) 0.002(2) -0.026(3) -0.007(2) C12 0.063(4) 0.037(3) 0.054(4) 0.009(3) -0.010(3) -0.022(3) C13 0.042(3) 0.048(3) 0.065(4) 0.002(3) 0.007(3) -0.020(3) C14 0.034(3) 0.038(3) 0.050(3) -0.005(2) 0.001(2) -0.008(2) C15 0.021(2) 0.042(3) 0.058(3) -0.007(2) -0.001(2) -0.006(2) C16 0.024(2) 0.034(2) 0.040(3) -0.0071(19) -0.0059(18) -0.0065(18) C17 0.031(2) 0.034(2) 0.046(3) -0.004(2) -0.002(2) -0.0128(19) C18 0.035(2) 0.027(2) 0.035(2) -0.0053(18) -0.0078(19) -0.0070(18) C19 0.045(3) 0.028(2) 0.055(3) -0.004(2) -0.007(2) -0.005(2) C20 0.039(3) 0.049(3) 0.047(3) -0.009(2) -0.022(2) 0.007(2) C21 0.034(2) 0.033(2) 0.035(2) -0.0032(19) -0.016(2) -0.0049(19) C22 0.040(3) 0.048(3) 0.032(2) -0.004(2) -0.016(2) -0.005(2) C23 0.032(2) 0.042(3) 0.032(2) -0.008(2) -0.0076(19) -0.006(2) C24 0.037(3) 0.071(4) 0.037(3) -0.021(3) -0.005(2) 0.002(3) O1S 0.035(2) 0.058(3) 0.083(3) -0.021(2) -0.015(2) 0.0036(19) N1S 0.034(2) 0.038(2) 0.049(3) -0.011(2) -0.0070(19) -0.0048(18) C1S 0.032(3) 0.051(3) 0.046(3) -0.012(3) -0.008(2) -0.010(2) C2S 0.057(4) 0.052(4) 0.080(5) -0.019(3) -0.017(4) 0.011(3) C3S 0.036(3) 0.060(4) 0.083(5) -0.018(3) -0.006(3) -0.017(3) O2S 0.069(3) 0.052(2) 0.053(3) -0.006(2) -0.020(2) -0.019(2) N2S 0.045(3) 0.044(2) 0.046(3) -0.016(2) -0.011(2) -0.005(2) C4S 0.043(3) 0.054(3) 0.047(3) -0.014(3) -0.015(3) -0.003(3) C5S 0.054(4) 0.079(5) 0.105(7) -0.048(5) 0.005(4) -0.008(4) C6S 0.067(4) 0.048(3) 0.087(5) -0.020(3) -0.037(4) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.935(3) . ? Mo1 O2 1.974(5) . ? Mo1 N4 2.211(4) . ? Mo1 N2 2.219(4) . ? Mo1 Cl2 2.2888(16) . ? Mo1 Cl1 2.3212(15) . ? O1 C2 1.390(5) . ? N1 C16 1.359(6) . ? N1 N2 1.377(5) . ? N1 C1 1.448(5) . ? N2 C18 1.344(6) . ? N3 C21 1.354(6) . ? N3 N4 1.375(5) . ? N3 C1 1.458(6) . ? N4 C23 1.333(6) . ? C1 C2 1.564(6) . ? C2 C3 1.529(6) . ? C2 C9 1.535(6) . ? C3 C8 1.393(6) . ? C3 C4 1.397(6) . ? C4 C5 1.376(7) . ? C5 C6 1.378(8) . ? C6 C7 1.381(8) . ? C7 C8 1.387(7) . ? C9 C14 1.384(7) . ? C9 C10 1.393(7) . ? C10 C11 1.388(7) . ? C11 C12 1.377(9) . ? C12 C13 1.378(9) . ? C13 C14 1.385(8) . ? C15 C16 1.492(7) . ? C16 C17 1.368(7) . ? C17 C18 1.385(7) . ? C18 C19 1.481(7) . ? C20 C21 1.486(7) . ? C21 C22 1.373(7) . ? C22 C23 1.394(7) . ? C23 C24 1.492(7) . ? O1S C1S 1.216(7) . ? N1S C1S 1.334(7) . ? N1S C3S 1.450(7) . ? N1S C2S 1.455(8) . ? O2S C4S 1.222(8) . ? N2S C4S 1.319(8) . ? N2S C6S 1.437(8) . ? N2S C5S 1.447(8) . ? 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 O1 Mo1 O2 167.70(16) . . ? O1 Mo1 N4 79.96(14) . . ? O2 Mo1 N4 90.76(16) . . ? O1 Mo1 N2 79.96(13) . . ? O2 Mo1 N2 90.52(15) . . ? N4 Mo1 N2 79.86(14) . . ? O1 Mo1 Cl2 91.41(10) . . ? O2 Mo1 Cl2 97.08(12) . . ? N4 Mo1 Cl2 92.45(11) . . ? N2 Mo1 Cl2 169.28(10) . . ? O1 Mo1 Cl1 93.71(10) . . ? O2 Mo1 Cl1 94.53(13) . . ? N4 Mo1 Cl1 170.99(11) . . ? N2 Mo1 Cl1 92.80(11) . . ? Cl2 Mo1 Cl1 94.12(6) . . ? C2 O1 Mo1 136.4(3) . . ? C16 N1 N2 110.6(4) . . ? C16 N1 C1 128.6(4) . . ? N2 N1 C1 119.7(3) . . ? C18 N2 N1 105.6(4) . . ? C18 N2 Mo1 134.5(3) . . ? N1 N2 Mo1 119.5(3) . . ? C21 N3 N4 111.1(4) . . ? C21 N3 C1 129.2(4) . . ? N4 N3 C1 119.5(4) . . ? C23 N4 N3 105.8(4) . . ? C23 N4 Mo1 134.2(3) . . ? N3 N4 Mo1 119.8(3) . . ? N1 C1 N3 109.0(4) . . ? N1 C1 C2 111.5(3) . . ? N3 C1 C2 110.4(3) . . ? O1 C2 C3 108.8(3) . . ? O1 C2 C9 109.3(3) . . ? C3 C2 C9 111.8(3) . . ? O1 C2 C1 107.2(3) . . ? C3 C2 C1 111.0(3) . . ? C9 C2 C1 108.5(3) . . ? C8 C3 C4 118.1(4) . . ? C8 C3 C2 119.0(4) . . ? C4 C3 C2 122.8(4) . . ? C5 C4 C3 120.6(5) . . ? C4 C5 C6 121.0(5) . . ? C5 C6 C7 119.1(5) . . ? C6 C7 C8 120.5(5) . . ? C7 C8 C3 120.7(5) . . ? C14 C9 C10 119.1(4) . . ? C14 C9 C2 119.4(4) . . ? C10 C9 C2 121.5(4) . . ? C11 C10 C9 120.2(5) . . ? C12 C11 C10 120.2(5) . . ? C13 C12 C11 119.7(5) . . ? C12 C13 C14 120.5(5) . . ? C9 C14 C13 120.3(5) . . ? N1 C16 C17 106.6(4) . . ? N1 C16 C15 123.3(4) . . ? C17 C16 C15 130.2(4) . . ? C16 C17 C18 107.3(4) . . ? N2 C18 C17 109.9(4) . . ? N2 C18 C19 121.5(4) . . ? C17 C18 C19 128.5(4) . . ? N3 C21 C22 106.1(4) . . ? N3 C21 C20 123.7(5) . . ? C22 C21 C20 130.2(5) . . ? C21 C22 C23 107.1(4) . . ? N4 C23 C22 109.8(4) . . ? N4 C23 C24 122.4(5) . . ? C22 C23 C24 127.7(5) . . ? C1S N1S C3S 120.3(5) . . ? C1S N1S C2S 121.6(5) . . ? C3S N1S C2S 118.0(5) . . ? O1S C1S N1S 125.0(6) . . ? C4S N2S C6S 123.8(6) . . ? C4S N2S C5S 120.8(6) . . ? C6S N2S C5S 115.4(6) . . ? O2S C4S N2S 125.5(6) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 2.845 _refine_diff_density_min -1.515 _refine_diff_density_rms 0.122 # Attachment 'Justin103.cif' data_justin103_Compound_7 _database_code_depnum_ccdc_archive 'CCDC 603447' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Cl3 Mo N5 O2' _chemical_formula_weight 696.90 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3441(11) _cell_length_b 15.8510(14) _cell_length_c 15.9522(15) _cell_angle_alpha 93.312(4) _cell_angle_beta 91.687(4) _cell_angle_gamma 93.927(4) _cell_volume 3107.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8231 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.17 _exptl_crystal_description rod _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type SADABS-multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 57348 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 28.46 _reflns_number_total 15147 _reflns_number_gt 9868 _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^)+(0.0733P)^2^+2.0491P] 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 15147 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.72772(2) 0.20613(2) 0.567869(18) 0.02592(9) Uani 1 1 d . . . Cl1 Cl 0.57494(8) 0.18436(7) 0.65955(6) 0.0443(3) Uani 1 1 d . . . O1 O 0.8298(2) 0.24305(16) 0.63669(15) 0.0337(6) Uani 1 1 d . . . O2 O 0.62597(19) 0.17821(14) 0.46711(14) 0.0262(5) Uani 1 1 d . . . N2 N 0.8407(2) 0.22043(18) 0.46370(17) 0.0257(6) Uani 1 1 d . . . N1 N 0.8095(2) 0.26524(18) 0.39705(18) 0.0263(6) Uani 1 1 d . . . N4 N 0.6872(2) 0.33454(18) 0.53952(17) 0.0267(6) Uani 1 1 d . . . N3 N 0.6839(2) 0.35620(17) 0.45760(17) 0.0257(6) Uani 1 1 d . . . N5 N 0.7448(2) 0.07322(19) 0.58262(19) 0.0311(7) Uani 1 1 d . . . C1 C 0.8855(3) 0.3258(3) 0.2669(2) 0.0441(10) Uani 1 1 d . . . H1B H 0.8132 0.3437 0.2605 0.066 Uiso 1 1 calc R . . H1C H 0.9011 0.2893 0.2194 0.066 Uiso 1 1 calc R . . H1D H 0.9366 0.3745 0.2707 0.066 Uiso 1 1 calc R . . C2 C 0.8946(3) 0.2788(2) 0.3456(2) 0.0330(9) Uani 1 1 d . . . C3 C 0.9812(3) 0.2418(2) 0.3802(2) 0.0349(9) Uani 1 1 d . . . H3A H 1.0506 0.2407 0.3591 0.042 Uiso 1 1 calc R . . C4 C 0.9452(3) 0.2063(2) 0.4529(2) 0.0319(8) Uani 1 1 d . . . C5 C 1.0072(3) 0.1581(3) 0.5133(3) 0.0485(11) Uani 1 1 d . . . H5A H 0.9608 0.1413 0.5576 0.073 Uiso 1 1 calc R . . H5B H 1.0683 0.1933 0.5367 0.073 Uiso 1 1 calc R . . H5C H 1.0323 0.1086 0.4845 0.073 Uiso 1 1 calc R . . C6 C 0.6338(4) 0.4757(3) 0.3696(3) 0.0443(10) Uani 1 1 d . . . H6A H 0.6516 0.4371 0.3243 0.066 Uiso 1 1 calc R . . H6B H 0.6808 0.5265 0.3696 0.066 Uiso 1 1 calc R . . H6C H 0.5597 0.4893 0.3625 0.066 Uiso 1 1 calc R . . C7 C 0.6485(3) 0.4353(2) 0.4514(2) 0.0323(8) Uani 1 1 d . . . C8 C 0.6327(3) 0.4656(2) 0.5315(3) 0.0387(10) Uani 1 1 d . . . H8A H 0.6100 0.5187 0.5476 0.046 Uiso 1 1 calc R . . C9 C 0.6568(3) 0.4024(2) 0.5849(2) 0.0340(9) Uani 1 1 d . . . C10 C 0.6550(4) 0.4048(3) 0.6783(3) 0.0498(11) Uani 1 1 d . . . H10A H 0.6752 0.3516 0.6974 0.075 Uiso 1 1 calc R . . H10B H 0.5832 0.4150 0.6960 0.075 Uiso 1 1 calc R . . H10C H 0.7054 0.4495 0.7015 0.075 Uiso 1 1 calc R . . C11 C 0.7006(3) 0.2928(2) 0.3907(2) 0.0259(8) Uani 1 1 d . . . H11A H 0.6926 0.3192 0.3371 0.031 Uiso 1 1 calc R . . C12 C 0.6119(3) 0.2172(2) 0.3917(2) 0.0260(8) Uani 1 1 d . . . C13 C 0.5003(3) 0.2555(2) 0.3896(2) 0.0259(8) Uani 1 1 d . . . C14 C 0.4478(3) 0.2690(2) 0.4648(2) 0.0327(8) Uani 1 1 d . . . H14A H 0.4793 0.2535 0.5147 0.039 Uiso 1 1 calc R . . C15 C 0.3481(3) 0.3055(2) 0.4656(3) 0.0385(9) Uani 1 1 d . . . H15A H 0.3133 0.3137 0.5160 0.046 Uiso 1 1 calc R . . C16 C 0.3009(3) 0.3297(2) 0.3921(3) 0.0376(9) Uani 1 1 d . . . H16A H 0.2343 0.3537 0.3930 0.045 Uiso 1 1 calc R . . C17 C 0.3524(3) 0.3182(2) 0.3177(3) 0.0387(10) Uani 1 1 d . . . H17A H 0.3212 0.3350 0.2682 0.046 Uiso 1 1 calc R . . C18 C 0.4520(3) 0.2812(2) 0.3165(2) 0.0317(8) Uani 1 1 d . . . H18A H 0.4866 0.2737 0.2659 0.038 Uiso 1 1 calc R . . C19 C 0.6245(3) 0.1536(2) 0.3166(2) 0.0284(8) Uani 1 1 d . . . C20 C 0.6086(3) 0.0672(3) 0.3271(3) 0.0427(10) Uani 1 1 d . . . H20A H 0.5903 0.0490 0.3796 0.051 Uiso 1 1 calc R . . C21 C 0.6192(4) 0.0080(3) 0.2615(3) 0.0563(13) Uani 1 1 d . . . H21A H 0.6066 -0.0494 0.2699 0.068 Uiso 1 1 calc R . . C22 C 0.6487(4) 0.0335(3) 0.1834(3) 0.0538(12) Uani 1 1 d . . . H22A H 0.6578 -0.0063 0.1395 0.065 Uiso 1 1 calc R . . C23 C 0.6641(4) 0.1182(3) 0.1717(3) 0.0473(11) Uani 1 1 d . . . H23A H 0.6826 0.1359 0.1191 0.057 Uiso 1 1 calc R . . C24 C 0.6525(3) 0.1779(3) 0.2369(2) 0.0383(9) Uani 1 1 d . . . H24A H 0.6636 0.2352 0.2275 0.046 Uiso 1 1 calc R . . C25 C 0.6698(4) 0.0159(3) 0.5459(3) 0.0621(14) Uani 1 1 d . . . H25A H 0.6156 0.0354 0.5119 0.074 Uiso 1 1 calc R . . C26 C 0.6689(5) -0.0683(3) 0.5557(3) 0.0687(15) Uani 1 1 d . . . H26A H 0.6163 -0.1053 0.5276 0.082 Uiso 1 1 calc R . . C27 C 0.7467(4) -0.0992(3) 0.6077(3) 0.0574(13) Uani 1 1 d . . . H27A H 0.7481 -0.1569 0.6150 0.069 Uiso 1 1 calc R . . C28 C 0.8208(4) -0.0425(3) 0.6476(3) 0.0564(13) Uani 1 1 d . . . H28A H 0.8734 -0.0610 0.6838 0.068 Uiso 1 1 calc R . . C29 C 0.8183(3) 0.0428(3) 0.6346(3) 0.0427(10) Uani 1 1 d . . . H29A H 0.8696 0.0807 0.6629 0.051 Uiso 1 1 calc R . . Mo2 Mo 0.75772(2) -0.231597(19) 0.930709(18) 0.02545(9) Uani 1 1 d . . . Cl2 Cl 0.87673(8) -0.23516(7) 0.81060(6) 0.0394(2) Uani 1 1 d . . . O3 O 0.64235(19) -0.28368(16) 0.88703(15) 0.0323(6) Uani 1 1 d . . . O4 O 0.88119(18) -0.18281(15) 1.00701(14) 0.0276(5) Uani 1 1 d . . . N7 N 0.8401(2) -0.34942(18) 1.06370(18) 0.0278(7) Uani 1 1 d . . . N6 N 0.8132(2) -0.34897(19) 0.97968(18) 0.0284(7) Uani 1 1 d . . . N9 N 0.7246(2) -0.24863(18) 1.12099(17) 0.0278(7) Uani 1 1 d . . . N8 N 0.6772(2) -0.21949(18) 1.05049(17) 0.0269(7) Uani 1 1 d . . . N10 N 0.7244(2) -0.10525(19) 0.89616(18) 0.0285(7) Uani 1 1 d . . . C30 C 0.9089(4) -0.4458(3) 1.1704(3) 0.0538(12) Uani 1 1 d . . . H30A H 0.9062 -0.3959 1.2072 0.081 Uiso 1 1 calc R . . H30B H 0.9821 -0.4627 1.1694 0.081 Uiso 1 1 calc R . . H30C H 0.8622 -0.4907 1.1904 0.081 Uiso 1 1 calc R . . C31 C 0.8719(3) -0.4272(2) 1.0835(3) 0.0378(9) Uani 1 1 d . . . C32 C 0.8619(3) -0.4769(3) 1.0110(3) 0.0415(10) Uani 1 1 d . . . H32A H 0.8761 -0.5338 1.0048 0.050 Uiso 1 1 calc R . . C33 C 0.8264(3) -0.4271(2) 0.9478(2) 0.0358(9) Uani 1 1 d . . . C34 C 0.8024(4) -0.4515(3) 0.8567(3) 0.0489(11) Uani 1 1 d . . . H34A H 0.7800 -0.4032 0.8289 0.073 Uiso 1 1 calc R . . H34B H 0.7453 -0.4959 0.8515 0.073 Uiso 1 1 calc R . . H34C H 0.8665 -0.4710 0.8315 0.073 Uiso 1 1 calc R . . C35 C 0.6789(4) -0.2837(3) 1.2689(3) 0.0543(12) Uani 1 1 d . . . H35A H 0.7526 -0.2995 1.2711 0.081 Uiso 1 1 calc R . . H35B H 0.6306 -0.3323 1.2776 0.081 Uiso 1 1 calc R . . H35C H 0.6695 -0.2402 1.3119 0.081 Uiso 1 1 calc R . . C36 C 0.6538(3) -0.2515(2) 1.1848(2) 0.0345(9) Uani 1 1 d . . . C37 C 0.5595(3) -0.2218(3) 1.1540(2) 0.0374(9) Uani 1 1 d . . . H37A H 0.4961 -0.2157 1.1831 0.045 Uiso 1 1 calc R . . C38 C 0.5763(3) -0.2026(2) 1.0710(2) 0.0319(8) Uani 1 1 d . . . C39 C 0.4998(3) -0.1688(3) 1.0097(3) 0.0447(11) Uani 1 1 d . . . H39A H 0.5349 -0.1619 0.9574 0.067 Uiso 1 1 calc R . . H39B H 0.4781 -0.1149 1.0314 0.067 Uiso 1 1 calc R . . H39C H 0.4368 -0.2076 1.0007 0.067 Uiso 1 1 calc R . . C40 C 0.8361(3) -0.2731(2) 1.1177(2) 0.0285(8) Uani 1 1 d . . . H40A H 0.8596 -0.2858 1.1745 0.034 Uiso 1 1 calc R . . C41 C 0.9161(3) -0.2010(2) 1.0876(2) 0.0270(8) Uani 1 1 d . . . C42 C 0.9190(3) -0.1205(2) 1.1458(2) 0.0341(9) Uani 1 1 d . . . C43 C 0.9554(3) -0.0449(3) 1.1122(3) 0.0442(10) Uani 1 1 d . . . H43A H 0.9764 -0.0457 1.0567 0.053 Uiso 1 1 calc R . . C44 C 0.9609(4) 0.0314(3) 1.1593(4) 0.0655(15) Uani 1 1 d . . . H44A H 0.9871 0.0811 1.1363 0.079 Uiso 1 1 calc R . . C45 C 0.9270(4) 0.0329(3) 1.2410(4) 0.0708(17) Uani 1 1 d . . . H45A H 0.9263 0.0843 1.2720 0.085 Uiso 1 1 calc R . . C46 C 0.8943(4) -0.0405(4) 1.2767(3) 0.0661(15) Uani 1 1 d . . . H46A H 0.8742 -0.0389 1.3324 0.079 Uiso 1 1 calc R . . C47 C 0.8911(4) -0.1183(3) 1.2295(3) 0.0488(11) Uani 1 1 d . . . H47A H 0.8702 -0.1683 1.2544 0.059 Uiso 1 1 calc R . . C48 C 1.0303(3) -0.2349(2) 1.0850(2) 0.0291(8) Uani 1 1 d . . . C49 C 1.0905(3) -0.2458(3) 1.1582(2) 0.0374(9) Uani 1 1 d . . . H49A H 1.0613 -0.2328 1.2101 0.045 Uiso 1 1 calc R . . C50 C 1.1928(3) -0.2758(3) 1.1552(3) 0.0431(10) Uani 1 1 d . . . H50A H 1.2323 -0.2825 1.2046 0.052 Uiso 1 1 calc R . . C51 C 1.2361(3) -0.2956(3) 1.0788(3) 0.0424(10) Uani 1 1 d . . . H51A H 1.3045 -0.3165 1.0764 0.051 Uiso 1 1 calc R . . C52 C 1.1778(3) -0.2845(3) 1.0058(3) 0.0439(10) Uani 1 1 d . . . H52A H 1.2076 -0.2973 0.9541 0.053 Uiso 1 1 calc R . . C53 C 1.0748(3) -0.2541(2) 1.0087(2) 0.0345(9) Uani 1 1 d . . . H53A H 1.0360 -0.2468 0.9590 0.041 Uiso 1 1 calc R . . C54 C 0.6705(4) -0.0931(3) 0.8240(3) 0.0452(11) Uani 1 1 d . . . H54A H 0.6460 -0.1404 0.7897 0.054 Uiso 1 1 calc R . . C55 C 0.6494(4) -0.0145(3) 0.7982(3) 0.0517(12) Uani 1 1 d . . . H55A H 0.6085 -0.0095 0.7491 0.062 Uiso 1 1 calc R . . C56 C 0.6889(4) 0.0561(3) 0.8451(3) 0.0474(11) Uani 1 1 d . . . H56A H 0.6780 0.1100 0.8276 0.057 Uiso 1 1 calc R . . C57 C 0.7451(4) 0.0457(3) 0.9188(3) 0.0493(11) Uani 1 1 d . . . H57A H 0.7726 0.0926 0.9525 0.059 Uiso 1 1 calc R . . C58 C 0.7604(3) -0.0348(3) 0.9423(3) 0.0433(10) Uani 1 1 d . . . H58A H 0.7977 -0.0409 0.9929 0.052 Uiso 1 1 calc R . . Cl6 Cl 0.94020(15) 0.50129(10) 0.62676(11) 0.0918(5) Uani 1 1 d . . . Cl4 Cl 1.35726(14) -0.39912(11) 0.85908(12) 0.0946(5) Uani 1 1 d . . . Cl5 Cl 1.10584(13) 0.38692(14) 0.58829(12) 0.1098(7) Uani 1 1 d . . . Cl3 Cl 1.47390(17) -0.54884(11) 0.87685(13) 0.1089(6) Uani 1 1 d . . . C101 C 0.9687(4) 0.4041(3) 0.5768(3) 0.0638(14) Uani 1 1 d . . . H10D H 0.9257 0.3586 0.6008 0.077 Uiso 1 1 calc R . . H10E H 0.9487 0.4039 0.5175 0.077 Uiso 1 1 calc R . . C100 C 1.4738(7) -0.4398(4) 0.8906(6) 0.132(3) Uani 1 1 d . . . H10F H 1.4877 -0.4235 0.9497 0.159 Uiso 1 1 calc R . . H10G H 1.5332 -0.4146 0.8599 0.159 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 0.02833(17) 0.02785(17) 0.02227(17) 0.00221(12) 0.00154(12) 0.00612(13) Cl1 0.0432(6) 0.0570(7) 0.0360(6) 0.0127(5) 0.0160(4) 0.0120(5) O1 0.0364(14) 0.0379(15) 0.0270(14) 0.0019(11) -0.0030(11) 0.0058(12) O2 0.0293(13) 0.0229(12) 0.0265(13) 0.0032(10) -0.0001(10) 0.0016(10) N2 0.0274(16) 0.0270(16) 0.0238(15) 0.0052(12) 0.0029(12) 0.0047(13) N1 0.0278(16) 0.0270(16) 0.0245(15) 0.0032(12) 0.0053(12) 0.0029(13) N4 0.0303(16) 0.0274(16) 0.0230(16) -0.0008(12) 0.0024(12) 0.0065(13) N3 0.0304(16) 0.0232(15) 0.0238(16) 0.0021(12) -0.0012(12) 0.0036(13) N5 0.0365(18) 0.0282(16) 0.0295(17) 0.0050(13) 0.0027(14) 0.0050(14) C1 0.040(2) 0.058(3) 0.036(2) 0.016(2) 0.0111(19) 0.005(2) C2 0.037(2) 0.034(2) 0.028(2) 0.0015(16) 0.0059(17) 0.0022(17) C3 0.030(2) 0.042(2) 0.034(2) 0.0027(17) 0.0107(17) 0.0102(18) C4 0.032(2) 0.035(2) 0.029(2) 0.0016(16) 0.0051(16) 0.0074(17) C5 0.037(2) 0.068(3) 0.044(3) 0.013(2) 0.0071(19) 0.022(2) C6 0.055(3) 0.030(2) 0.049(3) 0.0061(19) -0.008(2) 0.0082(19) C7 0.037(2) 0.0256(19) 0.035(2) 0.0008(16) 0.0008(17) 0.0050(16) C8 0.045(2) 0.024(2) 0.047(2) -0.0067(18) -0.0061(19) 0.0109(17) C9 0.038(2) 0.029(2) 0.035(2) -0.0050(17) -0.0007(17) 0.0066(17) C10 0.070(3) 0.041(2) 0.038(2) -0.0118(19) -0.001(2) 0.013(2) C11 0.0262(18) 0.0278(19) 0.0241(18) 0.0009(14) 0.0011(14) 0.0063(15) C12 0.0290(18) 0.0251(18) 0.0239(18) 0.0024(14) -0.0017(14) 0.0023(15) C13 0.0268(18) 0.0223(17) 0.0277(19) -0.0031(14) -0.0016(15) 0.0011(14) C14 0.032(2) 0.034(2) 0.031(2) -0.0024(16) -0.0016(16) 0.0064(17) C15 0.033(2) 0.039(2) 0.043(2) -0.0080(18) 0.0039(18) 0.0080(18) C16 0.031(2) 0.032(2) 0.049(3) -0.0038(18) -0.0020(18) 0.0063(17) C17 0.044(2) 0.029(2) 0.042(2) 0.0010(17) -0.0133(19) 0.0016(18) C18 0.033(2) 0.030(2) 0.031(2) -0.0015(16) -0.0046(16) 0.0007(16) C19 0.0253(18) 0.034(2) 0.0257(19) -0.0034(15) -0.0025(14) 0.0056(15) C20 0.052(3) 0.034(2) 0.042(2) -0.0021(18) 0.003(2) 0.0051(19) C21 0.076(3) 0.035(2) 0.057(3) -0.012(2) 0.002(3) 0.009(2) C22 0.053(3) 0.062(3) 0.045(3) -0.023(2) -0.001(2) 0.012(2) C23 0.052(3) 0.063(3) 0.026(2) -0.011(2) 0.0005(18) 0.008(2) C24 0.042(2) 0.040(2) 0.033(2) -0.0021(18) -0.0006(18) 0.0066(19) C25 0.084(4) 0.037(3) 0.064(3) 0.013(2) -0.027(3) -0.006(2) C26 0.096(4) 0.037(3) 0.071(4) 0.008(2) -0.017(3) -0.007(3) C27 0.071(3) 0.027(2) 0.076(4) 0.012(2) 0.009(3) 0.009(2) C28 0.045(3) 0.046(3) 0.083(4) 0.028(3) 0.003(3) 0.015(2) C29 0.037(2) 0.039(2) 0.052(3) 0.010(2) -0.003(2) 0.0043(19) Mo2 0.02610(17) 0.02927(18) 0.02106(16) 0.00037(12) 0.00080(12) 0.00355(13) Cl2 0.0367(5) 0.0534(6) 0.0282(5) 0.0001(4) 0.0089(4) 0.0029(5) O3 0.0303(13) 0.0381(15) 0.0281(14) -0.0023(11) -0.0012(11) 0.0039(11) O4 0.0280(13) 0.0292(13) 0.0255(13) 0.0036(10) -0.0029(10) 0.0014(10) N7 0.0291(16) 0.0275(16) 0.0279(16) 0.0052(13) 0.0033(13) 0.0052(13) N6 0.0295(16) 0.0313(17) 0.0244(16) 0.0005(13) 0.0034(13) 0.0018(13) N9 0.0301(16) 0.0326(17) 0.0213(15) 0.0029(13) 0.0009(12) 0.0060(13) N8 0.0301(16) 0.0306(16) 0.0207(15) 0.0018(12) 0.0015(12) 0.0067(13) N10 0.0276(16) 0.0324(17) 0.0259(16) 0.0038(13) 0.0031(13) 0.0034(13) C30 0.066(3) 0.044(3) 0.055(3) 0.018(2) -0.005(2) 0.014(2) C31 0.037(2) 0.033(2) 0.045(2) 0.0106(18) 0.0023(18) 0.0059(17) C32 0.045(2) 0.026(2) 0.054(3) 0.0012(19) 0.002(2) 0.0092(18) C33 0.037(2) 0.031(2) 0.040(2) -0.0043(17) 0.0012(17) 0.0092(17) C34 0.062(3) 0.041(2) 0.043(3) -0.018(2) -0.004(2) 0.014(2) C35 0.055(3) 0.077(3) 0.034(2) 0.021(2) 0.012(2) 0.016(3) C36 0.037(2) 0.041(2) 0.027(2) 0.0013(17) 0.0070(17) 0.0082(18) C37 0.034(2) 0.048(2) 0.032(2) 0.0029(18) 0.0127(17) 0.0109(18) C38 0.031(2) 0.038(2) 0.027(2) 0.0002(16) 0.0041(16) 0.0061(17) C39 0.032(2) 0.066(3) 0.040(2) 0.009(2) 0.0057(18) 0.019(2) C40 0.0300(19) 0.032(2) 0.0238(18) 0.0001(15) 0.0008(15) 0.0067(16) C41 0.0287(19) 0.0277(19) 0.0244(19) 0.0024(15) -0.0051(15) 0.0025(15) C42 0.031(2) 0.035(2) 0.035(2) -0.0054(17) -0.0083(16) 0.0087(17) C43 0.046(2) 0.033(2) 0.053(3) -0.001(2) -0.012(2) 0.0045(19) C44 0.069(3) 0.038(3) 0.086(4) -0.009(3) -0.031(3) 0.008(2) C45 0.066(3) 0.048(3) 0.094(5) -0.038(3) -0.030(3) 0.021(3) C46 0.061(3) 0.081(4) 0.053(3) -0.033(3) -0.009(2) 0.019(3) C47 0.053(3) 0.046(3) 0.046(3) -0.016(2) -0.006(2) 0.003(2) C48 0.0286(19) 0.0241(18) 0.034(2) 0.0000(15) -0.0003(16) 0.0012(15) C49 0.037(2) 0.042(2) 0.033(2) 0.0047(18) -0.0054(17) 0.0075(18) C50 0.037(2) 0.046(2) 0.048(3) 0.009(2) -0.0128(19) 0.0069(19) C51 0.029(2) 0.040(2) 0.060(3) 0.007(2) -0.001(2) 0.0131(18) C52 0.042(2) 0.041(2) 0.048(3) -0.002(2) 0.011(2) 0.007(2) C53 0.033(2) 0.035(2) 0.035(2) -0.0026(17) -0.0024(17) 0.0046(17) C54 0.059(3) 0.040(2) 0.035(2) 0.0024(19) -0.011(2) 0.003(2) C55 0.059(3) 0.054(3) 0.045(3) 0.010(2) -0.006(2) 0.014(2) C56 0.051(3) 0.040(2) 0.055(3) 0.013(2) 0.008(2) 0.017(2) C57 0.051(3) 0.033(2) 0.064(3) -0.006(2) -0.007(2) 0.011(2) C58 0.050(3) 0.037(2) 0.042(2) -0.0043(19) -0.008(2) 0.014(2) Cl6 0.1018(12) 0.0704(10) 0.1032(12) -0.0044(9) -0.0053(10) 0.0178(9) Cl4 0.0846(11) 0.0921(12) 0.1128(13) 0.0173(10) 0.0337(10) 0.0251(9) Cl5 0.0560(9) 0.1527(17) 0.1171(14) -0.0352(13) -0.0036(9) 0.0201(10) Cl3 0.1299(16) 0.0628(10) 0.1340(16) 0.0021(10) -0.0004(13) 0.0128(10) C101 0.060(3) 0.056(3) 0.073(4) 0.003(3) -0.008(3) -0.011(3) C100 0.160(7) 0.049(4) 0.183(8) 0.025(4) -0.085(6) -0.012(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 Mo1 O1 1.697(2) . ? Mo1 O2 2.020(2) . ? Mo1 N5 2.157(3) . ? Mo1 N4 2.198(3) . ? Mo1 N2 2.212(3) . ? Mo1 Cl1 2.4385(10) . ? O2 C12 1.396(4) . ? N2 C4 1.339(4) . ? N2 N1 1.373(4) . ? N1 C2 1.365(4) . ? N1 C11 1.444(4) . ? N4 C9 1.342(4) . ? N4 N3 1.370(4) . ? N3 C7 1.364(4) . ? N3 C11 1.452(4) . ? N5 C29 1.343(5) . ? N5 C25 1.347(5) . ? C1 C2 1.500(5) . ? C2 C3 1.372(5) . ? C3 C4 1.390(5) . ? C4 C5 1.490(5) . ? C6 C7 1.498(5) . ? C7 C8 1.363(5) . ? C8 C9 1.394(5) . ? C9 C10 1.488(6) . ? C11 C12 1.567(5) . ? C12 C19 1.540(5) . ? C12 C13 1.543(5) . ? C13 C18 1.388(5) . ? C13 C14 1.392(5) . ? C14 C15 1.396(5) . ? C15 C16 1.379(6) . ? C16 C17 1.371(6) . ? C17 C18 1.398(5) . ? C19 C20 1.391(5) . ? C19 C24 1.395(5) . ? C20 C21 1.381(6) . ? C21 C22 1.384(7) . ? C22 C23 1.367(7) . ? C23 C24 1.383(5) . ? C25 C26 1.353(6) . ? C26 C27 1.383(7) . ? C27 C28 1.355(7) . ? C28 C29 1.383(6) . ? Mo2 O3 1.706(2) . ? Mo2 O4 2.006(2) . ? Mo2 N10 2.170(3) . ? Mo2 N8 2.184(3) . ? Mo2 N6 2.203(3) . ? Mo2 Cl2 2.4489(10) . ? O4 C41 1.397(4) . ? N7 C31 1.370(5) . ? N7 N6 1.372(4) . ? N7 C40 1.449(4) . ? N6 C33 1.334(5) . ? N9 C36 1.363(5) . ? N9 N8 1.371(4) . ? N9 C40 1.456(4) . ? N8 C38 1.337(5) . ? N10 C58 1.343(5) . ? N10 C54 1.343(5) . ? C30 C31 1.499(6) . ? C31 C32 1.359(6) . ? C32 C33 1.395(6) . ? C33 C34 1.498(5) . ? C35 C36 1.494(5) . ? C36 C37 1.373(5) . ? C37 C38 1.394(5) . ? C38 C39 1.487(5) . ? C40 C41 1.565(5) . ? C41 C42 1.532(5) . ? C41 C48 1.543(5) . ? C42 C47 1.388(6) . ? C42 C43 1.392(6) . ? C43 C44 1.383(6) . ? C44 C45 1.380(8) . ? C45 C46 1.365(8) . ? C46 C47 1.405(6) . ? C48 C53 1.377(5) . ? C48 C49 1.392(5) . ? C49 C50 1.381(5) . ? C50 C51 1.373(6) . ? C51 C52 1.377(6) . ? C52 C53 1.391(5) . ? C54 C55 1.375(6) . ? C55 C56 1.363(6) . ? C56 C57 1.372(6) . ? C57 C58 1.375(6) . ? Cl6 C101 1.755(5) . ? Cl4 C100 1.692(7) . ? Cl5 C101 1.739(5) . ? Cl3 C100 1.730(6) . ? 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 O1 Mo1 O2 166.70(11) . . ? O1 Mo1 N5 96.69(12) . . ? O2 Mo1 N5 90.73(10) . . ? O1 Mo1 N4 92.65(11) . . ? O2 Mo1 N4 80.25(10) . . ? N5 Mo1 N4 170.63(11) . . ? O1 Mo1 N2 89.27(11) . . ? O2 Mo1 N2 78.85(10) . . ? N5 Mo1 N2 97.00(11) . . ? N4 Mo1 N2 83.82(10) . . ? O1 Mo1 Cl1 102.39(9) . . ? O2 Mo1 Cl1 89.37(7) . . ? N5 Mo1 Cl1 83.52(8) . . ? N4 Mo1 Cl1 93.78(8) . . ? N2 Mo1 Cl1 168.21(8) . . ? C12 O2 Mo1 132.4(2) . . ? C4 N2 N1 106.1(3) . . ? C4 N2 Mo1 134.8(2) . . ? N1 N2 Mo1 118.2(2) . . ? C2 N1 N2 110.2(3) . . ? C2 N1 C11 129.5(3) . . ? N2 N1 C11 120.3(3) . . ? C9 N4 N3 105.7(3) . . ? C9 N4 Mo1 135.0(2) . . ? N3 N4 Mo1 119.2(2) . . ? C7 N3 N4 111.0(3) . . ? C7 N3 C11 128.6(3) . . ? N4 N3 C11 119.7(3) . . ? C29 N5 C25 116.1(4) . . ? C29 N5 Mo1 124.3(3) . . ? C25 N5 Mo1 119.1(3) . . ? N1 C2 C3 106.9(3) . . ? N1 C2 C1 122.8(3) . . ? C3 C2 C1 130.3(3) . . ? C2 C3 C4 106.6(3) . . ? N2 C4 C3 110.2(3) . . ? N2 C4 C5 121.5(3) . . ? C3 C4 C5 128.3(3) . . ? C8 C7 N3 106.2(3) . . ? C8 C7 C6 130.4(3) . . ? N3 C7 C6 123.5(3) . . ? C7 C8 C9 107.5(3) . . ? N4 C9 C8 109.6(3) . . ? N4 C9 C10 121.9(3) . . ? C8 C9 C10 128.5(3) . . ? N1 C11 N3 110.3(3) . . ? N1 C11 C12 112.3(3) . . ? N3 C11 C12 110.5(3) . . ? O2 C12 C19 110.3(3) . . ? O2 C12 C13 109.4(3) . . ? C19 C12 C13 112.1(3) . . ? O2 C12 C11 107.6(3) . . ? C19 C12 C11 110.2(3) . . ? C13 C12 C11 107.1(3) . . ? C18 C13 C14 118.2(3) . . ? C18 C13 C12 122.9(3) . . ? C14 C13 C12 118.8(3) . . ? C13 C14 C15 120.4(4) . . ? C16 C15 C14 120.4(4) . . ? C17 C16 C15 119.9(4) . . ? C16 C17 C18 119.9(4) . . ? C13 C18 C17 121.1(4) . . ? C20 C19 C24 117.1(3) . . ? C20 C19 C12 119.6(3) . . ? C24 C19 C12 123.3(3) . . ? C21 C20 C19 121.5(4) . . ? C20 C21 C22 120.3(4) . . ? C23 C22 C21 119.0(4) . . ? C22 C23 C24 121.0(4) . . ? C23 C24 C19 121.1(4) . . ? N5 C25 C26 123.8(5) . . ? C25 C26 C27 119.5(5) . . ? C28 C27 C26 117.8(4) . . ? C27 C28 C29 120.1(4) . . ? N5 C29 C28 122.6(4) . . ? O3 Mo2 O4 166.31(11) . . ? O3 Mo2 N10 97.60(11) . . ? O4 Mo2 N10 90.16(10) . . ? O3 Mo2 N8 89.28(11) . . ? O4 Mo2 N8 78.91(10) . . ? N10 Mo2 N8 93.95(11) . . ? O3 Mo2 N6 91.79(11) . . ? O4 Mo2 N6 80.23(10) . . ? N10 Mo2 N6 170.38(11) . . ? N8 Mo2 N6 84.03(11) . . ? O3 Mo2 Cl2 100.72(8) . . ? O4 Mo2 Cl2 91.00(7) . . ? N10 Mo2 Cl2 86.15(8) . . ? N8 Mo2 Cl2 169.91(8) . . ? N6 Mo2 Cl2 94.20(8) . . ? C41 O4 Mo2 132.6(2) . . ? C31 N7 N6 110.8(3) . . ? C31 N7 C40 128.9(3) . . ? N6 N7 C40 120.3(3) . . ? C33 N6 N7 105.7(3) . . ? C33 N6 Mo2 135.8(3) . . ? N7 N6 Mo2 118.5(2) . . ? C36 N9 N8 111.0(3) . . ? C36 N9 C40 130.1(3) . . ? N8 N9 C40 118.9(3) . . ? C38 N8 N9 106.1(3) . . ? C38 N8 Mo2 133.1(2) . . ? N9 N8 Mo2 119.6(2) . . ? C58 N10 C54 115.9(3) . . ? C58 N10 Mo2 122.9(3) . . ? C54 N10 Mo2 121.1(3) . . ? C32 C31 N7 106.1(3) . . ? C32 C31 C30 131.1(4) . . ? N7 C31 C30 122.8(4) . . ? C31 C32 C33 107.4(3) . . ? N6 C33 C32 109.9(3) . . ? N6 C33 C34 121.2(4) . . ? C32 C33 C34 128.8(4) . . ? N9 C36 C37 105.9(3) . . ? N9 C36 C35 124.3(3) . . ? C37 C36 C35 129.7(4) . . ? C36 C37 C38 107.4(3) . . ? N8 C38 C37 109.5(3) . . ? N8 C38 C39 121.6(3) . . ? C37 C38 C39 128.9(3) . . ? N7 C40 N9 109.7(3) . . ? N7 C40 C41 110.4(3) . . ? N9 C40 C41 112.6(3) . . ? O4 C41 C42 109.4(3) . . ? O4 C41 C48 110.0(3) . . ? C42 C41 C48 109.9(3) . . ? O4 C41 C40 107.5(3) . . ? C42 C41 C40 112.2(3) . . ? C48 C41 C40 107.7(3) . . ? C47 C42 C43 118.4(4) . . ? C47 C42 C41 124.6(4) . . ? C43 C42 C41 117.0(3) . . ? C44 C43 C42 121.6(5) . . ? C45 C44 C43 119.1(5) . . ? C46 C45 C44 120.6(4) . . ? C45 C46 C47 120.3(5) . . ? C42 C47 C46 119.8(5) . . ? C53 C48 C49 118.8(3) . . ? C53 C48 C41 119.7(3) . . ? C49 C48 C41 121.5(3) . . ? C50 C49 C48 121.1(4) . . ? C51 C50 C49 119.7(4) . . ? C50 C51 C52 119.9(4) . . ? C51 C52 C53 120.6(4) . . ? C48 C53 C52 120.0(4) . . ? N10 C54 C55 123.5(4) . . ? C56 C55 C54 119.5(4) . . ? C55 C56 C57 118.2(4) . . ? C56 C57 C58 119.2(4) . . ? N10 C58 C57 123.5(4) . . ? Cl5 C101 Cl6 111.1(3) . . ? Cl4 C100 Cl3 114.8(4) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.159 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.110 # Attachment 'justin60b.cif' data_justin60b_Compound_4 _database_code_depnum_ccdc_archive 'CCDC 603448' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H27 Cl2 Mo N4 O3.50' _chemical_formula_weight 606.35 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' 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 Pba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 9.5623(6) _cell_length_b 29.6352(18) _cell_length_c 9.4479(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2677.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6202 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.84 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type SADABS-multiscan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 66675 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.11 _reflns_number_total 6132 _reflns_number_gt 4852 _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^)+(0.1016P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(4) _refine_ls_number_reflns 6132 _refine_ls_number_parameters 321 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1294 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _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 0.05169(3) 0.938620(9) 0.68484(5) 0.02281(11) Uani 1 1 d . . . N1 N 0.0225(4) 0.93748(11) 0.9327(5) 0.0250(8) Uani 1 1 d . . . N2 N -0.0714(4) 0.90918(12) 0.9942(4) 0.0273(8) Uani 1 1 d . . . N3 N -0.1893(4) 0.93007(10) 0.7023(5) 0.0286(9) Uani 1 1 d . . . N4 N -0.2469(4) 0.90765(11) 0.8161(4) 0.0303(7) Uani 1 1 d . . . O1 O 0.0320(3) 0.87469(9) 0.7324(3) 0.0275(6) Uani 1 1 d . . . O2 O 0.0390(4) 0.93298(12) 0.5062(5) 0.0357(8) Uani 1 1 d . . . O3 O 0.0000 1.0000 0.7064(5) 0.0282(9) Uani 1 2 d S . . O4 O 0.2263(3) 0.94155(9) 0.7159(3) 0.0331(9) Uani 1 1 d . . . C1 C -0.1498(7) 0.88072(19) 1.2322(6) 0.0549(14) Uani 1 1 d . . . H1A H -0.2162 0.8643 1.1760 0.082 Uiso 1 1 calc R . . H1B H -0.1987 0.9000 1.2972 0.082 Uiso 1 1 calc R . . H1C H -0.0926 0.8599 1.2841 0.082 Uiso 1 1 calc R . . C2 C -0.0594(5) 0.90879(17) 1.1375(5) 0.0372(12) Uani 1 1 d . . . C3 C 0.0481(5) 0.93793(13) 1.1670(8) 0.0345(13) Uani 1 1 d . . . H3B H 0.0824 0.9449 1.2565 0.041 Uiso 1 1 calc R . . C4 C 0.0963(5) 0.95509(16) 1.0405(5) 0.0311(9) Uani 1 1 d . . . C5 C 0.2132(5) 0.98708(15) 1.0149(5) 0.0386(10) Uani 1 1 d . . . H5A H 0.2218 0.9926 0.9151 0.058 Uiso 1 1 calc R . . H5B H 0.2988 0.9743 1.0499 0.058 Uiso 1 1 calc R . . H5C H 0.1947 1.0150 1.0630 0.058 Uiso 1 1 calc R . . C6 C -0.4786(6) 0.8902(3) 0.9280(8) 0.0685(19) Uani 1 1 d . . . H6A H -0.4208 0.8739 0.9936 0.103 Uiso 1 1 calc R . . H6B H -0.5433 0.8698 0.8841 0.103 Uiso 1 1 calc R . . H6C H -0.5293 0.9132 0.9776 0.103 Uiso 1 1 calc R . . C7 C -0.3885(5) 0.91145(16) 0.8168(6) 0.0398(10) Uani 1 1 d . . . C8 C -0.4246(5) 0.93745(14) 0.7023(12) 0.0457(17) Uani 1 1 d . . . H8A H -0.5143 0.9461 0.6756 0.055 Uiso 1 1 calc R . . C9 C -0.3004(5) 0.94825(16) 0.6344(5) 0.0349(11) Uani 1 1 d . . . C10 C -0.2809(6) 0.97484(17) 0.5008(6) 0.0446(12) Uani 1 1 d . . . H10A H -0.1829 0.9770 0.4796 0.067 Uiso 1 1 calc R . . H10B H -0.3189 1.0046 0.5131 0.067 Uiso 1 1 calc R . . H10C H -0.3282 0.9600 0.4244 0.067 Uiso 1 1 calc R . . C11 C -0.1555(5) 0.88028(14) 0.9036(5) 0.0291(9) Uani 1 1 d . . . H11A H -0.2141 0.8612 0.9642 0.035 Uiso 1 1 calc R . . C12 C -0.0592(4) 0.84888(14) 0.8137(5) 0.0259(8) Uani 1 1 d . . . C13 C -0.1513(5) 0.81998(14) 0.7153(5) 0.0330(11) Uani 1 1 d . . . C14 C -0.2724(6) 0.79890(18) 0.7608(6) 0.0451(13) Uani 1 1 d . . . H14A H -0.3022 0.8023 0.8539 0.054 Uiso 1 1 calc R . . C15 C -0.3499(6) 0.7725(2) 0.6661(7) 0.0578(16) Uani 1 1 d . . . H15A H -0.4337 0.7595 0.6950 0.069 Uiso 1 1 calc R . . C16 C -0.3017(7) 0.7657(2) 0.5293(7) 0.0591(16) Uani 1 1 d . . . H16A H -0.3512 0.7472 0.4675 0.071 Uiso 1 1 calc R . . C17 C -0.1813(7) 0.78622(19) 0.4856(6) 0.0546(15) Uani 1 1 d . . . H17A H -0.1499 0.7819 0.3935 0.065 Uiso 1 1 calc R . . C18 C -0.1053(6) 0.81344(17) 0.5770(5) 0.0410(11) Uani 1 1 d . . . H18A H -0.0237 0.8273 0.5459 0.049 Uiso 1 1 calc R . . C19 C 0.0251(5) 0.82081(14) 0.9203(5) 0.0304(9) Uani 1 1 d . . . C20 C 0.1569(5) 0.83581(17) 0.9588(6) 0.0429(12) Uani 1 1 d . . . H20A H 0.1957 0.8606 0.9129 0.051 Uiso 1 1 calc R . . C21 C 0.2315(6) 0.81433(19) 1.0649(7) 0.0531(15) Uani 1 1 d . . . H21A H 0.3190 0.8251 1.0912 0.064 Uiso 1 1 calc R . . C22 C 0.1769(6) 0.7775(2) 1.1307(6) 0.0521(14) Uani 1 1 d . . . H22A H 0.2274 0.7631 1.2019 0.063 Uiso 1 1 calc R . . C23 C 0.0512(6) 0.7618(2) 1.0934(7) 0.0526(15) Uani 1 1 d . . . H23A H 0.0152 0.7365 1.1387 0.063 Uiso 1 1 calc R . . C24 C -0.0278(5) 0.78305(17) 0.9863(6) 0.0405(12) Uani 1 1 d . . . H24A H -0.1149 0.7717 0.9606 0.049 Uiso 1 1 calc R . . C25 C 0.3275(10) 0.8832(3) 1.4133(12) 0.102(3) Uani 1 1 d . . . H25A H 0.3147 0.8983 1.5035 0.122 Uiso 1 1 calc R . . H25B H 0.2357 0.8757 1.3766 0.122 Uiso 1 1 calc R . . Cl1 Cl 0.4167(6) 0.83606(14) 1.4389(7) 0.247(3) Uani 1 1 d . . . Cl2 Cl 0.4105(3) 0.92039(12) 1.2955(3) 0.1126(8) 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 Mo1 0.02448(16) 0.02424(16) 0.01972(17) 0.0000(2) 0.0015(2) -0.00128(11) N1 0.0266(19) 0.0238(18) 0.024(2) 0.0035(14) -0.0009(17) -0.0023(14) N2 0.035(2) 0.0262(17) 0.0208(18) 0.0005(14) 0.0030(14) 0.0016(14) N3 0.0330(17) 0.0257(15) 0.027(3) -0.0040(17) -0.0064(19) 0.0056(12) N4 0.0293(18) 0.0308(18) 0.0307(18) 0.0051(15) 0.0030(16) 0.0010(15) O1 0.0307(15) 0.0248(14) 0.0270(15) 0.0005(11) 0.0057(11) -0.0003(11) O2 0.043(2) 0.0423(19) 0.022(2) -0.0026(14) 0.0022(14) -0.0023(13) O3 0.0288(17) 0.0275(18) 0.028(3) 0.000 0.000 -0.0029(16) O4 0.0250(15) 0.0399(16) 0.035(3) 0.0018(12) 0.0019(13) -0.0010(12) C1 0.082(4) 0.053(3) 0.029(3) 0.000(2) 0.012(3) -0.015(3) C2 0.056(3) 0.034(2) 0.022(2) 0.0056(16) 0.0047(18) 0.005(2) C3 0.052(3) 0.036(2) 0.015(4) -0.0002(17) -0.0041(18) 0.0019(18) C4 0.037(2) 0.032(2) 0.024(2) -0.0053(18) -0.0052(18) 0.003(2) C5 0.044(3) 0.037(2) 0.035(3) -0.002(2) -0.005(2) 0.002(2) C6 0.042(3) 0.082(5) 0.081(5) 0.025(4) 0.021(3) 0.010(3) C7 0.023(2) 0.041(3) 0.056(3) 0.005(2) 0.001(2) 0.0038(19) C8 0.027(2) 0.047(3) 0.064(5) -0.001(3) -0.007(3) 0.0017(17) C9 0.025(2) 0.035(2) 0.045(3) -0.0045(18) -0.0093(18) 0.0008(18) C10 0.051(3) 0.042(3) 0.041(3) -0.001(2) -0.016(2) 0.005(2) C11 0.031(2) 0.029(2) 0.027(2) 0.0024(16) 0.0050(17) -0.0022(18) C12 0.028(2) 0.0223(19) 0.028(2) 0.0005(16) -0.0005(17) -0.0027(15) C13 0.037(2) 0.0285(19) 0.033(3) 0.0053(17) -0.0039(18) 0.0005(17) C14 0.062(3) 0.041(3) 0.033(3) 0.002(2) -0.001(2) -0.021(2) C15 0.061(3) 0.066(3) 0.046(4) 0.001(3) -0.009(3) -0.034(3) C16 0.075(4) 0.053(3) 0.049(3) -0.008(3) -0.015(3) -0.024(3) C17 0.079(4) 0.052(3) 0.032(3) -0.009(2) -0.002(3) -0.018(3) C18 0.051(3) 0.040(3) 0.032(3) -0.004(2) -0.004(2) -0.006(2) C19 0.034(2) 0.026(2) 0.031(2) -0.0017(18) 0.0030(18) 0.0046(18) C20 0.034(3) 0.040(3) 0.054(3) 0.007(2) -0.005(2) -0.002(2) C21 0.041(3) 0.057(4) 0.061(4) 0.008(3) -0.009(2) 0.004(3) C22 0.051(3) 0.064(4) 0.041(3) 0.012(3) -0.006(2) 0.014(3) C23 0.060(4) 0.049(3) 0.049(3) 0.027(3) 0.010(3) 0.005(2) C24 0.037(3) 0.037(3) 0.047(3) 0.010(2) -0.001(2) -0.004(2) C25 0.096(6) 0.097(6) 0.112(7) -0.011(5) 0.022(5) 0.016(5) Cl1 0.412(8) 0.102(2) 0.228(6) -0.005(3) -0.129(6) 0.077(4) Cl2 0.1013(16) 0.151(2) 0.0856(17) -0.0055(16) -0.0031(14) -0.0218(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 Mo1 O4 1.698(3) . ? Mo1 O2 1.701(4) . ? Mo1 O3 1.8959(5) . ? Mo1 O1 1.956(3) . ? Mo1 N3 2.324(4) . ? Mo1 N1 2.359(5) . ? N1 C4 1.344(6) . ? N1 N2 1.359(5) . ? N2 C2 1.358(6) . ? N2 C11 1.454(6) . ? N3 C9 1.353(6) . ? N3 N4 1.379(6) . ? N4 C7 1.359(6) . ? N4 C11 1.451(6) . ? O1 C12 1.392(5) . ? O3 Mo1 1.8959(6) 2_575 ? C1 C2 1.497(7) . ? C2 C3 1.371(7) . ? C3 C4 1.379(9) . ? C4 C5 1.486(7) . ? C6 C7 1.497(8) . ? C7 C8 1.372(10) . ? C8 C9 1.387(9) . ? C9 C10 1.499(8) . ? C11 C12 1.560(6) . ? C12 C19 1.535(6) . ? C12 C13 1.541(6) . ? C13 C18 1.392(7) . ? C13 C14 1.384(7) . ? C14 C15 1.401(8) . ? C15 C16 1.387(9) . ? C16 C17 1.366(8) . ? C17 C18 1.387(7) . ? C19 C24 1.378(7) . ? C19 C20 1.385(7) . ? C20 C21 1.385(8) . ? C21 C22 1.361(8) . ? C22 C23 1.337(8) . ? C23 C24 1.411(8) . ? C25 Cl1 1.654(10) . ? C25 Cl2 1.756(10) . ? 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 O4 Mo1 O2 104.29(17) . . ? O4 Mo1 O3 100.88(10) . . ? O2 Mo1 O3 100.50(18) . . ? O4 Mo1 O1 95.99(13) . . ? O2 Mo1 O1 97.23(15) . . ? O3 Mo1 O1 151.59(13) . . ? O4 Mo1 N3 165.59(16) . . ? O2 Mo1 N3 89.37(18) . . ? O3 Mo1 N3 80.71(8) . . ? O1 Mo1 N3 77.45(11) . . ? O4 Mo1 N1 86.86(15) . . ? O2 Mo1 N1 167.35(14) . . ? O3 Mo1 N1 82.90(16) . . ? O1 Mo1 N1 75.33(12) . . ? N3 Mo1 N1 79.10(16) . . ? C4 N1 N2 105.2(4) . . ? C4 N1 Mo1 133.2(3) . . ? N2 N1 Mo1 120.7(3) . . ? C2 N2 N1 112.0(4) . . ? C2 N2 C11 129.0(4) . . ? N1 N2 C11 118.5(4) . . ? C9 N3 N4 104.3(4) . . ? C9 N3 Mo1 134.6(3) . . ? N4 N3 Mo1 120.3(3) . . ? C7 N4 N3 111.2(4) . . ? C7 N4 C11 130.1(4) . . ? N3 N4 C11 118.2(3) . . ? C12 O1 Mo1 136.0(2) . . ? Mo1 O3 Mo1 167.7(3) . 2_575 ? N2 C2 C3 105.1(5) . . ? N2 C2 C1 123.5(5) . . ? C3 C2 C1 131.4(5) . . ? C4 C3 C2 107.8(6) . . ? N1 C4 C3 109.8(5) . . ? N1 C4 C5 121.3(4) . . ? C3 C4 C5 128.9(4) . . ? N4 C7 C8 107.0(4) . . ? N4 C7 C6 122.8(5) . . ? C8 C7 C6 130.2(5) . . ? C9 C8 C7 106.2(4) . . ? N3 C9 C8 111.2(5) . . ? N3 C9 C10 120.7(4) . . ? C8 C9 C10 128.1(5) . . ? N4 C11 N2 109.8(3) . . ? N4 C11 C12 112.3(3) . . ? N2 C11 C12 110.2(3) . . ? O1 C12 C19 109.3(3) . . ? O1 C12 C13 109.3(4) . . ? C19 C12 C13 113.3(3) . . ? O1 C12 C11 110.0(3) . . ? C19 C12 C11 106.0(4) . . ? C13 C12 C11 108.8(3) . . ? C18 C13 C14 119.5(5) . . ? C18 C13 C12 117.6(4) . . ? C14 C13 C12 122.8(4) . . ? C13 C14 C15 119.8(5) . . ? C16 C15 C14 120.0(5) . . ? C17 C16 C15 119.8(5) . . ? C16 C17 C18 120.9(5) . . ? C13 C18 C17 120.0(5) . . ? C24 C19 C20 118.4(5) . . ? C24 C19 C12 123.0(4) . . ? C20 C19 C12 118.4(4) . . ? C21 C20 C19 120.7(5) . . ? C22 C21 C20 120.2(5) . . ? C23 C22 C21 120.2(5) . . ? C22 C23 C24 121.1(5) . . ? C19 C24 C23 119.4(5) . . ? Cl1 C25 Cl2 112.9(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.11 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.449 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.243