# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1205 data_comd_1 _audit_creation_method SHELXL-97 _chemical_formula_moiety '[Mo2(DAniF)2]6[1,3,5-Ph(COO)3]4(22.1CH3CN)(2.3CH2CL2)' _chemical_formula_sum 'C262.50 H262.90 Cl4.60 Mo12 N46.10 O48' _chemical_formula_weight 6145.84 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.825(3) _cell_length_b 27.377(2) _cell_length_c 38.248(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.71(1) _cell_angle_gamma 90.00 _cell_volume 28809(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 232 _cell_measurement_theta_min 6.9 _cell_measurement_theta_max 20.8 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12507 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 0.879 _exptl_special_details ; The well-formed crystals produced excellent diffraction data, but provided measurable scattering only to about 1A resolution. The general structure of the complex is well-defined, but many of the p-anisyl groups of the ligands are disordered over two sites. One of the dinuclear Mo2 subunits resides on the crystallographic 2-fold axis, but the metal-metal vector is not exactly bisected by the 2-fold axis, so the metal atoms and formamidinate groups at this site are all disordered. Careful modeling and judicious use of restraints allowed successful refinement of the whole model. The model for the complete metal complex (including symmetry-equivalent atoms and many disordered atoms) contains 690 atoms. There are at least 66 additional atoms modeled as interstitial solvent; most of the solvent is acetonitrile, but a few molecules of CH2Cl2 are also included. The most prominent instance of CH2Cl2 is a disordered "ball" of the solvent located directly in the center of the metal-complex cage. Several of the acetonitrile molecules are associated with the "axial" positions of the Mo-Mo subunits. The existence of a substantial amount of interstitial solvent was apparent before any diffraction data were collected; unprotected crystals lost solvent and turned powdery immediately upon removal from the mother liquor. Of the 292 refined non-hydrogen atoms, only the metal atoms were allowed to refine with anisotropic displacement parameters. Hydrogen atoms were used in idealized positions on the metal cluster for structure factor calculations; no hydrogen atoms were included on the solvent molecules. ; _diffrn_ambient_temperature 173(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 'Nonius FAST area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'None (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34640 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 21.37 _reflns_number_total 13285 _reflns_number_obs 10797 _reflns_threshold_expression >2sigma(I) _computing_data_collection MADNES _computing_cell_refinement MADNES _computing_data_reduction PROCOR _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+1310.9772P] 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 13285 _refine_ls_number_parameters 1190 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.1231 _refine_ls_R_factor_obs 0.0976 _refine_ls_wR_factor_all 0.2406 _refine_ls_wR_factor_obs 0.2174 _refine_ls_goodness_of_fit_all 1.073 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/esd_max 0.017 _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_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.74101(4) -0.64865(4) -0.15225(4) 0.0338(4) Uani 1 d . . . Mo2 Mo 0.74870(4) -0.70112(4) -0.18957(4) 0.0360(4) Uani 1 d . . . Mo3 Mo 0.47406(4) -0.93628(4) -0.23771(4) 0.0406(4) Uani 1 d . . . N1 N 0.7922(4) -0.6008(4) -0.1598(3) 0.038(3) Uiso 1 d . . . N2 N 0.8031(4) -0.6593(4) -0.1982(3) 0.042(3) Uiso 1 d . . . N3 N 0.7934(4) -0.6827(4) -0.1048(3) 0.043(3) Uiso 1 d . . . N4 N 0.8003(4) -0.7412(4) -0.1450(3) 0.041(3) Uiso 1 d . . . N5 N 0.5677(5) -0.7027(4) -0.0159(4) 0.054(3) Uiso 1 d . . . N6 N 0.5048(5) -0.7574(5) -0.0371(4) 0.063(4) Uiso 1 d . . . N9 N 0.4286(5) -0.9876(5) -0.2771(4) 0.063(4) Uiso 1 d . . . N10 N 0.5136(4) -0.9874(4) -0.1957(3) 0.042(3) Uiso 1 d . . . O1 O 0.8290(5) -0.4107(5) -0.1031(4) 0.089(4) Uiso 1 d . . . O3 O 0.8639(6) -0.6126(5) 0.0437(5) 0.107(5) Uiso 1 d . . . O5 O 0.7641(5) -0.6663(4) 0.0691(4) 0.081(4) Uiso 1 d . . . O10 O 0.4695(5) -1.0457(5) -0.0742(4) 0.088(4) Uiso 1 d . . . O301 O 0.6850(3) -0.6122(3) -0.1967(3) 0.034(2) Uiso 1 d . . . O302 O 0.6928(3) -0.6676(3) -0.2369(3) 0.037(2) Uiso 1 d . . . O303 O 0.6847(3) -0.6895(3) -0.1454(3) 0.039(2) Uiso 1 d . . . O304 O 0.6916(3) -0.7450(3) -0.1847(3) 0.034(2) Uiso 1 d . . . O305 O 0.5619(3) -0.6947(3) -0.0946(3) 0.043(2) Uiso 1 d . . . O306 O 0.5016(3) -0.7488(3) -0.1145(3) 0.049(3) Uiso 1 d . . . O307 O 0.5655(3) -0.4845(3) -0.2375(3) 0.042(2) Uiso 1 d . . . O308 O 0.5066(3) -0.4845(3) -0.2959(3) 0.048(3) Uiso 1 d . . . O309 O 0.5100(4) -0.8806(3) -0.1999(3) 0.052(3) Uiso 1 d . . . O310 O 0.5656(4) -0.8790(4) -0.2258(3) 0.056(3) Uiso 1 d . . . O311 O 0.4918(3) -0.6148(3) -0.1132(3) 0.046(2) Uiso 1 d . . . O312 O 0.4322(4) -0.6692(4) -0.1320(3) 0.056(3) Uiso 1 d . . . C1 C 0.8138(5) -0.6159(5) -0.1815(4) 0.039(4) Uiso 1 d . . . H1 H 0.8374 -0.5958 -0.1854 0.046 Uiso 1 calc R . . C2 C 0.8124(5) -0.7234(5) -0.1110(4) 0.042(4) Uiso 1 d . . . H2 H 0.8355 -0.7404 -0.0901 0.050 Uiso 1 calc R . . C3 C 0.5496(6) -0.7441(6) -0.0130(5) 0.066(5) Uiso 1 d . . . H3 H 0.5681 -0.7659 0.0066 0.079 Uiso 1 calc R . . C5 C 0.4441(7) -1.0018(6) -0.3031(5) 0.070(5) Uiso 1 d . . . H5 H 0.4243 -1.0236 -0.3222 0.084 Uiso 1 calc R . . C11 C 0.8007(5) -0.5514(5) -0.1455(5) 0.049(4) Uiso 1 d . . . C12 C 0.8109(5) -0.5140(5) -0.1660(5) 0.049(4) Uiso 1 d . . . H12 H 0.8121 -0.5203 -0.1900 0.059 Uiso 1 calc R . . C13 C 0.8191(6) -0.4682(6) -0.1508(5) 0.064(5) Uiso 1 d . . . H13 H 0.8257 -0.4424 -0.1648 0.077 Uiso 1 calc R . . C14 C 0.8180(6) -0.4584(6) -0.1170(5) 0.058(4) Uiso 1 d . . . C15 C 0.8065(6) -0.4945(5) -0.0963(5) 0.055(4) Uiso 1 d . . . H15 H 0.8047 -0.4878 -0.0725 0.066 Uiso 1 calc R . . C16 C 0.7979(5) -0.5409(5) -0.1122(4) 0.046(4) Uiso 1 d . . . H16 H 0.7896 -0.5664 -0.0989 0.055 Uiso 1 calc R . . C17 C 0.8210(9) -0.3988(9) -0.0701(7) 0.116(8) Uiso 1 d . . . H17A H 0.8302 -0.3647 -0.0633 0.174 Uiso 1 calc R . . H17B H 0.8407 -0.4201 -0.0493 0.174 Uiso 1 calc R . . H17C H 0.7865 -0.4033 -0.0749 0.174 Uiso 1 calc R . . C21 C 0.8358(11) -0.6751(9) -0.2164(7) 0.029(10) Uiso 0.650(15) d PD A 1 C22 C 0.8872(9) -0.6691(9) -0.1963(7) 0.066(8) Uiso 0.650(15) d PD A 1 H22 H 0.8994 -0.6528 -0.1725 0.079 Uiso 0.650(15) calc PR A 1 C23 C 0.9186(10) -0.6866(10) -0.2114(8) 0.075(9) Uiso 0.650(15) d PD A 1 H23 H 0.9527 -0.6849 -0.1974 0.090 Uiso 0.650(15) calc PR A 1 C24 C 0.9003(11) -0.7071(10) -0.2474(9) 0.071(9) Uiso 0.650(15) d PD A 1 C25 C 0.8512(9) -0.7165(10) -0.2668(8) 0.059(8) Uiso 0.650(15) d PD A 1 H25 H 0.8395 -0.7340 -0.2901 0.071 Uiso 0.650(15) calc PR A 1 C26 C 0.8193(9) -0.6983(8) -0.2498(7) 0.055(7) Uiso 0.650(15) d PD A 1 H26 H 0.7853 -0.7028 -0.2627 0.066 Uiso 0.650(15) calc PR A 1 O2 O 0.9360(9) -0.7222(10) -0.2616(7) 0.118(9) Uiso 0.650(15) d PD A 1 C27 C 0.9183(14) -0.7354(15) -0.3006(10) 0.117(13) Uiso 0.650(15) d PD A 1 H27A H 0.9456 -0.7451 -0.3073 0.175 Uiso 0.650(15) calc PR A 1 H27B H 0.9015 -0.7075 -0.3162 0.175 Uiso 0.650(15) calc PR A 1 H27C H 0.8956 -0.7628 -0.3052 0.175 Uiso 0.650(15) calc PR A 1 C21' C 0.823(2) -0.6743(18) -0.2224(15) 0.06(3) Uiso 0.350(15) d PD A 2 C22' C 0.8475(14) -0.7200(12) -0.2182(11) 0.048(12) Uiso 0.350(15) d PD A 2 H22' H 0.8485 -0.7420 -0.1987 0.058 Uiso 0.350(15) calc PR A 2 C23' C 0.870(2) -0.7319(15) -0.2423(14) 0.079(17) Uiso 0.350(15) d PD A 2 H23' H 0.8855 -0.7626 -0.2398 0.095 Uiso 0.350(15) calc PR A 2 C24' C 0.870(2) -0.6995(16) -0.2703(15) 0.072(17) Uiso 0.350(15) d PD A 2 C25' C 0.8496(17) -0.6532(14) -0.2728(13) 0.074(16) Uiso 0.350(15) d PD A 2 H25' H 0.8492 -0.6308 -0.2919 0.089 Uiso 0.350(15) calc PR A 2 C26' C 0.8297(14) -0.6407(12) -0.2455(11) 0.047(12) Uiso 0.350(15) d PD A 2 H26' H 0.8212 -0.6077 -0.2435 0.057 Uiso 0.350(15) calc PR A 2 O2' O 0.8990(16) -0.7110(16) -0.2912(12) 0.124(17) Uiso 0.350(15) d PD A 2 C27' C 0.938(2) -0.745(3) -0.274(2) 0.13(3) Uiso 0.350(15) d PD A 2 H27D H 0.9552 -0.7499 -0.2910 0.194 Uiso 0.350(15) calc PR A 2 H27E H 0.9249 -0.7757 -0.2695 0.194 Uiso 0.350(15) calc PR A 2 H27F H 0.9605 -0.7311 -0.2499 0.194 Uiso 0.350(15) calc PR A 2 C31 C 0.8125(6) -0.6642(5) -0.0670(5) 0.049(4) Uiso 1 d . . . C32 C 0.8622(6) -0.6576(6) -0.0482(5) 0.058(4) Uiso 1 d . . . H32 H 0.8837 -0.6647 -0.0604 0.069 Uiso 1 calc R . . C33 C 0.8801(7) -0.6401(6) -0.0108(5) 0.070(5) Uiso 1 d . . . H33 H 0.9141 -0.6363 0.0028 0.084 Uiso 1 calc R . . C34 C 0.8503(7) -0.6289(7) 0.0055(6) 0.080(6) Uiso 1 d . . . C35 C 0.8007(7) -0.6333(6) -0.0119(5) 0.069(5) Uiso 1 d . . . H35 H 0.7799 -0.6249 0.0008 0.083 Uiso 1 calc R . . C36 C 0.7824(6) -0.6506(6) -0.0487(5) 0.059(4) Uiso 1 d . . . H36 H 0.7482 -0.6533 -0.0619 0.071 Uiso 1 calc R . . C37 C 0.9154(11) -0.6159(12) 0.0649(9) 0.166(12) Uiso 1 d . . . H37A H 0.9231 -0.6047 0.0909 0.249 Uiso 1 calc R . . H37B H 0.9324 -0.5955 0.0529 0.249 Uiso 1 calc R . . H37C H 0.9258 -0.6500 0.0653 0.249 Uiso 1 calc R . . C41 C 0.8182(12) -0.7900(8) -0.150(2) 0.039(4) Uiso 0.582(14) d PD B 1 C42 C 0.8455(8) -0.7960(7) -0.1729(7) 0.037(6) Uiso 0.582(14) d PD B 1 H42 H 0.8509 -0.7689 -0.1863 0.044 Uiso 0.582(14) calc PR B 1 C43 C 0.8642(8) -0.8412(8) -0.1756(7) 0.041(7) Uiso 0.582(14) d PD B 1 H43 H 0.8854 -0.8441 -0.1887 0.049 Uiso 0.582(14) calc PR B 1 C44 C 0.8531(12) -0.8818(10) -0.1600(10) 0.051(11) Uiso 0.582(14) d PD B 1 C45 C 0.8282(10) -0.8742(9) -0.1350(8) 0.064(9) Uiso 0.582(14) d PD B 1 H45 H 0.8245 -0.9001 -0.1198 0.077 Uiso 0.582(14) calc PR B 1 C46 C 0.8100(9) -0.8292(8) -0.1333(7) 0.046(7) Uiso 0.582(14) d PD B 1 H46 H 0.7899 -0.8258 -0.1192 0.055 Uiso 0.582(14) calc PR B 1 O4 O 0.8718(8) -0.9276(8) -0.1601(6) 0.061(6) Uiso 0.582(14) d PD B 1 C47 C 0.9008(10) -0.9327(10) -0.1808(8) 0.060(8) Uiso 0.582(14) d PD B 1 H47A H 0.9128 -0.9663 -0.1787 0.090 Uiso 0.582(14) calc PR B 1 H47B H 0.9284 -0.9102 -0.1710 0.090 Uiso 0.582(14) calc PR B 1 H47C H 0.8816 -0.9251 -0.2075 0.090 Uiso 0.582(14) calc PR B 1 C41' C 0.8205(15) -0.7847(11) -0.148(3) 0.039(4) Uiso 0.418(14) d PD B 2 C42' C 0.8714(10) -0.7912(10) -0.1291(10) 0.048(10) Uiso 0.418(14) d PD B 2 H42' H 0.8906 -0.7656 -0.1138 0.058 Uiso 0.418(14) calc PR B 2 C43' C 0.8932(11) -0.8338(11) -0.1326(10) 0.060(12) Uiso 0.418(14) d PD B 2 H43' H 0.9274 -0.8375 -0.1199 0.072 Uiso 0.418(14) calc PR B 2 C44' C 0.8662(11) -0.8706(10) -0.1542(12) 0.031(12) Uiso 0.418(14) d PD B 2 C45' C 0.8143(10) -0.8648(11) -0.1726(9) 0.048(10) Uiso 0.418(14) d PD B 2 H45' H 0.7945 -0.8901 -0.1878 0.058 Uiso 0.418(14) calc PR B 2 C46' C 0.7944(9) -0.8217(9) -0.1673(9) 0.032(8) Uiso 0.418(14) d PD B 2 H46' H 0.7600 -0.8183 -0.1783 0.038 Uiso 0.418(14) calc PR B 2 O4' O 0.8890(10) -0.9126(10) -0.1578(9) 0.074(11) Uiso 0.418(14) d PD B 2 C47' C 0.8594(19) -0.9495(17) -0.1794(18) 0.12(2) Uiso 0.418(14) d PD B 2 H47D H 0.8795 -0.9775 -0.1803 0.185 Uiso 0.418(14) calc PR B 2 H47E H 0.8414 -0.9376 -0.2052 0.185 Uiso 0.418(14) calc PR B 2 H47F H 0.8365 -0.9597 -0.1681 0.185 Uiso 0.418(14) calc PR B 2 C51 C 0.6184(5) -0.6954(5) 0.0061(5) 0.049(4) Uiso 1 d . . . C52 C 0.6330(8) -0.6535(8) 0.0266(6) 0.096(7) Uiso 1 d . . . H52 H 0.6095 -0.6300 0.0265 0.115 Uiso 1 calc R . . C53 C 0.6831(8) -0.6445(9) 0.0482(7) 0.104(7) Uiso 1 d . . . H53 H 0.6936 -0.6155 0.0627 0.125 Uiso 1 calc R . . C54 C 0.7157(6) -0.6796(6) 0.0472(5) 0.059(4) Uiso 1 d . . . C55 C 0.7023(5) -0.7197(5) 0.0258(4) 0.047(4) Uiso 1 d . . . H55 H 0.7257 -0.7427 0.0249 0.056 Uiso 1 calc R . . C56 C 0.6520(5) -0.7268(5) 0.0045(4) 0.044(4) Uiso 1 d . . . H56 H 0.6418 -0.7547 -0.0114 0.053 Uiso 1 calc R . . C57 C 0.8005(6) -0.7017(6) 0.0708(5) 0.068(5) Uiso 1 d . . . H57A H 0.8328 -0.6891 0.0866 0.102 Uiso 1 calc R . . H57B H 0.7991 -0.7081 0.0451 0.102 Uiso 1 calc R . . H57C H 0.7946 -0.7321 0.0818 0.102 Uiso 1 calc R . . C61 C 0.4897(9) -0.8188(10) -0.0377(8) 0.036(5) Uiso 0.514(11) d PD C 1 C62 C 0.4963(12) -0.8391(12) -0.0030(10) 0.078(8) Uiso 0.514(11) d PD C 1 H62 H 0.5128 -0.8219 0.0199 0.093 Uiso 0.514(11) calc PR C 1 C63 C 0.4779(16) -0.8855(14) -0.0029(11) 0.094(10) Uiso 0.514(11) d PD C 1 H63 H 0.4818 -0.9001 0.0206 0.113 Uiso 0.514(11) calc PR C 1 C64 C 0.4550(11) -0.9105(10) -0.0347(8) 0.063(7) Uiso 0.514(11) d PD C 1 C65 C 0.4524(15) -0.8923(13) -0.0694(11) 0.103(10) Uiso 0.514(11) d PD C 1 H65 H 0.4416 -0.9115 -0.0918 0.124 Uiso 0.514(11) calc PR C 1 C66 C 0.4674(13) -0.8426(12) -0.0686(10) 0.081(9) Uiso 0.514(11) d PD C 1 H66 H 0.4606 -0.8263 -0.0921 0.097 Uiso 0.514(11) calc PR C 1 O6 O 0.4382(10) -0.9580(9) -0.0350(8) 0.097(9) Uiso 0.514(11) d PD C 1 C67 C 0.4402(16) -0.9759(14) -0.0023(12) 0.091(10) Uiso 0.514(11) d PD C 1 H67A H 0.4273 -1.0093 -0.0061 0.137 Uiso 0.514(11) calc PR C 1 H67B H 0.4206 -0.9555 0.0074 0.137 Uiso 0.514(11) calc PR C 1 H67C H 0.4740 -0.9763 0.0159 0.137 Uiso 0.514(11) calc PR C 1 C61' C 0.4842(10) -0.7936(11) -0.0273(8) 0.036(5) Uiso 0.486(11) d PD C 2 C62' C 0.4915(13) -0.8032(14) 0.0100(10) 0.078(8) Uiso 0.486(11) d PD C 2 H62' H 0.5116 -0.7826 0.0299 0.093 Uiso 0.486(11) calc PR C 2 C63' C 0.4689(14) -0.8434(13) 0.0176(10) 0.094(10) Uiso 0.486(11) d PD C 2 H63' H 0.4668 -0.8464 0.0417 0.113 Uiso 0.486(11) calc PR C 2 C64' C 0.4498(14) -0.8783(11) -0.0084(9) 0.063(7) Uiso 0.486(11) d PD C 2 C65' C 0.4391(15) -0.8683(15) -0.0465(12) 0.103(10) Uiso 0.486(11) d PD C 2 H65' H 0.4223 -0.8907 -0.0661 0.124 Uiso 0.486(11) calc PR C 2 C66' C 0.4552(13) -0.8214(13) -0.0537(10) 0.081(9) Uiso 0.486(11) d PD C 2 H66' H 0.4440 -0.8102 -0.0792 0.097 Uiso 0.486(11) calc PR C 2 O6' O 0.4274(9) -0.9180(8) 0.0007(7) 0.083(8) Uiso 0.486(11) d PD C 2 C67' C 0.4234(17) -0.9591(14) -0.0180(15) 0.091(10) Uiso 0.486(11) d PD C 2 H67D H 0.4070 -0.9835 -0.0084 0.137 Uiso 0.486(11) calc PR C 2 H67E H 0.4558 -0.9710 -0.0146 0.137 Uiso 0.486(11) calc PR C 2 H67F H 0.4043 -0.9535 -0.0450 0.137 Uiso 0.486(11) calc PR C 2 Mo5 Mo 0.5275(3) -0.6534(2) -0.0633(3) 0.0320(15) Uani 0.663(9) d PD . 1 Mo6 Mo 0.4693(2) -0.7030(2) -0.08060(19) 0.0333(12) Uani 0.663(9) d PD C 1 C71 C 0.5245(8) -0.5766(9) -0.0034(5) 0.032(5) Uiso 0.663(9) d PD C 1 C72 C 0.5458(7) -0.5378(8) -0.0151(6) 0.037(5) Uiso 0.663(9) d PD C 1 H72 H 0.5413 -0.5347 -0.0410 0.044 Uiso 0.663(9) calc PR . 1 C73 C 0.5730(8) -0.5044(9) 0.0108(7) 0.054(6) Uiso 0.663(9) d PD C 1 H73 H 0.5894 -0.4793 0.0033 0.065 Uiso 0.663(9) calc PR . 1 C74 C 0.5770(8) -0.5070(8) 0.0480(6) 0.044(6) Uiso 0.663(9) d PD C 1 C75 C 0.5562(13) -0.5451(10) 0.0615(9) 0.060(8) Uiso 0.663(9) d PD C 1 H75 H 0.5598 -0.5474 0.0872 0.072 Uiso 0.663(9) calc PR . 1 C76 C 0.5306(8) -0.5787(8) 0.0346(6) 0.041(5) Uiso 0.663(9) d PD C 1 H76 H 0.5159 -0.6051 0.0423 0.050 Uiso 0.663(9) calc PR . 1 O7 O 0.6032(8) -0.4702(7) 0.0717(6) 0.068(7) Uiso 0.663(9) d PD C 1 C77 C 0.6006(10) -0.4655(9) 0.1077(7) 0.065(7) Uiso 0.663(9) d PD C 1 H77A H 0.6210 -0.4381 0.1213 0.098 Uiso 0.663(9) calc PR . 1 H77B H 0.6121 -0.4957 0.1221 0.098 Uiso 0.663(9) calc PR . 1 H77C H 0.5668 -0.4594 0.1044 0.098 Uiso 0.663(9) calc PR . 1 N7 N 0.4982(6) -0.6121(8) -0.0307(5) 0.043(5) Uiso 0.663(9) d PD C 1 C4 C 0.4570(9) -0.6277(10) -0.0292(7) 0.051(7) Uiso 0.663(9) d PD C 1 H4 H 0.4445 -0.6124 -0.0126 0.061 Uiso 0.663(9) calc PR . 1 N8 N 0.4324(6) -0.6659(9) -0.0515(6) 0.041(5) Uiso 0.663(9) d PD C 1 C81 C 0.3845(7) -0.6767(9) -0.0535(7) 0.046(6) Uiso 0.663(9) d PD C 1 C82 C 0.3692(9) -0.7223(11) -0.0570(8) 0.065(8) Uiso 0.663(9) d PD C 1 H82 H 0.3895 -0.7479 -0.0593 0.078 Uiso 0.663(9) calc PR . 1 C83 C 0.3219(10) -0.7334(10) -0.0575(9) 0.082(9) Uiso 0.663(9) d PD C 1 H83 H 0.3091 -0.7656 -0.0615 0.099 Uiso 0.663(9) calc PR . 1 C84 C 0.2977(10) -0.6969(10) -0.0523(9) 0.073(8) Uiso 0.663(9) d PD C 1 C85 C 0.3099(10) -0.6513(10) -0.0460(9) 0.083(9) Uiso 0.663(9) d PD C 1 H85 H 0.2898 -0.6271 -0.0416 0.100 Uiso 0.663(9) calc PR . 1 C86 C 0.3574(10) -0.6411(11) -0.0465(9) 0.086(9) Uiso 0.663(9) d PD C 1 H86 H 0.3698 -0.6088 -0.0418 0.103 Uiso 0.663(9) calc PR . 1 O8 O 0.2485(9) -0.7062(9) -0.0527(8) 0.128(9) Uiso 0.663(9) d PD C 1 C87 C 0.2319(19) -0.7566(18) -0.0607(17) 0.20(2) Uiso 0.663(9) d PD C 1 H87A H 0.1993 -0.7595 -0.0605 0.300 Uiso 0.663(9) calc PR . 1 H87B H 0.2543 -0.7780 -0.0412 0.300 Uiso 0.663(9) calc PR . 1 H87C H 0.2312 -0.7661 -0.0856 0.300 Uiso 0.663(9) calc PR . 1 Mo5' Mo 0.5242(6) -0.6693(4) -0.0630(5) 0.028(3) Uani 0.337(9) d PD C 2 Mo6' Mo 0.4694(4) -0.7220(3) -0.0840(4) 0.025(2) Uani 0.337(9) d PD C 2 C71' C 0.5118(12) -0.5989(13) -0.0020(7) 0.032(5) Uiso 0.337(9) d PD C 2 C72' C 0.5355(15) -0.5580(13) -0.0085(9) 0.037(5) Uiso 0.337(9) d PD C 2 H72' H 0.5374 -0.5528 -0.0324 0.044 Uiso 0.337(9) calc PR . 2 C73' C 0.5561(16) -0.5252(13) 0.0209(10) 0.054(6) Uiso 0.337(9) d PD C 2 H73' H 0.5695 -0.4955 0.0164 0.065 Uiso 0.337(9) calc PR . 2 C74' C 0.557(2) -0.5353(15) 0.0564(12) 0.044(6) Uiso 0.337(9) d PD C 2 C75' C 0.5340(16) -0.5763(13) 0.0647(10) 0.060(8) Uiso 0.337(9) d PD C 2 H75' H 0.5326 -0.5820 0.0888 0.072 Uiso 0.337(9) calc PR . 2 C76' C 0.5139(14) -0.6067(13) 0.0346(8) 0.041(5) Uiso 0.337(9) d PD C 2 H76' H 0.4999 -0.6362 0.0389 0.050 Uiso 0.337(9) calc PR . 2 O7' O 0.5752(13) -0.5018(11) 0.0854(9) 0.088(12) Uiso 0.337(9) d PD C 2 C77' C 0.600(2) -0.4605(18) 0.0795(19) 0.065(7) Uiso 0.337(9) d PD C 2 H77D H 0.6103 -0.4398 0.1021 0.098 Uiso 0.337(9) calc PR . 2 H77E H 0.5776 -0.4420 0.0577 0.098 Uiso 0.337(9) calc PR . 2 H77F H 0.6280 -0.4711 0.0745 0.098 Uiso 0.337(9) calc PR . 2 N7' N 0.4893(9) -0.6331(11) -0.0317(7) 0.024(9) Uiso 0.337(9) d PD C 2 C4' C 0.4459(12) -0.6501(16) -0.0354(12) 0.042(14) Uiso 0.337(9) d PD C 2 H4' H 0.4281 -0.6341 -0.0228 0.050 Uiso 0.337(9) calc PR . 2 N8' N 0.4267(8) -0.6905(13) -0.0572(8) 0.028(9) Uiso 0.337(9) d PD C 2 C81' C 0.3768(10) -0.7039(13) -0.0667(12) 0.034(11) Uiso 0.337(9) d PD C 2 C82' C 0.3639(12) -0.7503(14) -0.0733(15) 0.060(14) Uiso 0.337(9) d PD C 2 H82' H 0.3879 -0.7748 -0.0691 0.072 Uiso 0.337(9) calc PR . 2 C83' C 0.3135(12) -0.7633(13) -0.0866(14) 0.059(14) Uiso 0.337(9) d PD C 2 H83' H 0.3027 -0.7958 -0.0937 0.071 Uiso 0.337(9) calc PR . 2 C84' C 0.2834(13) -0.7283(15) -0.0884(18) 0.090(19) Uiso 0.337(9) d PD C 2 C85' C 0.2912(14) -0.6817(15) -0.0834(19) 0.10(2) Uiso 0.337(9) d PD C 2 H85' H 0.2663 -0.6577 -0.0898 0.124 Uiso 0.337(9) calc PR . 2 C86' C 0.3433(12) -0.6707(14) -0.0668(15) 0.067(15) Uiso 0.337(9) d PD C 2 H86' H 0.3538 -0.6395 -0.0558 0.080 Uiso 0.337(9) calc PR . 2 O8' O 0.2315(14) -0.7414(17) -0.0979(18) 0.16(2) Uiso 0.337(9) d PD C 2 C87' C 0.197(2) -0.702(3) -0.116(3) 0.20(2) Uiso 0.337(9) d PD C 2 H87D H 0.1637 -0.7138 -0.1213 0.300 Uiso 0.337(9) calc PR . 2 H87E H 0.1995 -0.6933 -0.1400 0.300 Uiso 0.337(9) calc PR . 2 H87F H 0.2039 -0.6739 -0.0993 0.300 Uiso 0.337(9) calc PR . 2 C91 C 0.3855(8) -1.0143(10) -0.2767(7) 0.042(6) Uiso 0.624(14) d PD D 1 C92 C 0.3762(10) -1.0618(9) -0.2841(8) 0.065(8) Uiso 0.624(14) d PD D 1 H92 H 0.3997 -1.0829 -0.2871 0.078 Uiso 0.624(14) calc PR D 1 C93 C 0.3299(10) -1.0796(10) -0.2873(9) 0.075(8) Uiso 0.624(14) d PD D 1 H93 H 0.3224 -1.1132 -0.2928 0.090 Uiso 0.624(14) calc PR D 1 C94 C 0.2983(9) -1.0519(10) -0.2830(8) 0.065(8) Uiso 0.624(14) d PD D 1 C95 C 0.3071(10) -1.0074(11) -0.2726(9) 0.067(7) Uiso 0.624(14) d PD D 1 H95 H 0.2842 -0.9887 -0.2666 0.080 Uiso 0.624(14) calc PR D 1 C96 C 0.3522(8) -0.9863(9) -0.2700(7) 0.046(7) Uiso 0.624(14) d PD D 1 H96 H 0.3587 -0.9527 -0.2637 0.055 Uiso 0.624(14) calc PR D 1 O9 O 0.2510(8) -1.0751(7) -0.2898(6) 0.091(7) Uiso 0.624(14) d PD D 1 C97 C 0.2136(12) -1.0420(12) -0.2883(12) 0.071(10) Uiso 0.624(14) d PD D 1 H97A H 0.1836 -1.0604 -0.2930 0.107 Uiso 0.624(14) calc PR D 1 H97B H 0.2074 -1.0167 -0.3077 0.107 Uiso 0.624(14) calc PR D 1 H97C H 0.2245 -1.0267 -0.2632 0.107 Uiso 0.624(14) calc PR D 1 C91' C 0.3785(11) -0.9849(17) -0.2794(11) 0.053(12) Uiso 0.376(14) d PD D 2 C92' C 0.3466(14) -1.0189(16) -0.2987(13) 0.084(16) Uiso 0.376(14) d PD D 2 H92' H 0.3538 -1.0421 -0.3142 0.100 Uiso 0.376(14) calc PR D 2 C93' C 0.3007(15) -1.0188(16) -0.2947(14) 0.075(8) Uiso 0.376(14) d PD D 2 H93' H 0.2774 -1.0432 -0.3071 0.090 Uiso 0.376(14) calc PR D 2 C94' C 0.2907(13) -0.9867(14) -0.2751(12) 0.056(13) Uiso 0.376(14) d PD D 2 C95' C 0.3185(12) -0.9515(14) -0.2580(13) 0.067(7) Uiso 0.376(14) d PD D 2 H95' H 0.3092 -0.9282 -0.2437 0.080 Uiso 0.376(14) calc PR D 2 C96' C 0.3646(13) -0.9490(15) -0.2614(13) 0.070(14) Uiso 0.376(14) d PD D 2 H96' H 0.3855 -0.9220 -0.2509 0.084 Uiso 0.376(14) calc PR D 2 O9' O 0.2450(12) -0.9940(14) -0.2688(12) 0.117(15) Uiso 0.376(14) d PD D 2 C97' C 0.229(3) -1.045(3) -0.272(3) 0.18(5) Uiso 0.376(14) d PD D 2 H97D H 0.1992 -1.0473 -0.2674 0.263 Uiso 0.376(14) calc PR D 2 H97E H 0.2545 -1.0649 -0.2539 0.263 Uiso 0.376(14) calc PR D 2 H97F H 0.2227 -1.0566 -0.2980 0.263 Uiso 0.376(14) calc PR D 2 C101 C 0.5014(5) -1.0030(5) -0.1663(5) 0.046(4) Uiso 1 d . . . C102 C 0.4577(6) -1.0166(6) -0.1704(5) 0.059(4) Uiso 1 d . . . H102 H 0.4333 -1.0166 -0.1954 0.071 Uiso 1 calc R . . C103 C 0.4445(7) -1.0308(6) -0.1411(5) 0.068(5) Uiso 1 d . . . H103 H 0.4116 -1.0393 -0.1462 0.082 Uiso 1 calc R . . C104 C 0.4775(7) -1.0328(6) -0.1059(6) 0.069(5) Uiso 1 d . . . C105 C 0.5239(10) -1.0159(9) -0.0998(8) 0.120(8) Uiso 1 d . . . H105 H 0.5478 -1.0140 -0.0747 0.144 Uiso 1 calc R . . C106 C 0.5353(9) -1.0019(8) -0.1296(7) 0.108(7) Uiso 1 d . . . H106 H 0.5674 -0.9913 -0.1250 0.129 Uiso 1 calc R . . C107 C 0.4239(7) -1.0632(7) -0.0783(6) 0.084(6) Uiso 1 d . . . H10A H 0.4237 -1.0707 -0.0534 0.126 Uiso 1 calc R . . H10B H 0.4166 -1.0928 -0.0939 0.126 Uiso 1 calc R . . H10C H 0.3993 -1.0383 -0.0907 0.126 Uiso 1 calc R . . Mo4 Mo 0.4721(4) -0.4291(2) -0.28498(19) 0.0280(13) Uani 0.50 d PD . -1 N11 N 0.5085(7) -0.3782(7) -0.3065(7) 0.031(5) Uiso 0.50 d PD E -1 C111 C 0.4894(10) -0.3561(9) -0.3431(9) 0.042(8) Uiso 0.50 d PD E -1 C112 C 0.4934(10) -0.3095(9) -0.3506(9) 0.050(8) Uiso 0.50 d PD E -1 H112 H 0.5082 -0.2875 -0.3301 0.060 Uiso 0.50 calc PR E -1 C113 C 0.4759(14) -0.2912(13) -0.3885(11) 0.080(13) Uiso 0.50 d PD E -1 H113 H 0.4826 -0.2583 -0.3926 0.096 Uiso 0.50 calc PR E -1 C114 C 0.4516(13) -0.3176(12) -0.4168(10) 0.095(13) Uiso 0.50 d PD E -1 C115 C 0.4486(13) -0.3648(13) -0.4100(10) 0.088(9) Uiso 0.50 d PD E -1 H115 H 0.4318 -0.3851 -0.4312 0.106 Uiso 0.50 calc PR E -1 C116 C 0.4675(11) -0.3873(11) -0.3749(9) 0.069(10) Uiso 0.50 d PD E -1 H116 H 0.4659 -0.4217 -0.3722 0.083 Uiso 0.50 calc PR E -1 O11 O 0.4128(11) -0.2891(13) -0.4519(10) 0.135(13) Uiso 0.50 d PD E -1 C117 C 0.455(2) -0.260(2) -0.4661(17) 0.20(3) Uiso 0.50 d PD E -1 H11A H 0.4382 -0.2393 -0.4883 0.294 Uiso 0.50 calc PR E -1 H11B H 0.4748 -0.2842 -0.4725 0.294 Uiso 0.50 calc PR E -1 H11C H 0.4767 -0.2392 -0.4453 0.294 Uiso 0.50 calc PR E -1 C6 C 0.4476(9) -0.3533(9) -0.2407(8) 0.035(7) Uiso 0.50 d PD F -1 H6 H 0.4297 -0.3281 -0.2349 0.042 Uiso 0.50 calc PR F -1 N12 N 0.4307(6) -0.3740(6) -0.2742(7) 0.032(6) Uiso 0.50 d PD F -1 C121 C 0.3831(9) -0.3583(11) -0.2975(10) 0.038(8) Uiso 0.50 d PD F -1 C122 C 0.3466(8) -0.3500(9) -0.2833(8) 0.034(7) Uiso 0.50 d PD F -1 H122 H 0.3554 -0.3531 -0.2568 0.040 Uiso 0.50 calc PR F -1 C123 C 0.3013(13) -0.338(2) -0.3038(13) 0.089(11) Uiso 0.50 d PD F -1 H123 H 0.2778 -0.3342 -0.2930 0.106 Uiso 0.50 calc PR F -1 C124 C 0.2899(8) -0.3326(9) -0.3423(7) 0.027(6) Uiso 0.50 d PD F -1 C125 C 0.3248(10) -0.3399(12) -0.3594(10) 0.066(7) Uiso 0.50 d PD F -1 H125 H 0.3172 -0.3363 -0.3858 0.079 Uiso 0.50 calc PR F -1 C126 C 0.3709(8) -0.3526(9) -0.3334(8) 0.036(7) Uiso 0.50 d PD F -1 H126 H 0.3955 -0.3574 -0.3430 0.043 Uiso 0.50 calc PR F -1 O12 O 0.2436(6) -0.3173(7) -0.3704(6) 0.047(5) Uiso 0.50 d PD F -1 C127 C 0.2055(9) -0.3095(12) -0.3585(10) 0.059(9) Uiso 0.50 d PD F -1 H12A H 0.1764 -0.2992 -0.3801 0.088 Uiso 0.50 calc PR F -1 H12B H 0.2147 -0.2840 -0.3390 0.088 Uiso 0.50 calc PR F -1 H12C H 0.1985 -0.3399 -0.3479 0.088 Uiso 0.50 calc PR F -1 Mo4B Mo 0.5270(4) -0.4256(2) -0.23025(18) 0.0299(15) Uani 0.50 d PD . -1 N11B N 0.4910(7) -0.3681(7) -0.2143(7) 0.039(6) Uiso 0.50 d PD F -1 C11O C 0.5069(10) -0.3408(9) -0.1801(9) 0.050(8) Uiso 0.50 d PD F -1 C11P C 0.4976(11) -0.2939(9) -0.1765(9) 0.053(8) Uiso 0.50 d PD F -1 H11R H 0.4770 -0.2765 -0.1983 0.064 Uiso 0.50 calc PR F -1 C11Q C 0.5175(12) -0.2686(12) -0.1411(10) 0.074(11) Uiso 0.50 d PD F -1 H11S H 0.5078 -0.2359 -0.1393 0.088 Uiso 0.50 calc PR F -1 C11R C 0.5480(13) -0.2897(11) -0.1119(9) 0.055(10) Uiso 0.50 d PD F -1 C11T C 0.5575(13) -0.3368(12) -0.1139(10) 0.088(9) Uiso 0.50 d PD F -1 H11T H 0.5787 -0.3525 -0.0915 0.106 Uiso 0.50 calc PR F -1 C11U C 0.5387(11) -0.3643(11) -0.1466(9) 0.057(9) Uiso 0.50 d PD F -1 H11U H 0.5467 -0.3979 -0.1467 0.069 Uiso 0.50 calc PR F -1 O11B O 0.5671(10) -0.2591(10) -0.0746(8) 0.100(9) Uiso 0.50 d PD F -1 C11V C 0.5620(18) -0.3055(14) -0.0444(12) 0.105(15) Uiso 0.50 d PD F -1 H11V H 0.5728 -0.2929 -0.0184 0.157 Uiso 0.50 calc PR F -1 H11W H 0.5824 -0.3333 -0.0450 0.157 Uiso 0.50 calc PR F -1 H11X H 0.5280 -0.3161 -0.0529 0.157 Uiso 0.50 calc PR F -1 C6'A C 0.5525(9) -0.3628(9) -0.2813(8) 0.042(8) Uiso 0.50 d PD E -1 H6'A H 0.5710 -0.3411 -0.2898 0.051 Uiso 0.50 calc PR E -1 N12B N 0.5703(6) -0.3767(7) -0.2456(8) 0.036(6) Uiso 0.50 d PD E -1 C12O C 0.6193(9) -0.3633(10) -0.2248(9) 0.049(8) Uiso 0.50 d PD E -1 C12P C 0.6551(9) -0.3653(12) -0.2405(9) 0.062(9) Uiso 0.50 d PD E -1 H12R H 0.6457 -0.3760 -0.2660 0.075 Uiso 0.50 calc PR E -1 C12Q C 0.7008(12) -0.3530(15) -0.2216(11) 0.089(11) Uiso 0.50 d PD E -1 H12S H 0.7246 -0.3559 -0.2324 0.106 Uiso 0.50 calc PR E -1 C12R C 0.7123(10) -0.3358(14) -0.1853(9) 0.047(9) Uiso 0.50 d PD E -1 C12T C 0.6790(10) -0.3332(12) -0.1663(10) 0.066(7) Uiso 0.50 d PD E -1 H12T H 0.6871 -0.3218 -0.1411 0.079 Uiso 0.50 calc PR E -1 C12U C 0.6328(10) -0.3499(13) -0.1902(10) 0.057(11) Uiso 0.50 d PD E -1 H12U H 0.6090 -0.3515 -0.1795 0.068 Uiso 0.50 calc PR E -1 O12B O 0.7608(9) -0.3199(13) -0.1595(10) 0.136(12) Uiso 0.50 d PD E -1 C12V C 0.7977(3) -0.3228(3) -0.1734(2) 0.16(2) Uiso 0.50 d PD E -1 H12V H 0.8282 -0.3109 -0.1540 0.236 Uiso 0.50 calc PR E -1 H12W H 0.7891 -0.3026 -0.1962 0.236 Uiso 0.50 calc PR E -1 H12X H 0.8017 -0.3568 -0.1796 0.236 Uiso 0.50 calc PR E -1 C301 C 0.6719(3) -0.6312(3) -0.2300(2) 0.031(3) Uiso 1 d R . . C302 C 0.6294(3) -0.6080(3) -0.2598(2) 0.037(3) Uiso 1 d R . . C303 C 0.6086(3) -0.5674(3) -0.2520(2) 0.037(3) Uiso 1 d R . . H303 H 0.6217 -0.5535 -0.2274 0.044 Uiso 1 calc R . . C304 C 0.5673(5) -0.5455(5) -0.2806(4) 0.038(4) Uiso 1 d . . . C305 C 0.5488(5) -0.5676(5) -0.3159(4) 0.040(4) Uiso 1 d . . . H305 H 0.5206 -0.5543 -0.3351 0.048 Uiso 1 calc R . . C306 C 0.5698(5) -0.6077(5) -0.3236(4) 0.036(3) Uiso 1 d . . . C307 C 0.6096(5) -0.6293(5) -0.2963(4) 0.036(3) Uiso 1 d . . . H307 H 0.6235 -0.6581 -0.3018 0.043 Uiso 1 calc R . . C308 C 0.5464(5) -0.5024(5) -0.2695(4) 0.041(4) Uiso 1 d . . . C309 C 0.5471(5) -0.6324(5) -0.3619(4) 0.046(4) Uiso 1 d . . . C401 C 0.6716(5) -0.7283(5) -0.1646(4) 0.035(3) Uiso 1 d . . . C402 C 0.6278(5) -0.7534(5) -0.1618(4) 0.037(3) Uiso 1 d . . . C403 C 0.6093(5) -0.7948(5) -0.1833(4) 0.040(4) Uiso 1 d . . . H403 H 0.6235 -0.8073 -0.1998 0.048 Uiso 1 calc R . . C404 C 0.5687(6) -0.8181(5) -0.1800(5) 0.053(4) Uiso 1 d . . . C405 C 0.5477(6) -0.7978(5) -0.1569(4) 0.052(4) Uiso 1 d . . . H405 H 0.5204 -0.8133 -0.1547 0.062 Uiso 1 calc R . . C406 C 0.5660(5) -0.7549(5) -0.1368(4) 0.038(3) Uiso 1 d . . . C407 C 0.6062(5) -0.7335(5) -0.1390(4) 0.036(3) Uiso 1 d . . . H407 H 0.6194 -0.7048 -0.1248 0.044 Uiso 1 calc R . . C408 C 0.5426(5) -0.7318(5) -0.1135(4) 0.043(4) Uiso 1 d . . . C409 C 0.5466(6) -0.8620(6) -0.2034(5) 0.054(4) Uiso 1 d . . . N1S N 0.5628(9) -0.1997(10) -0.4016(7) 0.150(9) Uiso 1 d . G 1 C1S C 0.5637(14) -0.2484(15) -0.4067(11) 0.079(11) Uiso 0.50 d P G 1 C2S C 0.5564(17) -0.2982(17) -0.4183(14) 0.107(10) Uiso 0.50 d P G 1 C1S' C 0.5512(16) -0.1741(17) -0.3831(14) 0.097(14) Uiso 0.50 d P G 1 C2S' C 0.5405(17) -0.1596(17) -0.3460(14) 0.107(10) Uiso 0.50 d P G 1 N2S N 0.7690(8) -0.2703(9) -0.2503(7) 0.142(8) Uiso 1 d . . . C3S C 0.7739(12) -0.3113(13) -0.2594(9) 0.151(11) Uiso 1 d . . . C4S C 0.7860(15) -0.3641(16) -0.2658(12) 0.206(16) Uiso 1 d . . . N3S N 0.8989(6) -0.1008(6) -0.4434(5) 0.083(5) Uiso 1 d . . . C5S C 0.8633(10) -0.0807(9) -0.4569(7) 0.109(8) Uiso 1 d . . . C6S C 0.8154(12) -0.0540(12) -0.4771(10) 0.165(12) Uiso 1 d . . . N4S N 0.8173(6) -0.0808(6) -0.3842(5) 0.089(5) Uiso 1 d . . . C7S C 0.8582(7) -0.0881(6) -0.3676(6) 0.071(5) Uiso 1 d . . . C8S C 0.9080(7) -0.0944(7) -0.3447(6) 0.081(6) Uiso 1 d . . . N5S N 1.1965(13) -0.1723(13) -0.3361(11) 0.102(11) Uiso 0.50 d P H 1 C9S C 1.2340(13) -0.1787(12) -0.3461(10) 0.064(9) Uiso 0.50 d P H 1 C10S C 1.2694(13) -0.1812(13) -0.3535(10) 0.067(10) Uiso 0.50 d P H 1 C53S C 0.277(2) -0.514(2) -0.0974(18) 0.039(15) Uiso 0.25 d P I 1 Cl7 Cl 0.2870(8) -0.4758(8) -0.1046(7) 0.083(6) Uiso 0.25 d P I 1 Cl8 Cl 0.2899(10) -0.5426(10) -0.0529(8) 0.118(8) Uiso 0.25 d P I 1 N6S N 0.281(3) -0.483(3) -0.078(2) 0.11(3) Uiso 0.25 d P J 2 C11S C 0.260(4) -0.544(4) -0.104(3) 0.08(3) Uiso 0.25 d P J 2 C12S C 0.269(3) -0.554(3) -0.117(2) 0.05(2) Uiso 0.25 d P J 2 N7S N 0.3957(7) -0.4618(6) -0.3470(6) 0.026(6) Uiso 0.521(19) d PD K 1 C13S C 0.3610(13) -0.4659(16) -0.3397(13) 0.102(14) Uiso 0.521(19) d PD K 1 C14S C 0.3189(15) -0.4716(18) -0.3267(15) 0.107(16) Uiso 0.521(19) d PD K 1 N8S N 0.2809(11) -0.4427(11) -0.2575(9) 0.093(10) Uiso 0.57(2) d PD L 2 C15S C 0.2948(12) -0.4564(12) -0.2800(9) 0.075(10) Uiso 0.57(2) d PD L 2 C16S C 0.3064(11) -0.4725(11) -0.3136(8) 0.054(8) Uiso 0.57(2) d PD L 2 N9S N 0.2867(13) -0.4415(13) -0.4310(10) 0.081(13) Uiso 0.41(2) d PD M 3 C17S C 0.3188(14) -0.4624(15) -0.4083(12) 0.074(14) Uiso 0.41(2) d PD M 3 C18S C 0.3665(12) -0.4645(12) -0.3734(11) 0.046(10) Uiso 0.41(2) d PD M 3 C19S C 0.3306(13) -0.9100(13) -0.3607(10) 0.122(11) Uiso 0.80 d P . . N10S N 0.2005(13) -0.3965(13) -0.1509(10) 0.098(11) Uiso 0.50 d P . 1 C20S C 0.3658(13) -0.9169(12) -0.3695(10) 0.065(10) Uiso 0.50 d P N 1 N11S N 0.343(2) -0.977(2) -0.3810(18) 0.098(18) Uiso 0.30 d P N 2 C21S C 0.336(2) -0.948(2) -0.3699(17) 0.058(15) Uiso 0.30 d P N 2 N12S N 0.4014(16) -0.4445(15) -0.4482(13) 0.120(13) Uiso 0.50 d P . . C23S C 0.4300(19) -0.4678(19) -0.4239(16) 0.113(16) Uiso 0.50 d P . . C24S C 0.4679(12) -0.4922(12) -0.3925(10) 0.060(9) Uiso 0.50 d P . . N13S N 0.152(2) -0.588(3) -0.1059(19) 0.20(3) Uiso 0.50 d P . . C25S C 0.141(3) -0.626(3) -0.115(2) 0.16(3) Uiso 0.50 d P . . C26S C 0.087(5) -0.644(4) -0.111(3) 0.32(6) Uiso 0.50 d P . . C51S C 0.4274(16) -0.8065(16) -0.2012(13) 0.093(13) Uiso 0.50 d P . 1 Cl1 Cl 0.8775(7) -0.2755(7) -0.2255(5) 0.153(6) Uiso 0.50 d P . 1 Cl2 Cl 0.4151(6) -0.8639(7) -0.1779(5) 0.153(6) Uiso 0.50 d P . 1 N14S N 0.3876(10) -0.7791(10) -0.1563(8) 0.061(7) Uiso 0.50 d P . 2 C27S C 0.3940(12) -0.7725(11) -0.1808(10) 0.054(8) Uiso 0.50 d P . 2 C28S C 0.910(2) -0.2599(19) -0.2108(15) 0.107(15) Uiso 0.50 d P . 2 N15S N 0.4003(11) -0.9054(11) -0.2042(10) 0.073(9) Uiso 0.50 d P O 3 C29S C 0.4206(12) -0.9055(12) -0.1731(11) 0.051(8) Uiso 0.50 d P O 3 C30S C 0.4423(16) -0.8975(16) -0.1328(13) 0.094(13) Uiso 0.50 d P O 3 C52S C 0.5386(15) -0.6822(15) -0.2461(12) 0.160(14) Uiso 0.80 d P . . Cl3 Cl 0.5000 -0.6320(11) -0.2500 0.102(8) Uiso 0.30 d SP . . Cl4 Cl 0.5038(10) -0.7302(10) -0.2325(7) 0.115(8) Uiso 0.25 d P . . Cl5 Cl 0.4951(10) -0.6528(10) -0.2271(8) 0.114(8) Uiso 0.25 d P . . Cl6 Cl 0.4989(17) -0.7036(17) -0.2122(14) 0.117(14) Uiso 0.15 d P . . N16S N 1.0385(17) -0.6193(15) -0.1945(13) 0.122(14) Uiso 0.50 d P . . C31S C 1.0067(15) -0.6226(14) -0.2177(13) 0.073(11) Uiso 0.50 d P . . C32S C 1.0000 -0.608(2) -0.2500 0.23(3) Uiso 1 d S . . N17S N 0.793(2) -0.4919(18) -0.0029(17) 0.143(19) Uiso 0.50 d P . . C33S C 0.818(3) -0.496(2) 0.021(3) 0.13(2) Uiso 0.50 d P . . C34S C 0.820(4) -0.505(4) 0.044(3) 0.26(6) Uiso 0.50 d P . . N18S N 0.262(4) -0.627(4) 0.014(3) 0.32(5) Uiso 0.50 d P . . C35S C 0.302(2) -0.642(2) 0.0278(17) 0.127(18) Uiso 0.50 d P . . C36S C 0.2895(12) -0.3364(12) -0.4374(10) 0.059(9) Uiso 0.50 d P . . N19S N 0.313(2) -0.829(2) 0.0101(17) 0.17(2) Uiso 0.50 d P . . C37S C 0.343(6) -0.811(6) 0.011(4) 0.35(8) Uiso 0.50 d P . . C38S C 0.350(3) -0.864(3) 0.023(2) 0.18(3) Uiso 0.50 d P . . 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 0.0250(7) 0.0368(7) 0.0299(9) -0.0004(6) 0.0001(7) -0.0013(5) Mo2 0.0209(6) 0.0397(7) 0.0382(10) -0.0037(6) 0.0013(7) 0.0025(5) Mo3 0.0376(7) 0.0335(7) 0.0433(10) 0.0045(6) 0.0077(7) 0.0040(6) Mo5 0.0247(17) 0.043(4) 0.0218(19) -0.001(3) 0.0014(14) -0.002(2) Mo6 0.0275(14) 0.042(3) 0.028(2) 0.005(2) 0.0073(14) -0.001(2) Mo5' 0.028(4) 0.029(6) 0.025(4) 0.001(5) 0.009(3) 0.001(4) Mo6' 0.024(3) 0.028(5) 0.022(3) -0.006(4) 0.008(2) -0.003(4) Mo4 0.0301(18) 0.0289(19) 0.022(4) 0.002(2) 0.006(3) 0.0020(15) Mo4B 0.0303(18) 0.0315(19) 0.023(5) 0.001(2) 0.005(4) -0.0027(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo2 2.0992(17) . y Mo1 N3 2.101(12) . ? Mo1 N1 2.113(10) . ? Mo1 O303 2.115(8) . ? Mo1 O301 2.117(9) . ? Mo2 N4 2.111(12) . ? Mo2 N2 2.112(11) . ? Mo2 O302 2.137(9) . ? Mo2 O304 2.149(8) . ? Mo3 O309 2.089(10) . ? Mo3 Mo3 2.098(2) 2_654 y Mo3 N10 2.113(12) . ? Mo3 N9 2.121(14) . ? Mo3 O310 2.130(10) 2_654 ? N1 C1 1.301(16) . ? N1 C11 1.444(18) . ? N2 C1 1.328(17) . ? N2 C21' 1.34(3) . ? N2 C21 1.46(2) . ? N3 C2 1.312(16) . ? N3 C31 1.428(18) . ? N4 C2 1.303(17) . ? N4 C41' 1.36(3) . ? N4 C41 1.48(2) . ? N5 C3 1.279(19) . ? N5 C51 1.432(19) . ? N5 Mo5' 1.99(2) . ? N5 Mo5 2.205(16) . ? N6 C61' 1.30(3) . ? N6 C3 1.35(2) . ? N6 C61 1.74(3) . ? N6 Mo6' 1.951(19) . ? N6 Mo6 2.179(15) . ? N9 C5 1.31(2) . ? N9 C91' 1.46(3) . ? N9 C91 1.49(2) . ? N10 C5 1.338(19) 2_654 ? N10 C101 1.378(18) . ? O1 C14 1.398(19) . ? O1 C17 1.41(2) . ? O3 C34 1.43(2) . ? O3 C37 1.44(3) . ? O5 C54 1.409(19) . ? O5 C57 1.438(19) . ? O10 C104 1.37(2) . ? O10 C107 1.39(2) . ? O301 C301 1.290(11) . ? O302 C301 1.255(11) . ? O303 C401 1.265(15) . ? O304 C401 1.231(14) . ? O305 C408 1.251(16) . ? O305 Mo5' 2.064(16) . ? O305 Mo5 2.171(11) . ? O306 C408 1.295(16) . ? O306 Mo6' 1.923(14) . ? O306 Mo6 2.270(11) . ? O307 C308 1.235(15) . ? O307 Mo4B 2.061(11) . ? O307 Mo4 2.245(11) 2_654 ? O308 C308 1.320(16) . ? O308 Mo4 1.967(11) . ? O308 Mo4B 2.321(11) 2_654 ? O309 C409 1.258(16) . ? O310 C409 1.281(17) . ? O310 Mo3 2.129(10) 2_654 ? O311 C309 1.276(16) 2_654 ? O311 Mo5 2.081(13) . ? O311 Mo5' 2.33(2) . ? O312 C309 1.251(16) 2_654 ? O312 Mo6 2.067(12) . ? O312 Mo6' 2.264(16) . ? C5 N10 1.338(19) 2_654 ? C11 C16 1.34(2) . ? C11 C12 1.39(2) . ? C12 C13 1.37(2) . ? C13 C14 1.33(2) . ? C14 C15 1.39(2) . ? C15 C16 1.39(2) . ? C21 C26 1.34(3) . ? C21 C22 1.44(4) . ? C22 C23 1.36(3) . ? C23 C24 1.39(4) . ? C24 C25 1.39(4) . ? C24 O2 1.43(3) . ? C25 C26 1.43(3) . ? O2 C27 1.42(3) . ? C21' C26' 1.35(3) . ? C21' C22' 1.43(4) . ? C22' C23' 1.37(3) . ? C23' C24' 1.39(4) . ? C24' C25' 1.39(4) . ? C24' O2' 1.43(3) . ? C25' C26' 1.43(3) . ? O2' C27' 1.43(3) . ? C31 C32 1.39(2) . ? C31 C36 1.39(2) . ? C32 C33 1.41(2) . ? C33 C34 1.30(2) . ? C34 C35 1.37(2) . ? C35 C36 1.38(2) . ? C41 C46 1.32(5) . ? C41 C42 1.42(5) . ? C42 C43 1.38(3) . ? C43 C44 1.36(3) . ? C44 O4 1.37(2) . ? C44 C45 1.44(3) . ? C45 C46 1.36(3) . ? O4 C47 1.39(3) . ? C41' C46' 1.32(5) . ? C41' C42' 1.42(5) . ? C42' C43' 1.37(3) . ? C43' C44' 1.35(4) . ? C44' O4' 1.37(2) . ? C44' C45' 1.44(3) . ? C45' C46' 1.37(3) . ? O4' C47' 1.39(3) . ? C51 C56 1.341(19) . ? C51 C52 1.36(2) . ? C52 C53 1.42(3) . ? C53 C54 1.38(3) . ? C54 C55 1.33(2) . ? C55 C56 1.42(2) . ? C61 C66 1.29(3) . ? C61 C62 1.38(3) . ? C62 C63 1.38(4) . ? C63 C64 1.33(4) . ? C64 C65 1.39(4) . ? C64 O6 1.39(3) . ? C65 C66 1.43(4) . ? O6 C67 1.32(4) . ? C61' C66' 1.29(4) . ? C61' C62' 1.38(3) . ? C62' C63' 1.38(4) . ? C63' C64' 1.34(4) . ? C64' O6' 1.39(3) . ? C64' C65' 1.39(4) . ? C65' C66' 1.44(4) . ? O6' C67' 1.32(4) . ? Mo5 Mo6 2.100(6) . y Mo5 N7 2.107(15) . ? Mo5 N3S 2.555(18) 4_644 ? Mo6 N8 2.103(17) . ? C71 C76 1.39(2) . ? C71 C72 1.40(3) . ? C71 N7 1.42(3) . ? C72 C73 1.36(3) . ? C73 C74 1.38(3) . ? C74 O7 1.38(3) . ? C74 C75 1.41(4) . ? C75 C76 1.37(3) . ? O7 C77 1.42(3) . ? N7 C4 1.32(3) . ? C4 N8 1.37(4) . ? N8 C81 1.43(2) . ? C81 C82 1.32(4) . ? C81 C86 1.36(3) . ? C82 C83 1.44(3) . ? C83 C84 1.29(3) . ? C84 C85 1.30(3) . ? C84 O8 1.48(3) . ? C85 C86 1.45(3) . ? O8 C87 1.46(5) . ? Mo5' Mo6' 2.093(11) . y Mo5' N7' 2.112(18) . ? Mo6' N8' 2.10(2) . ? C71' C76' 1.39(3) . ? C71' C72' 1.40(3) . ? C71' N7' 1.42(3) . ? C72' C73' 1.38(3) . ? C73' C74' 1.38(3) . ? C74' O7' 1.38(3) . ? C74' C75' 1.42(4) . ? C75' C76' 1.36(3) . ? O7' C77' 1.41(3) . ? N7' C4' 1.33(3) . ? C4' N8' 1.37(4) . ? N8' C81' 1.44(3) . ? C81' C82' 1.32(4) . ? C81' C86' 1.35(3) . ? C82' C83' 1.43(3) . ? C83' C84' 1.30(3) . ? C84' C85' 1.30(4) . ? C84' O8' 1.49(3) . ? C85' C86' 1.46(4) . ? O8' C87' 1.46(5) . ? C91 C92 1.34(3) . ? C91 C96 1.36(3) . ? C92 C93 1.43(3) . ? C93 C94 1.27(3) . ? C94 C95 1.28(4) . ? C94 O9 1.48(3) . ? C95 C96 1.43(3) . ? O9 C97 1.46(4) . ? C91' C92' 1.33(3) . ? C91' C96' 1.36(3) . ? C92' C93' 1.43(3) . ? C93' C94' 1.26(4) . ? C94' C95' 1.28(4) . ? C94' O9' 1.49(3) . ? C95' C96' 1.43(3) . ? O9' C97' 1.46(4) . ? C101 C102 1.31(2) . ? C101 C106 1.38(3) . ? C102 C103 1.38(2) . ? C103 C104 1.33(2) . ? C104 C105 1.39(3) . ? C105 C106 1.36(3) . ? Mo4 N12 2.089(17) . ? Mo4 Mo4B 2.104(5) . y Mo4 N11 2.119(16) . ? Mo4 O307 2.245(11) 2_654 ? N11 C6'A 1.36(3) . ? N11 C111 1.42(3) . ? C111 C112 1.32(3) . ? C111 C116 1.42(4) . ? C112 C113 1.43(4) . ? C113 C114 1.27(4) . ? C114 C115 1.33(4) . ? C114 O11 1.60(4) . ? C115 C116 1.38(3) . ? O11 C117 1.75(4) . ? C6 N12 1.31(3) . ? C6 N11B 1.36(3) . ? N12 C121 1.42(3) . ? C121 C126 1.29(4) . ? C121 C122 1.41(3) . ? C122 C123 1.31(3) . ? C123 C124 1.38(5) . ? C124 C125 1.44(4) . ? C124 O12 1.45(3) . ? C125 C126 1.39(3) . ? O12 C127 1.40(3) . ? Mo4B N12B 2.094(18) . ? Mo4B N11B 2.122(16) . ? Mo4B O308 2.321(11) 2_654 ? N11B C11O 1.42(3) . ? C11O C11P 1.33(3) . ? C11O C11U 1.42(4) . ? C11P C11Q 1.43(4) . ? C11Q C11R 1.27(4) . ? C11R C11T 1.33(4) . ? C11R O11B 1.56(3) . ? C11T C11U 1.38(3) . ? O11B C11V 1.76(4) . ? C6'A N12B 1.32(3) . ? N12B C12O 1.41(3) . ? C12O C12U 1.28(4) . ? C12O C12P 1.41(3) . ? C12P C12Q 1.32(3) . ? C12Q C12R 1.38(5) . ? C12R C12T 1.45(4) . ? C12R O12B 1.47(3) . ? C12T C12U 1.40(3) . ? O12B C12V 1.40(3) . ? C301 C302 1.4814 . ? C302 C303 1.3592 . ? C302 C307 1.416(15) . ? C303 C304 1.424(16) . ? C304 C305 1.386(19) . ? C304 C308 1.470(19) . ? C305 C306 1.352(18) . ? C306 C307 1.376(18) . ? C306 C309 1.51(2) . ? C309 O312 1.251(16) 2_654 ? C309 O311 1.276(16) 2_654 ? C401 C402 1.517(18) . ? C402 C407 1.379(18) . ? C402 C403 1.383(19) . ? C403 C404 1.416(19) . ? C404 C405 1.38(2) . ? C404 C409 1.49(2) . ? C405 C406 1.39(2) . ? C406 C407 1.368(17) . ? C406 C408 1.469(19) . ? N1S C1S' 1.14(4) . ? N1S C1S 1.35(4) . ? C1S C2S 1.43(6) . ? C1S' C2S' 1.62(6) . ? N2S C3S 1.20(3) . ? C3S C4S 1.53(4) . ? N3S C5S 1.13(3) . ? N3S Mo5 2.555(18) 4_654 ? C5S C6S 1.52(4) . ? N4S C7S 1.16(2) . ? C7S C8S 1.41(3) . ? N5S C9S 1.33(4) . ? C9S C10S 1.20(4) . ? C53S Cl7 1.16(6) . ? C53S Cl8 1.77(7) . ? N6S C11S 1.92(13) . ? N7S C13S 1.17(3) . ? C13S C14S 1.53(3) . ? N8S C15S 1.15(3) . ? C15S C16S 1.52(3) . ? N9S C17S 1.16(3) . ? C17S C18S 1.53(3) . ? C19S C21S 1.13(6) . ? C19S N10S 1.23(4) 4_544 ? C19S C20S 1.23(4) . ? N10S C19S 1.23(4) 4_554 ? N11S C21S 0.96(7) . ? N12S C23S 1.17(6) . ? C23S C24S 1.46(6) . ? N13S C25S 1.11(8) . ? C25S C26S 1.76(12) . ? C51S Cl1 1.65(5) 3_445 ? C51S Cl2 1.91(5) . ? Cl1 C51S 1.65(5) 3 ? N14S C27S 1.04(4) . ? C27S C28S 1.45(6) 3_445 ? C28S C27S 1.45(6) 3 ? N15S C29S 1.11(4) . ? C29S C30S 1.44(5) . ? C52S Cl6 1.66(6) 2_654 ? C52S Cl3 1.76(5) . ? C52S Cl4 1.79(5) 2_654 ? C52S Cl4 1.87(4) . ? C52S Cl5 1.89(4) . ? C52S Cl6 2.15(6) . ? Cl3 C52S 1.76(5) 2_654 ? Cl4 C52S 1.79(5) 2_654 ? Cl6 C52S 1.66(6) 2_654 ? N16S C31S 1.02(5) . ? C31S C32S 1.24(4) . ? C32S C31S 1.24(4) 2_754 ? N17S C33S 0.96(8) . ? N17S C34S 1.69(12) . ? C33S C34S 0.88(12) . ? N18S C35S 1.18(10) . ? C35S C36S 1.63(6) 6_546 ? C36S C35S 1.63(6) 6_545 ? N19S C37S 1.04(15) . ? N19S C38S 1.40(8) . ? C37S C38S 1.51(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Mo2 Mo1 N3 92.5(3) . . ? Mo2 Mo1 N1 93.3(3) . . ? N3 Mo1 N1 93.3(4) . . ? Mo2 Mo1 O303 91.3(2) . . ? N3 Mo1 O303 91.1(4) . . ? N1 Mo1 O303 173.5(4) . . ? Mo2 Mo1 O301 92.0(2) . . ? N3 Mo1 O301 174.7(4) . . ? N1 Mo1 O301 89.2(4) . . ? O303 Mo1 O301 86.1(3) . . ? Mo1 Mo2 N4 92.5(3) . . ? Mo1 Mo2 N2 91.6(3) . . ? N4 Mo2 N2 92.5(4) . . ? Mo1 Mo2 O302 91.6(2) . . ? N4 Mo2 O302 174.0(4) . . ? N2 Mo2 O302 91.7(4) . . ? Mo1 Mo2 O304 91.5(2) . . ? N4 Mo2 O304 89.7(4) . . ? N2 Mo2 O304 176.2(4) . . ? O302 Mo2 O304 85.9(3) . . ? O309 Mo3 Mo3 92.3(3) . 2_654 ? O309 Mo3 N10 88.3(4) . . ? Mo3 Mo3 N10 92.8(3) 2_654 . ? O309 Mo3 N9 172.1(4) . . ? Mo3 Mo3 N9 93.5(4) 2_654 . ? N10 Mo3 N9 96.8(5) . . ? O309 Mo3 O310 85.6(4) . 2_654 ? Mo3 Mo3 O310 91.5(3) 2_654 2_654 ? N10 Mo3 O310 172.6(4) . 2_654 ? N9 Mo3 O310 88.9(5) . 2_654 ? C1 N1 C11 118.7(11) . . ? C1 N1 Mo1 116.9(9) . . ? C11 N1 Mo1 124.1(9) . . ? C1 N2 C21' 121(3) . . ? C1 N2 C21 114.3(14) . . ? C21' N2 C21 14(3) . . ? C1 N2 Mo2 117.8(9) . . ? C21' N2 Mo2 121(3) . . ? C21 N2 Mo2 127.3(13) . . ? C2 N3 C31 116.8(12) . . ? C2 N3 Mo1 116.8(10) . . ? C31 N3 Mo1 126.2(9) . . ? C2 N4 C41' 116(4) . . ? C2 N4 C41 120(3) . . ? C41' N4 C41 5(4) . . ? C2 N4 Mo2 116.5(9) . . ? C41' N4 Mo2 127(4) . . ? C41 N4 Mo2 124(3) . . ? C3 N5 C51 117.3(14) . . ? C3 N5 Mo5' 109.7(12) . . ? C51 N5 Mo5' 129.7(11) . . ? C3 N5 Mo5 120.0(12) . . ? C51 N5 Mo5 120.9(10) . . ? Mo5' N5 Mo5 10.7(4) . . ? C61' N6 C3 117.6(18) . . ? C61' N6 C61 27.7(13) . . ? C3 N6 C61 117.0(15) . . ? C61' N6 Mo6' 119.8(16) . . ? C3 N6 Mo6' 122.4(12) . . ? C61 N6 Mo6' 115.0(12) . . ? C61' N6 Mo6 126.8(15) . . ? C3 N6 Mo6 113.6(11) . . ? C61 N6 Mo6 127.1(12) . . ? Mo6' N6 Mo6 13.5(3) . . ? C5 N9 C91' 128(2) . . ? C5 N9 C91 115.0(16) . . ? C91' N9 C91 32.5(15) . . ? C5 N9 Mo3 114.9(12) . . ? C91' N9 Mo3 111.6(17) . . ? C91 N9 Mo3 129.6(12) . . ? C5 N10 C101 119.0(14) 2_654 . ? C5 N10 Mo3 115.2(11) 2_654 . ? C101 N10 Mo3 125.5(9) . . ? C14 O1 C17 117.3(15) . . ? C34 O3 C37 112.2(19) . . ? C54 O5 C57 115.8(13) . . ? C104 O10 C107 118.9(16) . . ? C301 O301 Mo1 116.6(6) . . ? C301 O302 Mo2 116.8(7) . . ? C401 O303 Mo1 117.1(8) . . ? C401 O304 Mo2 116.0(8) . . ? C408 O305 Mo5' 112.3(9) . . ? C408 O305 Mo5 122.1(9) . . ? Mo5' O305 Mo5 11.7(4) . . ? C408 O306 Mo6' 122.2(10) . . ? C408 O306 Mo6 113.0(9) . . ? Mo6' O306 Mo6 11.2(4) . . ? C308 O307 Mo4B 112.2(9) . . ? C308 O307 Mo4 122.8(9) . 2_654 ? Mo4B O307 Mo4 14.7(2) . 2_654 ? C308 O308 Mo4 120.9(9) . . ? C308 O308 Mo4B 109.8(9) . 2_654 ? Mo4 O308 Mo4B 12.4(4) . 2_654 ? C409 O309 Mo3 117.2(10) . . ? C409 O310 Mo3 115.3(9) . 2_654 ? C309 O311 Mo5 119.3(9) 2_654 . ? C309 O311 Mo5' 110.1(9) 2_654 . ? Mo5 O311 Mo5' 9.7(5) . . ? C309 O312 Mo6 114.7(10) 2_654 . ? C309 O312 Mo6' 122.9(10) 2_654 . ? Mo6 O312 Mo6' 13.2(3) . . ? N1 C1 N2 120.3(12) . . ? N4 C2 N3 121.6(14) . . ? N5 C3 N6 121.3(17) . . ? N9 C5 N10 123.5(17) . 2_654 ? C16 C11 C12 119.0(14) . . ? C16 C11 N1 119.5(13) . . ? C12 C11 N1 121.5(14) . . ? C13 C12 C11 118.7(16) . . ? C14 C13 C12 122.0(17) . . ? C13 C14 C15 120.9(16) . . ? C13 C14 O1 117.7(15) . . ? C15 C14 O1 121.4(15) . . ? C14 C15 C16 116.5(16) . . ? C11 C16 C15 122.8(15) . . ? C26 C21 C22 119(2) . . ? C26 C21 N2 122(3) . . ? C22 C21 N2 119(2) . . ? C23 C22 C21 120(2) . . ? C22 C23 C24 119(3) . . ? C25 C24 C23 122(2) . . ? C25 C24 O2 122(2) . . ? C23 C24 O2 115(2) . . ? C24 C25 C26 116(2) . . ? C21 C26 C25 122(2) . . ? C27 O2 C24 116(2) . . ? N2 C21' C26' 118(3) . . ? N2 C21' C22' 122(3) . . ? C26' C21' C22' 118(3) . . ? C23' C22' C21' 120(3) . . ? C22' C23' C24' 121(3) . . ? C25' C24' C23' 121(3) . . ? C25' C24' O2' 120(3) . . ? C23' C24' O2' 118(3) . . ? C24' C25' C26' 117(3) . . ? C21' C26' C25' 122(3) . . ? C27' O2' C24' 117(3) . . ? C32 C31 C36 118.3(16) . . ? C32 C31 N3 120.1(13) . . ? C36 C31 N3 121.5(14) . . ? C31 C32 C33 118.9(16) . . ? C34 C33 C32 120.2(19) . . ? C33 C34 C35 124(2) . . ? C33 C34 O3 125.6(19) . . ? C35 C34 O3 110.5(17) . . ? C34 C35 C36 116.7(18) . . ? C35 C36 C31 121.9(16) . . ? C46 C41 C42 117.5(18) . . ? C46 C41 N4 122(4) . . ? C42 C41 N4 120(3) . . ? C43 C42 C41 120(2) . . ? C44 C43 C42 122(2) . . ? C43 C44 O4 125(2) . . ? C43 C44 C45 117(2) . . ? O4 C44 C45 117(2) . . ? C46 C45 C44 119(2) . . ? C41 C46 C45 124(2) . . ? C44 O4 C47 115.9(19) . . ? C46' C41' N4 122(4) . . ? C46' C41' C42' 118(2) . . ? N4 C41' C42' 120(4) . . ? C43' C42' C41' 121(3) . . ? C44' C43' C42' 120(2) . . ? C43' C44' O4' 119(2) . . ? C43' C44' C45' 119(2) . . ? O4' C44' C45' 122(3) . . ? C46' C45' C44' 118(2) . . ? C41' C46' C45' 123(2) . . ? C44' O4' C47' 117(3) . . ? C56 C51 C52 119.1(16) . . ? C56 C51 N5 121.4(14) . . ? C52 C51 N5 119.2(15) . . ? C51 C52 C53 121(2) . . ? C54 C53 C52 117(2) . . ? C55 C54 C53 122.8(18) . . ? C55 C54 O5 124.9(15) . . ? C53 C54 O5 112.1(16) . . ? C54 C55 C56 117.7(14) . . ? C51 C56 C55 122.0(14) . . ? C66 C61 C62 121(3) . . ? C66 C61 N6 123(2) . . ? C62 C61 N6 116(2) . . ? C61 C62 C63 117(3) . . ? C64 C63 C62 122(3) . . ? C63 C64 C65 120(3) . . ? C63 C64 O6 123(3) . . ? C65 C64 O6 116(3) . . ? C64 C65 C66 115(3) . . ? C61 C66 C65 123(3) . . ? C67 O6 C64 117(3) . . ? C66' C61' N6 118(3) . . ? C66' C61' C62' 119(3) . . ? N6 C61' C62' 123(3) . . ? C63' C62' C61' 118(3) . . ? C64' C63' C62' 121(3) . . ? C63' C64' O6' 119(3) . . ? C63' C64' C65' 120(3) . . ? O6' C64' C65' 119(3) . . ? C64' C65' C66' 115(3) . . ? C61' C66' C65' 123(3) . . ? C67' O6' C64' 119(3) . . ? O311 Mo5 Mo6 88.3(5) . . ? O311 Mo5 N7 95.1(6) . . ? Mo6 Mo5 N7 93.0(6) . . ? O311 Mo5 O305 86.6(5) . . ? Mo6 Mo5 O305 90.0(4) . . ? N7 Mo5 O305 176.6(7) . . ? O311 Mo5 N5 171.2(6) . . ? Mo6 Mo5 N5 89.1(4) . . ? N7 Mo5 N5 93.4(7) . . ? O305 Mo5 N5 85.0(5) . . ? O311 Mo5 N3S 85.5(5) . 4_644 ? Mo6 Mo5 N3S 166.0(6) . 4_644 ? N7 Mo5 N3S 100.0(7) . 4_644 ? O305 Mo5 N3S 77.2(5) . 4_644 ? N5 Mo5 N3S 95.1(6) . 4_644 ? O312 Mo6 Mo5 94.8(4) . . ? O312 Mo6 N8 95.1(6) . . ? Mo5 Mo6 N8 93.3(7) . . ? O312 Mo6 N6 163.2(5) . . ? Mo5 Mo6 N6 95.8(5) . . ? N8 Mo6 N6 97.2(7) . . ? O312 Mo6 O306 83.8(4) . . ? Mo5 Mo6 O306 93.1(4) . . ? N8 Mo6 O306 173.5(7) . . ? N6 Mo6 O306 82.6(5) . . ? C76 C71 C72 118(2) . . ? C76 C71 N7 123(2) . . ? C72 C71 N7 118.3(17) . . ? C73 C72 C71 119(2) . . ? C72 C73 C74 120(2) . . ? O7 C74 C73 116.1(19) . . ? O7 C74 C75 121(2) . . ? C73 C74 C75 123(3) . . ? C76 C75 C74 115(3) . . ? C75 C76 C71 124(2) . . ? C74 O7 C77 118.4(17) . . ? C4 N7 C71 116.7(17) . . ? C4 N7 Mo5 117.1(18) . . ? C71 N7 Mo5 124.4(13) . . ? N7 C4 N8 120.2(19) . . ? C4 N8 C81 118.4(19) . . ? C4 N8 Mo6 115.8(13) . . ? C81 N8 Mo6 125.8(19) . . ? C82 C81 C86 119(2) . . ? C82 C81 N8 120(2) . . ? C86 C81 N8 120(2) . . ? C81 C82 C83 120(2) . . ? C84 C83 C82 116(3) . . ? C83 C84 C85 130(3) . . ? C83 C84 O8 118(2) . . ? C85 C84 O8 112(2) . . ? C84 C85 C86 113(3) . . ? C81 C86 C85 122(3) . . ? C87 O8 C84 115(3) . . ? N5 Mo5' O305 93.6(8) . . ? N5 Mo5' Mo6' 99.7(8) . . ? O305 Mo5' Mo6' 93.7(7) . . ? N5 Mo5' N7' 89.7(11) . . ? O305 Mo5' N7' 171.7(11) . . ? Mo6' Mo5' N7' 93.2(8) . . ? N5 Mo5' O311 163.7(8) . . ? O305 Mo5' O311 83.0(7) . . ? Mo6' Mo5' O311 96.4(8) . . ? N7' Mo5' O311 91.7(10) . . ? O306 Mo6' N6 98.6(7) . . ? O306 Mo6' Mo5' 89.8(6) . . ? N6 Mo6' Mo5' 85.7(8) . . ? O306 Mo6' N8' 172.6(11) . . ? N6 Mo6' N8' 88.3(10) . . ? Mo5' Mo6' N8' 93.5(9) . . ? O306 Mo6' O312 87.3(6) . . ? N6 Mo6' O312 170.1(7) . . ? Mo5' Mo6' O312 86.4(7) . . ? N8' Mo6' O312 86.3(10) . . ? C76' C71' C72' 118(3) . . ? C76' C71' N7' 122(3) . . ? C72' C71' N7' 120(2) . . ? C73' C72' C71' 118(3) . . ? C74' C73' C72' 120(3) . . ? C73' C74' O7' 121(3) . . ? C73' C74' C75' 124(3) . . ? O7' C74' C75' 115(3) . . ? C76' C75' C74' 113(3) . . ? C75' C76' C71' 126(3) . . ? C74' O7' C77' 118(3) . . ? C4' N7' C71' 117(2) . . ? C4' N7' Mo5' 117(2) . . ? C71' N7' Mo5' 125.2(18) . . ? N7' C4' N8' 120(2) . . ? C4' N8' C81' 121(2) . . ? C4' N8' Mo6' 115.9(16) . . ? C81' N8' Mo6' 122(2) . . ? C82' C81' C86' 119(3) . . ? C82' C81' N8' 119(3) . . ? C86' C81' N8' 121(3) . . ? C81' C82' C83' 120(3) . . ? C84' C83' C82' 116(3) . . ? C85' C84' C83' 130(3) . . ? C85' C84' O8' 113(3) . . ? C83' C84' O8' 118(3) . . ? C84' C85' C86' 111(3) . . ? C81' C86' C85' 122(3) . . ? C87' O8' C84' 115(3) . . ? C92 C91 C96 119(2) . . ? C92 C91 N9 126(2) . . ? C96 C91 N9 115(2) . . ? C91 C92 C93 118(2) . . ? C94 C93 C92 122(3) . . ? C93 C94 C95 123(3) . . ? C93 C94 O9 115(2) . . ? C95 C94 O9 122(2) . . ? C94 C95 C96 119(3) . . ? C91 C96 C95 120(2) . . ? C97 O9 C94 115(2) . . ? C92' C91' C96' 120(3) . . ? C92' C91' N9 120(3) . . ? C96' C91' N9 121(3) . . ? C91' C92' C93' 117(3) . . ? C94' C93' C92' 121(3) . . ? C93' C94' C95' 125(3) . . ? C93' C94' O9' 117(3) . . ? C95' C94' O9' 118(3) . . ? C94' C95' C96' 117(3) . . ? C91' C96' C95' 120(3) . . ? C97' O9' C94' 113(3) . . ? C102 C101 C106 115.9(17) . . ? C102 C101 N10 123.7(16) . . ? C106 C101 N10 120.3(16) . . ? C101 C102 C103 124.5(18) . . ? C104 C103 C102 120.1(18) . . ? C103 C104 O10 126.4(17) . . ? C103 C104 C105 117(2) . . ? O10 C104 C105 116(2) . . ? C106 C105 C104 120(3) . . ? C105 C106 C101 122(2) . . ? O308 Mo4 N12 175.5(7) . . ? O308 Mo4 Mo4B 88.7(5) . . ? N12 Mo4 Mo4B 93.6(7) . . ? O308 Mo4 N11 92.0(7) . . ? N12 Mo4 N11 91.8(8) . . ? Mo4B Mo4 N11 92.2(7) . . ? O308 Mo4 O307 86.6(4) . 2_654 ? N12 Mo4 O307 89.6(7) . 2_654 ? Mo4B Mo4 O307 87.8(4) . 2_654 ? N11 Mo4 O307 178.6(7) . 2_654 ? C6'A N11 C111 118.2(19) . . ? C6'A N11 Mo4 115.3(17) . . ? C111 N11 Mo4 126.2(15) . . ? C112 C111 C116 116(3) . . ? C112 C111 N11 126(3) . . ? C116 C111 N11 118(2) . . ? C111 C112 C113 122(3) . . ? C114 C113 C112 122(3) . . ? C113 C114 C115 116(3) . . ? C113 C114 O11 115(3) . . ? C115 C114 O11 124(3) . . ? C114 C115 C116 126(3) . . ? C115 C116 C111 116(3) . . ? C114 O11 C117 96(2) . . ? N12 C6 N11B 120(2) . . ? C6 N12 C121 113(2) . . ? C6 N12 Mo4 118.2(15) . . ? C121 N12 Mo4 128.1(19) . . ? C126 C121 C122 117(2) . . ? C126 C121 N12 121(3) . . ? C122 C121 N12 123(3) . . ? C123 C122 C121 125(3) . . ? C122 C123 C124 116(4) . . ? C123 C124 C125 123(2) . . ? C123 C124 O12 126(3) . . ? C125 C124 O12 111(2) . . ? C126 C125 C124 113(3) . . ? C121 C126 C125 126(3) . . ? C127 O12 C124 118(2) . . ? O307 Mo4B N12B 91.5(7) . . ? O307 Mo4B Mo4 95.2(5) . . ? N12B Mo4B Mo4 94.5(7) . . ? O307 Mo4B N11B 171.6(8) . . ? N12B Mo4B N11B 92.4(9) . . ? Mo4 Mo4B N11B 92.0(7) . . ? O307 Mo4B O308 82.5(4) . 2_654 ? N12B Mo4B O308 168.7(8) . 2_654 ? Mo4 Mo4B O308 95.6(4) . 2_654 ? N11B Mo4B O308 92.3(7) . 2_654 ? C6 N11B C11O 114.3(19) . . ? C6 N11B Mo4B 116.7(17) . . ? C11O N11B Mo4B 129.0(16) . . ? C11P C11O C11U 116(3) . . ? C11P C11O N11B 126(3) . . ? C11U C11O N11B 118(2) . . ? C11O C11P C11Q 123(3) . . ? C11R C11Q C11P 120(3) . . ? C11Q C11R C11T 119(3) . . ? C11Q C11R O11B 116(3) . . ? C11T C11R O11B 124(3) . . ? C11R C11T C11U 124(3) . . ? C11T C11U C11O 118(3) . . ? C11R O11B C11V 97(2) . . ? N12B C6'A N11 123(2) . . ? C6'A N12B C12O 115(2) . . ? C6'A N12B Mo4B 115.5(15) . . ? C12O N12B Mo4B 128.5(19) . . ? C12U C12O C12P 117(2) . . ? C12U C12O N12B 120(3) . . ? C12P C12O N12B 122(3) . . ? C12Q C12P C12O 123(3) . . ? C12P C12Q C12R 116(4) . . ? C12Q C12R C12T 125(3) . . ? C12Q C12R O12B 125(3) . . ? C12T C12R O12B 110(3) . . ? C12U C12T C12R 110(3) . . ? C12O C12U C12T 127(3) . . ? C12V O12B C12R 116(2) . . ? O302 C301 O301 122.8(8) . . ? O302 C301 C302 121.8(6) . . ? O301 C301 C302 115.4(5) . . ? C303 C302 C307 120.0(6) . . ? C303 C302 C301 120.8 . . ? C307 C302 C301 119.2(6) . . ? C302 C303 C304 120.6(6) . . ? C305 C304 C303 117.7(11) . . ? C305 C304 C308 125.2(13) . . ? C303 C304 C308 117.1(12) . . ? C306 C305 C304 121.5(14) . . ? C305 C306 C307 121.4(14) . . ? C305 C306 C309 120.0(13) . . ? C307 C306 C309 118.3(12) . . ? C306 C307 C302 118.7(11) . . ? O307 C308 O308 123.0(12) . . ? O307 C308 C304 121.3(13) . . ? O308 C308 C304 115.7(13) . . ? O312 C309 O311 122.4(14) 2_654 2_654 ? O312 C309 C306 118.1(13) 2_654 . ? O311 C309 C306 119.5(12) 2_654 . ? O304 C401 O303 124.0(12) . . ? O304 C401 C402 121.1(12) . . ? O303 C401 C402 114.9(11) . . ? C407 C402 C403 121.6(12) . . ? C407 C402 C401 119.4(12) . . ? C403 C402 C401 119.0(12) . . ? C402 C403 C404 118.3(13) . . ? C405 C404 C403 119.3(14) . . ? C405 C404 C409 120.3(14) . . ? C403 C404 C409 120.2(13) . . ? C404 C405 C406 121.0(14) . . ? C407 C406 C405 119.5(13) . . ? C407 C406 C408 119.0(12) . . ? C405 C406 C408 121.5(12) . . ? C406 C407 C402 120.2(13) . . ? O305 C408 O306 121.8(12) . . ? O305 C408 C406 118.8(12) . . ? O306 C408 C406 119.3(13) . . ? O309 C409 O310 123.4(14) . . ? O309 C409 C404 117.5(14) . . ? O310 C409 C404 119.1(13) . . ? C1S' N1S C1S 136(4) . . ? N1S C1S C2S 169(4) . . ? N1S C1S' C2S' 155(5) . . ? N2S C3S C4S 172(4) . . ? C5S N3S Mo5 160.4(19) . 4_654 ? N3S C5S C6S 177(3) . . ? N4S C7S C8S 175(2) . . ? C10S C9S N5S 175(4) . . ? Cl7 C53S Cl8 130(5) . . ? C12S C11S N6S 126(10) . . ? N7S C13S C14S 175(5) . . ? N8S C15S C16S 172(4) . . ? N9S C17S C18S 153(4) . . ? C21S C19S N10S 128(5) . 4_544 ? N10S C19S C20S 170(4) 4_544 . ? N11S C21S C19S 168(8) . . ? N12S C23S C24S 174(5) . . ? N13S C25S C26S 113(8) . . ? Cl1 C51S Cl2 113(2) 3_445 . ? N14S C27S C28S 171(4) . 3_445 ? N15S C29S C30S 170(4) . . ? Cl6 C52S Cl3 91(3) 2_654 . ? Cl5 C52S Cl4 85(3) 2_654 2_654 ? Cl3 C52S Cl4 102(2) . 2_654 ? Cl5 C52S Cl4 107(3) 2_654 . ? Cl6 C52S Cl4 77(3) 2_654 . ? Cl3 C52S Cl4 99(2) . . ? Cl6 C52S Cl5 102(3) 2_654 . ? Cl4 C52S Cl5 91(2) 2_654 . ? Cl4 C52S Cl5 69.9(18) . . ? Cl5 C52S Cl6 101(3) 2_654 . ? Cl6 C52S Cl6 99(3) 2_654 . ? Cl3 C52S Cl6 76.7(19) . . ? Cl4 C52S Cl6 68(2) 2_654 . ? N16S C31S C32S 125(5) . . ? C31S C32S C31S 143(8) 2_754 . ? C34S C33S N17S 134(10) . . ? N18S C35S C36S 88(6) . 6_546 ? C37S N19S C38S 75(9) . . ? N19S C37S C38S 63(9) . . ? _diffrn_measured_fraction_theta_max 0.398 _diffrn_reflns_theta_full 21.37 _diffrn_measured_fraction_theta_full 0.398 _refine_diff_density_max 1.043 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.142 #===END