# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ? _publ_contact_author_email yonggewei@mail.tsinghua.edu.cn _publ_contact_author_phone ? _publ_author_name 'Yongge Wei' _publ_contact_author_name 'Wei, Yongge' data_di-chex _database_code_depnum_ccdc_archive 'CCDC 869447' #TrackingRef '- Di-cHex-R1.cif' _audit_creation_date 2012-04-24 _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H22 Mo6 N2 O17, 2(C16 H36 N), 2(C2 H3 N)' _chemical_formula_sum 'C48 H100 Mo6 N6 O17' _chemical_formula_weight 1608.98 _chemical_absolute_configuration unk _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 43 _space_group_name_H-M_alt 'F d d 2' _space_group_name_Hall 'F 2 -2d' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, z' 3 'x+1/4, -y+1/4, z+1/4' 4 '-x+1/4, y+1/4, z+1/4' 5 'x, y+1/2, z+1/2' 6 '-x, -y+1/2, z+1/2' 7 'x+1/4, -y+3/4, z+3/4' 8 '-x+1/4, y+3/4, z+3/4' 9 'x+1/2, y, z+1/2' 10 '-x+1/2, -y, z+1/2' 11 'x+3/4, -y+1/4, z+3/4' 12 '-x+3/4, y+1/4, z+3/4' 13 'x+1/2, y+1/2, z' 14 '-x+1/2, -y+1/2, z' 15 'x+3/4, -y+3/4, z+1/4' 16 '-x+3/4, y+3/4, z+1/4' _cell_length_a 30.813(6) _cell_length_b 32.507(7) _cell_length_c 13.740(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13763(5) _cell_formula_units_Z 8 _cell_measurement_reflns_used 8539 _cell_measurement_temperature 143(2) _cell_measurement_theta_max 27.4621 _cell_measurement_theta_min 3.1091 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_T_max 0.7052 _exptl_absorpt_correction_T_min 0.6977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2000))' _exptl_crystal_colour Red _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 6544 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.34 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_unetI/netI 0.0332 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 25636 _diffrn_reflns_theta_full 24.50 _diffrn_reflns_theta_max 24.50 _diffrn_reflns_theta_min 3.11 _diffrn_ambient_temperature 143(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; #_diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_method dtprofit.ref _reflns_number_gt 4661 _reflns_number_total 5685 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.899 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.088 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(9) _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.242 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 339 _refine_ls_number_reflns 5685 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0686 _refine_ls_restrained_S_all 1.242 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+91.0507P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1419 _refine_ls_wR_factor_ref 0.1496 _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. The disorder in cyclohexyl ring was modelled using the DFIX instruction of the same C-C distances of 1.53 angstrom with a deviation 0f 0.005angstrom. Also, the disorderly tetrabutyl ammonium cation was modelled with the C-C bond length of 1.53 angstrom (C111-C112, C112-C113, C113-C114, C122-C123, C123-C124, C142-C143, C143-C144, C132-C133, C133-C134) within a deviation 0f 0.01angstrom. An acetonitrile molecule was modelled with the interatomic distance of N3-C7, C7-C8, N3-C8 fixed at 1.18, 1.48 and 2.72, respecively, at the deviation level of 0.01 angstrom. The butyl chain C141-C142-C143-C144, the acetonitrile sovent N3-C7-C8, and the cyclohexyl ring C1- C2- C3- C4- C5- C6 and N1, were modelled with the DELU and SiMU instructions to have the similar thermal motion. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.54853(4) 0.01847(3) 0.16095(10) 0.0974(4) Uani 1 1 d D . . Mo2 Mo 0.54920(3) 0.01897(3) -0.07455(10) 0.0887(4) Uani 1 1 d . . . Mo3 Mo 0.47185(3) 0.06742(2) 0.04531(12) 0.0784(3) Uani 1 1 d . . . O1 O 0.5000 0.0000 0.0506(9) 0.064(2) Uani 1 2 d S . . O2 O 0.5839(4) 0.0334(3) -0.1642(8) 0.133(4) Uani 1 1 d . . . O3 O 0.4518(3) 0.1156(2) 0.0385(9) 0.115(3) Uani 1 1 d . . . O4 O 0.5000 0.0000 0.2402(10) 0.108(4) Uani 1 2 d S . . O5 O 0.4381(2) 0.0383(2) -0.0524(7) 0.094(3) Uani 1 1 d . . . O6 O 0.4366(3) 0.0404(3) 0.1399(7) 0.095(3) Uani 1 1 d . . . O7 O 0.57933(17) 0.0297(2) 0.0404(9) 0.104(2) Uani 1 1 d . . . O8 O 0.5000 0.0000 -0.1464(8) 0.080(3) Uani 1 2 d S . . O9 O 0.5168(3) 0.0703(2) 0.1398(6) 0.085(2) Uani 1 1 d . . . O10 O 0.5163(3) 0.0688(2) -0.0532(7) 0.096(3) Uani 1 1 d . . . N1 N 0.5878(4) 0.0332(4) 0.2425(10) 0.141(5) Uani 1 1 d DU . . N2 N 0.5994(2) 0.1663(2) 0.0070(6) 0.070(2) Uani 1 1 d . . . C1 C 0.6246(5) 0.0468(5) 0.3061(12) 0.168(6) Uani 1 1 d DU . . H1 H 0.6379 0.0722 0.2777 0.201 Uiso 1 1 calc R . . C2 C 0.6586(5) 0.0128(6) 0.3084(16) 0.190(7) Uani 1 1 d DU . . H2A H 0.6705 0.0083 0.2422 0.228 Uiso 1 1 calc R . . H2B H 0.6453 -0.0132 0.3308 0.228 Uiso 1 1 calc R . . C3 C 0.6951(6) 0.0255(8) 0.3779(14) 0.212(9) Uani 1 1 d DU . . H3A H 0.7187 0.0049 0.3761 0.254 Uiso 1 1 calc R . . H3B H 0.7072 0.0524 0.3578 0.254 Uiso 1 1 calc R . . C4 C 0.6766(7) 0.0286(7) 0.4806(15) 0.218(9) Uani 1 1 d DU . . H4A H 0.6999 0.0333 0.5289 0.262 Uiso 1 1 calc R . . H4B H 0.6605 0.0033 0.4982 0.262 Uiso 1 1 calc R . . C5 C 0.6459(7) 0.0657(7) 0.4755(16) 0.227(9) Uani 1 1 d DU . . H5A H 0.6620 0.0899 0.4513 0.273 Uiso 1 1 calc R . . H5B H 0.6350 0.0721 0.5415 0.273 Uiso 1 1 calc R . . C6 C 0.6076(6) 0.0567(8) 0.4076(13) 0.213(9) Uani 1 1 d DU . . H6A H 0.5907 0.0331 0.4329 0.256 Uiso 1 1 calc R . . H6B H 0.5882 0.0809 0.4048 0.256 Uiso 1 1 calc R . . C111 C 0.6026(3) 0.2127(3) -0.0045(9) 0.082(3) Uani 1 1 d D . . H11A H 0.6204 0.2237 0.0497 0.099 Uiso 1 1 calc R . . H11B H 0.6183 0.2187 -0.0658 0.099 Uiso 1 1 calc R . . C112 C 0.5598(3) 0.2356(3) -0.0061(10) 0.095(3) Uani 1 1 d D . . H11C H 0.5423 0.2274 0.0510 0.114 Uiso 1 1 calc R . . H11D H 0.5435 0.2279 -0.0655 0.114 Uiso 1 1 calc R . . C113 C 0.5666(4) 0.2822(3) -0.0044(12) 0.113(4) Uani 1 1 d D . . H11E H 0.5825 0.2897 0.0555 0.135 Uiso 1 1 calc R . . H11F H 0.5847 0.2902 -0.0608 0.135 Uiso 1 1 calc R . . C114 C 0.5244(5) 0.3060(5) -0.0078(14) 0.150(7) Uani 1 1 d D . . H11G H 0.5087 0.2991 -0.0676 0.225 Uiso 1 1 calc R . . H11H H 0.5306 0.3356 -0.0068 0.225 Uiso 1 1 calc R . . H11I H 0.5066 0.2988 0.0488 0.225 Uiso 1 1 calc R . . C121 C 0.5739(3) 0.1537(4) 0.0967(8) 0.076(3) Uani 1 1 d . . . H12A H 0.5437 0.1635 0.0889 0.091 Uiso 1 1 calc R . . H12B H 0.5730 0.1233 0.0992 0.091 Uiso 1 1 calc R . . C122 C 0.5907(4) 0.1691(4) 0.1925(8) 0.089(3) Uani 1 1 d D . . H12C H 0.5926 0.1995 0.1907 0.106 Uiso 1 1 calc R . . H12D H 0.6202 0.1581 0.2036 0.106 Uiso 1 1 calc R . . C123 C 0.5614(3) 0.1562(4) 0.2758(6) 0.084(3) Uani 1 1 d D . . H12E H 0.5598 0.1258 0.2787 0.100 Uiso 1 1 calc R . . H12F H 0.5317 0.1669 0.2645 0.100 Uiso 1 1 calc R . . C124 C 0.5786(4) 0.1728(5) 0.3719(8) 0.109(4) Uani 1 1 d D . . H12G H 0.6093 0.1654 0.3787 0.163 Uiso 1 1 calc R . . H12H H 0.5620 0.1607 0.4257 0.163 Uiso 1 1 calc R . . H12I H 0.5755 0.2028 0.3732 0.163 Uiso 1 1 calc R . . C131 C 0.6460(2) 0.1510(3) 0.0150(7) 0.069(3) Uani 1 1 d . . . H13A H 0.6602 0.1653 0.0702 0.082 Uiso 1 1 calc R . . H13B H 0.6618 0.1590 -0.0450 0.082 Uiso 1 1 calc R . . C132 C 0.6509(2) 0.1048(3) 0.0295(8) 0.071(2) Uani 1 1 d D . . H13C H 0.6358 0.0900 -0.0236 0.085 Uiso 1 1 calc R . . H13D H 0.6374 0.0966 0.0920 0.085 Uiso 1 1 calc R . . C133 C 0.6994(3) 0.0930(3) 0.0299(10) 0.095(3) Uani 1 1 d D . . H13E H 0.7129 0.1015 -0.0322 0.114 Uiso 1 1 calc R . . H13F H 0.7144 0.1076 0.0835 0.114 Uiso 1 1 calc R . . C134 C 0.7044(4) 0.0466(4) 0.0432(14) 0.131(5) Uani 1 1 d D . . H13G H 0.6931 0.0324 -0.0145 0.196 Uiso 1 1 calc R . . H13H H 0.6880 0.0378 0.1007 0.196 Uiso 1 1 calc R . . H13I H 0.7351 0.0399 0.0518 0.196 Uiso 1 1 calc R . . C141 C 0.5760(3) 0.1473(3) -0.0803(9) 0.075(3) Uani 1 1 d U . . H14A H 0.5716 0.1176 -0.0669 0.090 Uiso 1 1 calc R . . H14B H 0.5470 0.1601 -0.0854 0.090 Uiso 1 1 calc R . . C142 C 0.5982(4) 0.1513(4) -0.1771(7) 0.092(3) Uani 1 1 d DU . . H14C H 0.6260 0.1361 -0.1764 0.110 Uiso 1 1 calc R . . H14D H 0.6043 0.1806 -0.1912 0.110 Uiso 1 1 calc R . . C143 C 0.5683(4) 0.1335(5) -0.2550(8) 0.111(4) Uani 1 1 d DU . . H14E H 0.5602 0.1050 -0.2368 0.133 Uiso 1 1 calc R . . H14F H 0.5413 0.1500 -0.2576 0.133 Uiso 1 1 calc R . . C144 C 0.5889(7) 0.1331(7) -0.3549(10) 0.175(8) Uani 1 1 d DU . . H14G H 0.5688 0.1208 -0.4018 0.262 Uiso 1 1 calc R . . H14H H 0.6157 0.1168 -0.3528 0.262 Uiso 1 1 calc R . . H14I H 0.5957 0.1613 -0.3747 0.262 Uiso 1 1 calc R . . N3 N 0.4610(11) 0.0703(12) -0.4576(19) 0.383(17) Uiso 1 1 d DU . . C7 C 0.4657(12) 0.0753(14) -0.544(2) 0.297(16) Uiso 1 1 d DU . . C8 C 0.4606(8) 0.0806(8) -0.6518(18) 0.213(10) Uiso 1 1 d DU . . H8A H 0.4846 0.0668 -0.6853 0.319 Uiso 1 1 calc R . . H8B H 0.4609 0.1100 -0.6678 0.319 Uiso 1 1 calc R . . H8C H 0.4330 0.0685 -0.6726 0.319 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0829(8) 0.0819(8) 0.1272(10) -0.0161(6) -0.0327(7) 0.0011(6) Mo2 0.0747(7) 0.0558(6) 0.1356(10) -0.0089(5) 0.0328(7) -0.0067(5) Mo3 0.0631(5) 0.0511(4) 0.1210(7) -0.0035(6) 0.0079(6) 0.0087(4) O1 0.038(4) 0.045(4) 0.108(6) 0.000 0.000 0.003(3) O2 0.143(8) 0.080(6) 0.176(10) -0.003(6) 0.072(7) 0.006(6) O3 0.132(6) 0.062(4) 0.149(7) -0.006(6) 0.032(7) 0.030(4) O4 0.119(11) 0.087(9) 0.120(9) 0.000 0.000 0.014(8) O5 0.056(5) 0.068(5) 0.159(8) 0.016(5) 0.001(5) 0.013(4) O6 0.061(5) 0.095(6) 0.130(7) 0.008(5) 0.025(4) 0.020(4) O7 0.042(3) 0.112(5) 0.159(7) -0.022(7) -0.011(6) -0.001(3) O8 0.094(8) 0.062(6) 0.082(7) 0.000 0.000 0.025(6) O9 0.104(6) 0.064(5) 0.087(5) -0.019(4) 0.005(4) -0.001(4) O10 0.099(6) 0.050(5) 0.138(8) 0.010(4) 0.013(5) -0.014(4) N1 0.123(9) 0.130(10) 0.170(11) -0.044(8) -0.072(8) -0.010(8) N2 0.063(5) 0.061(5) 0.086(6) 0.001(4) 0.008(4) -0.021(4) C1 0.178(12) 0.167(13) 0.158(10) -0.046(11) -0.111(10) 0.034(9) C2 0.143(12) 0.262(18) 0.165(13) -0.038(14) -0.049(11) 0.065(11) C3 0.146(15) 0.29(2) 0.197(15) -0.018(16) -0.074(12) 0.063(14) C4 0.212(18) 0.26(2) 0.182(12) -0.072(16) -0.101(13) 0.102(14) C5 0.272(18) 0.224(18) 0.185(13) -0.094(13) -0.136(13) 0.097(14) C6 0.202(16) 0.246(19) 0.191(13) -0.088(14) -0.095(11) 0.092(14) C111 0.079(7) 0.066(6) 0.101(8) -0.006(5) -0.003(6) -0.009(5) C112 0.085(8) 0.082(8) 0.117(9) 0.012(6) -0.016(7) -0.011(6) C113 0.105(10) 0.083(8) 0.150(12) 0.022(8) -0.006(9) -0.004(7) C114 0.160(15) 0.112(12) 0.179(16) 0.027(10) -0.025(12) 0.039(11) C121 0.047(5) 0.095(8) 0.086(7) 0.001(6) 0.009(5) -0.004(5) C122 0.063(7) 0.095(8) 0.109(10) -0.008(7) 0.033(6) -0.008(6) C123 0.056(5) 0.121(8) 0.073(8) 0.026(6) 0.012(5) -0.004(5) C124 0.109(10) 0.130(11) 0.088(9) -0.003(8) 0.025(8) -0.003(9) C131 0.038(4) 0.084(6) 0.083(7) -0.007(5) 0.001(4) -0.013(4) C132 0.056(5) 0.087(6) 0.069(7) 0.015(5) 0.007(5) -0.010(4) C133 0.066(6) 0.118(9) 0.101(9) 0.000(8) -0.022(7) 0.023(6) C134 0.093(8) 0.154(12) 0.145(12) 0.031(13) 0.023(11) 0.052(8) C141 0.046(5) 0.077(7) 0.102(7) 0.008(6) -0.010(5) -0.019(5) C142 0.078(7) 0.097(8) 0.100(7) 0.006(6) -0.014(5) -0.012(6) C143 0.085(8) 0.142(11) 0.106(7) -0.002(8) -0.021(6) 0.022(8) C144 0.25(2) 0.169(18) 0.108(9) -0.004(11) -0.003(11) -0.033(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 2.212(8) . ? Mo1 O4 1.945(8) . ? Mo1 O6 1.990(8) 2_655 ? Mo1 O7 1.943(11) . ? Mo1 O9 1.970(8) . ? Mo1 N1 1.716(8) . ? Mo2 O1 2.374(9) . ? Mo2 O2 1.698(9) . ? Mo2 O5 1.926(8) 2_655 ? Mo2 O7 1.865(11) . ? Mo2 O8 1.911(6) . ? Mo2 O10 1.934(8) . ? Mo3 O1 2.3583(9) . ? Mo3 O3 1.686(6) . ? Mo3 O5 1.945(9) . ? Mo3 O6 1.908(8) . ? Mo3 O9 1.900(9) . ? Mo3 O10 1.927(9) . ? O1 Mo1 2.212(8) 2_655 ? O1 Mo2 2.374(9) 2_655 ? O1 Mo3 2.3583(9) 2_655 ? O4 Mo1 1.945(8) 2_655 ? O5 Mo2 1.926(8) 2_655 ? O6 Mo1 1.990(8) 2_655 ? O8 Mo2 1.911(6) 2_655 ? N1 C1 1.500(15) . ? N2 C111 1.519(12) . ? N2 C121 1.517(11) . ? N2 C131 1.524(11) . ? N2 C141 1.530(13) . ? C1 H1 1.0000 . ? C1 C2 1.524(5) . ? C1 C6 1.524(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.532(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.527(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.532(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.533(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C111 H11A 0.9900 . ? C111 H11B 0.9900 . ? C111 C112 1.515(8) . ? C112 H11C 0.9900 . ? C112 H11D 0.9900 . ? C112 C113 1.528(9) . ? C113 H11E 0.9900 . ? C113 H11F 0.9900 . ? C113 C114 1.513(9) . ? C114 H11G 0.9800 . ? C114 H11H 0.9800 . ? C114 H11I 0.9800 . ? C121 H12A 0.9900 . ? C121 H12B 0.9900 . ? C121 C122 1.499(15) . ? C122 H12C 0.9900 . ? C122 H12D 0.9900 . ? C122 C123 1.516(8) . ? C123 H12E 0.9900 . ? C123 H12F 0.9900 . ? C123 C124 1.520(9) . ? C124 H12G 0.9800 . ? C124 H12H 0.9800 . ? C124 H12I 0.9800 . ? C131 H13A 0.9900 . ? C131 H13B 0.9900 . ? C131 C132 1.525(12) . ? C132 H13C 0.9900 . ? C132 H13D 0.9900 . ? C132 C133 1.541(8) . ? C133 H13E 0.9900 . ? C133 H13F 0.9900 . ? C133 C134 1.526(9) . ? C134 H13G 0.9800 . ? C134 H13H 0.9800 . ? C134 H13I 0.9800 . ? C141 H14A 0.9900 . ? C141 H14B 0.9900 . ? C141 C142 1.501(15) . ? C142 H14C 0.9900 . ? C142 H14D 0.9900 . ? C142 C143 1.526(9) . ? C143 H14E 0.9900 . ? C143 H14F 0.9900 . ? C143 C144 1.513(9) . ? C144 H14G 0.9800 . ? C144 H14H 0.9800 . ? C144 H14I 0.9800 . ? N3 C7 1.211(9) . ? C7 C8 1.495(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mo1 O1 77.3(4) . . ? O4 Mo1 O6 87.8(3) . 2_655 ? O4 Mo1 O9 88.0(3) . . ? O6 Mo1 O1 78.2(2) 2_655 . ? O7 Mo1 O1 78.3(3) . . ? O7 Mo1 O4 155.6(4) . . ? O7 Mo1 O6 86.8(4) . 2_655 ? O7 Mo1 O9 87.5(3) . . ? O9 Mo1 O1 78.2(2) . . ? O9 Mo1 O6 156.3(3) . 2_655 ? N1 Mo1 O1 177.5(6) . . ? N1 Mo1 O4 105.2(7) . . ? N1 Mo1 O6 101.6(5) . 2_655 ? N1 Mo1 O7 99.2(6) . . ? N1 Mo1 O9 102.0(6) . . ? O2 Mo2 O1 178.9(3) . . ? O2 Mo2 O5 104.7(4) . 2_655 ? O2 Mo2 O7 104.4(5) . . ? O2 Mo2 O8 102.4(5) . . ? O2 Mo2 O10 102.0(4) . . ? O5 Mo2 O1 76.4(3) 2_655 . ? O5 Mo2 O10 153.2(4) 2_655 . ? O7 Mo2 O1 75.7(3) . . ? O7 Mo2 O5 86.9(4) . 2_655 ? O7 Mo2 O8 153.2(4) . . ? O7 Mo2 O10 88.6(4) . . ? O8 Mo2 O1 77.5(3) . . ? O8 Mo2 O5 86.0(2) . 2_655 ? O8 Mo2 O10 86.2(3) . . ? O10 Mo2 O1 76.9(3) . . ? O3 Mo3 O1 178.6(5) . . ? O3 Mo3 O5 102.6(5) . . ? O3 Mo3 O6 104.8(4) . . ? O3 Mo3 O9 105.0(5) . . ? O3 Mo3 O10 101.5(4) . . ? O5 Mo3 O1 76.4(3) . . ? O6 Mo3 O1 76.2(3) . . ? O6 Mo3 O5 86.7(3) . . ? O6 Mo3 O10 153.5(3) . . ? O9 Mo3 O1 75.9(3) . . ? O9 Mo3 O5 152.3(3) . . ? O9 Mo3 O6 88.4(4) . . ? O9 Mo3 O10 87.7(3) . . ? O10 Mo3 O1 77.4(3) . . ? O10 Mo3 O5 84.7(4) . . ? Mo1 O1 Mo1 93.5(5) . 2_655 ? Mo1 O1 Mo2 89.67(5) . . ? Mo1 O1 Mo2 176.8(4) 2_655 . ? Mo1 O1 Mo2 176.8(4) . 2_655 ? Mo1 O1 Mo2 89.67(5) 2_655 2_655 ? Mo1 O1 Mo3 91.0(2) 2_655 2_655 ? Mo1 O1 Mo3 91.4(2) . 2_655 ? Mo1 O1 Mo3 91.0(2) . . ? Mo1 O1 Mo3 91.4(2) 2_655 . ? Mo2 O1 Mo2 87.2(4) . 2_655 ? Mo3 O1 Mo2 88.3(2) 2_655 2_655 ? Mo3 O1 Mo2 89.1(2) . 2_655 ? Mo3 O1 Mo2 88.3(2) . . ? Mo3 O1 Mo2 89.1(2) 2_655 . ? Mo3 O1 Mo3 176.5(6) 2_655 . ? Mo1 O4 Mo1 111.9(7) . 2_655 ? Mo2 O5 Mo3 118.1(4) 2_655 . ? Mo3 O6 Mo1 114.2(4) . 2_655 ? Mo2 O7 Mo1 116.4(3) . . ? Mo2 O8 Mo2 117.8(5) . 2_655 ? Mo3 O9 Mo1 114.9(4) . . ? Mo3 O10 Mo2 117.3(4) . . ? C1 N1 Mo1 174.9(14) . . ? C111 N2 C131 105.6(6) . . ? C111 N2 C141 110.6(8) . . ? C121 N2 C111 112.7(8) . . ? C121 N2 C131 110.0(7) . . ? C121 N2 C141 106.5(7) . . ? C131 N2 C141 111.6(7) . . ? N1 C1 H1 109.0 . . ? N1 C1 C2 108.5(12) . . ? N1 C1 C6 109.5(13) . . ? C2 C1 H1 109.0 . . ? C6 C1 H1 109.0 . . ? C6 C1 C2 111.8(16) . . ? C1 C2 H2A 110.0 . . ? C1 C2 H2B 110.0 . . ? C1 C2 C3 108.7(14) . . ? H2A C2 H2B 108.3 . . ? C3 C2 H2A 110.0 . . ? C3 C2 H2B 110.0 . . ? C2 C3 H3A 110.0 . . ? C2 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? C4 C3 C2 108.6(17) . . ? C4 C3 H3A 110.0 . . ? C4 C3 H3B 110.0 . . ? C3 C4 H4A 111.0 . . ? C3 C4 H4B 111.0 . . ? C3 C4 C5 103.8(18) . . ? H4A C4 H4B 109.0 . . ? C5 C4 H4A 111.0 . . ? C5 C4 H4B 111.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 C6 110.7(15) . . ? H5A C5 H5B 108.1 . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C1 C6 C5 109.3(14) . . ? C1 C6 H6A 109.8 . . ? C1 C6 H6B 109.8 . . ? C5 C6 H6A 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N2 C111 H11A 108.4 . . ? N2 C111 H11B 108.4 . . ? H11A C111 H11B 107.4 . . ? C112 C111 N2 115.6(8) . . ? C112 C111 H11A 108.4 . . ? C112 C111 H11B 108.4 . . ? C111 C112 H11C 109.3 . . ? C111 C112 H11D 109.3 . . ? C111 C112 C113 111.7(8) . . ? H11C C112 H11D 108.0 . . ? C113 C112 H11C 109.3 . . ? C113 C112 H11D 109.3 . . ? C112 C113 H11E 109.0 . . ? C112 C113 H11F 109.0 . . ? H11E C113 H11F 107.8 . . ? C114 C113 C112 113.0(11) . . ? C114 C113 H11E 109.0 . . ? C114 C113 H11F 109.0 . . ? C113 C114 H11G 109.5 . . ? C113 C114 H11H 109.5 . . ? C113 C114 H11I 109.5 . . ? H11G C114 H11H 109.5 . . ? H11G C114 H11I 109.5 . . ? H11H C114 H11I 109.5 . . ? N2 C121 H12A 108.2 . . ? N2 C121 H12B 108.2 . . ? H12A C121 H12B 107.3 . . ? C122 C121 N2 116.5(8) . . ? C122 C121 H12A 108.2 . . ? C122 C121 H12B 108.2 . . ? C121 C122 H12C 109.3 . . ? C121 C122 H12D 109.3 . . ? C121 C122 C123 111.5(9) . . ? H12C C122 H12D 108.0 . . ? C123 C122 H12C 109.3 . . ? C123 C122 H12D 109.3 . . ? C122 C123 H12E 109.5 . . ? C122 C123 H12F 109.5 . . ? C122 C123 C124 110.6(9) . . ? H12E C123 H12F 108.1 . . ? C124 C123 H12E 109.5 . . ? C124 C123 H12F 109.5 . . ? C123 C124 H12G 109.5 . . ? C123 C124 H12H 109.5 . . ? C123 C124 H12I 109.5 . . ? H12G C124 H12H 109.5 . . ? H12G C124 H12I 109.5 . . ? H12H C124 H12I 109.5 . . ? N2 C131 H13A 108.5 . . ? N2 C131 H13B 108.5 . . ? N2 C131 C132 115.1(6) . . ? H13A C131 H13B 107.5 . . ? C132 C131 H13A 108.5 . . ? C132 C131 H13B 108.5 . . ? C131 C132 H13C 109.7 . . ? C131 C132 H13D 109.7 . . ? C131 C132 C133 109.9(7) . . ? H13C C132 H13D 108.2 . . ? C133 C132 H13C 109.7 . . ? C133 C132 H13D 109.7 . . ? C132 C133 H13E 109.6 . . ? C132 C133 H13F 109.6 . . ? H13E C133 H13F 108.2 . . ? C134 C133 C132 110.1(8) . . ? C134 C133 H13E 109.6 . . ? C134 C133 H13F 109.6 . . ? C133 C134 H13G 109.5 . . ? C133 C134 H13H 109.5 . . ? C133 C134 H13I 109.5 . . ? H13G C134 H13H 109.5 . . ? H13G C134 H13I 109.5 . . ? H13H C134 H13I 109.5 . . ? N2 C141 H14A 108.2 . . ? N2 C141 H14B 108.2 . . ? H14A C141 H14B 107.3 . . ? C142 C141 N2 116.5(7) . . ? C142 C141 H14A 108.2 . . ? C142 C141 H14B 108.2 . . ? C141 C142 H14C 110.0 . . ? C141 C142 H14D 110.0 . . ? C141 C142 C143 108.3(9) . . ? H14C C142 H14D 108.4 . . ? C143 C142 H14C 110.0 . . ? C143 C142 H14D 110.0 . . ? C142 C143 H14E 109.1 . . ? C142 C143 H14F 109.1 . . ? H14E C143 H14F 107.8 . . ? C144 C143 C142 112.6(12) . . ? C144 C143 H14E 109.1 . . ? C144 C143 H14F 109.1 . . ? C143 C144 H14G 109.5 . . ? C143 C144 H14H 109.5 . . ? C143 C144 H14I 109.5 . . ? H14G C144 H14H 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? N3 C7 C8 167(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1 O3 1.00 2.83 3.72(2) 148.6 3 C3 H3B O3 0.99 2.83 3.75(3) 154.4 3 C5 H5A O3 0.99 2.93 3.81(3) 149.2 3 data_w _database_code_depnum_ccdc_archive 'CCDC 869448' _audit_creation_date 2012-04-24 _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C8 H18 Mo6 N2 O17, 2(C16 H36 N)' _chemical_formula_sum 'C40 H90 Mo6 N4 O17' _chemical_formula_weight 1474.80 _chemical_melting_point ? 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 16.492(3) _cell_length_b 17.087(3) _cell_length_c 22.417(5) _cell_angle_alpha 106.72(3) _cell_angle_beta 103.00(3) _cell_angle_gamma 96.29(3) _cell_volume 5791(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 37624 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.50 _cell_measurement_theta_min 3.00 _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2000))' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 2984 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_unetI/netI 0.0462 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 56187 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 3.00 _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.952 _diffrn_measured_fraction_theta_max 0.952 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_detector_area_resol_mean 28.5714 _diffrn_measurement_method dtprofit.ref _reflns_number_gt 15877 _reflns_number_total 25299 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.206 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.101 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1207 _refine_ls_number_reflns 25299 _refine_ls_number_restraints 863 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0553 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0954P)^2^+2.7186P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1582 _refine_ls_wR_factor_ref 0.1820 _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. The disorder in tert-butyl was modelled using the DFIX instruction of the same C-C distances of 1.53 angstrom with a deviation 0f 0.01angstrom. Also, the disorderly tetrabutyl ammonium cations was modelled with the 1, 2 C-C bond length of 1.53 angstrom 1,3 C-C distance of 2.50 angstrom. All the butyl chains in all the four tetrabutyl ammonium cations were modelled to have the same geometry with the SAME instruction. One butyl chain in two tetrabutyl ammonium cations, two butyl chain in the third tetrabutyl ammonium cation, and all the four butyl chains in the 4th tetrabutyl ammonium cation were modelled with the DELU and SiMU instructions to have the similar thermal motion. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.97156(3) 0.53692(3) 0.15945(3) 0.05433(14) Uani 1 1 d . . . Mo2 Mo 1.15519(3) 0.51363(4) 0.22887(3) 0.06062(15) Uani 1 1 d . . . Mo3 Mo 1.04286(4) 0.61499(3) 0.31590(3) 0.05616(14) Uani 1 1 d . . . Mo4 Mo 1.00163(4) 0.35263(3) 0.16220(3) 0.05889(15) Uani 1 1 d . . . Mo5 Mo 0.88589(3) 0.45330(3) 0.24988(3) 0.05451(14) Uani 1 1 d . . . Mo6 Mo 1.07576(4) 0.42981(3) 0.32162(3) 0.05868(15) Uani 1 1 d . . . Mo7 Mo 0.55464(4) 0.92683(4) 0.34598(3) 0.06552(16) Uani 1 1 d . . . Mo8 Mo 0.36995(3) 0.92922(3) 0.26341(3) 0.05647(14) Uani 1 1 d . . . Mo9 Mo 0.49684(4) 0.83111(3) 0.19061(3) 0.06414(16) Uani 1 1 d . . . Mo10 Mo 0.50888(3) 1.10016(3) 0.32628(3) 0.05580(14) Uani 1 1 d . . . Mo11 Mo 0.64041(3) 1.00433(4) 0.25346(3) 0.06783(17) Uani 1 1 d . . . Mo12 Mo 0.45043(4) 1.00635(4) 0.16836(3) 0.06603(16) Uani 1 1 d . . . O1 O 1.0237(2) 0.4857(2) 0.23868(16) 0.0420(8) Uani 1 1 d . . . O3 O 1.0561(4) 0.7079(3) 0.3731(2) 0.0830(15) Uani 1 1 d . . . O4 O 0.9868(4) 0.2569(3) 0.1087(3) 0.0904(16) Uani 1 1 d . . . O5 O 0.7871(3) 0.4313(3) 0.2581(3) 0.0825(15) Uani 1 1 d . . . O6 O 1.1116(4) 0.3883(3) 0.3797(2) 0.0883(16) Uani 1 1 d . . . O7 O 1.0904(3) 0.5533(3) 0.1651(2) 0.0576(10) Uani 1 1 d . . . O8 O 0.9952(3) 0.6349(2) 0.2377(2) 0.0560(10) Uani 1 1 d . . . O9 O 0.9639(3) 0.4202(3) 0.11138(19) 0.0603(10) Uani 1 1 d . . . O10 O 0.8696(2) 0.5016(3) 0.1824(2) 0.0575(10) Uani 1 1 d . . . O11 O 1.1480(3) 0.6146(3) 0.2959(2) 0.0608(10) Uani 1 1 d . . . O12 O 1.1150(3) 0.4003(3) 0.1694(2) 0.0653(11) Uani 1 1 d . . . O13 O 0.9285(3) 0.5636(2) 0.3093(2) 0.0570(10) Uani 1 1 d . . . O14 O 0.8960(3) 0.3542(2) 0.1865(2) 0.0596(10) Uani 1 1 d . . . O15 O 0.9554(3) 0.4157(2) 0.3132(2) 0.0594(10) Uani 1 1 d . . . O16 O 1.0790(3) 0.5446(3) 0.36769(19) 0.0640(11) Uani 1 1 d . . . O17 O 1.1737(3) 0.4642(3) 0.2993(2) 0.0671(12) Uani 1 1 d . . . O18 O 1.0474(3) 0.3350(2) 0.2438(2) 0.0651(11) Uani 1 1 d . . . O19 O 0.4135(5) 1.0339(4) 0.1030(3) 0.119(2) Uani 1 1 d . . . O20 O 0.7383(4) 1.0356(4) 0.2508(4) 0.117(2) Uani 1 1 d . . . O21 O 0.5119(4) 1.1985(3) 0.3731(3) 0.0879(16) Uani 1 1 d . . . O22 O 0.4981(4) 0.7361(3) 0.1414(3) 0.102(2) Uani 1 1 d . . . O23 O 0.4607(3) 0.8902(3) 0.1318(2) 0.0694(12) Uani 1 1 d . . . O24 O 0.4353(3) 0.9023(3) 0.3351(2) 0.0672(12) Uani 1 1 d . . . O25 O 0.5491(3) 1.0466(3) 0.3855(2) 0.0659(11) Uani 1 1 d . . . O26 O 0.3909(3) 0.8244(2) 0.2072(2) 0.0663(12) Uani 1 1 d . . . O27 O 0.5458(3) 0.8260(3) 0.2759(2) 0.0685(12) Uani 1 1 d . . . O28 O 0.6581(3) 0.9710(3) 0.3279(2) 0.0753(13) Uani 1 1 d . . . O29 O 0.5024(2) 0.9653(2) 0.25933(17) 0.0434(8) Uani 1 1 d . . . O30 O 0.3507(3) 0.9635(3) 0.1863(2) 0.0663(11) Uani 1 1 d . . . O31 O 0.6120(3) 0.8918(3) 0.2019(2) 0.0693(12) Uani 1 1 d . . . O32 O 0.5716(3) 1.0289(3) 0.1830(2) 0.0794(15) Uani 1 1 d . . . O33 O 0.4614(3) 1.1039(2) 0.2378(2) 0.0668(12) Uani 1 1 d . . . O34 O 0.6153(3) 1.1068(3) 0.3064(2) 0.0733(13) Uani 1 1 d . . . O35 O 0.3951(3) 1.0451(2) 0.3153(2) 0.0562(10) Uani 1 1 d . . . N1 N 0.9337(3) 0.5768(3) 0.0989(3) 0.0642(13) Uani 1 1 d . . . N2 N 1.2552(3) 0.5363(4) 0.2214(3) 0.0773(17) Uani 1 1 d . . . N3 N 0.5895(5) 0.9008(5) 0.4149(3) 0.094(2) Uani 1 1 d . . . N4 N 0.2712(3) 0.8938(4) 0.2681(3) 0.0787(17) Uani 1 1 d . . . N5 N 1.2030(4) 0.6829(4) 0.5649(3) 0.094(2) Uani 1 1 d . . . N6 N 1.2178(4) 0.1818(4) 0.2429(3) 0.0771(16) Uani 1 1 d . . . N7 N 0.7532(4) 0.7143(4) 0.2686(3) 0.0880(19) Uani 1 1 d D . . N8 N 1.3554(5) 0.7995(5) -0.0663(3) 0.138(3) Uani 1 1 d DU . . C1 C 0.9115(4) 0.6118(4) 0.0480(3) 0.0688(17) Uani 1 1 d D . . C2 C 0.8316(8) 0.6439(12) 0.0506(7) 0.286(14) Uani 1 1 d D . . H2A H 0.8409 0.6883 0.0905 0.429 Uiso 1 1 calc R . . H2B H 0.7881 0.5999 0.0481 0.429 Uiso 1 1 calc R . . H2C H 0.8141 0.6643 0.0150 0.429 Uiso 1 1 calc R . . C3 C 0.9849(7) 0.6734(10) 0.0517(7) 0.265(13) Uani 1 1 d D . . H3A H 0.9991 0.7172 0.0924 0.398 Uiso 1 1 calc R . . H3B H 0.9705 0.6963 0.0171 0.398 Uiso 1 1 calc R . . H3C H 1.0326 0.6465 0.0480 0.398 Uiso 1 1 calc R . . C4 C 0.8877(10) 0.5439(7) -0.0167(4) 0.166(6) Uani 1 1 d D . . H4A H 0.8385 0.5056 -0.0198 0.249 Uiso 1 1 calc R . . H4B H 0.9339 0.5148 -0.0205 0.249 Uiso 1 1 calc R . . H4C H 0.8756 0.5679 -0.0507 0.249 Uiso 1 1 calc R . . C5 C 1.3372(4) 0.5535(6) 0.2101(4) 0.094(3) Uani 1 1 d D . . C6 C 1.3243(8) 0.5454(16) 0.1398(6) 0.289(14) Uani 1 1 d D . . H6A H 1.2913 0.5851 0.1296 0.434 Uiso 1 1 calc R . . H6B H 1.2951 0.4903 0.1135 0.434 Uiso 1 1 calc R . . H6C H 1.3784 0.5558 0.1313 0.434 Uiso 1 1 calc R . . C7 C 1.3805(7) 0.6413(6) 0.2513(7) 0.158(5) Uani 1 1 d D . . H7A H 1.3483 0.6799 0.2383 0.237 Uiso 1 1 calc R . . H7B H 1.4364 0.6518 0.2460 0.237 Uiso 1 1 calc R . . H7C H 1.3843 0.6478 0.2959 0.237 Uiso 1 1 calc R . . C8 C 1.3875(7) 0.4921(8) 0.2279(9) 0.184(7) Uani 1 1 d . . . H8A H 1.3601 0.4370 0.2003 0.276 Uiso 1 1 calc R . . H8B H 1.3913 0.4962 0.2721 0.276 Uiso 1 1 calc R . . H8C H 1.4434 0.5038 0.2229 0.276 Uiso 1 1 calc R . . C9 C 0.6036(7) 0.8878(7) 0.4770(5) 0.113(4) Uani 1 1 d D . . C10 C 0.6834(10) 0.8524(11) 0.4901(7) 0.218(9) Uani 1 1 d . . . H10A H 0.7314 0.8926 0.4939 0.327 Uiso 1 1 calc R . . H10B H 0.6793 0.8028 0.4550 0.327 Uiso 1 1 calc R . . H10C H 0.6902 0.8393 0.5296 0.327 Uiso 1 1 calc R . . C11 C 0.6133(9) 0.9683(9) 0.5309(5) 0.196(8) Uani 1 1 d D . . H11A H 0.6655 1.0039 0.5364 0.294 Uiso 1 1 calc R . . H11B H 0.6138 0.9567 0.5704 0.294 Uiso 1 1 calc R . . H11C H 0.5668 0.9955 0.5201 0.294 Uiso 1 1 calc R . . C12 C 0.5223(12) 0.8311(9) 0.4720(7) 0.191(7) Uani 1 1 d . . . H12A H 0.5157 0.7788 0.4389 0.286 Uiso 1 1 calc R . . H12B H 0.4746 0.8569 0.4612 0.286 Uiso 1 1 calc R . . H12C H 0.5253 0.8219 0.5126 0.286 Uiso 1 1 calc R . . C13 C 0.2014(5) 0.8495(5) 0.2812(5) 0.097(3) Uani 1 1 d D . . C14 C 0.1452(9) 0.9100(8) 0.3028(10) 0.237(10) Uani 1 1 d D . . H14A H 0.1218 0.9303 0.2682 0.356 Uiso 1 1 calc R . . H14B H 0.1781 0.9558 0.3396 0.356 Uiso 1 1 calc R . . H14C H 0.1002 0.8823 0.3143 0.356 Uiso 1 1 calc R . . C15 C 0.1580(8) 0.7762(7) 0.2218(5) 0.163(6) Uani 1 1 d D . . H15A H 0.1327 0.7958 0.1872 0.244 Uiso 1 1 calc R . . H15B H 0.1149 0.7427 0.2311 0.244 Uiso 1 1 calc R . . H15C H 0.1988 0.7435 0.2093 0.244 Uiso 1 1 calc R . . C16 C 0.2393(7) 0.8152(7) 0.3355(5) 0.148(5) Uani 1 1 d D . . H16A H 0.2659 0.8607 0.3745 0.222 Uiso 1 1 calc R . . H16B H 0.2806 0.7831 0.3232 0.222 Uiso 1 1 calc R . . H16C H 0.1951 0.7806 0.3427 0.222 Uiso 1 1 calc R . . C111 C 1.1648(6) 0.7439(6) 0.5324(5) 0.122(4) Uani 1 1 d DU . . H11D H 1.1491 0.7171 0.4859 0.146 Uiso 1 1 calc R . . H11E H 1.1131 0.7536 0.5448 0.146 Uiso 1 1 calc R . . C112 C 1.2209(8) 0.8274(7) 0.5480(7) 0.173(6) Uani 1 1 d DU . . H11F H 1.2649 0.8210 0.5257 0.208 Uiso 1 1 calc R . . H11G H 1.2477 0.8500 0.5942 0.208 Uiso 1 1 calc R . . C113 C 1.1666(10) 0.8862(9) 0.5266(9) 0.264(10) Uani 1 1 d DU . . H11H H 1.1251 0.8558 0.4859 0.316 Uiso 1 1 calc R . . H11I H 1.1363 0.9072 0.5585 0.316 Uiso 1 1 calc R . . C114 C 1.2191(16) 0.9577(13) 0.5187(14) 0.43(2) Uani 1 1 d DU . . H11J H 1.1837 0.9820 0.4916 0.651 Uiso 1 1 calc R . . H11K H 1.2625 0.9383 0.4993 0.651 Uiso 1 1 calc R . . H11L H 1.2448 0.9987 0.5603 0.651 Uiso 1 1 calc R . . C121 C 1.2193(5) 0.7190(5) 0.6376(4) 0.091(3) Uani 1 1 d D . . H12D H 1.2335 0.6759 0.6562 0.110 Uiso 1 1 calc R . . H12E H 1.2687 0.7632 0.6536 0.110 Uiso 1 1 calc R . . C122 C 1.1489(6) 0.7533(5) 0.6626(5) 0.107(3) Uani 1 1 d D . . H12F H 1.0977 0.7112 0.6445 0.128 Uiso 1 1 calc R . . H12G H 1.1381 0.8006 0.6484 0.128 Uiso 1 1 calc R . . C123 C 1.1701(7) 0.7802(5) 0.7356(5) 0.113(3) Uani 1 1 d D . . H12H H 1.1768 0.7320 0.7496 0.136 Uiso 1 1 calc R . . H12I H 1.2236 0.8191 0.7536 0.136 Uiso 1 1 calc R . . C124 C 1.1030(7) 0.8206(7) 0.7617(7) 0.151(5) Uani 1 1 d D . . H12J H 1.1191 0.8363 0.8081 0.227 Uiso 1 1 calc R . . H12K H 1.0500 0.7821 0.7447 0.227 Uiso 1 1 calc R . . H12L H 1.0970 0.8692 0.7490 0.227 Uiso 1 1 calc R . . C131 C 1.1368(4) 0.6030(5) 0.5392(4) 0.082(2) Uani 1 1 d D . . H13A H 1.1191 0.5871 0.4923 0.099 Uiso 1 1 calc R . . H13B H 1.0876 0.6148 0.5547 0.099 Uiso 1 1 calc R . . C132 C 1.1647(5) 0.5289(5) 0.5576(4) 0.087(2) Uani 1 1 d D . . H13C H 1.2097 0.5120 0.5383 0.105 Uiso 1 1 calc R . . H13D H 1.1862 0.5445 0.6042 0.105 Uiso 1 1 calc R . . C133 C 1.0910(5) 0.4583(4) 0.5341(4) 0.084(2) Uani 1 1 d D . . H13E H 1.0654 0.4486 0.4885 0.101 Uiso 1 1 calc R . . H13F H 1.0490 0.4743 0.5571 0.101 Uiso 1 1 calc R . . C134 C 1.1133(7) 0.3776(5) 0.5426(5) 0.113(3) Uani 1 1 d D . . H13G H 1.0630 0.3353 0.5265 0.169 Uiso 1 1 calc R . . H13H H 1.1372 0.3860 0.5877 0.169 Uiso 1 1 calc R . . H13I H 1.1537 0.3603 0.5191 0.169 Uiso 1 1 calc R . . C141 C 1.2860(5) 0.6655(7) 0.5513(5) 0.125(4) Uani 1 1 d D . . H14D H 1.3063 0.6271 0.5731 0.150 Uiso 1 1 calc R . . H14E H 1.3273 0.7169 0.5694 0.150 Uiso 1 1 calc R . . C142 C 1.2805(7) 0.6291(11) 0.4797(6) 0.174(6) Uani 1 1 d D . . H14F H 1.2457 0.5738 0.4616 0.209 Uiso 1 1 calc R . . H14G H 1.2558 0.6640 0.4560 0.209 Uiso 1 1 calc R . . C143 C 1.3703(8) 0.6254(14) 0.4753(7) 0.231(9) Uani 1 1 d D . . H14H H 1.4064 0.6793 0.4992 0.277 Uiso 1 1 calc R . . H14I H 1.3918 0.5848 0.4941 0.277 Uiso 1 1 calc R . . C144 C 1.3711(12) 0.602(2) 0.4056(8) 0.36(2) Uani 1 1 d D . . H14J H 1.4275 0.5965 0.4024 0.540 Uiso 1 1 calc R . . H14K H 1.3530 0.6437 0.3879 0.540 Uiso 1 1 calc R . . H14L H 1.3335 0.5494 0.3818 0.540 Uiso 1 1 calc R . . C211 C 1.1981(6) 0.2287(6) 0.1943(4) 0.094(3) Uani 1 1 d D . . H21A H 1.1435 0.2018 0.1639 0.113 Uiso 1 1 calc R . . H21B H 1.1934 0.2848 0.2174 0.113 Uiso 1 1 calc R . . C212 C 1.2627(6) 0.2338(7) 0.1567(5) 0.113(3) Uani 1 1 d D . . H21C H 1.3136 0.2723 0.1851 0.135 Uiso 1 1 calc R . . H21D H 1.2775 0.1795 0.1417 0.135 Uiso 1 1 calc R . . C213 C 1.2305(10) 0.2619(8) 0.0997(6) 0.158(6) Uani 1 1 d D . . H21E H 1.2768 0.2754 0.0821 0.190 Uiso 1 1 calc R . . H21F H 1.2068 0.3115 0.1131 0.190 Uiso 1 1 calc R . . C214 C 1.1623(12) 0.1924(12) 0.0478(7) 0.236(10) Uani 1 1 d D . . H21G H 1.1412 0.2106 0.0115 0.354 Uiso 1 1 calc R . . H21H H 1.1167 0.1793 0.0654 0.354 Uiso 1 1 calc R . . H21I H 1.1864 0.1439 0.0340 0.354 Uiso 1 1 calc R . . C221 C 1.2219(5) 0.0932(4) 0.2088(4) 0.086(2) Uani 1 1 d D . . H22A H 1.2364 0.0655 0.2409 0.103 Uiso 1 1 calc R . . H22B H 1.2670 0.0932 0.1875 0.103 Uiso 1 1 calc R . . C222 C 1.1407(6) 0.0435(6) 0.1589(5) 0.109(3) Uani 1 1 d D . . H22C H 1.0981 0.0338 0.1809 0.131 Uiso 1 1 calc R . . H22D H 1.1201 0.0756 0.1314 0.131 Uiso 1 1 calc R . . C223 C 1.1523(7) -0.0386(6) 0.1178(5) 0.133(4) Uani 1 1 d D . . H22E H 1.1728 -0.0707 0.1454 0.160 Uiso 1 1 calc R . . H22F H 1.1950 -0.0289 0.0959 0.160 Uiso 1 1 calc R . . C224 C 1.0713(7) -0.0885(7) 0.0678(6) 0.150(5) Uani 1 1 d D . . H22G H 1.0827 -0.1391 0.0416 0.224 Uiso 1 1 calc R . . H22H H 1.0501 -0.0566 0.0408 0.224 Uiso 1 1 calc R . . H22I H 1.0299 -0.1014 0.0892 0.224 Uiso 1 1 calc R . . C231 C 1.1486(6) 0.1876(6) 0.2776(4) 0.101(3) Uani 1 1 d D . . H23A H 1.1470 0.2458 0.2968 0.121 Uiso 1 1 calc R . . H23B H 1.0946 0.1620 0.2458 0.121 Uiso 1 1 calc R . . C232 C 1.1573(8) 0.1477(9) 0.3295(6) 0.145(5) Uani 1 1 d D . . H23C H 1.2119 0.1708 0.3610 0.174 Uiso 1 1 calc R . . H23D H 1.1542 0.0884 0.3108 0.174 Uiso 1 1 calc R . . C233 C 1.0866(9) 0.1631(12) 0.3625(7) 0.197(7) Uani 1 1 d D . . H23E H 1.0864 0.2223 0.3762 0.236 Uiso 1 1 calc R . . H23F H 1.0329 0.1357 0.3310 0.236 Uiso 1 1 calc R . . C234 C 1.0924(13) 0.1340(13) 0.4196(8) 0.259(10) Uani 1 1 d D . . H23G H 1.0458 0.1467 0.4374 0.388 Uiso 1 1 calc R . . H23H H 1.1448 0.1616 0.4517 0.388 Uiso 1 1 calc R . . H23I H 1.0904 0.0750 0.4065 0.388 Uiso 1 1 calc R . . C241 C 1.3046(5) 0.2221(5) 0.2911(4) 0.093(2) Uani 1 1 d DU . . H24A H 1.3150 0.1923 0.3221 0.111 Uiso 1 1 calc R . . H24B H 1.3476 0.2151 0.2678 0.111 Uiso 1 1 calc R . . C242 C 1.3148(7) 0.3124(6) 0.3274(6) 0.153(5) Uani 1 1 d DU . . H24C H 1.2675 0.3206 0.3461 0.184 Uiso 1 1 calc R . . H24D H 1.3122 0.3432 0.2970 0.184 Uiso 1 1 calc R . . C243 C 1.3965(8) 0.3484(8) 0.3808(7) 0.203(7) Uani 1 1 d DU . . H24E H 1.4144 0.4066 0.3863 0.244 Uiso 1 1 calc R . . H24F H 1.4409 0.3187 0.3703 0.244 Uiso 1 1 calc R . . C244 C 1.3794(15) 0.3391(19) 0.4426(9) 0.377(17) Uani 1 1 d DU . . H24G H 1.4307 0.3593 0.4772 0.566 Uiso 1 1 calc R . . H24H H 1.3596 0.2815 0.4361 0.566 Uiso 1 1 calc R . . H24I H 1.3370 0.3706 0.4536 0.566 Uiso 1 1 calc R . . C311 C 0.7570(7) 0.6370(7) 0.2173(5) 0.133(4) Uani 1 1 d DU . . H31A H 0.7635 0.5926 0.2360 0.159 Uiso 1 1 calc R . . H31B H 0.8064 0.6472 0.2020 0.159 Uiso 1 1 calc R . . C312 C 0.6774(8) 0.6088(8) 0.1597(6) 0.160(5) Uani 1 1 d DU . . H31C H 0.6271 0.6106 0.1752 0.192 Uiso 1 1 calc R . . H31D H 0.6779 0.6459 0.1341 0.192 Uiso 1 1 calc R . . C313 C 0.6760(12) 0.5198(10) 0.1178(9) 0.283(11) Uani 1 1 d DU . . H31E H 0.7239 0.5189 0.0994 0.340 Uiso 1 1 calc R . . H31F H 0.6801 0.4835 0.1442 0.340 Uiso 1 1 calc R . . C314 C 0.5941(13) 0.4896(13) 0.0642(10) 0.324(14) Uani 1 1 d DU . . H31G H 0.5894 0.4317 0.0414 0.487 Uiso 1 1 calc R . . H31H H 0.5940 0.5208 0.0347 0.487 Uiso 1 1 calc R . . H31I H 0.5470 0.4972 0.0824 0.487 Uiso 1 1 calc R . . C321 C 0.7458(8) 0.7865(7) 0.2413(6) 0.139(4) Uani 1 1 d DU . . H32A H 0.7434 0.8361 0.2749 0.167 Uiso 1 1 calc R . . H32B H 0.6943 0.7728 0.2064 0.167 Uiso 1 1 calc R . . C322 C 0.8232(9) 0.8024(8) 0.2161(6) 0.154(5) Uani 1 1 d DU . . H32C H 0.8740 0.7995 0.2465 0.185 Uiso 1 1 calc R . . H32D H 0.8169 0.7598 0.1751 0.185 Uiso 1 1 calc R . . C323 C 0.8313(11) 0.8864(10) 0.2074(11) 0.241(8) Uani 1 1 d DU . . H32E H 0.8328 0.9278 0.2479 0.289 Uiso 1 1 calc R . . H32F H 0.7814 0.8874 0.1753 0.289 Uiso 1 1 calc R . . C324 C 0.9084(9) 0.9102(10) 0.1869(10) 0.232(9) Uani 1 1 d DU . . H32G H 0.9090 0.9641 0.1818 0.347 Uiso 1 1 calc R . . H32H H 0.9071 0.8701 0.1465 0.347 Uiso 1 1 calc R . . H32I H 0.9583 0.9116 0.2192 0.347 Uiso 1 1 calc R . . C331 C 0.6815(7) 0.7030(9) 0.2977(6) 0.163(6) Uani 1 1 d D . . H33A H 0.6286 0.6935 0.2649 0.195 Uiso 1 1 calc R . . H33B H 0.6845 0.7539 0.3321 0.195 Uiso 1 1 calc R . . C332 C 0.6815(6) 0.6306(8) 0.3251(6) 0.129(4) Uani 1 1 d D . . H33C H 0.6810 0.5802 0.2911 0.155 Uiso 1 1 calc R . . H33D H 0.7335 0.6413 0.3591 0.155 Uiso 1 1 calc R . . C333 C 0.6081(8) 0.6165(10) 0.3518(8) 0.227(9) Uani 1 1 d D . . H33E H 0.5560 0.6061 0.3179 0.273 Uiso 1 1 calc R . . H33F H 0.6086 0.6668 0.3860 0.273 Uiso 1 1 calc R . . C334 C 0.6081(9) 0.5448(10) 0.3784(8) 0.189(7) Uani 1 1 d D . . H33G H 0.5599 0.5396 0.3952 0.283 Uiso 1 1 calc R . . H33H H 0.6591 0.5549 0.4124 0.283 Uiso 1 1 calc R . . H33I H 0.6054 0.4944 0.3445 0.283 Uiso 1 1 calc R . . C341 C 0.8384(5) 0.7365(6) 0.3209(4) 0.120(3) Uani 1 1 d D . . H34A H 0.8474 0.6888 0.3350 0.143 Uiso 1 1 calc R . . H34B H 0.8839 0.7492 0.3023 0.143 Uiso 1 1 calc R . . C342 C 0.8413(7) 0.8111(7) 0.3795(5) 0.132(4) Uani 1 1 d D . . H34C H 0.8076 0.7935 0.4053 0.159 Uiso 1 1 calc R . . H34D H 0.8165 0.8533 0.3646 0.159 Uiso 1 1 calc R . . C343 C 0.9324(9) 0.8487(11) 0.4219(7) 0.188(6) Uani 1 1 d D . . H34E H 0.9300 0.8852 0.4633 0.225 Uiso 1 1 calc R . . H34F H 0.9601 0.8041 0.4299 0.225 Uiso 1 1 calc R . . C344 C 0.9862(12) 0.8974(14) 0.3931(12) 0.308(14) Uani 1 1 d D . . H34G H 1.0432 0.9143 0.4204 0.463 Uiso 1 1 calc R . . H34H H 0.9633 0.9458 0.3899 0.463 Uiso 1 1 calc R . . H34I H 0.9861 0.8631 0.3509 0.463 Uiso 1 1 calc R . . C411 C 1.3591(8) 0.7384(6) -0.1312(4) 0.135(4) Uani 1 1 d DU . . H41A H 1.3832 0.6924 -0.1220 0.162 Uiso 1 1 calc R . . H41B H 1.3014 0.7159 -0.1576 0.162 Uiso 1 1 calc R . . C412 C 1.4072(8) 0.7703(8) -0.1706(5) 0.171(5) Uani 1 1 d DU . . H41C H 1.4667 0.7871 -0.1471 0.206 Uiso 1 1 calc R . . H41D H 1.3869 0.8189 -0.1778 0.206 Uiso 1 1 calc R . . C413 C 1.3978(8) 0.7061(11) -0.2343(6) 0.237(9) Uani 1 1 d DU . . H41E H 1.3759 0.7287 -0.2684 0.284 Uiso 1 1 calc R . . H41F H 1.3562 0.6584 -0.2390 0.284 Uiso 1 1 calc R . . C414 C 1.4784(11) 0.6769(13) -0.2435(11) 0.333(15) Uani 1 1 d DU . . H41G H 1.4651 0.6266 -0.2796 0.500 Uiso 1 1 calc R . . H41H H 1.5076 0.6664 -0.2051 0.500 Uiso 1 1 calc R . . H41I H 1.5140 0.7189 -0.2514 0.500 Uiso 1 1 calc R . . C421 C 1.3138(8) 0.8644(7) -0.0874(6) 0.198(6) Uani 1 1 d DU . . H42A H 1.2650 0.8368 -0.1240 0.238 Uiso 1 1 calc R . . H42B H 1.3533 0.8959 -0.1020 0.238 Uiso 1 1 calc R . . C422 C 1.2853(16) 0.9242(12) -0.0358(9) 0.322(11) Uani 1 1 d DU . . H42C H 1.3338 0.9566 -0.0003 0.386 Uiso 1 1 calc R . . H42D H 1.2477 0.8940 -0.0189 0.386 Uiso 1 1 calc R . . C423 C 1.2392(15) 0.9815(13) -0.0666(11) 0.336(13) Uani 1 1 d DU . . H42E H 1.2657 1.0388 -0.0422 0.403 Uiso 1 1 calc R . . H42F H 1.2449 0.9706 -0.1102 0.403 Uiso 1 1 calc R . . C424 C 1.1454(16) 0.970(2) -0.0691(15) 0.420(18) Uani 1 1 d DU . . H42G H 1.1246 1.0196 -0.0717 0.630 Uiso 1 1 calc R . . H42H H 1.1379 0.9591 -0.0308 0.630 Uiso 1 1 calc R . . H42I H 1.1145 0.9239 -0.1065 0.630 Uiso 1 1 calc R . . C431 C 1.3033(8) 0.7465(6) -0.0388(5) 0.201(5) Uani 1 1 d DU . . H43A H 1.2488 0.7225 -0.0703 0.241 Uiso 1 1 calc R . . H43B H 1.3317 0.7010 -0.0342 0.241 Uiso 1 1 calc R . . C432 C 1.2875(14) 0.7897(10) 0.0252(7) 0.315(11) Uani 1 1 d DU . . H43C H 1.2709 0.8423 0.0250 0.378 Uiso 1 1 calc R . . H43D H 1.3391 0.8009 0.0597 0.378 Uiso 1 1 calc R . . C433 C 1.2170(11) 0.7343(13) 0.0371(13) 0.294(12) Uani 1 1 d DU . . H43E H 1.2154 0.7555 0.0818 0.353 Uiso 1 1 calc R . . H43F H 1.1625 0.7345 0.0096 0.353 Uiso 1 1 calc R . . C434 C 1.2346(14) 0.6462(12) 0.0222(16) 0.328(14) Uani 1 1 d DU . . H43G H 1.1940 0.6124 0.0335 0.492 Uiso 1 1 calc R . . H43H H 1.2906 0.6471 0.0469 0.492 Uiso 1 1 calc R . . H43I H 1.2303 0.6235 -0.0231 0.492 Uiso 1 1 calc R . . C441 C 1.4459(5) 0.8361(8) -0.0266(5) 0.200(6) Uani 1 1 d DU . . H44A H 1.4717 0.8686 -0.0488 0.240 Uiso 1 1 calc R . . H44B H 1.4444 0.8744 0.0144 0.240 Uiso 1 1 calc R . . C442 C 1.5030(11) 0.7781(12) -0.0123(7) 0.276(9) Uani 1 1 d DU . . H44C H 1.5057 0.7386 -0.0524 0.332 Uiso 1 1 calc R . . H44D H 1.4812 0.7474 0.0128 0.332 Uiso 1 1 calc R . . C443 C 1.5924(11) 0.8290(14) 0.0262(8) 0.337(11) Uani 1 1 d DU . . H44E H 1.6153 0.8590 0.0011 0.405 Uiso 1 1 calc R . . H44F H 1.5904 0.8687 0.0664 0.405 Uiso 1 1 calc R . . C444 C 1.6468(15) 0.7654(19) 0.0396(11) 0.460(19) Uani 1 1 d DU . . H44G H 1.7039 0.7935 0.0623 0.690 Uiso 1 1 calc R . . H44H H 1.6464 0.7254 -0.0007 0.690 Uiso 1 1 calc R . . H44I H 1.6241 0.7374 0.0654 0.690 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0547(3) 0.0612(3) 0.0533(3) 0.0285(3) 0.0112(2) 0.0161(2) Mo2 0.0435(3) 0.0716(3) 0.0727(4) 0.0292(3) 0.0185(3) 0.0130(2) Mo3 0.0651(3) 0.0408(2) 0.0552(3) 0.0079(2) 0.0117(3) 0.0094(2) Mo4 0.0693(3) 0.0461(3) 0.0575(3) 0.0074(2) 0.0189(3) 0.0167(2) Mo5 0.0479(3) 0.0519(3) 0.0694(3) 0.0217(3) 0.0237(3) 0.0102(2) Mo6 0.0701(3) 0.0596(3) 0.0557(3) 0.0289(3) 0.0158(3) 0.0253(3) Mo7 0.0631(3) 0.0806(4) 0.0659(4) 0.0388(3) 0.0150(3) 0.0305(3) Mo8 0.0372(2) 0.0544(3) 0.0741(4) 0.0164(3) 0.0149(2) 0.0051(2) Mo9 0.0654(3) 0.0412(3) 0.0805(4) 0.0057(3) 0.0279(3) 0.0088(2) Mo10 0.0605(3) 0.0416(2) 0.0542(3) 0.0045(2) 0.0102(2) 0.0050(2) Mo11 0.0479(3) 0.0683(4) 0.0811(4) 0.0141(3) 0.0250(3) -0.0030(3) Mo12 0.0849(4) 0.0650(3) 0.0465(3) 0.0212(3) 0.0095(3) 0.0152(3) O1 0.0430(19) 0.0406(18) 0.046(2) 0.0162(16) 0.0142(16) 0.0112(15) O3 0.109(4) 0.050(2) 0.075(3) 0.000(2) 0.021(3) 0.013(3) O4 0.119(4) 0.057(3) 0.089(4) 0.002(3) 0.039(3) 0.024(3) O5 0.057(3) 0.085(3) 0.112(4) 0.033(3) 0.037(3) 0.008(2) O6 0.115(4) 0.097(4) 0.076(3) 0.054(3) 0.026(3) 0.043(3) O7 0.058(2) 0.065(2) 0.061(3) 0.032(2) 0.024(2) 0.0147(19) O8 0.066(3) 0.043(2) 0.063(3) 0.0207(19) 0.017(2) 0.0158(18) O9 0.067(3) 0.062(2) 0.047(2) 0.0119(19) 0.013(2) 0.011(2) O10 0.044(2) 0.062(2) 0.067(3) 0.024(2) 0.0117(19) 0.0131(18) O11 0.053(2) 0.058(2) 0.064(3) 0.018(2) 0.008(2) -0.0009(19) O12 0.071(3) 0.065(3) 0.070(3) 0.020(2) 0.033(2) 0.029(2) O13 0.061(2) 0.053(2) 0.060(2) 0.0136(19) 0.027(2) 0.0198(19) O14 0.060(2) 0.047(2) 0.067(3) 0.0116(19) 0.019(2) 0.0017(18) O15 0.072(3) 0.055(2) 0.066(3) 0.030(2) 0.031(2) 0.016(2) O16 0.074(3) 0.068(3) 0.045(2) 0.017(2) 0.008(2) 0.011(2) O17 0.053(2) 0.085(3) 0.074(3) 0.040(3) 0.014(2) 0.028(2) O18 0.082(3) 0.048(2) 0.077(3) 0.027(2) 0.029(2) 0.029(2) O19 0.172(7) 0.131(5) 0.068(4) 0.059(4) 0.016(4) 0.043(5) O20 0.067(3) 0.124(5) 0.155(6) 0.029(4) 0.053(4) -0.011(3) O21 0.115(4) 0.053(3) 0.079(3) -0.002(2) 0.027(3) 0.007(3) O22 0.122(5) 0.047(3) 0.128(5) -0.009(3) 0.067(4) 0.009(3) O23 0.078(3) 0.064(3) 0.050(2) 0.001(2) 0.012(2) 0.006(2) O24 0.075(3) 0.066(3) 0.082(3) 0.038(2) 0.039(3) 0.024(2) O25 0.061(3) 0.074(3) 0.049(2) 0.010(2) 0.001(2) 0.013(2) O26 0.056(2) 0.044(2) 0.090(3) 0.007(2) 0.026(2) -0.0031(18) O27 0.074(3) 0.062(3) 0.094(3) 0.040(3) 0.040(3) 0.035(2) O28 0.043(2) 0.094(3) 0.081(3) 0.023(3) 0.005(2) 0.019(2) O29 0.0368(18) 0.0397(18) 0.048(2) 0.0118(16) 0.0057(15) 0.0037(14) O30 0.050(2) 0.072(3) 0.061(3) 0.014(2) -0.007(2) 0.013(2) O31 0.064(3) 0.071(3) 0.080(3) 0.020(2) 0.035(2) 0.020(2) O32 0.103(4) 0.064(3) 0.078(3) 0.018(2) 0.054(3) -0.006(3) O33 0.092(3) 0.049(2) 0.064(3) 0.025(2) 0.018(2) 0.017(2) O34 0.066(3) 0.057(2) 0.078(3) 0.005(2) 0.016(2) -0.016(2) O35 0.058(2) 0.055(2) 0.058(2) 0.0142(19) 0.021(2) 0.0209(19) N1 0.064(3) 0.073(3) 0.060(3) 0.030(3) 0.013(3) 0.019(3) N2 0.048(3) 0.097(4) 0.096(4) 0.043(4) 0.022(3) 0.016(3) N3 0.106(5) 0.119(6) 0.088(5) 0.055(4) 0.037(4) 0.062(4) N4 0.053(3) 0.067(3) 0.114(5) 0.019(3) 0.033(3) 0.007(3) N5 0.057(3) 0.116(5) 0.091(5) 0.057(4) -0.024(3) -0.028(3) N6 0.072(4) 0.078(4) 0.089(4) 0.034(3) 0.016(3) 0.040(3) N7 0.095(5) 0.100(5) 0.091(5) 0.039(4) 0.033(4) 0.070(4) N8 0.201(8) 0.138(7) 0.053(4) 0.022(4) -0.006(4) 0.051(6) C1 0.082(5) 0.070(4) 0.067(4) 0.033(4) 0.023(4) 0.027(4) C2 0.35(2) 0.53(3) 0.254(18) 0.31(2) 0.235(18) 0.37(3) C3 0.230(18) 0.28(2) 0.234(17) 0.204(17) -0.098(14) -0.140(16) C4 0.238(16) 0.164(11) 0.076(7) 0.035(7) 0.010(8) 0.028(11) C5 0.042(4) 0.128(7) 0.122(7) 0.052(6) 0.025(4) 0.014(4) C6 0.103(10) 0.65(4) 0.158(14) 0.21(2) 0.043(9) 0.014(16) C7 0.101(8) 0.125(9) 0.262(17) 0.081(11) 0.061(10) 0.004(7) C8 0.079(7) 0.131(10) 0.36(2) 0.079(12) 0.077(10) 0.046(7) C9 0.138(9) 0.153(9) 0.100(7) 0.077(7) 0.057(7) 0.095(8) C10 0.242(18) 0.33(2) 0.175(14) 0.167(16) 0.063(12) 0.190(17) C11 0.174(13) 0.31(2) 0.088(9) 0.024(11) 0.057(9) 0.049(14) C12 0.31(2) 0.144(12) 0.158(13) 0.071(10) 0.093(14) 0.064(13) C13 0.060(4) 0.074(5) 0.155(9) 0.029(5) 0.043(5) 0.000(4) C14 0.147(12) 0.170(13) 0.46(3) 0.089(17) 0.202(17) 0.058(10) C15 0.157(11) 0.137(9) 0.131(9) 0.040(8) -0.027(8) -0.082(9) C16 0.166(11) 0.128(9) 0.120(9) 0.027(7) 0.039(8) -0.061(8) C111 0.110(7) 0.128(7) 0.105(7) 0.065(6) -0.028(6) -0.028(6) C112 0.166(11) 0.156(9) 0.174(11) 0.104(9) -0.028(9) -0.050(8) C113 0.283(19) 0.189(12) 0.282(17) 0.179(13) -0.092(15) -0.035(12) C114 0.49(4) 0.26(2) 0.45(4) 0.25(2) -0.15(3) -0.14(2) C121 0.077(5) 0.092(5) 0.081(5) 0.040(5) -0.022(4) -0.025(4) C122 0.086(6) 0.089(6) 0.133(9) 0.053(6) -0.002(6) -0.015(5) C123 0.139(9) 0.065(5) 0.114(8) 0.024(5) 0.018(7) -0.024(5) C124 0.132(10) 0.117(9) 0.181(13) 0.017(9) 0.045(10) 0.006(8) C131 0.059(4) 0.097(5) 0.074(5) 0.037(4) -0.012(3) -0.011(4) C132 0.067(5) 0.104(6) 0.090(6) 0.039(5) 0.011(4) 0.008(4) C133 0.084(5) 0.093(5) 0.070(5) 0.023(4) 0.016(4) 0.013(4) C134 0.139(9) 0.099(7) 0.108(7) 0.042(6) 0.036(7) 0.032(6) C141 0.062(5) 0.185(11) 0.118(8) 0.069(8) 0.002(5) -0.028(6) C142 0.096(9) 0.30(2) 0.134(11) 0.090(12) 0.035(8) 0.006(10) C143 0.151(14) 0.35(3) 0.150(14) 0.038(16) 0.046(12) -0.013(15) C144 0.185(19) 0.70(6) 0.186(19) 0.11(3) 0.103(16) 0.04(3) C211 0.106(6) 0.093(6) 0.102(6) 0.044(5) 0.028(5) 0.057(5) C212 0.115(8) 0.137(9) 0.115(8) 0.060(7) 0.048(6) 0.048(6) C213 0.232(17) 0.143(11) 0.155(13) 0.065(10) 0.107(13) 0.100(11) C214 0.35(3) 0.26(2) 0.171(17) 0.116(17) 0.124(19) 0.13(2) C221 0.091(6) 0.069(4) 0.098(6) 0.027(4) 0.018(5) 0.034(4) C222 0.094(7) 0.106(7) 0.130(8) 0.038(6) 0.031(6) 0.027(5) C223 0.116(8) 0.105(7) 0.131(9) -0.001(7) -0.010(7) 0.020(6) C224 0.118(9) 0.144(10) 0.143(11) 0.009(8) 0.002(8) 0.016(8) C231 0.107(7) 0.110(7) 0.107(7) 0.042(6) 0.043(6) 0.055(5) C232 0.170(12) 0.178(12) 0.146(11) 0.103(10) 0.078(9) 0.068(10) C233 0.167(14) 0.28(2) 0.194(16) 0.150(16) 0.058(12) 0.044(13) C234 0.28(3) 0.30(3) 0.27(2) 0.14(2) 0.14(2) 0.10(2) C241 0.093(6) 0.083(5) 0.104(6) 0.034(4) 0.015(5) 0.037(4) C242 0.131(9) 0.106(7) 0.179(11) 0.013(7) -0.003(8) 0.032(7) C243 0.171(13) 0.136(10) 0.206(14) -0.025(10) -0.046(10) 0.060(9) C244 0.33(3) 0.55(4) 0.172(14) 0.01(2) 0.006(17) 0.15(3) C311 0.143(9) 0.131(8) 0.122(8) 0.026(6) 0.030(6) 0.067(7) C312 0.149(10) 0.172(11) 0.133(10) 0.037(8) 0.003(7) 0.029(9) C313 0.27(2) 0.212(16) 0.225(18) -0.020(12) -0.088(14) 0.049(15) C314 0.26(2) 0.28(2) 0.27(2) -0.013(17) -0.113(18) 0.02(2) C321 0.169(11) 0.137(9) 0.139(10) 0.066(8) 0.044(8) 0.078(8) C322 0.199(12) 0.163(10) 0.125(9) 0.069(8) 0.062(9) 0.039(9) C323 0.215(16) 0.204(14) 0.39(2) 0.155(15) 0.146(15) 0.076(13) C324 0.147(13) 0.205(16) 0.35(3) 0.119(17) 0.075(14) -0.017(11) C331 0.104(8) 0.267(18) 0.131(10) 0.054(11) 0.033(7) 0.113(10) C332 0.099(7) 0.198(12) 0.143(10) 0.099(9) 0.056(7) 0.078(8) C333 0.134(13) 0.27(2) 0.212(18) 0.033(17) 0.023(12) -0.067(14) C334 0.141(12) 0.226(17) 0.247(18) 0.152(16) 0.056(12) 0.016(11) C341 0.086(6) 0.128(8) 0.148(10) 0.047(8) 0.021(6) 0.054(6) C342 0.147(11) 0.129(9) 0.096(8) -0.001(7) 0.035(7) 0.019(8) C343 0.157(14) 0.199(16) 0.193(16) 0.055(13) 0.045(12) 0.004(12) C344 0.21(2) 0.31(3) 0.44(4) 0.25(3) 0.02(2) 0.009(19) C411 0.206(11) 0.098(6) 0.083(5) 0.023(5) 0.032(6) -0.013(6) C412 0.181(11) 0.184(11) 0.102(7) 0.036(7) 0.014(7) -0.080(9) C413 0.164(12) 0.33(2) 0.144(11) -0.014(11) 0.068(11) -0.062(12) C414 0.194(18) 0.23(2) 0.43(3) -0.04(2) 0.018(19) 0.026(17) C421 0.268(14) 0.175(11) 0.171(13) 0.093(9) 0.025(11) 0.087(10) C422 0.51(3) 0.247(19) 0.227(18) 0.075(14) 0.057(18) 0.217(16) C423 0.48(3) 0.37(2) 0.212(19) 0.115(17) 0.07(2) 0.29(2) C424 0.56(4) 0.56(4) 0.36(3) 0.27(3) 0.27(3) 0.37(3) C431 0.326(14) 0.212(13) 0.156(11) 0.120(10) 0.119(10) 0.152(10) C432 0.31(2) 0.37(2) 0.280(17) 0.061(16) 0.193(16) 0.024(18) C433 0.122(13) 0.40(3) 0.300(19) 0.04(2) 0.076(13) -0.041(17) C434 0.150(18) 0.41(3) 0.40(4) 0.13(4) 0.07(2) -0.03(2) C441 0.196(9) 0.282(15) 0.072(7) -0.021(8) 0.005(6) 0.115(8) C442 0.294(15) 0.48(2) 0.117(11) 0.111(14) 0.069(11) 0.263(16) C443 0.251(15) 0.70(3) 0.128(13) 0.160(18) 0.066(11) 0.279(18) C444 0.36(2) 0.98(5) 0.24(2) 0.33(3) 0.148(18) 0.46(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo2 3.2017(12) . ? Mo1 O1 2.243(3) . ? Mo1 O7 1.919(4) . ? Mo1 O8 1.972(4) . ? Mo1 O9 1.951(4) . ? Mo1 O10 1.950(4) . ? Mo1 N1 1.715(5) . ? Mo2 O1 2.242(3) . ? Mo2 O7 1.916(4) . ? Mo2 O11 1.970(4) . ? Mo2 O12 1.950(5) . ? Mo2 O17 1.975(4) . ? Mo2 N2 1.709(5) . ? Mo3 O1 2.319(3) . ? Mo3 O3 1.685(4) . ? Mo3 O8 1.895(4) . ? Mo3 O11 1.886(4) . ? Mo3 O13 1.947(4) . ? Mo3 O16 1.949(4) . ? Mo4 O1 2.353(3) . ? Mo4 O4 1.681(5) . ? Mo4 O9 1.900(4) . ? Mo4 O12 1.908(4) . ? Mo4 O14 1.939(4) . ? Mo4 O18 1.936(5) . ? Mo5 O1 2.366(3) . ? Mo5 O5 1.693(4) . ? Mo5 O10 1.905(4) . ? Mo5 O13 1.914(4) . ? Mo5 O14 1.923(4) . ? Mo5 O15 1.922(4) . ? Mo6 O1 2.364(3) . ? Mo6 O6 1.681(5) . ? Mo6 O15 1.933(4) . ? Mo6 O16 1.924(4) . ? Mo6 O17 1.879(4) . ? Mo6 O18 1.931(5) . ? Mo7 Mo8 3.1998(13) . ? Mo7 O24 1.912(5) . ? Mo7 O25 2.003(5) . ? Mo7 O27 1.935(5) . ? Mo7 O28 1.962(5) . ? Mo7 O29 2.248(4) . ? Mo7 N3 1.722(6) . ? Mo8 O24 1.926(5) . ? Mo8 O26 1.986(4) . ? Mo8 O29 2.233(3) . ? Mo8 O30 1.951(5) . ? Mo8 O35 1.930(4) . ? Mo8 N4 1.712(5) . ? Mo9 O22 1.685(5) . ? Mo9 O23 1.912(5) . ? Mo9 O26 1.866(4) . ? Mo9 O27 1.931(5) . ? Mo9 O29 2.345(3) . ? Mo9 O31 1.987(4) . ? Mo10 O21 1.695(5) . ? Mo10 O25 1.865(5) . ? Mo10 O29 2.336(3) . ? Mo10 O33 1.984(4) . ? Mo10 O34 1.905(5) . ? Mo10 O35 1.934(4) . ? Mo11 O20 1.664(5) . ? Mo11 O28 1.887(5) . ? Mo11 O29 2.344(3) . ? Mo11 O31 1.879(5) . ? Mo11 O32 1.907(6) . ? Mo11 O34 1.957(5) . ? Mo12 O19 1.673(5) . ? Mo12 O23 1.960(5) . ? Mo12 O29 2.356(4) . ? Mo12 O30 1.900(5) . ? Mo12 O32 1.926(5) . ? Mo12 O33 1.884(4) . ? N1 C1 1.431(8) . ? N2 C5 1.446(8) . ? N3 C9 1.445(10) . ? N4 C13 1.440(9) . ? N5 C111 1.544(11) . ? N5 C121 1.516(10) . ? N5 C131 1.526(8) . ? N5 C141 1.509(12) . ? N6 C211 1.527(9) . ? N6 C221 1.504(9) . ? N6 C231 1.517(10) . ? N6 C241 1.533(10) . ? N7 C311 1.500(10) . ? N7 C321 1.531(11) . ? N7 C331 1.492(12) . ? N7 C341 1.541(5) . ? N8 C411 1.546(7) . ? N8 C421 1.499(7) . ? N8 C431 1.524(5) . ? N8 C441 1.514(5) . ? C1 C2 1.490(8) . ? C1 C3 1.484(8) . ? C1 C4 1.509(8) . ? C5 C6 1.505(9) . ? C5 C7 1.511(8) . ? C5 C8 1.494(14) . ? C9 C10 1.511(15) . ? C9 C11 1.512(9) . ? C9 C12 1.529(17) . ? C13 C14 1.511(8) . ? C13 C15 1.506(8) . ? C13 C16 1.537(8) . ? C111 C112 1.515(10) . ? C112 C113 1.524(12) . ? C113 C114 1.495(8) . ? C121 C122 1.502(10) . ? C122 C123 1.513(10) . ? C123 C124 1.507(10) . ? C131 C132 1.526(9) . ? C132 C133 1.495(8) . ? C133 C134 1.519(9) . ? C141 C142 1.523(11) . ? C142 C143 1.513(12) . ? C143 C144 1.502(8) . ? C211 C212 1.509(9) . ? C212 C213 1.500(11) . ? C213 C214 1.533(12) . ? C221 C222 1.515(9) . ? C222 C223 1.499(10) . ? C223 C224 1.514(10) . ? C231 C232 1.495(10) . ? C232 C233 1.523(12) . ? C233 C234 1.488(8) . ? C241 C242 1.494(10) . ? C242 C243 1.515(11) . ? C243 C244 1.522(5) . ? C311 C312 1.538(11) . ? C312 C313 1.534(12) . ? C313 C314 1.515(13) . ? C321 C322 1.535(11) . ? C322 C323 1.500(12) . ? C323 C324 1.500(10) . ? C331 C332 1.531(11) . ? C332 C333 1.493(8) . ? C333 C334 1.508(13) . ? C341 C342 1.532(10) . ? C342 C343 1.540(11) . ? C343 C344 1.516(13) . ? C411 C412 1.485(9) . ? C412 C413 1.493(8) . ? C413 C414 1.506(5) . ? C421 C422 1.508(5) . ? C422 C423 1.526(13) . ? C423 C424 1.524(12) . ? C431 C432 1.506(5) . ? C432 C433 1.538(5) . ? C433 C434 1.519(5) . ? C441 C442 1.490(10) . ? C442 C443 1.545(14) . ? C443 C444 1.536(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 Mo2 44.43(9) . . ? O7 Mo1 Mo2 33.38(12) . . ? O7 Mo1 O1 77.81(15) . . ? O7 Mo1 O8 88.52(18) . . ? O7 Mo1 O9 88.05(18) . . ? O7 Mo1 O10 155.93(17) . . ? O8 Mo1 Mo2 82.51(13) . . ? O8 Mo1 O1 77.55(14) . . ? O9 Mo1 Mo2 81.34(13) . . ? O9 Mo1 O1 78.04(15) . . ? O9 Mo1 O8 155.52(17) . . ? O10 Mo1 Mo2 122.55(12) . . ? O10 Mo1 O1 78.12(15) . . ? O10 Mo1 O8 86.34(18) . . ? O10 Mo1 O9 86.97(18) . . ? N1 Mo1 Mo2 134.46(18) . . ? N1 Mo1 O1 178.9(2) . . ? N1 Mo1 O7 101.1(2) . . ? N1 Mo1 O8 102.3(2) . . ? N1 Mo1 O9 102.1(2) . . ? N1 Mo1 O10 103.0(2) . . ? O1 Mo2 Mo1 44.47(9) . . ? O7 Mo2 Mo1 33.44(11) . . ? O7 Mo2 O1 77.90(15) . . ? O7 Mo2 O11 88.45(18) . . ? O7 Mo2 O12 89.21(19) . . ? O7 Mo2 O17 155.77(17) . . ? O11 Mo2 Mo1 82.07(13) . . ? O11 Mo2 O1 76.86(15) . . ? O11 Mo2 O17 85.15(19) . . ? O12 Mo2 Mo1 82.24(14) . . ? O12 Mo2 O1 78.17(15) . . ? O12 Mo2 O11 154.85(17) . . ? O12 Mo2 O17 86.8(2) . . ? O17 Mo2 Mo1 122.36(13) . . ? O17 Mo2 O1 77.89(15) . . ? N2 Mo2 Mo1 135.0(2) . . ? N2 Mo2 O1 179.2(2) . . ? N2 Mo2 O7 101.6(2) . . ? N2 Mo2 O11 102.6(3) . . ? N2 Mo2 O12 102.5(3) . . ? N2 Mo2 O17 102.6(2) . . ? O3 Mo3 O1 178.7(2) . . ? O3 Mo3 O8 103.9(2) . . ? O3 Mo3 O11 104.2(2) . . ? O3 Mo3 O13 102.4(2) . . ? O3 Mo3 O16 102.0(2) . . ? O8 Mo3 O1 77.14(15) . . ? O8 Mo3 O13 86.29(18) . . ? O8 Mo3 O16 153.98(17) . . ? O11 Mo3 O1 76.52(16) . . ? O11 Mo3 O8 89.96(19) . . ? O11 Mo3 O13 153.25(17) . . ? O11 Mo3 O16 86.86(19) . . ? O13 Mo3 O1 76.83(14) . . ? O13 Mo3 O16 85.05(18) . . ? O16 Mo3 O1 77.00(15) . . ? O4 Mo4 O1 178.9(2) . . ? O4 Mo4 O9 104.8(2) . . ? O4 Mo4 O12 103.6(2) . . ? O4 Mo4 O14 103.5(2) . . ? O4 Mo4 O18 102.4(2) . . ? O9 Mo4 O1 76.26(15) . . ? O9 Mo4 O12 87.98(19) . . ? O9 Mo4 O14 87.28(19) . . ? O9 Mo4 O18 152.78(17) . . ? O12 Mo4 O1 76.21(15) . . ? O12 Mo4 O14 152.82(17) . . ? O12 Mo4 O18 86.2(2) . . ? O14 Mo4 O1 76.67(14) . . ? O18 Mo4 O1 76.53(15) . . ? O18 Mo4 O14 85.89(19) . . ? O5 Mo5 O1 179.33(19) . . ? O5 Mo5 O10 103.7(2) . . ? O5 Mo5 O13 103.2(2) . . ? O5 Mo5 O14 104.0(2) . . ? O5 Mo5 O15 103.7(2) . . ? O10 Mo5 O1 75.92(14) . . ? O10 Mo5 O13 87.41(18) . . ? O10 Mo5 O14 86.63(18) . . ? O10 Mo5 O15 152.56(17) . . ? O13 Mo5 O1 76.27(15) . . ? O13 Mo5 O14 152.89(17) . . ? O13 Mo5 O15 86.75(18) . . ? O14 Mo5 O1 76.62(15) . . ? O15 Mo5 O1 76.65(15) . . ? O15 Mo5 O14 86.47(19) . . ? O6 Mo6 O1 178.9(2) . . ? O6 Mo6 O15 103.0(2) . . ? O6 Mo6 O16 104.6(2) . . ? O6 Mo6 O17 103.8(2) . . ? O6 Mo6 O18 102.7(2) . . ? O15 Mo6 O1 76.51(14) . . ? O16 Mo6 O1 76.36(15) . . ? O16 Mo6 O15 85.41(19) . . ? O16 Mo6 O18 152.58(18) . . ? O17 Mo6 O1 76.66(15) . . ? O17 Mo6 O15 153.18(17) . . ? O17 Mo6 O16 88.3(2) . . ? O17 Mo6 O18 88.0(2) . . ? O18 Mo6 O1 76.34(15) . . ? O18 Mo6 O15 85.78(19) . . ? O24 Mo7 Mo8 33.66(13) . . ? O24 Mo7 O25 87.30(19) . . ? O24 Mo7 O27 90.0(2) . . ? O24 Mo7 O28 155.65(19) . . ? O24 Mo7 O29 77.91(16) . . ? O25 Mo7 Mo8 80.56(13) . . ? O25 Mo7 O29 77.04(15) . . ? O27 Mo7 Mo8 83.76(14) . . ? O27 Mo7 O25 155.52(18) . . ? O27 Mo7 O28 87.7(2) . . ? O27 Mo7 O29 78.60(16) . . ? O28 Mo7 Mo8 122.07(14) . . ? O28 Mo7 O25 84.9(2) . . ? O28 Mo7 O29 77.88(17) . . ? O29 Mo7 Mo8 44.26(9) . . ? N3 Mo7 Mo8 132.7(2) . . ? N3 Mo7 O24 99.1(3) . . ? N3 Mo7 O25 100.1(3) . . ? N3 Mo7 O27 104.4(3) . . ? N3 Mo7 O28 104.9(3) . . ? N3 Mo7 O29 175.9(2) . . ? O24 Mo8 Mo7 33.37(13) . . ? O24 Mo8 O26 86.4(2) . . ? O24 Mo8 O29 77.99(16) . . ? O24 Mo8 O30 156.26(18) . . ? O24 Mo8 O35 90.01(19) . . ? O26 Mo8 Mo7 80.48(14) . . ? O26 Mo8 O29 77.34(15) . . ? O29 Mo8 Mo7 44.62(9) . . ? O30 Mo8 Mo7 123.03(13) . . ? O30 Mo8 O26 85.6(2) . . ? O30 Mo8 O29 78.47(16) . . ? O35 Mo8 Mo7 83.81(13) . . ? O35 Mo8 O26 156.58(16) . . ? O35 Mo8 O29 79.28(15) . . ? O35 Mo8 O30 88.59(18) . . ? N4 Mo8 Mo7 131.3(2) . . ? N4 Mo8 O24 98.0(3) . . ? N4 Mo8 O26 99.2(2) . . ? N4 Mo8 O29 174.8(2) . . ? N4 Mo8 O30 105.3(3) . . ? N4 Mo8 O35 104.3(2) . . ? O22 Mo9 O23 103.3(3) . . ? O22 Mo9 O26 106.1(2) . . ? O22 Mo9 O27 103.3(3) . . ? O22 Mo9 O29 177.1(2) . . ? O22 Mo9 O31 101.5(2) . . ? O23 Mo9 O27 152.52(18) . . ? O23 Mo9 O29 76.77(15) . . ? O23 Mo9 O31 84.6(2) . . ? O26 Mo9 O23 90.0(2) . . ? O26 Mo9 O27 89.0(2) . . ? O26 Mo9 O29 76.85(15) . . ? O26 Mo9 O31 152.35(18) . . ? O27 Mo9 O29 76.26(16) . . ? O27 Mo9 O31 83.6(2) . . ? O31 Mo9 O29 75.52(15) . . ? O21 Mo10 O25 104.1(2) . . ? O21 Mo10 O29 178.4(2) . . ? O21 Mo10 O33 102.4(2) . . ? O21 Mo10 O34 103.3(2) . . ? O21 Mo10 O35 102.9(2) . . ? O25 Mo10 O29 77.48(16) . . ? O25 Mo10 O33 153.52(18) . . ? O25 Mo10 O34 89.7(2) . . ? O25 Mo10 O35 89.03(19) . . ? O33 Mo10 O29 76.07(15) . . ? O34 Mo10 O29 76.99(16) . . ? O34 Mo10 O33 85.6(2) . . ? O34 Mo10 O35 153.23(17) . . ? O35 Mo10 O29 76.64(14) . . ? O35 Mo10 O33 83.75(19) . . ? O20 Mo11 O28 103.2(3) . . ? O20 Mo11 O29 177.9(3) . . ? O20 Mo11 O31 104.6(3) . . ? O20 Mo11 O32 103.0(3) . . ? O20 Mo11 O34 102.1(3) . . ? O28 Mo11 O29 76.90(16) . . ? O28 Mo11 O32 153.50(19) . . ? O28 Mo11 O34 86.7(2) . . ? O31 Mo11 O28 89.2(2) . . ? O31 Mo11 O29 77.49(16) . . ? O31 Mo11 O32 87.8(2) . . ? O31 Mo11 O34 153.28(18) . . ? O32 Mo11 O29 76.75(16) . . ? O32 Mo11 O34 84.2(2) . . ? O34 Mo11 O29 75.87(15) . . ? O19 Mo12 O23 103.4(3) . . ? O19 Mo12 O29 179.1(3) . . ? O19 Mo12 O30 103.6(3) . . ? O19 Mo12 O32 103.9(3) . . ? O19 Mo12 O33 103.6(3) . . ? O23 Mo12 O29 75.63(16) . . ? O30 Mo12 O23 86.3(2) . . ? O30 Mo12 O29 76.39(15) . . ? O30 Mo12 O32 152.4(2) . . ? O32 Mo12 O23 84.4(2) . . ? O32 Mo12 O29 76.10(17) . . ? O33 Mo12 O23 153.00(19) . . ? O33 Mo12 O29 77.38(15) . . ? O33 Mo12 O30 88.1(2) . . ? O33 Mo12 O32 88.4(2) . . ? Mo1 O1 Mo3 90.88(12) . . ? Mo1 O1 Mo4 90.20(12) . . ? Mo1 O1 Mo5 90.16(12) . . ? Mo1 O1 Mo6 178.74(17) . . ? Mo2 O1 Mo1 91.09(12) . . ? Mo2 O1 Mo3 91.21(12) . . ? Mo2 O1 Mo4 90.32(12) . . ? Mo2 O1 Mo5 178.55(17) . . ? Mo2 O1 Mo6 90.03(12) . . ? Mo3 O1 Mo4 178.11(16) . . ? Mo3 O1 Mo5 89.50(12) . . ? Mo3 O1 Mo6 89.66(12) . . ? Mo4 O1 Mo5 88.95(12) . . ? Mo4 O1 Mo6 89.23(11) . . ? Mo6 O1 Mo5 88.71(11) . . ? Mo2 O7 Mo1 113.18(18) . . ? Mo3 O8 Mo1 114.42(18) . . ? Mo4 O9 Mo1 115.5(2) . . ? Mo5 O10 Mo1 115.8(2) . . ? Mo3 O11 Mo2 115.4(2) . . ? Mo4 O12 Mo2 115.3(2) . . ? Mo5 O13 Mo3 117.40(19) . . ? Mo5 O14 Mo4 117.76(19) . . ? Mo5 O15 Mo6 118.13(19) . . ? Mo6 O16 Mo3 117.0(2) . . ? Mo6 O17 Mo2 115.4(2) . . ? Mo6 O18 Mo4 117.90(19) . . ? Mo9 O23 Mo12 117.8(2) . . ? Mo7 O24 Mo8 113.0(2) . . ? Mo10 O25 Mo7 114.8(2) . . ? Mo9 O26 Mo8 115.25(19) . . ? Mo9 O27 Mo7 114.8(2) . . ? Mo11 O28 Mo7 115.1(2) . . ? Mo7 O29 Mo9 90.27(12) . . ? Mo7 O29 Mo10 90.65(13) . . ? Mo7 O29 Mo11 89.99(12) . . ? Mo7 O29 Mo12 178.86(16) . . ? Mo8 O29 Mo7 91.12(13) . . ? Mo8 O29 Mo9 90.54(12) . . ? Mo8 O29 Mo10 90.19(13) . . ? Mo8 O29 Mo11 178.88(18) . . ? Mo8 O29 Mo12 90.02(12) . . ? Mo9 O29 Mo12 89.68(12) . . ? Mo10 O29 Mo9 178.82(17) . . ? Mo10 O29 Mo11 89.66(11) . . ? Mo10 O29 Mo12 89.38(12) . . ? Mo11 O29 Mo9 89.60(13) . . ? Mo11 O29 Mo12 88.87(12) . . ? Mo12 O30 Mo8 115.0(2) . . ? Mo11 O31 Mo9 117.4(2) . . ? Mo11 O32 Mo12 118.3(2) . . ? Mo12 O33 Mo10 117.1(2) . . ? Mo10 O34 Mo11 117.4(2) . . ? Mo8 O35 Mo10 113.85(19) . . ? C1 N1 Mo1 173.6(5) . . ? C5 N2 Mo2 175.8(6) . . ? C9 N3 Mo7 167.1(6) . . ? C13 N4 Mo8 163.4(6) . . ? C121 N5 C111 109.6(8) . . ? C121 N5 C131 109.8(6) . . ? C131 N5 C111 106.2(5) . . ? C141 N5 C111 113.2(7) . . ? C141 N5 C121 107.5(6) . . ? C141 N5 C131 110.6(8) . . ? C211 N6 C241 109.9(6) . . ? C221 N6 C211 110.4(6) . . ? C221 N6 C231 112.1(7) . . ? C221 N6 C241 107.4(5) . . ? C231 N6 C211 106.7(5) . . ? C231 N6 C241 110.4(7) . . ? C311 N7 C321 110.6(8) . . ? C311 N7 C341 106.2(6) . . ? C321 N7 C341 107.9(8) . . ? C331 N7 C311 112.9(9) . . ? C331 N7 C321 109.0(7) . . ? C331 N7 C341 110.1(7) . . ? C421 N8 C411 102.3(8) . . ? C421 N8 C431 115.6(6) . . ? C421 N8 C441 110.3(6) . . ? C431 N8 C411 104.3(5) . . ? C441 N8 C411 107.0(8) . . ? C441 N8 C431 115.9(6) . . ? N1 C1 C2 108.8(6) . . ? N1 C1 C3 109.4(7) . . ? N1 C1 C4 109.8(7) . . ? C2 C1 C4 103.5(10) . . ? C3 C1 C2 115.6(8) . . ? C3 C1 C4 109.6(10) . . ? N2 C5 C6 108.5(7) . . ? N2 C5 C7 109.1(7) . . ? N2 C5 C8 107.6(8) . . ? C6 C5 C7 109.5(12) . . ? C8 C5 C6 111.4(13) . . ? C8 C5 C7 110.6(9) . . ? N3 C9 C10 109.5(8) . . ? N3 C9 C11 111.3(9) . . ? N3 C9 C12 104.3(10) . . ? C10 C9 C11 108.7(12) . . ? C10 C9 C12 115.0(11) . . ? C11 C9 C12 108.0(10) . . ? N4 C13 C14 108.3(7) . . ? N4 C13 C15 108.3(7) . . ? N4 C13 C16 107.0(7) . . ? C14 C13 C16 110.7(12) . . ? C15 C13 C14 114.7(11) . . ? C15 C13 C16 107.6(8) . . ? C112 C111 N5 116.3(7) . . ? C111 C112 C113 108.7(10) . . ? C114 C113 C112 111.6(13) . . ? C122 C121 N5 117.2(7) . . ? C121 C122 C123 112.0(8) . . ? C124 C123 C122 112.6(10) . . ? N5 C131 C132 115.9(6) . . ? C133 C132 C131 109.5(6) . . ? C132 C133 C134 114.3(7) . . ? N5 C141 C142 114.1(8) . . ? C143 C142 C141 106.3(9) . . ? C144 C143 C142 109.2(12) . . ? C212 C211 N6 115.0(7) . . ? C213 C212 C211 112.3(8) . . ? C212 C213 C214 109.4(11) . . ? N6 C221 C222 114.6(6) . . ? C223 C222 C221 112.6(7) . . ? C222 C223 C224 112.8(9) . . ? C232 C231 N6 115.6(7) . . ? C231 C232 C233 109.5(9) . . ? C234 C233 C232 115.3(12) . . ? C242 C241 N6 115.4(7) . . ? C241 C242 C243 114.6(9) . . ? C242 C243 C244 107.4(13) . . ? N7 C311 C312 112.5(9) . . ? C313 C312 C311 109.2(10) . . ? C314 C313 C312 109.2(13) . . ? N7 C321 C322 109.0(8) . . ? C323 C322 C321 110.0(10) . . ? C322 C323 C324 114.1(12) . . ? N7 C331 C332 113.4(8) . . ? C333 C332 C331 113.9(9) . . ? C332 C333 C334 113.7(12) . . ? C342 C341 N7 112.2(7) . . ? C341 C342 C343 112.0(10) . . ? C344 C343 C342 114.7(13) . . ? C412 C411 N8 118.3(8) . . ? C411 C412 C413 111.6(9) . . ? C412 C413 C414 114.6(8) . . ? N8 C421 C422 114.6(7) . . ? C421 C422 C423 107.6(13) . . ? C424 C423 C422 112.8(18) . . ? C432 C431 N8 116.9(7) . . ? C431 C432 C433 109.7(10) . . ? C434 C433 C432 108.9(7) . . ? C442 C441 N8 118.3(11) . . ? C441 C442 C443 109.0(13) . . ? C444 C443 C442 105.8(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4C O12 0.96 2.90 3.803(12) 157.5 2_765 C7 H7A O26 0.96 2.81 3.541(12) 133.5 1_655 C11 H11B O35 0.96 2.61 3.553(13) 168.0 2_676 C12 H12C O21 0.96 2.87 3.803(15) 164.5 2_676 C15 H15B O8 0.96 2.61 3.560(11) 170.7 1_455 C16 H16C O3 0.96 2.80 3.745(11) 169.2 1_455 C16 H16C O11 0.96 2.68 3.366(10) 128.6 1_455