# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1539 data_VG9611 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H30 N6 O6 F6 S2 Mo' _chemical_formula_weight 916.72 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Ia loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z' 'x+1/2, y+1/2, z+1/2' 'x+1, -y+1/2, z+1/2' _cell_length_a 18.8743(12) _cell_length_b 10.7534(5) _cell_length_c 19.5999(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.967(4) _cell_angle_gamma 90.00 _cell_volume 3939.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 10.79 _cell_measurement_theta_max 27.47 _exptl_crystal_description Prisms _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method ? _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 4.431 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.1000 _exptl_absorpt_correction_T_max 0.2056 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.28 _diffrn_reflns_number 3366 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.56 _diffrn_reflns_theta_max 63.99 _reflns_number_total 3332 _reflns_number_observed 3009 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 15 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+2.4771P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00123(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 3317 _refine_ls_number_parameters 491 _refine_ls_number_restraints 212 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_obs 0.0456 _refine_ls_wR_factor_all 0.1179 _refine_ls_wR_factor_obs 0.1128 _refine_ls_goodness_of_fit_all 1.030 _refine_ls_goodness_of_fit_obs 1.041 _refine_ls_restrained_S_all 1.033 _refine_ls_restrained_S_obs 1.042 _refine_ls_shift/esd_max -0.021 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.36724(4) 0.62167(5) 0.86184(3) 0.0386(2) Uani 1 d . . N1 N 0.3214(4) 0.4782(6) 0.8615(4) 0.043(2) Uani 1 d . . N2 N 0.2944(4) 0.3711(6) 0.8796(4) 0.0428(14) Uani 1 d . . C21 C 0.2538(3) 0.3225(6) 0.7588(3) 0.054(2) Uani 1 d G . H21A H 0.2838(3) 0.3843(6) 0.7460(3) 0.065 Uiso 1 calc R . C22 C 0.2127(4) 0.2521(7) 0.7086(3) 0.070(3) Uani 1 d G . H22A H 0.2152(6) 0.2666(11) 0.6623(3) 0.084 Uiso 1 calc R . C23 C 0.1678(4) 0.1598(7) 0.7278(4) 0.079(4) Uani 1 d G . H23A H 0.1403(6) 0.1126(10) 0.6942(4) 0.094 Uiso 1 calc R . C24 C 0.1640(4) 0.1380(6) 0.7971(4) 0.075(3) Uani 1 d G . H24A H 0.1340(5) 0.0762(8) 0.8099(5) 0.090 Uiso 1 calc R . C25 C 0.2051(4) 0.2084(6) 0.8472(3) 0.059(2) Uani 1 d G . H25A H 0.2026(6) 0.1939(9) 0.8936(3) 0.071 Uiso 1 calc R . C26 C 0.2500(3) 0.3007(5) 0.8281(3) 0.046(2) Uani 1 d G . C27 C 0.3332(4) 0.2080(5) 0.9633(3) 0.054(2) Uani 1 d G . H27A H 0.3385(4) 0.1539(5) 0.9273(3) 0.064 Uiso 1 calc R . C28 C 0.3490(4) 0.1681(5) 1.0311(4) 0.070(3) Uani 1 d G . H28A H 0.3649(6) 0.0872(6) 1.0406(5) 0.084 Uiso 1 calc R . C29 C 0.3411(5) 0.2490(7) 1.0849(3) 0.075(3) Uani 1 d G . H29A H 0.3517(7) 0.2223(9) 1.1303(3) 0.090 Uiso 1 calc R . C30 C 0.3173(5) 0.3698(6) 1.0707(3) 0.083(4) Uani 1 d G . H30A H 0.3120(7) 0.4240(8) 1.1067(3) 0.099 Uiso 1 calc R . C31 C 0.3015(4) 0.4098(4) 1.0029(3) 0.060(2) Uani 1 d G . H31A H 0.2856(6) 0.4906(5) 0.9934(5) 0.072 Uiso 1 calc R . C32 C 0.3094(4) 0.3289(5) 0.9492(2) 0.049(2) Uani 1 d G . N3 N 0.4243(4) 0.6222(7) 0.9412(4) 0.046(2) Uani 1 d . . N4 N 0.4707(5) 0.6084(7) 0.9962(4) 0.051(2) Uani 1 d . . C41 C 0.4871(4) 0.3844(6) 0.9811(3) 0.056(2) Uani 1 d G . H41A H 0.4647(4) 0.3896(6) 0.9359(3) 0.067 Uiso 1 calc R . C42 C 0.5155(5) 0.2719(5) 1.0069(4) 0.073(4) Uani 1 d G . H42A H 0.5120(7) 0.2017(6) 0.9789(5) 0.088 Uiso 1 calc R . C43 C 0.5490(5) 0.2642(5) 1.0746(5) 0.084(4) Uani 1 d G . H43A H 0.5680(7) 0.1889(7) 1.0918(6) 0.101 Uiso 1 calc R . C44 C 0.5542(5) 0.3691(7) 1.1164(4) 0.091(5) Uani 1 d G . H44A H 0.5766(7) 0.3639(10) 1.1617(4) 0.109 Uiso 1 calc R . C45 C 0.5258(5) 0.4816(6) 1.0906(3) 0.078(4) Uani 1 d G . H45A H 0.5293(7) 0.5518(7) 1.1186(4) 0.094 Uiso 1 calc R . C46 C 0.4923(4) 0.4893(5) 1.0230(3) 0.051(2) Uani 1 d G . C47 C 0.5867(4) 0.7163(6) 1.0098(4) 0.064(3) Uani 1 d G . H47A H 0.6062(4) 0.6501(6) 0.9883(4) 0.077 Uiso 1 calc R . C48 C 0.6293(3) 0.8174(7) 1.0330(4) 0.080(4) Uani 1 d G . H48A H 0.6773(3) 0.8188(11) 1.0269(6) 0.096 Uiso 1 calc R . C49 C 0.6001(4) 0.9164(6) 1.0652(5) 0.083(4) Uani 1 d G . H49A H 0.6286(6) 0.9841(8) 1.0807(6) 0.099 Uiso 1 calc R . C50 C 0.5284(4) 0.9144(6) 1.0743(4) 0.078(3) Uani 1 d G . H50A H 0.5089(6) 0.9806(8) 1.0959(6) 0.093 Uiso 1 calc R . C51 C 0.4858(3) 0.8133(7) 1.0511(4) 0.067(3) Uani 1 d G . H51A H 0.4378(3) 0.8119(10) 1.0572(6) 0.080 Uiso 1 calc R . C52 C 0.5150(3) 0.7143(5) 1.0189(4) 0.049(2) Uani 1 d G . O5 O 0.4087(4) 0.8107(6) 0.8349(4) 0.060(2) Uani 1 d . . S5 S 0.44750(15) 0.9191(2) 0.86272(14) 0.0573(6) Uani 1 d D . O51 O 0.4187(6) 0.9760(9) 0.9193(5) 0.092(3) Uani 1 d . . O52 O 0.5224(6) 0.9014(12) 0.8733(6) 0.107(3) Uani 1 d . . C53 C 0.4298(10) 1.0278(13) 0.7942(8) 0.187(16) Uani 1 d D . F54 F 0.3593(8) 1.0493(12) 0.7784(8) 0.152(8) Uani 0.75 d PD 1 F55 F 0.4606(11) 1.1379(10) 0.8167(8) 0.153(6) Uani 0.75 d PDU 1 F56 F 0.4554(10) 0.9919(14) 0.7390(6) 0.165(9) Uani 0.75 d PD 1 F54' F 0.3953(32) 1.1289(33) 0.8139(23) 0.225(25) Uiso 0.25 d PDU 2 F55' F 0.4939(17) 1.0750(46) 0.7792(24) 0.161(18) Uiso 0.25 d PDU 2 F56' F 0.3946(29) 0.9862(39) 0.7372(14) 0.179(21) Uiso 0.25 d PDU 2 O6 O 0.3149(4) 0.6647(8) 0.7569(4) 0.066(2) Uani 1 d . . S6 S 0.2837(2) 0.6456(2) 0.68610(14) 0.0622(6) Uani 1 d D . O61 O 0.2108(6) 0.6198(13) 0.6777(7) 0.128(5) Uani 1 d . . O62 O 0.3229(9) 0.5668(13) 0.6474(7) 0.140(5) Uani 1 d . . C63 C 0.2873(8) 0.7979(14) 0.6493(7) 0.105(6) Uani 1 d D . F64 F 0.2537(9) 0.8793(10) 0.6852(8) 0.128(6) Uani 0.75 d PD 1 F65 F 0.2580(11) 0.8018(13) 0.5844(6) 0.150(7) Uani 0.75 d PD 1 F66 F 0.3560(7) 0.8344(14) 0.6534(9) 0.136(6) Uani 0.75 d PD 1 F64' F 0.2947(29) 0.8867(22) 0.6958(18) 0.143(21) Uiso 0.25 d PDU 2 F65' F 0.2251(21) 0.8193(37) 0.6071(26) 0.196(27) Uiso 0.25 d PDU 2 F66' F 0.3395(25) 0.8057(37) 0.6104(26) 0.204(28) Uiso 0.25 d PDU 2 N7 N 0.2761(4) 0.7247(7) 0.8946(4) 0.050(2) Uani 1 d . . C71 C 0.2859(6) 0.8161(11) 0.9414(6) 0.065(3) Uani 1 d . . H71A H 0.3320(6) 0.8318(11) 0.9633(6) 0.078 Uiso 1 calc R . C72 C 0.2300(7) 0.8883(11) 0.9584(8) 0.078(4) Uani 1 d . . H72A H 0.2386(7) 0.9505(11) 0.9915(8) 0.094 Uiso 1 calc R . C73 C 0.1624(7) 0.8673(13) 0.9262(7) 0.080(3) Uani 1 d . . H73A H 0.1239(7) 0.9149(13) 0.9360(7) 0.096 Uiso 1 calc R . C74 C 0.1535(8) 0.7734(19) 0.8789(9) 0.111(6) Uani 1 d . . H74A H 0.1079(8) 0.7545(19) 0.8568(9) 0.134 Uiso 1 calc R . C75 C 0.2099(7) 0.7082(15) 0.8638(8) 0.090(5) Uani 1 d . . H75A H 0.2020(7) 0.6477(15) 0.8297(8) 0.108 Uiso 1 calc R . N8 N 0.4544(4) 0.5438(6) 0.8102(4) 0.045(2) Uani 1 d . . C81 C 0.4456(6) 0.4357(10) 0.7743(7) 0.064(3) Uani 1 d . . H81A H 0.4023(6) 0.3937(10) 0.7721(7) 0.077 Uiso 1 calc R . C82 C 0.4981(7) 0.3871(11) 0.7415(7) 0.070(3) Uani 1 d . . H82A H 0.4901(7) 0.3128(11) 0.7174(7) 0.084 Uiso 1 calc R . C83 C 0.5623(6) 0.4457(11) 0.7435(6) 0.066(3) Uani 1 d . . H83A H 0.5983(6) 0.4143(11) 0.7204(6) 0.079 Uiso 1 calc R . C84 C 0.5713(7) 0.5523(12) 0.7810(8) 0.083(4) Uani 1 d . . H84A H 0.6149(7) 0.5937(12) 0.7850(8) 0.100 Uiso 1 calc R . C85 C 0.5170(6) 0.5997(9) 0.8130(6) 0.064(3) Uani 1 d . . H85A H 0.5246(6) 0.6738(9) 0.8374(6) 0.076 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0439(3) 0.0266(3) 0.0448(3) -0.0009(4) 0.0043(2) -0.0010(3) N1 0.049(4) 0.026(3) 0.057(4) -0.002(3) 0.016(3) 0.004(3) N2 0.051(4) 0.030(3) 0.048(4) -0.002(3) 0.008(3) -0.010(3) C21 0.057(5) 0.048(5) 0.058(6) -0.001(5) 0.010(4) -0.003(4) C22 0.053(7) 0.087(8) 0.066(7) -0.021(7) -0.002(6) -0.001(6) C23 0.075(8) 0.074(8) 0.079(8) -0.024(6) -0.015(6) -0.008(6) C24 0.069(7) 0.050(5) 0.104(9) 0.002(6) -0.002(6) -0.025(5) C25 0.065(6) 0.048(5) 0.064(6) -0.002(4) 0.011(5) -0.015(4) C26 0.047(4) 0.033(4) 0.056(5) -0.002(3) 0.005(4) -0.004(3) C27 0.066(6) 0.032(4) 0.061(5) -0.002(4) 0.006(5) 0.008(4) C28 0.075(7) 0.058(6) 0.076(7) 0.018(5) 0.008(6) 0.016(5) C29 0.084(8) 0.081(8) 0.061(6) 0.019(6) 0.009(6) 0.003(7) C30 0.128(11) 0.070(7) 0.052(6) -0.009(5) 0.021(6) -0.009(8) C31 0.083(7) 0.045(5) 0.054(5) -0.006(4) 0.014(5) 0.002(5) C32 0.061(5) 0.037(4) 0.047(5) -0.003(4) 0.004(4) 0.006(4) N3 0.047(4) 0.040(4) 0.052(5) -0.004(3) 0.012(3) 0.003(3) N4 0.069(5) 0.036(3) 0.045(4) -0.002(3) -0.009(4) 0.002(3) C41 0.062(6) 0.035(4) 0.072(6) 0.001(4) 0.012(5) 0.001(4) C42 0.094(10) 0.045(6) 0.082(9) 0.003(6) 0.017(8) 0.014(6) C43 0.086(8) 0.051(6) 0.112(11) 0.017(6) 0.003(8) -0.005(6) C44 0.099(9) 0.072(7) 0.090(9) 0.037(7) -0.033(7) -0.011(7) C45 0.100(9) 0.053(6) 0.073(7) 0.012(5) -0.022(7) -0.014(6) C46 0.053(5) 0.045(5) 0.052(5) 0.006(4) -0.001(4) -0.006(4) C47 0.068(6) 0.060(6) 0.062(6) -0.005(5) 0.001(5) -0.010(5) C48 0.094(9) 0.073(8) 0.068(7) 0.002(6) -0.006(6) -0.030(7) C49 0.100(10) 0.062(7) 0.077(8) 0.008(6) -0.019(7) -0.028(7) C50 0.091(9) 0.048(6) 0.089(8) -0.017(6) -0.009(7) 0.001(6) C51 0.074(7) 0.058(7) 0.065(7) -0.014(5) -0.005(5) 0.002(6) C52 0.062(5) 0.042(4) 0.041(4) -0.004(4) -0.002(4) -0.002(4) O5 0.064(4) 0.032(3) 0.087(5) -0.001(3) 0.019(4) -0.017(3) S5 0.0650(14) 0.0352(10) 0.072(2) -0.0009(10) 0.0090(12) -0.0029(10) O51 0.114(7) 0.071(6) 0.096(7) -0.024(5) 0.026(6) 0.015(5) O52 0.072(6) 0.124(9) 0.121(9) -0.022(7) 0.002(6) -0.013(6) C53 0.353(42) 0.083(12) 0.100(14) 0.042(11) -0.060(20) -0.116(19) F54 0.212(18) 0.076(8) 0.140(12) 0.012(8) -0.075(13) 0.057(10) F55 0.233(15) 0.052(6) 0.167(12) 0.021(7) 0.005(11) -0.069(8) F56 0.242(21) 0.183(17) 0.068(7) 0.032(9) 0.020(10) -0.122(16) O6 0.071(5) 0.067(5) 0.056(5) 0.012(4) -0.005(4) 0.003(4) S6 0.077(2) 0.0504(13) 0.0572(14) 0.0039(11) 0.0019(12) -0.0052(12) O61 0.088(7) 0.138(11) 0.147(11) 0.022(9) -0.026(7) -0.055(7) O62 0.206(15) 0.102(8) 0.117(9) -0.030(7) 0.035(9) 0.067(9) C63 0.148(17) 0.080(10) 0.081(10) 0.017(8) -0.011(10) -0.002(10) F64 0.151(14) 0.052(6) 0.173(15) 0.002(7) -0.008(11) 0.037(7) F65 0.253(21) 0.127(11) 0.058(6) 0.049(7) -0.018(9) 0.009(12) F66 0.144(12) 0.110(10) 0.162(15) 0.024(10) 0.054(11) -0.055(9) N7 0.053(4) 0.035(4) 0.062(5) -0.005(3) 0.012(4) 0.003(3) C71 0.055(6) 0.061(6) 0.077(7) -0.025(5) 0.004(5) -0.003(5) C72 0.073(7) 0.056(6) 0.108(10) -0.032(7) 0.022(7) -0.002(6) C73 0.070(7) 0.078(8) 0.096(9) -0.018(7) 0.023(6) 0.021(6) C74 0.062(7) 0.147(15) 0.122(13) -0.057(12) 0.001(8) 0.016(9) C75 0.056(6) 0.109(11) 0.103(10) -0.050(9) 0.006(6) 0.003(6) N8 0.047(4) 0.032(3) 0.054(4) 0.001(3) 0.002(3) -0.005(3) C81 0.062(6) 0.044(5) 0.090(8) -0.018(5) 0.022(6) 0.002(4) C82 0.075(7) 0.057(6) 0.079(7) -0.021(6) 0.014(6) 0.001(5) C83 0.069(6) 0.062(6) 0.069(6) -0.011(5) 0.022(5) 0.016(5) C84 0.068(7) 0.067(7) 0.122(11) -0.006(7) 0.039(7) -0.009(6) C85 0.060(6) 0.042(5) 0.091(8) -0.024(5) 0.021(5) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo N3 1.765(8) . ? Mo N1 1.768(7) . ? Mo O6 2.203(7) . ? Mo N8 2.212(8) . ? Mo N7 2.216(8) . ? Mo O5 2.266(6) . ? N1 N2 1.328(10) . ? N2 C32 1.428(8) . ? N2 C26 1.435(8) . ? C21 C22 1.39 . ? C21 C26 1.39 . ? C22 C23 1.39 . ? C23 C24 1.39 . ? C24 C25 1.39 . ? C25 C26 1.39 . ? C27 C28 1.39 . ? C27 C32 1.39 . ? C28 C29 1.39 . ? C29 C30 1.39 . ? C30 C31 1.39 . ? C31 C32 1.39 . ? N3 N4 1.299(11) . ? N4 C46 1.422(8) . ? N4 C52 1.446(8) . ? C41 C42 1.39 . ? C41 C46 1.39 . ? C42 C43 1.39 . ? C43 C44 1.39 . ? C44 C45 1.39 . ? C45 C46 1.39 . ? C47 C48 1.39 . ? C47 C52 1.39 . ? C48 C49 1.39 . ? C49 C50 1.39 . ? C50 C51 1.39 . ? C51 C52 1.39 . ? O5 S5 1.443(7) . ? S5 O52 1.414(11) . ? S5 O51 1.438(10) . ? S5 C53 1.78(2) . ? C53 F56' 1.30(2) . ? C53 F56 1.30(2) . ? C53 F54 1.34(2) . ? C53 F54' 1.35(2) . ? C53 F55 1.366(14) . ? C53 F55' 1.38(2) . ? O6 S6 1.446(8) . ? S6 O61 1.390(11) . ? S6 O62 1.413(11) . ? S6 C63 1.79(2) . ? C63 F64' 1.31(2) . ? C63 F65 1.316(14) . ? C63 F66' 1.33(2) . ? C63 F64 1.34(2) . ? C63 F66 1.35(2) . ? C63 F65' 1.36(2) . ? N7 C75 1.321(14) . ? N7 C71 1.339(13) . ? C71 C72 1.39(2) . ? C72 C73 1.36(2) . ? C73 C74 1.37(2) . ? C74 C75 1.34(2) . ? N8 C85 1.320(13) . ? N8 C81 1.357(13) . ? C81 C82 1.36(2) . ? C82 C83 1.36(2) . ? C83 C84 1.36(2) . ? C84 C85 1.37(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Mo N1 104.1(3) . . ? N3 Mo O6 164.1(4) . . ? N1 Mo O6 91.4(3) . . ? N3 Mo N8 90.1(3) . . ? N1 Mo N8 93.6(3) . . ? O6 Mo N8 85.3(3) . . ? N3 Mo N7 98.4(3) . . ? N1 Mo N7 92.2(3) . . ? O6 Mo N7 84.3(3) . . ? N8 Mo N7 168.2(3) . . ? N3 Mo O5 90.8(3) . . ? N1 Mo O5 165.0(3) . . ? O6 Mo O5 73.6(3) . . ? N8 Mo O5 86.0(3) . . ? N7 Mo O5 85.8(3) . . ? N2 N1 Mo 164.2(6) . . ? N1 N2 C32 119.9(6) . . ? N1 N2 C26 118.6(6) . . ? C32 N2 C26 121.6(6) . . ? C22 C21 C26 120.0 . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 N2 120.3(5) . . ? C21 C26 N2 119.6(5) . . ? C28 C27 C32 120.0 . . ? C29 C28 C27 120.0 . . ? C30 C29 C28 120.0 . . ? C29 C30 C31 120.0 . . ? C30 C31 C32 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 N2 119.8(5) . . ? C27 C32 N2 120.2(5) . . ? N4 N3 Mo 171.7(7) . . ? N3 N4 C46 122.4(7) . . ? N3 N4 C52 117.4(7) . . ? C46 N4 C52 118.1(6) . . ? C42 C41 C46 120.0 . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 N4 118.4(5) . . ? C41 C46 N4 121.3(5) . . ? C48 C47 C52 120.0 . . ? C49 C48 C47 120.0 . . ? C50 C49 C48 120.0 . . ? C51 C50 C49 120.0 . . ? C50 C51 C52 120.0 . . ? C51 C52 C47 120.0 . . ? C51 C52 N4 119.7(6) . . ? C47 C52 N4 120.3(6) . . ? S5 O5 Mo 144.1(5) . . ? O52 S5 O51 114.9(7) . . ? O52 S5 O5 113.1(6) . . ? O51 S5 O5 114.2(6) . . ? O52 S5 C53 106.2(8) . . ? O51 S5 C53 104.5(7) . . ? O5 S5 C53 102.3(6) . . ? F56 C53 F54 109.2(14) . . ? F56' C53 F54' 108.4(20) . . ? F56 C53 F55 109.5(13) . . ? F54 C53 F55 106.9(14) . . ? F56' C53 F55' 107.6(19) . . ? F54' C53 F55' 103.6(18) . . ? F56' C53 S5 116.3(17) . . ? F56 C53 S5 112.3(12) . . ? F54 C53 S5 111.4(11) . . ? F54' C53 S5 111.2(17) . . ? F55 C53 S5 107.4(11) . . ? F55' C53 S5 108.9(16) . . ? S6 O6 Mo 159.5(6) . . ? O61 S6 O62 113.6(10) . . ? O61 S6 O6 114.0(7) . . ? O62 S6 O6 115.3(7) . . ? O61 S6 C63 103.1(8) . . ? O62 S6 C63 106.3(8) . . ? O6 S6 C63 102.9(6) . . ? F64' C63 F66' 109.6(20) . . ? F65 C63 F64 108.7(14) . . ? F65 C63 F66 108.7(14) . . ? F64 C63 F66 107.5(13) . . ? F64' C63 F65' 107.4(19) . . ? F66' C63 F65' 106.6(19) . . ? F64' C63 S6 113.0(17) . . ? F65 C63 S6 112.6(11) . . ? F66' C63 S6 111.1(17) . . ? F64 C63 S6 109.8(11) . . ? F66 C63 S6 109.4(11) . . ? F65' C63 S6 108.8(17) . . ? C75 N7 C71 116.4(10) . . ? C75 N7 Mo 121.5(7) . . ? C71 N7 Mo 121.7(7) . . ? N7 C71 C72 122.5(11) . . ? C73 C72 C71 119.4(11) . . ? C72 C73 C74 117.1(11) . . ? C75 C74 C73 120.6(14) . . ? N7 C75 C74 123.9(13) . . ? C85 N8 C81 117.1(9) . . ? C85 N8 Mo 121.8(6) . . ? C81 N8 Mo 121.1(7) . . ? N8 C81 C82 122.0(11) . . ? C81 C82 C83 120.8(11) . . ? C84 C83 C82 116.7(10) . . ? C83 C84 C85 121.1(11) . . ? N8 C85 C84 122.2(10) . . ? _refine_diff_density_max 0.517 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.071 data_VG9609 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C47.50 H40 N3 O5 F3 S Cl4 Mo' _chemical_formula_weight 1059.63 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 12.900(2) _cell_length_b 14.588(3) _cell_length_c 14.795(3) _cell_angle_alpha 119.41(2) _cell_angle_beta 91.321(14) _cell_angle_gamma 95.50(2) _cell_volume 2406.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 4.95 _cell_measurement_theta_max 12.35 _exptl_crystal_description Prisms _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method ? _exptl_crystal_F_000 1078 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.7888 _exptl_absorpt_correction_T_max 0.9515 _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6069 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0885 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5708 _reflns_number_observed 4210 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+0.3727P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5707 _refine_ls_number_parameters 514 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_obs 0.0628 _refine_ls_wR_factor_all 0.1705 _refine_ls_wR_factor_obs 0.1494 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_goodness_of_fit_obs 1.094 _refine_ls_restrained_S_all 1.057 _refine_ls_restrained_S_obs 1.094 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.23943(5) 0.01775(5) 0.27770(5) 0.0232(2) Uani 1 d . . Cl Cl 0.07129(15) -0.0843(2) 0.21285(15) 0.0380(5) Uani 1 d . . O1 O 0.1868(4) 0.1455(4) 0.3172(4) 0.0281(12) Uani 1 d . . C1 C 0.1219(6) 0.2159(6) 0.3925(6) 0.028(2) Uani 1 d . . C2 C 0.0544(6) 0.1488(6) 0.4293(6) 0.031(2) Uani 1 d . . H2A H 0.0046(6) 0.1927(6) 0.4757(6) 0.038 Uiso 1 calc R . H2B H 0.0139(6) 0.0894(6) 0.3685(6) 0.038 Uiso 1 calc R . C3 C 0.1142(6) 0.1055(6) 0.4851(6) 0.029(2) Uani 1 d . . N3 N 0.1996(4) 0.0570(5) 0.4440(4) 0.0225(13) Uani 1 d . . C4 C 0.0821(6) 0.1176(6) 0.5800(6) 0.033(2) Uani 1 d . . H4A H 0.0210(6) 0.1486(6) 0.6059(6) 0.040 Uiso 1 calc R . C5 C 0.1383(7) 0.0853(7) 0.6333(6) 0.039(2) Uani 1 d . . H5A H 0.1171(7) 0.0942(7) 0.6971(6) 0.047 Uiso 1 calc R . C6 C 0.2280(6) 0.0387(6) 0.5949(6) 0.032(2) Uani 1 d . . H6A H 0.2685(6) 0.0167(6) 0.6328(6) 0.039 Uiso 1 calc R . C7 C 0.2570(6) 0.0249(6) 0.4996(5) 0.026(2) Uani 1 d . . C8 C 0.3530(6) -0.0259(6) 0.4576(5) 0.026(2) Uani 1 d . . H8A H 0.3843(6) -0.0442(6) 0.5067(5) 0.032 Uiso 1 calc R . H8B H 0.4038(6) 0.0252(6) 0.4521(5) 0.032 Uiso 1 calc R . C9 C 0.3312(6) -0.1270(6) 0.3498(5) 0.027(2) Uani 1 d . . O9 O 0.2956(4) -0.0959(4) 0.2786(3) 0.0265(12) Uani 1 d . . C10 C 0.0349(5) 0.2013(4) 0.2285(4) 0.059(3) Uani 1 d G . H10A H 0.0704(5) 0.1426(4) 0.1883(4) 0.070 Uiso 1 calc R . C11 C -0.0333(6) 0.2350(6) 0.1799(3) 0.082(4) Uani 1 d G . H11A H -0.0439(8) 0.1991(8) 0.1069(3) 0.098 Uiso 1 calc R . C12 C -0.0857(5) 0.3218(6) 0.2393(4) 0.065(3) Uani 1 d G . H12A H -0.1318(7) 0.3446(8) 0.2065(6) 0.078 Uiso 1 calc R . C13 C -0.0699(5) 0.3749(4) 0.3473(4) 0.050(2) Uani 1 d G . H13A H -0.1054(7) 0.4336(6) 0.3875(6) 0.060 Uiso 1 calc R . C14 C -0.0017(4) 0.3412(4) 0.3958(3) 0.042(2) Uani 1 d G . H14A H 0.0090(7) 0.3771(6) 0.4688(3) 0.050 Uiso 1 calc R . C15 C 0.0507(4) 0.2544(4) 0.3364(4) 0.032(2) Uani 1 d G . C16 C 0.2776(4) 0.3566(4) 0.4539(3) 0.047(2) Uani 1 d G . H16A H 0.2911(4) 0.3283(4) 0.3836(3) 0.057 Uiso 1 calc R . C17 C 0.3411(4) 0.4448(4) 0.5304(4) 0.059(3) Uani 1 d G . H17A H 0.3975(5) 0.4762(6) 0.5118(6) 0.070 Uiso 1 calc R . C18 C 0.3211(4) 0.4867(4) 0.6344(4) 0.051(3) Uani 1 d G . H18A H 0.3640(5) 0.5463(5) 0.6861(5) 0.061 Uiso 1 calc R . C19 C 0.2377(4) 0.4404(4) 0.6619(3) 0.040(2) Uani 1 d G . H19A H 0.2242(6) 0.4687(6) 0.7323(3) 0.048 Uiso 1 calc R . C20 C 0.1742(3) 0.3521(4) 0.5854(3) 0.035(2) Uani 1 d G . H20A H 0.1178(5) 0.3208(6) 0.6041(5) 0.042 Uiso 1 calc R . C21 C 0.1942(4) 0.3103(3) 0.4815(3) 0.029(2) Uani 1 d G . C22 C 0.2473(4) -0.2304(4) 0.4326(3) 0.040(2) Uani 1 d G . H22A H 0.2941(4) -0.1882(4) 0.4917(3) 0.048 Uiso 1 calc R . C23 C 0.1787(4) -0.3122(5) 0.4283(4) 0.049(2) Uani 1 d G . H23A H 0.1792(6) -0.3255(7) 0.4844(5) 0.059 Uiso 1 calc R . C24 C 0.1094(4) -0.3745(4) 0.3409(5) 0.054(3) Uani 1 d G . H24A H 0.0630(6) -0.4299(5) 0.3380(6) 0.065 Uiso 1 calc R . C25 C 0.1087(4) -0.3549(4) 0.2580(4) 0.055(3) Uani 1 d G . H25A H 0.0618(6) -0.3970(6) 0.1990(5) 0.066 Uiso 1 calc R . C26 C 0.1772(4) -0.2731(4) 0.2624(3) 0.042(2) Uani 1 d G . H26A H 0.1767(6) -0.2598(6) 0.2063(4) 0.050 Uiso 1 calc R . C27 C 0.2465(4) -0.2108(4) 0.3497(3) 0.028(2) Uani 1 d G . C28 C 0.4884(4) -0.2059(4) 0.3765(3) 0.034(2) Uani 1 d G . H28A H 0.4672(4) -0.1883(4) 0.4430(3) 0.041 Uiso 1 calc R . C29 C 0.5764(4) -0.2576(5) 0.3421(4) 0.040(2) Uani 1 d G . H29A H 0.6148(5) -0.2749(7) 0.3852(5) 0.048 Uiso 1 calc R . C30 C 0.6077(4) -0.2837(5) 0.2439(4) 0.046(2) Uani 1 d G . H30A H 0.6672(5) -0.3187(7) 0.2206(6) 0.055 Uiso 1 calc R . C31 C 0.5509(4) -0.2582(5) 0.1801(3) 0.049(2) Uani 1 d G . H31A H 0.5720(6) -0.2758(7) 0.1137(4) 0.059 Uiso 1 calc R . C32 C 0.4628(4) -0.2065(4) 0.2146(3) 0.035(2) Uani 1 d G . H32A H 0.4244(5) -0.1892(7) 0.1714(4) 0.043 Uiso 1 calc R . C33 C 0.4315(3) -0.1804(4) 0.3128(3) 0.027(2) Uani 1 d G . N34 N 0.2667(5) -0.0149(5) 0.1498(4) 0.0283(15) Uani 1 d . . N35 N 0.2867(5) -0.0567(5) 0.0522(4) 0.030(2) Uani 1 d . . C36 C 0.2629(6) -0.0520(5) -0.1083(4) 0.058(3) Uani 1 d G . H36A H 0.2622(6) -0.1260(5) -0.1462(4) 0.070 Uiso 1 calc R . C37 C 0.2506(7) 0.0043(6) -0.1603(4) 0.080(4) Uani 1 d G . H37A H 0.2415(10) -0.0316(8) -0.2334(4) 0.096 Uiso 1 calc R . C38 C 0.2517(7) 0.1138(6) -0.1043(6) 0.076(4) Uani 1 d G . H38A H 0.2433(9) 0.1518(8) -0.1394(8) 0.092 Uiso 1 calc R . C39 C 0.2651(7) 0.1669(4) 0.0038(6) 0.094(5) Uani 1 d G . H39A H 0.2658(10) 0.2409(4) 0.0417(8) 0.112 Uiso 1 calc R . C40 C 0.2774(6) 0.1106(5) 0.0558(4) 0.064(3) Uani 1 d G . H40A H 0.2865(9) 0.1466(6) 0.1289(4) 0.077 Uiso 1 calc R . C41 C 0.2763(5) 0.0012(5) -0.0002(4) 0.035(2) Uani 1 d G . C42 C 0.2597(3) -0.2409(4) 0.0076(4) 0.042(2) Uani 1 d G . H42A H 0.1952(3) -0.2292(4) 0.0372(4) 0.050 Uiso 1 calc R . C43 C 0.2934(5) -0.3404(4) -0.0338(5) 0.055(3) Uani 1 d G . H43A H 0.2518(7) -0.3960(4) -0.0322(7) 0.066 Uiso 1 calc R . C44 C 0.3888(5) -0.3577(4) -0.0776(5) 0.061(3) Uani 1 d G . H44A H 0.4116(7) -0.4250(4) -0.1056(7) 0.074 Uiso 1 calc R . C45 C 0.4504(4) -0.2755(5) -0.0800(5) 0.058(3) Uani 1 d G . H45A H 0.5148(5) -0.2872(7) -0.1096(7) 0.069 Uiso 1 calc R . C46 C 0.4166(4) -0.1760(4) -0.0386(4) 0.047(2) Uani 1 d G . H46A H 0.4583(5) -0.1204(5) -0.0402(7) 0.056 Uiso 1 calc R . C47 C 0.3213(4) -0.1587(3) 0.0052(4) 0.033(2) Uani 1 d G . O48 O 0.3891(4) 0.1150(4) 0.3480(4) 0.0316(13) Uani 1 d . . S S 0.49166(14) 0.1061(2) 0.30240(14) 0.0295(5) Uani 1 d . . O49 O 0.5656(4) 0.0731(5) 0.3505(4) 0.0394(14) Uani 1 d . . O50 O 0.4851(4) 0.0588(5) 0.1914(4) 0.045(2) Uani 1 d . . C51 C 0.5400(7) 0.2450(8) 0.3505(7) 0.047(2) Uani 1 d . . F52 F 0.6353(4) 0.2535(5) 0.3222(5) 0.071(2) Uani 1 d . . F53 F 0.4792(5) 0.2877(5) 0.3104(5) 0.065(2) Uani 1 d . . F54 F 0.5411(5) 0.3011(4) 0.4527(4) 0.0601(15) Uani 1 d . . C70 C 0.3598(13) 0.5330(12) 0.2208(13) 0.113(6) Uani 1 d . . H70A H 0.4200(13) 0.5880(12) 0.2515(13) 0.135 Uiso 0.60 calc PR 1 H70B H 0.2968(13) 0.5684(12) 0.2432(13) 0.135 Uiso 0.60 calc PR 1 H70C H 0.3209(13) 0.5928(12) 0.2489(13) 0.135 Uiso 0.40 d PR 2 H70D H 0.4304(13) 0.5564(12) 0.2514(13) 0.135 Uiso 0.40 d PR 2 Cl71 Cl 0.3576(4) 0.4756(4) 0.0860(4) 0.1128(13) Uani 1 d . . Cl72 Cl 0.3657(8) 0.4566(6) 0.2673(5) 0.110(3) Uani 0.60 d P 1 Cl73 Cl 0.2963(12) 0.4252(13) 0.2476(13) 0.135(6) Uiso 0.40 d P 2 C80 C 0.0808(18) 0.3374(19) -0.0181(19) 0.120(7) Uiso 0.40 d PU 1 H80A H 0.0640(18) 0.2616(19) -0.0418(19) 0.144 Uiso 0.40 calc PR 1 H80B H 0.1325(18) 0.3665(19) 0.0418(19) 0.144 Uiso 0.40 calc PR 1 Cl81 Cl 0.1398(5) 0.3485(6) -0.1162(5) 0.065(2) Uiso 0.40 d P 1 Cl82 Cl -0.0227(5) 0.3921(5) 0.0223(5) 0.062(2) Uiso 0.40 d PU 1 C85 C -0.0227(5) 0.3921(5) 0.0223(5) 0.062(2) Uiso 0.10 d PU 2 H85A H -0.0282(129) 0.4156(2967) 0.0963(2967) 0.074(2) Uiso 0.10 calc PR 2 H85B H -0.0856(129) 0.3446(2967) -0.0181(2967) 0.074 Uiso 0.10 calc PR 2 Cl86 Cl 0.0808(18) 0.3374(19) -0.0181(19) 0.120(7) Uiso 0.10 d PU 2 Cl87 Cl 0.0000 0.5000 0.0000(19) 0.147(13) Uiso 0.20 d SP 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0251(3) 0.0268(4) 0.0182(3) 0.0110(3) 0.0045(2) 0.0059(3) Cl 0.0323(10) 0.0394(12) 0.0354(10) 0.0139(9) 0.0031(8) 0.0002(9) O1 0.026(3) 0.032(3) 0.027(3) 0.014(2) 0.007(2) 0.008(2) C1 0.028(4) 0.021(4) 0.027(4) 0.006(3) 0.003(3) 0.004(3) C2 0.030(4) 0.032(5) 0.030(4) 0.013(3) 0.006(3) 0.008(3) C3 0.031(4) 0.023(4) 0.026(4) 0.009(3) 0.004(3) 0.002(3) N3 0.025(3) 0.023(3) 0.020(3) 0.011(3) 0.002(2) -0.001(3) C4 0.039(4) 0.032(5) 0.031(4) 0.015(4) 0.017(3) 0.005(4) C5 0.045(5) 0.041(5) 0.023(4) 0.009(4) 0.015(3) 0.007(4) C6 0.042(4) 0.034(5) 0.027(4) 0.019(4) 0.010(3) 0.011(4) C7 0.030(4) 0.022(4) 0.023(4) 0.011(3) -0.004(3) -0.006(3) C8 0.030(4) 0.023(4) 0.021(3) 0.008(3) 0.001(3) 0.001(3) C9 0.032(4) 0.026(4) 0.019(3) 0.007(3) 0.005(3) 0.003(3) O9 0.029(3) 0.033(3) 0.018(2) 0.012(2) 0.000(2) 0.005(2) C10 0.059(6) 0.063(7) 0.044(5) 0.016(5) -0.005(4) 0.030(5) C11 0.095(9) 0.092(10) 0.046(6) 0.022(6) -0.010(6) 0.035(8) C12 0.064(7) 0.074(8) 0.066(7) 0.041(6) -0.009(5) 0.022(6) C13 0.048(5) 0.048(6) 0.057(6) 0.027(5) 0.001(4) 0.019(4) C14 0.038(5) 0.044(5) 0.041(5) 0.019(4) 0.004(4) 0.010(4) C15 0.033(4) 0.026(4) 0.034(4) 0.014(4) -0.001(3) 0.000(3) C16 0.052(5) 0.030(5) 0.048(5) 0.012(4) 0.010(4) -0.004(4) C17 0.045(5) 0.054(6) 0.062(6) 0.020(5) 0.010(5) -0.012(5) C18 0.048(5) 0.032(5) 0.052(6) 0.004(4) -0.006(4) 0.007(4) C19 0.045(5) 0.035(5) 0.036(4) 0.014(4) 0.000(4) 0.008(4) C20 0.037(4) 0.035(5) 0.030(4) 0.012(4) 0.004(3) 0.009(4) C21 0.028(4) 0.028(4) 0.028(4) 0.010(3) 0.002(3) 0.008(3) C22 0.037(4) 0.049(6) 0.036(4) 0.023(4) 0.005(3) -0.002(4) C23 0.045(5) 0.047(6) 0.069(6) 0.041(5) 0.012(4) -0.003(5) C24 0.042(5) 0.050(6) 0.070(7) 0.032(5) 0.007(5) -0.004(5) C25 0.042(5) 0.041(6) 0.070(7) 0.022(5) -0.015(5) -0.017(4) C26 0.047(5) 0.039(5) 0.039(5) 0.019(4) -0.003(4) 0.005(4) C27 0.023(4) 0.024(4) 0.029(4) 0.008(3) -0.002(3) -0.002(3) C28 0.040(4) 0.039(5) 0.026(4) 0.016(4) 0.003(3) 0.006(4) C29 0.031(4) 0.037(5) 0.056(5) 0.025(4) 0.003(4) 0.010(4) C30 0.040(5) 0.044(6) 0.054(5) 0.023(4) 0.016(4) 0.018(4) C31 0.048(5) 0.060(6) 0.039(5) 0.021(4) 0.018(4) 0.023(5) C32 0.037(4) 0.044(5) 0.028(4) 0.019(4) 0.005(3) 0.011(4) C33 0.033(4) 0.022(4) 0.025(4) 0.010(3) 0.008(3) 0.002(3) N34 0.030(3) 0.031(4) 0.022(3) 0.012(3) 0.003(2) 0.004(3) N35 0.040(4) 0.032(4) 0.020(3) 0.014(3) 0.005(3) 0.005(3) C36 0.088(8) 0.064(7) 0.032(5) 0.028(5) 0.020(5) 0.030(6) C37 0.100(9) 0.120(12) 0.057(7) 0.067(8) 0.028(6) 0.038(9) C38 0.089(8) 0.103(11) 0.081(8) 0.080(8) -0.006(7) 0.007(8) C39 0.124(12) 0.074(9) 0.110(11) 0.074(9) -0.044(9) -0.022(8) C40 0.094(8) 0.046(7) 0.053(6) 0.029(5) -0.031(6) -0.013(6) C41 0.026(4) 0.063(6) 0.027(4) 0.033(4) 0.001(3) 0.003(4) C42 0.048(5) 0.045(6) 0.025(4) 0.010(4) 0.005(4) 0.006(4) C43 0.089(8) 0.027(5) 0.040(5) 0.010(4) -0.006(5) 0.006(5) C44 0.087(8) 0.051(7) 0.034(5) 0.007(4) 0.005(5) 0.034(6) C45 0.068(7) 0.060(7) 0.042(5) 0.018(5) 0.018(5) 0.036(6) C46 0.046(5) 0.055(6) 0.042(5) 0.024(4) 0.013(4) 0.015(5) C47 0.042(4) 0.034(5) 0.019(4) 0.009(3) 0.002(3) 0.011(4) O48 0.031(3) 0.035(3) 0.028(3) 0.015(2) 0.003(2) 0.002(2) S 0.0269(10) 0.0386(12) 0.0267(9) 0.0193(9) 0.0032(7) 0.0019(8) O49 0.032(3) 0.055(4) 0.036(3) 0.025(3) 0.001(2) 0.012(3) O50 0.034(3) 0.071(4) 0.025(3) 0.022(3) 0.006(2) 0.002(3) C51 0.038(5) 0.054(6) 0.052(6) 0.030(5) 0.006(4) -0.001(4) F52 0.045(3) 0.068(4) 0.101(5) 0.046(4) 0.021(3) -0.009(3) F53 0.067(4) 0.073(4) 0.084(4) 0.060(4) 0.016(3) 0.014(3) F54 0.068(4) 0.043(3) 0.056(3) 0.017(3) 0.002(3) -0.005(3) C70 0.097(11) 0.076(10) 0.120(13) 0.011(9) 0.022(9) 0.027(8) Cl71 0.128(3) 0.107(3) 0.123(3) 0.070(3) 0.008(3) 0.026(3) Cl72 0.184(9) 0.090(5) 0.069(4) 0.040(3) 0.028(5) 0.068(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo N34 1.763(6) . ? Mo O1 1.861(5) . ? Mo O9 1.878(5) . ? Mo O48 2.181(5) . ? Mo N3 2.319(6) . ? Mo Cl 2.393(2) . ? O1 C1 1.444(8) . ? C1 C15 1.539(9) . ? C1 C2 1.548(11) . ? C1 C21 1.553(8) . ? C2 C3 1.501(11) . ? C3 N3 1.356(9) . ? C3 C4 1.404(11) . ? N3 C7 1.364(10) . ? C4 C5 1.332(12) . ? C5 C6 1.388(11) . ? C6 C7 1.390(11) . ? C7 C8 1.493(10) . ? C8 C9 1.545(10) . ? C9 O9 1.419(9) . ? C9 C33 1.545(8) . ? C9 C27 1.558(8) . ? C10 C11 1.39 . ? C10 C15 1.39 . ? C11 C12 1.39 . ? C12 C13 1.39 . ? C13 C14 1.39 . ? C14 C15 1.39 . ? C16 C17 1.39 . ? C16 C21 1.39 . ? C17 C18 1.39 . ? C18 C19 1.39 . ? C19 C20 1.39 . ? C20 C21 1.39 . ? C22 C23 1.39 . ? C22 C27 1.39 . ? C23 C24 1.39 . ? C24 C25 1.39 . ? C25 C26 1.39 . ? C26 C27 1.39 . ? C28 C29 1.39 . ? C28 C33 1.39 . ? C29 C30 1.39 . ? C30 C31 1.39 . ? C31 C32 1.39 . ? C32 C33 1.39 . ? N34 N35 1.306(8) . ? N35 C41 1.412(8) . ? N35 C47 1.422(8) . ? C36 C37 1.39 . ? C36 C41 1.39 . ? C37 C38 1.39 . ? C38 C39 1.39 . ? C39 C40 1.39 . ? C40 C41 1.39 . ? C42 C43 1.39 . ? C42 C47 1.39 . ? C43 C44 1.39 . ? C44 C45 1.39 . ? C45 C46 1.39 . ? C46 C47 1.39 . ? O48 S 1.487(5) . ? S O49 1.428(6) . ? S O50 1.432(6) . ? S C51 1.823(10) . ? C51 F54 1.318(11) . ? C51 F52 1.323(10) . ? C51 F53 1.338(11) . ? C70 Cl72 1.58(2) . ? C70 Cl71 1.74(2) . ? C70 Cl73 1.92(2) . ? C80 Cl82 1.60(2) . ? C80 Cl81 1.72(2) . ? C85 Cl86 1.60(2) . ? C85 Cl87 1.761(7) . ? Cl87 C85 1.761(7) 2_565 ? 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 N34 Mo O1 98.6(3) . . ? N34 Mo O9 96.9(3) . . ? O1 Mo O9 163.8(2) . . ? N34 Mo O48 94.3(2) . . ? O1 Mo O48 85.5(2) . . ? O9 Mo O48 88.8(2) . . ? N34 Mo N3 178.4(2) . . ? O1 Mo N3 81.8(2) . . ? O9 Mo N3 82.8(2) . . ? O48 Mo N3 87.3(2) . . ? N34 Mo Cl 89.8(2) . . ? O1 Mo Cl 93.3(2) . . ? O9 Mo Cl 91.4(2) . . ? O48 Mo Cl 175.90(15) . . ? N3 Mo Cl 88.68(15) . . ? C1 O1 Mo 140.2(5) . . ? O1 C1 C15 107.7(5) . . ? O1 C1 C2 106.4(6) . . ? C15 C1 C2 109.5(6) . . ? O1 C1 C21 108.3(5) . . ? C15 C1 C21 111.1(6) . . ? C2 C1 C21 113.6(6) . . ? C3 C2 C1 115.1(6) . . ? N3 C3 C4 121.1(7) . . ? N3 C3 C2 119.5(6) . . ? C4 C3 C2 119.4(7) . . ? C3 N3 C7 118.5(6) . . ? C3 N3 Mo 120.7(5) . . ? C7 N3 Mo 120.6(5) . . ? C5 C4 C3 119.9(7) . . ? C4 C5 C6 120.3(7) . . ? C5 C6 C7 118.8(8) . . ? N3 C7 C6 121.3(7) . . ? N3 C7 C8 119.6(6) . . ? C6 C7 C8 119.1(7) . . ? C7 C8 C9 113.0(6) . . ? O9 C9 C8 107.5(6) . . ? O9 C9 C33 109.0(5) . . ? C8 C9 C33 111.1(6) . . ? O9 C9 C27 108.9(5) . . ? C8 C9 C27 112.6(5) . . ? C33 C9 C27 107.8(6) . . ? C9 O9 Mo 140.1(4) . . ? C11 C10 C15 120.0 . . ? C12 C11 C10 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 C1 118.8(4) . . ? C10 C15 C1 121.2(4) . . ? C17 C16 C21 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C19 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C20 C21 C16 120.0 . . ? C20 C21 C1 122.0(4) . . ? C16 C21 C1 117.9(4) . . ? C23 C22 C27 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C22 120.0 . . ? C26 C27 C9 120.0(4) . . ? C22 C27 C9 119.7(4) . . ? C29 C28 C33 120.0 . . ? C30 C29 C28 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C28 120.0 . . ? C32 C33 C9 120.3(4) . . ? C28 C33 C9 119.7(4) . . ? N35 N34 Mo 169.5(6) . . ? N34 N35 C41 119.5(6) . . ? N34 N35 C47 117.1(6) . . ? C41 N35 C47 123.3(5) . . ? C37 C36 C41 120.0 . . ? C36 C37 C38 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C41 C40 C39 120.0 . . ? C40 C41 C36 120.0 . . ? C40 C41 N35 120.3(4) . . ? C36 C41 N35 119.7(4) . . ? C43 C42 C47 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C47 C46 C45 120.0 . . ? C46 C47 C42 120.0 . . ? C46 C47 N35 121.3(4) . . ? C42 C47 N35 118.6(4) . . ? S O48 Mo 129.1(3) . . ? O49 S O50 118.3(4) . . ? O49 S O48 112.0(3) . . ? O50 S O48 114.6(3) . . ? O49 S C51 103.2(4) . . ? O50 S C51 104.7(4) . . ? O48 S C51 101.4(4) . . ? F54 C51 F52 109.4(7) . . ? F54 C51 F53 107.6(8) . . ? F52 C51 F53 107.4(8) . . ? F54 C51 S 111.5(6) . . ? F52 C51 S 110.2(7) . . ? F53 C51 S 110.6(6) . . ? Cl72 C70 Cl71 116.9(9) . . ? Cl71 C70 Cl73 106.2(9) . . ? Cl82 C80 Cl81 118.8(15) . . ? Cl86 C85 Cl87 100.3(10) . . ? C85 Cl87 C85 180.0 2_565 . ? _refine_diff_density_max 1.033 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.105 data_VG9617 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C56 H62 N10 Cl4 Mo2' _chemical_formula_weight 1208.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6091(6) _cell_length_b 18.777(2) _cell_length_c 14.6059(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.569(5) _cell_angle_gamma 90.00 _cell_volume 2788.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.63 _cell_measurement_theta_max 22.10 _exptl_crystal_description Rhombs _exptl_crystal_colour Orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method ? _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 5.806 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.3870 _exptl_absorpt_correction_T_max 0.5227 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 25.10 _diffrn_reflns_number 4892 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0933 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 63.99 _reflns_number_total 4621 _reflns_number_observed 3289 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+0.5745P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00071(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4619 _refine_ls_number_parameters 286 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_obs 0.0588 _refine_ls_wR_factor_all 0.5182 _refine_ls_wR_factor_obs 0.1330 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 4.052 _refine_ls_restrained_S_obs 1.079 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.05200(5) 0.04876(3) 0.13230(3) 0.0346(2) Uani 1 d . . Cl1 Cl 0.0172(2) 0.07467(8) -0.04571(10) 0.0405(4) Uani 1 d . . Cl2 Cl -0.1841(2) 0.07450(10) 0.10440(13) 0.0495(4) Uani 1 d . . N1 N 0.0978(6) 0.1378(3) 0.1609(4) 0.0402(12) Uani 1 d . . N2 N 0.1206(7) 0.2037(3) 0.1957(4) 0.0420(13) Uani 1 d . . N3 N 0.0635(6) 0.0044(3) 0.2402(4) 0.0382(12) Uani 1 d . . N4 N 0.0638(6) -0.0379(3) 0.3126(4) 0.0386(12) Uani 1 d . . N5 N 0.2434(6) 0.0019(3) 0.1226(4) 0.0411(12) Uani 1 d D . H5A H 0.2578(75) -0.0312(28) 0.1689(37) 0.035(18) Uiso 1 d D . H5B H 0.2350(118) -0.0206(54) 0.0667(41) 0.079(34) Uiso 1 d D . C6 C 0.1072(6) 0.2519(2) 0.0381(3) 0.050(2) Uani 1 d G . H6A H 0.1136(6) 0.2060(2) 0.0161(3) 0.059 Uiso 1 calc R . C7 C 0.0968(6) 0.3096(3) -0.0232(3) 0.061(2) Uani 1 d G . H7A H 0.0964(10) 0.3023(4) -0.0863(3) 0.073 Uiso 1 calc R . C8 C 0.0871(7) 0.3783(2) 0.0096(4) 0.061(2) Uani 1 d G . H8A H 0.0802(10) 0.4169(3) -0.0314(5) 0.073 Uiso 1 calc R . C9 C 0.0878(7) 0.3893(2) 0.1039(4) 0.061(2) Uani 1 d G . H9A H 0.0813(10) 0.4352(2) 0.1259(5) 0.073 Uiso 1 calc R . C10 C 0.0981(6) 0.3316(2) 0.1652(3) 0.052(2) Uani 1 d G . H10A H 0.0985(9) 0.3390(3) 0.2283(3) 0.062 Uiso 1 calc R . C11 C 0.1078(6) 0.2629(2) 0.1324(3) 0.0410(14) Uani 1 d G . C12 C 0.2374(5) 0.2463(3) 0.3552(4) 0.061(2) Uani 1 d G . H12A H 0.3113(5) 0.2551(3) 0.3348(4) 0.073 Uiso 1 calc R . C13 C 0.2380(6) 0.2640(4) 0.4478(4) 0.078(3) Uani 1 d G . H13A H 0.3122(7) 0.2846(5) 0.4892(5) 0.093 Uiso 1 calc R . C14 C 0.1275(8) 0.2509(4) 0.4784(3) 0.085(4) Uani 1 d G . H14A H 0.1279(10) 0.2627(5) 0.5403(4) 0.102 Uiso 1 calc R . C15 C 0.0165(6) 0.2200(4) 0.4164(4) 0.069(3) Uani 1 d G . H15A H -0.0574(7) 0.2112(5) 0.4369(6) 0.083 Uiso 1 calc R . C16 C 0.0160(5) 0.2024(3) 0.3239(4) 0.054(2) Uani 1 d G . H16A H -0.0583(6) 0.1818(5) 0.2825(5) 0.065 Uiso 1 calc R . C17 C 0.1264(5) 0.2155(3) 0.2933(3) 0.045(2) Uani 1 d G . C18 C 0.2017(5) 0.0451(2) 0.4245(3) 0.048(2) Uani 1 d G . H18A H 0.2114(5) 0.0715(2) 0.3731(3) 0.058 Uiso 1 calc R . C19 C 0.2645(5) 0.0667(3) 0.5173(4) 0.062(2) Uani 1 d G . H19A H 0.3161(7) 0.1076(3) 0.5280(5) 0.075 Uiso 1 calc R . C20 C 0.2500(6) 0.0273(3) 0.5942(2) 0.069(3) Uani 1 d G . H20A H 0.2920(8) 0.0417(4) 0.6564(3) 0.082 Uiso 1 calc R . C21 C 0.1729(6) -0.0338(3) 0.5783(3) 0.062(2) Uani 1 d G . H21A H 0.1632(8) -0.0602(4) 0.6298(3) 0.074 Uiso 1 calc R . C22 C 0.1101(5) -0.0555(2) 0.4855(3) 0.048(2) Uani 1 d G . H22A H 0.0585(7) -0.0964(3) 0.4748(5) 0.058 Uiso 1 calc R . C23 C 0.1246(5) -0.0160(2) 0.4086(2) 0.0392(14) Uani 1 d G . C24 C -0.1345(5) -0.1042(2) 0.2331(4) 0.053(2) Uani 1 d G . H24A H -0.1753(5) -0.0614(2) 0.2097(4) 0.064 Uiso 1 calc R . C25 C -0.2033(4) -0.1679(3) 0.2114(4) 0.066(2) Uani 1 d G . H25A H -0.2902(5) -0.1677(4) 0.1735(6) 0.079 Uiso 1 calc R . C26 C -0.1424(6) -0.2318(2) 0.2465(4) 0.068(2) Uani 1 d G . H26A H -0.1884(8) -0.2744(3) 0.2320(6) 0.081 Uiso 1 calc R . C27 C -0.0125(6) -0.2320(2) 0.3032(4) 0.070(3) Uani 1 d G . H27A H 0.0282(8) -0.2748(2) 0.3266(6) 0.083 Uiso 1 calc R . C28 C 0.0563(4) -0.1683(3) 0.3249(4) 0.056(2) Uani 1 d G . H28A H 0.1432(5) -0.1685(4) 0.3628(5) 0.067 Uiso 1 calc R . C29 C -0.0047(5) -0.1044(2) 0.2898(3) 0.0405(14) Uani 1 d G . C30 C 0.3751(8) 0.0372(4) 0.1393(5) 0.048(2) Uani 1 d . . C31 C 0.4759(10) -0.0208(5) 0.1361(7) 0.065(2) Uani 1 d . . H31A H 0.4800(10) -0.0550(5) 0.1858(7) 0.098 Uiso 1 calc R . H31B H 0.5609(10) 0.0005(5) 0.1455(7) 0.098 Uiso 1 calc R . H31C H 0.4499(10) -0.0442(5) 0.0752(7) 0.098 Uiso 1 calc R . C32 C 0.3676(10) 0.0913(5) 0.0618(6) 0.059(2) Uani 1 d . . H32A H 0.3425(10) 0.0681(5) 0.0007(6) 0.089 Uiso 1 calc R . H32B H 0.4521(10) 0.1133(5) 0.0715(6) 0.089 Uiso 1 calc R . H32C H 0.3036(10) 0.1269(5) 0.0638(6) 0.089 Uiso 1 calc R . C33 C 0.4150(9) 0.0723(5) 0.2381(6) 0.062(2) Uani 1 d . . H33A H 0.4191(9) 0.0368(5) 0.2862(6) 0.093 Uiso 1 calc R . H33B H 0.3513(9) 0.1078(5) 0.2412(6) 0.093 Uiso 1 calc R . H33C H 0.4998(9) 0.0942(5) 0.2489(6) 0.093 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0480(3) 0.0279(3) 0.0247(2) -0.0028(2) 0.0054(2) -0.0058(2) Cl1 0.0614(9) 0.0292(6) 0.0276(6) -0.0020(5) 0.0074(6) -0.0092(6) Cl2 0.0525(9) 0.0454(8) 0.0488(8) 0.0015(7) 0.0112(7) 0.0017(7) N1 0.049(3) 0.031(3) 0.039(3) -0.006(2) 0.010(2) -0.002(2) N2 0.068(4) 0.022(2) 0.034(3) -0.007(2) 0.011(3) -0.007(2) N3 0.045(3) 0.035(3) 0.033(2) -0.002(2) 0.010(2) -0.006(2) N4 0.055(3) 0.029(3) 0.029(2) 0.004(2) 0.007(2) -0.004(2) N5 0.045(3) 0.034(3) 0.040(3) -0.004(2) 0.006(2) 0.001(2) C6 0.071(5) 0.037(3) 0.036(3) 0.000(3) 0.009(3) -0.009(3) C7 0.077(6) 0.058(5) 0.044(4) 0.004(3) 0.012(4) -0.009(4) C8 0.066(5) 0.044(4) 0.073(5) 0.016(4) 0.020(4) 0.002(4) C9 0.081(6) 0.036(4) 0.065(5) 0.001(3) 0.019(4) 0.006(4) C10 0.063(5) 0.039(4) 0.057(4) -0.007(3) 0.023(3) -0.001(3) C11 0.054(4) 0.027(3) 0.042(3) -0.001(2) 0.014(3) -0.006(3) C12 0.070(5) 0.058(5) 0.046(4) -0.021(4) 0.004(4) -0.008(4) C13 0.099(8) 0.078(7) 0.045(5) -0.026(4) 0.003(5) -0.006(6) C14 0.133(11) 0.076(6) 0.040(4) -0.012(4) 0.016(5) 0.019(7) C15 0.098(8) 0.058(5) 0.065(5) 0.007(4) 0.045(5) 0.015(5) C16 0.067(5) 0.049(4) 0.048(4) 0.000(3) 0.020(4) -0.004(4) C17 0.063(4) 0.038(3) 0.031(3) -0.005(3) 0.007(3) 0.001(3) C18 0.049(4) 0.052(4) 0.038(3) 0.001(3) 0.003(3) 0.002(3) C19 0.058(5) 0.072(6) 0.050(4) -0.021(4) 0.004(4) 0.004(4) C20 0.066(5) 0.095(7) 0.037(4) -0.016(4) 0.003(3) 0.025(5) C21 0.068(5) 0.084(6) 0.032(3) 0.014(4) 0.012(3) 0.028(5) C22 0.051(4) 0.054(4) 0.038(3) 0.012(3) 0.011(3) 0.007(3) C23 0.044(3) 0.044(3) 0.026(3) 0.002(2) 0.005(2) 0.008(3) C24 0.060(5) 0.051(4) 0.047(4) 0.002(3) 0.013(3) -0.005(4) C25 0.071(6) 0.068(6) 0.053(4) -0.008(4) 0.011(4) -0.024(5) C26 0.088(7) 0.061(5) 0.061(5) -0.015(4) 0.033(5) -0.022(5) C27 0.100(8) 0.037(4) 0.080(6) 0.001(4) 0.040(6) 0.005(4) C28 0.063(5) 0.037(4) 0.069(5) 0.007(3) 0.022(4) 0.002(3) C29 0.052(4) 0.039(3) 0.033(3) 0.000(2) 0.017(3) -0.004(3) C30 0.052(4) 0.044(4) 0.048(4) -0.001(3) 0.015(3) 0.000(3) C31 0.058(5) 0.063(5) 0.073(6) -0.004(4) 0.016(4) 0.010(4) C32 0.066(5) 0.058(5) 0.054(4) 0.008(4) 0.017(4) -0.005(4) C33 0.063(5) 0.064(5) 0.046(4) -0.010(4) -0.004(4) -0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo N3 1.755(6) . ? Mo N1 1.758(6) . ? Mo N5 2.255(6) . ? Mo Cl2 2.468(2) . ? Mo Cl1 2.5662(14) . ? Mo Cl1 2.6420(15) 3 ? Cl1 Mo 2.6420(15) 3 ? N1 N2 1.333(8) . ? N2 C17 1.427(6) . ? N2 C11 1.428(6) . ? N3 N4 1.321(8) . ? N4 C23 1.427(6) . ? N4 C29 1.436(6) . ? N5 C30 1.502(10) . ? C6 C7 1.39 . ? C6 C11 1.39 . ? C7 C8 1.39 . ? C8 C9 1.39 . ? C9 C10 1.39 . ? C10 C11 1.39 . ? C12 C13 1.39 . ? C12 C17 1.39 . ? C13 C14 1.39 . ? C14 C15 1.39 . ? C15 C16 1.39 . ? C16 C17 1.39 . ? C18 C19 1.39 . ? C18 C23 1.39 . ? C19 C20 1.39 . ? C20 C21 1.39 . ? C21 C22 1.39 . ? C22 C23 1.39 . ? C24 C25 1.39 . ? C24 C29 1.39 . ? C25 C26 1.39 . ? C26 C27 1.39 . ? C27 C28 1.39 . ? C28 C29 1.39 . ? C30 C32 1.506(11) . ? C30 C33 1.533(10) . ? C30 C31 1.537(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Mo N1 107.1(3) . . ? N3 Mo N5 92.2(2) . . ? N1 Mo N5 101.2(3) . . ? N3 Mo Cl2 92.8(2) . . ? N1 Mo Cl2 93.0(2) . . ? N5 Mo Cl2 162.93(15) . . ? N3 Mo Cl1 162.3(2) . . ? N1 Mo Cl1 90.6(2) . . ? N5 Mo Cl1 83.2(2) . . ? Cl2 Mo Cl1 87.10(6) . . ? N3 Mo Cl1 87.3(2) . 3 ? N1 Mo Cl1 165.6(2) . 3 ? N5 Mo Cl1 76.09(15) . 3 ? Cl2 Mo Cl1 87.85(6) . 3 ? Cl1 Mo Cl1 75.00(5) . 3 ? Mo Cl1 Mo 105.00(5) . 3 ? N2 N1 Mo 168.9(5) . . ? N1 N2 C17 118.4(5) . . ? N1 N2 C11 120.2(5) . . ? C17 N2 C11 119.6(5) . . ? N4 N3 Mo 170.7(5) . . ? N3 N4 C23 120.7(5) . . ? N3 N4 C29 116.9(5) . . ? C23 N4 C29 122.3(4) . . ? C30 N5 Mo 129.0(4) . . ? C7 C6 C11 120.0 . . ? C6 C7 C8 120.0 . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C6 120.0 . . ? C10 C11 N2 120.1(4) . . ? C6 C11 N2 119.9(4) . . ? C13 C12 C17 120.0 . . ? C14 C13 C12 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C12 120.0 . . ? C16 C17 N2 119.6(4) . . ? C12 C17 N2 120.1(4) . . ? C19 C18 C23 120.0 . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 N4 121.2(4) . . ? C18 C23 N4 118.8(4) . . ? C25 C24 C29 120.0 . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C29 120.0 . . ? C28 C29 C24 120.0 . . ? C28 C29 N4 121.0(4) . . ? C24 C29 N4 119.0(4) . . ? N5 C30 C32 109.2(6) . . ? N5 C30 C33 109.7(6) . . ? C32 C30 C33 111.1(7) . . ? N5 C30 C31 107.8(6) . . ? C32 C30 C31 110.1(7) . . ? C33 C30 C31 108.9(7) . . ? _refine_diff_density_max 1.151 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.104 data_ESSEX _audit_creation_method MolEN _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H42 N10 B Cl Mo' _chemical_formula_weight 793.04 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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)/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 15.56(1) _cell_length_b 13.67(1) _cell_length_c 18.86(1) _cell_angle_alpha 90.00 _cell_angle_beta 105.09(3) _cell_angle_gamma 90.00 _cell_volume 3871(9) _cell_formula_units_z 4 _cell_measurement_temperature 291 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22.98 _cell_measurement_theta_max 24.02 _exptl_crystal_description Parallelepipeds _exptl_crystal_colour 'Golden brown' _exptl_crystal_size_max 0.85 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.36 _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 0.440 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.831 _exptl_special_details ; ? ; _diffrn_ambient_temperature 291 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method \w/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 2.44 _diffrn_reflns_number 8281 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 24.97 _reflns_number_total 7065 _reflns_number_observed 5027 _reflns_observed_criterion >3.0\s(I) _computing_data_collection CAD4_(Enraf-Nonius,_1977) _computing_cell_refinement CAD4_(Enraf-Nonius,_1977) _computing_data_reduction PROCESS_MolEN_(Fair,_1990) _computing_structure_solution Patterson_and_Fourier _computing_structure_refinement LSFM_MolEN_(Fair,_1990) _computing_molecular_graphics ORTEP_(Johnson,_1976) _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/ (\s^2^(Fo^2^) + 0.0016 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5027 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.077 _refine_ls_R_factor_obs 0.049 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.081 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.972 _refine_ls_shift/esd_max 0.001 _refine_diff_density_max 0.90 _refine_diff_density_min -0.18 _refine_ls_extinction_method none loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Mo 0.04633(3) 0.10783(3) 0.25800(2) 0.0330(1) Uani ? Cl1 0.1730(1) 0.0945(1) 0.36655(8) 0.0590(4) Uani ? N1 0.0852(3) 0.0184(3) 0.2043(2) 0.038(1) Uani ? N2 0.1088(3) -0.0421(3) 0.1589(2) 0.046(1) Uani ? N3 -0.0252(3) 0.0437(3) 0.3019(2) 0.039(1) Uani ? N4 -0.0760(3) -0.0030(3) 0.3362(2) 0.045(1) Uani ? N5 0.1233(3) 0.2253(3) 0.2145(2) 0.044(1) Uani ? N6 0.0796(3) 0.3069(3) 0.1798(3) 0.048(1) Uani ? N7 -0.0661(3) 0.1464(3) 0.1653(2) 0.040(1) Uani ? N8 -0.0773(3) 0.2399(3) 0.1376(2) 0.043(1) Uani ? N9 0.0086(3) 0.2522(3) 0.3053(2) 0.043(1) Uani ? N10 -0.0258(3) 0.3270(3) 0.2573(2) 0.047(1) Uani ? B -0.0176(4) 0.3235(5) 0.1776(4) 0.048(2) Uani ? C1 0.0670(3) -0.1338(4) 0.1421(3) 0.046(2) Uani ? C2 0.0282(4) -0.1790(4) 0.1917(3) 0.050(2) Uani ? C3 -0.0153(4) -0.2677(5) 0.1739(4) 0.066(2) Uani ? C4 -0.0213(4) -0.3112(5) 0.1071(4) 0.069(2) Uani ? C5 0.0175(5) -0.2665(5) 0.0588(4) 0.083(2) Uani ? C6 0.0611(4) -0.1800(4) 0.0751(3) 0.063(2) Uani ? C7 0.1742(4) -0.0089(4) 0.1217(3) 0.050(2) Uani ? C8 0.1597(5) 0.0718(6) 0.0800(4) 0.075(2) Uani ? C9 0.2258(6) 0.1020(6) 0.0467(4) 0.104(3) Uani ? C10 0.3022(5) 0.0496(7) 0.0565(4) 0.115(3) Uani ? C11 0.3145(4) -0.0288(7) 0.0979(4) 0.099(3) Uani ? C12 0.2523(4) -0.0631(6) 0.1317(4) 0.072(2) Uani ? C13 -0.1368(3) 0.0500(4) 0.3666(3) 0.046(2) Uani ? C14 -0.1505(4) 0.0226(5) 0.4335(3) 0.054(2) Uani ? C15 -0.2075(4) 0.0772(6) 0.4632(4) 0.071(2) Uani ? C16 -0.2493(4) 0.1581(6) 0.4261(4) 0.080(2) Uani ? C17 -0.2348(5) 0.1842(6) 0.3599(5) 0.081(3) Uani ? C18 -0.1777(4) 0.1315(5) 0.3294(4) 0.059(2) Uani ? C19 -0.0608(4) -0.1059(4) 0.3498(3) 0.045(1) Uani ? C20 -0.1316(4) -0.1702(5) 0.3401(3) 0.057(2) Uani ? C21 -0.1137(5) -0.2692(5) 0.3539(4) 0.069(2) Uani ? C22 -0.0278(5) -0.3020(5) 0.3751(3) 0.066(2) Uani ? C23 0.0408(5) -0.2387(5) 0.3841(4) 0.062(2) Uani ? C24 0.0256(4) -0.1397(4) 0.3724(3) 0.051(2) Uani ? C25 0.2102(3) 0.2347(4) 0.2126(3) 0.045(1) Uani ? C26 0.2193(4) 0.3200(4) 0.1772(4) 0.055(2) Uani ? C27 0.1377(4) 0.3644(4) 0.1569(4) 0.052(2) Uani ? C28 0.2794(4) 0.1621(5) 0.2453(3) 0.057(2) Uani ? C29 0.1101(5) 0.4577(5) 0.1168(4) 0.078(2) Uani ? C30 -0.1346(4) 0.0920(4) 0.1263(3) 0.046(2) Uani ? C31 -0.1879(4) 0.1552(5) 0.0741(3) 0.057(2) Uani ? C32 -0.1525(4) 0.2454(4) 0.0821(3) 0.047(2) Uani ? C33 -0.1467(4) -0.0123(5) 0.1414(4) 0.066(2) Uani ? C34 -0.1861(5) 0.3347(5) 0.0405(4) 0.070(2) Uani ? C35 -0.0055(4) 0.2762(4) 0.3708(3) 0.050(2) Uani ? C36 -0.0501(4) 0.3651(5) 0.3629(3) 0.063(2) Uani ? C37 -0.0634(4) 0.3937(4) 0.2923(4) 0.060(2) Uani ? C38 0.0242(4) 0.2159(5) 0.4377(3) 0.065(2) Uani ? C39 -0.1097(5) 0.4829(5) 0.2528(5) 0.086(3) Uani ? H -0.0374 0.3860 0.1507 0.0623 Uiso calc H2 0.0315 -0.1493 0.2378 0.0653 Uiso calc H3 -0.0414 -0.2988 0.2083 0.0863 Uiso calc H4 -0.0519 -0.3715 0.0948 0.0896 Uiso calc H5 0.0140 -0.2965 0.0127 0.1073 Uiso calc H6 0.0880 -0.1507 0.0405 0.0814 Uiso calc H8 0.1058 0.1076 0.0732 0.0974 Uiso calc H9 0.2172 0.1594 0.0172 0.1354 Uiso calc H10 0.3466 0.0698 0.0333 0.1499 Uiso calc H11 0.3691 -0.0634 0.1050 0.1284 Uiso calc H12 0.2619 -0.1211 0.1604 0.0931 Uiso calc H14 -0.1211 -0.0331 0.4588 0.0702 Uiso calc H15 -0.2178 0.0591 0.5089 0.0920 Uiso calc H16 -0.2882 0.1960 0.4464 0.1046 Uiso calc H17 -0.2647 0.2397 0.3346 0.1058 Uiso calc H18 -0.1669 0.1508 0.2841 0.0767 Uiso calc H20 -0.1912 -0.1473 0.3243 0.0739 Uiso calc H21 -0.1615 -0.3143 0.3486 0.0896 Uiso calc H22 -0.0163 -0.3699 0.3836 0.0860 Uiso calc H23 0.1002 -0.2625 0.3988 0.0808 Uiso calc H24 0.0741 -0.0954 0.3797 0.0668 Uiso calc H26 0.2728 0.3441 0.1682 0.0719 Uiso calc H31 -0.2409 0.1369 0.0386 0.0735 Uiso calc H36 -0.0682 0.3995 0.4003 0.0819 Uiso calc H28a 0.2509 0.1053 0.2682 0.0740 Uiso calc H28b 0.3070 0.1343 0.2049 0.0740 Uiso calc H28c 0.3289 0.1954 0.2861 0.0740 Uiso calc H29a 0.0425 0.4691 0.1108 0.1010 Uiso calc H29b 0.1461 0.5154 0.1463 0.1010 Uiso calc H29c 0.1224 0.4539 0.0653 0.1010 Uiso calc H33a -0.0939 -0.0357 0.1841 0.0863 Uiso calc H33b -0.2061 -0.0213 0.1561 0.0863 Uiso calc H33c -0.1484 -0.0533 0.0945 0.0863 Uiso calc H34a -0.1431 0.3925 0.0603 0.0916 Uiso calc H34b -0.1899 0.3236 -0.0148 0.0916 Uiso calc H34c -0.2491 0.3510 0.0466 0.0916 Uiso calc H38a 0.0558 0.1534 0.4257 0.0841 Uiso calc H38b 0.0683 0.2559 0.4782 0.0841 Uiso calc H38c -0.0307 0.1959 0.4563 0.0841 Uiso calc H39a -0.1073 0.4812 0.1983 0.1113 Uiso calc H39b -0.1758 0.4833 0.2551 0.1113 Uiso calc H39c -0.0781 0.5457 0.2779 0.1113 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo 0.0333(2) 0.0321(2) 0.0326(2) 0.0007(2) 0.0067(1) -0.0006(2) Cl1 0.0459(7) 0.078(1) 0.0444(7) 0.0008(7) -0.0036(6) -0.0000(8) N1 0.041(2) 0.029(2) 0.041(2) 0.003(2) 0.006(2) -0.002(2) N2 0.048(2) 0.052(3) 0.043(2) 0.000(2) 0.019(2) -0.006(2) N3 0.037(2) 0.039(2) 0.040(2) 0.002(2) 0.007(2) 0.003(2) N4 0.045(2) 0.042(2) 0.052(2) 0.002(2) 0.022(2) 0.002(2) N5 0.044(2) 0.043(2) 0.046(2) -0.000(2) 0.014(2) -0.002(2) N6 0.049(2) 0.043(2) 0.051(2) 0.001(2) 0.013(2) 0.006(2) N7 0.040(2) 0.039(2) 0.038(2) 0.005(2) 0.007(2) 0.001(2) N8 0.045(2) 0.050(3) 0.034(2) 0.009(2) 0.009(2) 0.006(2) N9 0.046(2) 0.041(2) 0.042(2) -0.002(2) 0.013(2) -0.005(2) N10 0.047(2) 0.039(2) 0.055(3) 0.002(2) 0.014(2) -0.006(2) B 0.048(3) 0.042(3) 0.054(3) 0.004(3) 0.014(3) 0.009(3) C1 0.038(3) 0.052(3) 0.051(3) 0.001(2) 0.015(2) -0.010(3) C2 0.059(3) 0.043(3) 0.050(3) 0.001(3) 0.018(2) 0.005(3) C3 0.068(3) 0.047(3) 0.091(4) -0.005(3) 0.032(3) 0.008(3) C4 0.054(3) 0.044(3) 0.108(5) -0.005(3) 0.019(3) -0.018(3) C5 0.084(4) 0.072(4) 0.102(4) -0.031(3) 0.044(3) -0.049(3) C6 0.071(3) 0.052(3) 0.080(3) -0.018(3) 0.045(2) -0.026(3) C7 0.060(3) 0.053(3) 0.041(3) -0.009(3) 0.018(2) -0.010(3) C8 0.097(5) 0.077(4) 0.053(3) -0.010(4) 0.023(3) 0.001(4) C9 0.179(6) 0.080(4) 0.067(4) -0.067(4) 0.054(4) -0.011(4) C10 0.130(4) 0.147(6) 0.095(4) -0.090(4) 0.077(3) -0.065(4) C11 0.064(4) 0.153(7) 0.092(4) -0.040(4) 0.044(3) -0.054(5) C12 0.053(3) 0.104(5) 0.062(4) 0.003(4) 0.021(3) -0.013(4) C13 0.036(2) 0.052(3) 0.052(3) 0.002(2) 0.013(2) -0.007(3) C14 0.050(3) 0.052(3) 0.065(3) -0.006(3) 0.023(2) -0.008(3) C15 0.064(3) 0.082(4) 0.076(4) -0.019(3) 0.037(3) -0.030(3) C16 0.063(4) 0.071(4) 0.118(5) -0.008(3) 0.042(3) -0.038(4) C17 0.049(3) 0.076(5) 0.113(6) 0.007(4) 0.010(4) -0.011(5) C18 0.046(3) 0.052(3) 0.076(4) 0.010(3) 0.011(3) -0.001(3) C19 0.054(3) 0.045(3) 0.037(2) 0.004(3) 0.018(2) 0.003(2) C20 0.057(3) 0.053(3) 0.064(3) -0.003(3) 0.022(3) -0.004(3) C21 0.094(4) 0.047(3) 0.074(4) -0.019(3) 0.036(3) -0.007(3) C22 0.101(4) 0.043(3) 0.059(3) 0.007(3) 0.030(3) 0.006(3) C23 0.076(4) 0.054(4) 0.057(3) 0.013(3) 0.018(3) 0.007(3) C24 0.056(3) 0.049(3) 0.051(3) 0.001(3) 0.017(2) 0.007(3) C25 0.039(2) 0.052(3) 0.044(3) -0.015(2) 0.013(2) -0.013(2) C26 0.047(3) 0.047(3) 0.076(3) -0.010(3) 0.024(2) -0.003(3) C27 0.061(3) 0.028(3) 0.068(3) -0.006(2) 0.019(3) 0.001(3) C28 0.040(3) 0.063(4) 0.067(3) 0.009(3) 0.014(3) -0.009(3) C29 0.084(4) 0.039(3) 0.111(5) 0.002(3) 0.026(4) 0.026(3) C30 0.041(3) 0.051(3) 0.043(3) 0.004(2) 0.004(2) -0.008(3) C31 0.045(3) 0.078(4) 0.039(3) 0.015(3) -0.004(3) -0.005(3) C32 0.043(3) 0.061(3) 0.036(3) 0.006(3) 0.006(2) 0.001(3) C33 0.060(4) 0.055(4) 0.070(4) -0.013(3) -0.009(3) -0.008(3) C34 0.068(4) 0.071(4) 0.062(4) 0.020(3) -0.001(3) 0.020(3) C35 0.057(3) 0.047(3) 0.048(3) -0.009(3) 0.017(2) -0.014(3) C36 0.076(4) 0.056(3) 0.065(3) -0.006(3) 0.031(3) -0.029(3) C37 0.056(3) 0.046(3) 0.079(4) -0.004(3) 0.019(3) -0.020(3) C38 0.076(4) 0.084(4) 0.036(3) -0.013(4) 0.017(3) -0.012(3) C39 0.093(5) 0.042(3) 0.120(6) 0.028(3) 0.024(4) -0.012(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Mo Cl1 2.451(2) ? Mo N1 1.790(4) ? Mo N3 1.780(4) ? Mo N5 2.279(5) ? Mo N7 2.191(4) ? Mo N9 2.303(5) ? N1 N2 1.310(6) ? N2 C1 1.411(8) ? N2 C7 1.450(7) ? N3 N4 1.312(6) ? N4 C13 1.424(7) ? N4 C19 1.437(7) ? N5 N6 1.379(6) ? N5 C25 1.369(7) ? N6 B 1.520(9) ? N6 C27 1.349(8) ? N7 N8 1.374(6) ? N7 C30 1.350(7) ? N8 B 1.540(9) ? N8 C32 1.354(7) ? N9 N10 1.378(7) ? N9 C35 1.352(7) ? N10 B 1.540(9) ? N10 C37 1.346(8) ? C1 C2 1.383(8) ? C1 C6 1.394(9) ? C2 C3 1.387(9) ? C3 C4 1.37(1) ? C4 C5 1.36(1) ? C5 C6 1.358(9) ? C7 C8 1.34(1) ? C7 C12 1.39(1) ? C8 C9 1.40(1) ? C9 C10 1.36(2) ? C10 C11 1.31(2) ? C11 C12 1.37(1) ? C13 C14 1.385(9) ? C13 C18 1.381(9) ? C14 C15 1.385(9) ? C15 C16 1.38(1) ? C16 C17 1.37(1) ? C17 C18 1.38(1) ? C19 C20 1.384(9) ? C19 C24 1.379(9) ? C20 C21 1.39(1) ? C21 C22 1.37(1) ? C22 C23 1.35(1) ? C23 C24 1.382(9) ? C25 C26 1.369(9) ? C25 C28 1.476(9) ? C26 C27 1.369(9) ? C27 C29 1.488(9) ? C30 C31 1.406(9) ? C30 C33 1.475(9) ? C31 C32 1.342(9) ? C32 C34 1.471(9) ? C35 C36 1.388(9) ? C35 C38 1.476(9) ? C36 C37 1.35(1) ? C37 C39 1.51(1) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl1 Mo N1 96.0(1) ? Cl1 Mo N3 92.2(1) ? Cl1 Mo N5 88.3(1) ? Cl1 Mo N7 170.2(1) ? Cl1 Mo N9 88.3(1) ? N1 Mo N3 105.8(2) ? N1 Mo N5 89.5(2) ? N1 Mo N7 91.7(2) ? N1 Mo N9 164.0(2) ? N3 Mo N5 164.6(2) ? N3 Mo N7 91.4(2) ? N3 Mo N9 89.4(2) ? N5 Mo N7 85.9(2) ? N5 Mo N9 75.3(2) ? N7 Mo N9 82.6(2) ? Mo N1 N2 174.0(4) ? N1 N2 C1 121.1(5) ? N1 N2 C7 118.0(5) ? C1 N2 C7 120.7(5) ? Mo N3 N4 178.2(4) ? N3 N4 C13 120.0(5) ? N3 N4 C19 118.1(4) ? C13 N4 C19 121.5(5) ? Mo N5 N6 120.1(3) ? Mo N5 C25 133.7(4) ? N6 N5 C25 106.2(5) ? N5 N6 B 119.7(5) ? N5 N6 C27 109.6(5) ? B N6 C27 130.5(5) ? Mo N7 N8 121.6(3) ? Mo N7 C30 131.0(4) ? N8 N7 C30 107.5(4) ? N7 N8 B 120.2(4) ? N7 N8 C32 110.1(5) ? B N8 C32 128.9(5) ? Mo N9 N10 118.4(3) ? Mo N9 C35 132.9(4) ? N10 N9 C35 107.1(5) ? N9 N10 B 120.1(5) ? N9 N10 C37 108.9(5) ? B N10 C37 131.1(6) ? N6 B N8 111.8(5) ? N6 B N10 108.2(5) ? N8 B N10 108.0(5) ? N2 C1 C2 120.1(5) ? N2 C1 C6 121.6(6) ? C2 C1 C6 118.3(6) ? C1 C2 C3 119.9(6) ? C2 C3 C4 120.7(7) ? C3 C4 C5 119.0(6) ? C4 C5 C6 121.4(7) ? C1 C6 C5 120.7(7) ? N2 C7 C8 120.6(6) ? N2 C7 C12 117.7(6) ? C8 C7 C12 121.6(7) ? C7 C8 C9 118.4(9) ? C8 C9 C10 120.(1) ? C9 C10 C11 119.9(9) ? C10 C11 C12 123(1) ? C7 C12 C11 116.8(9) ? N4 C13 C14 120.3(5) ? N4 C13 C18 118.2(6) ? C14 C13 C18 121.4(6) ? C13 C14 C15 119.3(7) ? C14 C15 C16 119.6(7) ? C15 C16 C17 120.3(7) ? C16 C17 C18 121.3(8) ? C13 C18 C17 118.1(7) ? N4 C19 C20 120.6(5) ? N4 C19 C24 119.0(5) ? C20 C19 C24 120.4(6) ? C19 C20 C21 118.6(6) ? C20 C21 C22 120.4(7) ? C21 C22 C23 120.5(7) ? C22 C23 C24 120.7(7) ? C19 C24 C23 119.3(6) ? N5 C25 C26 108.7(5) ? N5 C25 C28 122.9(5) ? C26 C25 C28 128.4(5) ? C25 C26 C27 107.9(5) ? N6 C27 C26 107.6(5) ? N6 C27 C29 122.2(6) ? C26 C27 C29 130.2(6) ? N7 C30 C31 106.4(6) ? N7 C30 C33 123.3(5) ? C31 C30 C33 130.3(6) ? C30 C31 C32 109.6(5) ? N8 C32 C31 106.4(5) ? N8 C32 C34 125.0(6) ? C31 C32 C34 128.6(6) ? N9 C35 C36 108.0(6) ?