# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wei, Yongge' _publ_contact_author_email yonggewei@mail.tsinghua.edu.cn _publ_author_name 'Yongge Wei' data_MEOBIPH _database_code_depnum_ccdc_archive 'CCDC 810527' #TrackingRef '- MEOBIPH.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H86 Mo6 N4 O20' _chemical_formula_weight 1590.83 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.638(3) _cell_length_b 12.773(3) _cell_length_c 20.309(4) _cell_angle_alpha 83.61(3) _cell_angle_beta 76.11(3) _cell_angle_gamma 79.62(3) _cell_volume 3122.3(11) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 20584 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1604 _exptl_absorpt_coefficient_mu 1.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8362 _exptl_absorpt_correction_T_max 0.8863 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean '100x100 micron' _diffrn_reflns_number 24659 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10730 _reflns_number_gt 7421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku RAPID AUTO Ver2.30' _computing_cell_refinement 'Rigaku RAPID AUTO Ver2.30' _computing_data_reduction 'Rigaku RAPID AUTO Ver2.30' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+3.7295P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10730 _refine_ls_number_parameters 679 _refine_ls_number_restraints 189 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.04926(4) 0.57573(4) 0.76107(3) 0.05770(16) Uani 1 1 d . . . Mo2 Mo -0.16818(4) 0.59177(4) 0.70025(4) 0.07106(19) Uani 1 1 d . . . Mo3 Mo -0.17501(5) 0.72794(5) 0.82977(3) 0.0744(2) Uani 1 1 d . . . Mo4 Mo 0.04646(4) 0.69570(5) 0.61229(3) 0.06505(17) Uani 1 1 d . . . Mo5 Mo 0.03907(5) 0.83238(4) 0.74110(3) 0.06959(18) Uani 1 1 d . . . Mo6 Mo -0.18208(4) 0.85156(4) 0.67973(3) 0.05823(16) Uani 1 1 d . . . O1 O -0.0635(3) 0.7095(3) 0.72168(17) 0.0497(9) Uani 1 1 d . . . O2 O -0.2474(4) 0.5079(4) 0.6854(4) 0.111(2) Uani 1 1 d . . . O3 O -0.2573(5) 0.7431(5) 0.9082(3) 0.111(2) Uani 1 1 d . . . O4 O 0.1244(4) 0.6858(5) 0.5326(2) 0.0966(16) Uani 1 1 d . . . O5 O 0.1154(4) 0.9203(4) 0.7544(3) 0.1025(18) Uani 1 1 d . . . O6 O -0.2648(4) 0.9542(3) 0.6494(2) 0.0784(13) Uani 1 1 d . . . O7 O -0.0573(3) 0.5014(3) 0.7375(2) 0.0719(12) Uani 1 1 d . . . O8 O -0.0624(4) 0.6145(3) 0.8425(2) 0.0751(12) Uani 1 1 d . . . O9 O 0.1174(3) 0.5844(3) 0.6653(2) 0.0621(10) Uani 1 1 d . . . O10 O 0.1137(3) 0.6975(3) 0.7700(2) 0.0663(11) Uani 1 1 d . . . O11 O -0.2396(3) 0.6322(3) 0.7921(3) 0.0826(14) Uani 1 1 d . . . O12 O -0.0613(4) 0.6025(3) 0.6175(2) 0.0731(12) Uani 1 1 d . . . O13 O -0.0697(4) 0.8241(4) 0.8240(2) 0.0791(13) Uani 1 1 d . . . O14 O 0.1088(3) 0.7937(3) 0.6491(2) 0.0692(11) Uani 1 1 d . . . O15 O -0.2426(3) 0.7300(3) 0.6720(2) 0.0713(12) Uani 1 1 d . . . O16 O -0.2459(3) 0.8391(3) 0.7745(2) 0.0706(11) Uani 1 1 d . . . O17 O -0.0693(3) 0.8106(4) 0.6001(2) 0.0708(11) Uani 1 1 d . . . O18 O -0.0746(3) 0.9207(3) 0.7026(2) 0.0696(11) Uani 1 1 d . . . O19 O 0.1441(5) 0.4573(4) 0.9246(3) 0.114(2) Uani 1 1 d . . . O20 O 0.3291(5) -0.0892(5) 1.0545(3) 0.1147(19) Uani 1 1 d . . . N1 N 0.1359(4) 0.4713(4) 0.7919(3) 0.0656(13) Uani 1 1 d . . . N2 N 0.5099(6) -0.1948(5) 0.9828(4) 0.124(3) Uani 1 1 d . . . H2A H 0.4791 -0.2184 1.0228 0.149 Uiso 1 1 calc R . . H2B H 0.5692 -0.2308 0.9604 0.149 Uiso 1 1 calc R . . N3 N -0.0033(4) 0.7864(4) 0.3660(2) 0.0611(12) Uani 1 1 d . . . N4 N 0.5794(6) 0.3472(8) 0.2163(4) 0.127(3) Uani 1 1 d . . . C1 C 0.1991(5) 0.3861(5) 0.8180(3) 0.0713(17) Uani 1 1 d . . . C2 C 0.1996(6) 0.3736(5) 0.8876(4) 0.083(2) Uani 1 1 d . . . C3 C 0.2542(6) 0.2805(6) 0.9138(4) 0.089(2) Uani 1 1 d . . . H3 H 0.2534 0.2718 0.9600 0.107 Uiso 1 1 calc R . . C4 C 0.3114(6) 0.1983(6) 0.8709(4) 0.083(2) Uani 1 1 d . . . C5 C 0.3164(7) 0.2147(6) 0.8017(4) 0.090(2) Uani 1 1 d . . . H5 H 0.3579 0.1637 0.7725 0.109 Uiso 1 1 calc R . . C6 C 0.2599(6) 0.3066(6) 0.7761(4) 0.083(2) Uani 1 1 d . . . H6 H 0.2624 0.3158 0.7297 0.099 Uiso 1 1 calc R . . C7 C 0.1413(10) 0.4462(9) 0.9962(4) 0.157(5) Uani 1 1 d . . . H7A H 0.1001 0.5096 1.0169 0.235 Uiso 1 1 calc R . . H7B H 0.2153 0.4357 1.0029 0.235 Uiso 1 1 calc R . . H7C H 0.1067 0.3859 1.0168 0.235 Uiso 1 1 calc R . . C8 C 0.4634(7) -0.0976(6) 0.9541(5) 0.096(2) Uani 1 1 d . . . C9 C 0.3685(7) -0.0418(6) 0.9911(4) 0.092(2) Uani 1 1 d . . . C10 C 0.3176(7) 0.0555(6) 0.9656(4) 0.092(2) Uani 1 1 d . . . H10 H 0.2535 0.0922 0.9914 0.111 Uiso 1 1 calc R . . C11 C 0.3652(7) 0.0968(6) 0.9002(4) 0.087(2) Uani 1 1 d . . . C12 C 0.4617(6) 0.0405(6) 0.8629(4) 0.093(2) Uani 1 1 d . . . H12 H 0.4944 0.0675 0.8199 0.111 Uiso 1 1 calc R . . C13 C 0.5084(7) -0.0556(6) 0.8901(5) 0.095(2) Uani 1 1 d . . . H13 H 0.5722 -0.0931 0.8644 0.114 Uiso 1 1 calc R . . C14 C 0.2424(9) -0.0299(9) 1.0970(6) 0.142(4) Uani 1 1 d . . . H14A H 0.2227 -0.0702 1.1397 0.214 Uiso 1 1 calc R . . H14B H 0.1801 -0.0133 1.0763 0.214 Uiso 1 1 calc R . . H14C H 0.2644 0.0351 1.1046 0.214 Uiso 1 1 calc R . . C111 C -0.0867(5) 0.7095(5) 0.3860(3) 0.0663(16) Uani 1 1 d DU . . H11A H -0.1580 0.7485 0.3811 0.080 Uiso 1 1 calc R . . H11B H -0.0656 0.6547 0.3538 0.080 Uiso 1 1 calc R . . C112 C -0.1006(6) 0.6555(5) 0.4562(3) 0.0790(19) Uani 1 1 d DU . . H11C H -0.1113 0.7084 0.4890 0.095 Uiso 1 1 calc R . . H11D H -0.0342 0.6055 0.4596 0.095 Uiso 1 1 calc R . . C113 C -0.1982(7) 0.5969(7) 0.4726(5) 0.116(3) Uani 1 1 d DU . . H11E H -0.2027 0.5663 0.4320 0.139 Uiso 1 1 calc R . . H11F H -0.1868 0.5387 0.5065 0.139 Uiso 1 1 calc R . . C114 C -0.3010(9) 0.6651(13) 0.4978(9) 0.251(9) Uani 1 1 d DU . . H11G H -0.3604 0.6242 0.5074 0.377 Uiso 1 1 calc R . . H11H H -0.3134 0.7220 0.4641 0.377 Uiso 1 1 calc R . . H11I H -0.2977 0.6943 0.5387 0.377 Uiso 1 1 calc R . . C121 C -0.0302(5) 0.8732(4) 0.4162(3) 0.0662(16) Uani 1 1 d D . . H12A H -0.0172 0.8401 0.4595 0.079 Uiso 1 1 calc R . . H12B H 0.0214 0.9232 0.4000 0.079 Uiso 1 1 calc R . . C122 C -0.1441(5) 0.9346(5) 0.4282(4) 0.0732(18) Uani 1 1 d D . . H12C H -0.1970 0.8862 0.4455 0.088 Uiso 1 1 calc R . . H12D H -0.1584 0.9694 0.3855 0.088 Uiso 1 1 calc R . . C123 C -0.1585(6) 1.0180(5) 0.4787(3) 0.0790(19) Uani 1 1 d D . . H12E H -0.1461 0.9827 0.5217 0.095 Uiso 1 1 calc R . . H12F H -0.1036 1.0646 0.4619 0.095 Uiso 1 1 calc R . . C124 C -0.2709(7) 1.0835(7) 0.4902(4) 0.106(3) Uani 1 1 d D . . H12G H -0.2767 1.1350 0.5224 0.158 Uiso 1 1 calc R . . H12H H -0.3254 1.0379 0.5075 0.158 Uiso 1 1 calc R . . H12I H -0.2828 1.1198 0.4480 0.158 Uiso 1 1 calc R . . C131 C -0.0099(6) 0.8400(5) 0.2969(3) 0.0713(17) Uani 1 1 d D . . H13A H 0.0347 0.8966 0.2873 0.086 Uiso 1 1 calc R . . H13B H -0.0857 0.8729 0.2982 0.086 Uiso 1 1 calc R . . C132 C 0.0280(7) 0.7666(5) 0.2384(3) 0.089(2) Uani 1 1 d D . . H13C H 0.1073 0.7446 0.2302 0.107 Uiso 1 1 calc R . . H13D H -0.0066 0.7031 0.2505 0.107 Uiso 1 1 calc R . . C133 C -0.0027(9) 0.8241(8) 0.1743(4) 0.127(3) Uani 1 1 d D . . H13E H -0.0824 0.8421 0.1819 0.153 Uiso 1 1 calc R . . H13F H 0.0278 0.8901 0.1642 0.153 Uiso 1 1 calc R . . C134 C 0.0391(12) 0.7578(12) 0.1156(5) 0.195(6) Uani 1 1 d D . . H13G H 0.0179 0.7961 0.0761 0.292 Uiso 1 1 calc R . . H13H H 0.0085 0.6928 0.1252 0.292 Uiso 1 1 calc R . . H13I H 0.1182 0.7414 0.1072 0.292 Uiso 1 1 calc R . . C141 C 0.1105(5) 0.7246(5) 0.3668(4) 0.0687(17) Uani 1 1 d D . . H14D H 0.1107 0.6943 0.4127 0.082 Uiso 1 1 calc R . . H14E H 0.1243 0.6657 0.3379 0.082 Uiso 1 1 calc R . . C142 C 0.2046(5) 0.7881(6) 0.3436(4) 0.091(2) Uani 1 1 d D . . H14F H 0.2103 0.8130 0.2961 0.109 Uiso 1 1 calc R . . H14G H 0.1896 0.8502 0.3699 0.109 Uiso 1 1 calc R . . C143 C 0.3124(6) 0.7214(6) 0.3520(5) 0.113(3) Uani 1 1 d D . . H14H H 0.3084 0.7020 0.4000 0.136 Uiso 1 1 calc R . . H14I H 0.3233 0.6560 0.3294 0.136 Uiso 1 1 calc R . . C144 C 0.4082(7) 0.7769(8) 0.3242(7) 0.169(6) Uani 1 1 d D . . H14J H 0.4742 0.7317 0.3319 0.253 Uiso 1 1 calc R . . H14K H 0.3980 0.8418 0.3463 0.253 Uiso 1 1 calc R . . H14L H 0.4148 0.7933 0.2762 0.253 Uiso 1 1 calc R . . C211 C 0.6858(8) 0.3169(11) 0.1640(5) 0.149(5) Uani 1 1 d D . . H21A H 0.7160 0.3815 0.1458 0.178 Uiso 1 1 calc R . . H21B H 0.7384 0.2722 0.1871 0.178 Uiso 1 1 calc R . . C212 C 0.6767(10) 0.2593(13) 0.1054(5) 0.198(7) Uani 1 1 d D . . H21C H 0.6554 0.1903 0.1222 0.238 Uiso 1 1 calc R . . H21D H 0.6196 0.3000 0.0842 0.238 Uiso 1 1 calc R . . C213 C 0.7841(12) 0.2441(17) 0.0535(6) 0.270(13) Uani 1 1 d D . . H21E H 0.7709 0.2220 0.0125 0.324 Uiso 1 1 calc R . . H21F H 0.8100 0.3123 0.0423 0.324 Uiso 1 1 calc R . . C214 C 0.8715(18) 0.166(2) 0.0749(10) 0.40(2) Uani 1 1 d D . . H21G H 0.9381 0.1639 0.0400 0.596 Uiso 1 1 calc R . . H21H H 0.8494 0.0968 0.0828 0.596 Uiso 1 1 calc R . . H21I H 0.8845 0.1862 0.1161 0.596 Uiso 1 1 calc R . . C221 C 0.5282(7) 0.2472(9) 0.2447(6) 0.139(4) Uani 1 1 d D . . H22A H 0.4586 0.2684 0.2763 0.167 Uiso 1 1 calc R . . H22B H 0.5120 0.2160 0.2076 0.167 Uiso 1 1 calc R . . C222 C 0.5981(8) 0.1627(9) 0.2805(6) 0.141(4) Uani 1 1 d D . . H22C H 0.6195 0.1940 0.3158 0.169 Uiso 1 1 calc R . . H22D H 0.6647 0.1353 0.2483 0.169 Uiso 1 1 calc R . . C223 C 0.5361(10) 0.0726(10) 0.3118(8) 0.171(5) Uani 1 1 d D . . H22E H 0.4687 0.1021 0.3426 0.205 Uiso 1 1 calc R . . H22F H 0.5149 0.0431 0.2758 0.205 Uiso 1 1 calc R . . C224 C 0.5942(14) -0.0150(13) 0.3491(10) 0.253(9) Uani 1 1 d D . . H22G H 0.5484 -0.0692 0.3647 0.379 Uiso 1 1 calc R . . H22H H 0.6104 0.0115 0.3873 0.379 Uiso 1 1 calc R . . H22I H 0.6618 -0.0448 0.3195 0.379 Uiso 1 1 calc R . . C231 C 0.6121(7) 0.3993(9) 0.2708(5) 0.124(3) Uani 1 1 d D . . H23A H 0.6671 0.3483 0.2885 0.149 Uiso 1 1 calc R . . H23B H 0.6473 0.4596 0.2491 0.149 Uiso 1 1 calc R . . C232 C 0.5216(8) 0.4381(10) 0.3304(6) 0.148(4) Uani 1 1 d D . . H23C H 0.4807 0.3806 0.3505 0.178 Uiso 1 1 calc R . . H23D H 0.4708 0.4962 0.3146 0.178 Uiso 1 1 calc R . . C233 C 0.5696(11) 0.4763(10) 0.3842(6) 0.154(4) Uani 1 1 d D . . H23E H 0.6298 0.5146 0.3620 0.185 Uiso 1 1 calc R . . H23F H 0.5132 0.5247 0.4122 0.185 Uiso 1 1 calc R . . C234 C 0.6100(9) 0.3855(12) 0.4267(7) 0.172(5) Uani 1 1 d D . . H23G H 0.6403 0.4104 0.4601 0.259 Uiso 1 1 calc R . . H23H H 0.6662 0.3379 0.3989 0.259 Uiso 1 1 calc R . . H23I H 0.5500 0.3485 0.4493 0.259 Uiso 1 1 calc R . . C241 C 0.4939(8) 0.4218(12) 0.1849(7) 0.214(6) Uani 1 1 d DU . . H24A H 0.4762 0.3853 0.1505 0.257 Uiso 1 1 calc R . . H24B H 0.4270 0.4370 0.2199 0.257 Uiso 1 1 calc R . . C242 C 0.5293(13) 0.5265(15) 0.1528(9) 0.288(7) Uani 1 1 d DU . . H24C H 0.5832 0.5138 0.1104 0.345 Uiso 1 1 calc R . . H24D H 0.5643 0.5552 0.1828 0.345 Uiso 1 1 calc R . . C243 C 0.4288(18) 0.6102(15) 0.1385(11) 0.358 Uani 1 1 d DU . . H24E H 0.3750 0.6235 0.1808 0.429 Uiso 1 1 calc R . . H24F H 0.4539 0.6770 0.1197 0.429 Uiso 1 1 calc R . . C244 C 0.3770(17) 0.5718(17) 0.0910(11) 0.340(12) Uani 1 1 d DU . . H24G H 0.3116 0.6208 0.0864 0.510 Uiso 1 1 calc R . . H24H H 0.3577 0.5029 0.1078 0.510 Uiso 1 1 calc R . . H24I H 0.4276 0.5663 0.0475 0.510 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 0.0546(3) 0.0492(3) 0.0600(3) 0.0059(2) -0.0094(2) 0.0051(2) Mo2 0.0541(3) 0.0470(3) 0.1135(5) -0.0101(3) -0.0202(3) -0.0072(2) Mo3 0.0732(4) 0.0714(4) 0.0564(3) 0.0015(3) 0.0049(3) 0.0164(3) Mo4 0.0576(3) 0.0753(4) 0.0508(3) 0.0018(3) -0.0042(2) 0.0044(3) Mo5 0.0690(4) 0.0510(3) 0.0957(5) -0.0039(3) -0.0347(3) -0.0067(3) Mo6 0.0522(3) 0.0465(3) 0.0714(4) 0.0053(2) -0.0160(3) 0.0011(2) O1 0.0466(19) 0.0409(19) 0.053(2) 0.0041(16) -0.0039(16) 0.0018(16) O2 0.078(3) 0.062(3) 0.209(7) -0.022(4) -0.048(4) -0.020(3) O3 0.104(4) 0.124(4) 0.065(3) -0.003(3) 0.017(3) 0.038(3) O4 0.085(3) 0.129(4) 0.054(3) -0.002(3) 0.003(2) 0.011(3) O5 0.100(4) 0.065(3) 0.163(5) -0.008(3) -0.066(4) -0.018(3) O6 0.067(3) 0.059(3) 0.102(3) 0.013(2) -0.028(2) 0.009(2) O7 0.061(2) 0.040(2) 0.108(3) -0.001(2) -0.014(2) -0.0003(18) O8 0.080(3) 0.071(3) 0.052(2) 0.011(2) -0.001(2) 0.017(2) O9 0.053(2) 0.061(2) 0.059(2) -0.0002(19) -0.0029(18) 0.0109(18) O10 0.068(3) 0.060(2) 0.077(3) -0.007(2) -0.033(2) 0.000(2) O11 0.057(2) 0.065(3) 0.100(3) 0.023(2) 0.010(2) 0.003(2) O12 0.076(3) 0.069(3) 0.078(3) -0.022(2) -0.028(2) 0.003(2) O13 0.098(3) 0.068(3) 0.075(3) -0.020(2) -0.035(3) 0.008(2) O14 0.054(2) 0.068(3) 0.080(3) 0.014(2) -0.011(2) -0.013(2) O15 0.054(2) 0.064(3) 0.099(3) -0.008(2) -0.026(2) -0.005(2) O16 0.064(3) 0.057(2) 0.078(3) -0.004(2) -0.009(2) 0.013(2) O17 0.063(2) 0.081(3) 0.059(3) 0.010(2) -0.011(2) 0.001(2) O18 0.072(3) 0.041(2) 0.098(3) 0.003(2) -0.030(2) -0.0076(19) O19 0.148(5) 0.084(4) 0.082(4) -0.009(3) -0.016(3) 0.048(4) O20 0.125(5) 0.094(4) 0.108(5) 0.022(3) -0.012(4) -0.008(4) N1 0.057(3) 0.053(3) 0.072(3) 0.010(2) -0.009(2) 0.010(2) N2 0.126(6) 0.082(5) 0.144(7) 0.023(5) -0.024(5) 0.013(4) N3 0.074(3) 0.046(3) 0.063(3) -0.004(2) -0.013(3) -0.012(2) N4 0.066(4) 0.202(9) 0.115(6) 0.027(6) -0.020(4) -0.045(5) C1 0.067(4) 0.065(4) 0.068(4) 0.006(3) -0.007(3) 0.010(3) C2 0.090(5) 0.060(4) 0.077(5) 0.004(3) -0.003(4) 0.023(4) C3 0.095(5) 0.074(5) 0.076(5) -0.002(4) -0.009(4) 0.030(4) C4 0.075(4) 0.064(4) 0.097(6) 0.002(4) -0.017(4) 0.011(3) C5 0.101(6) 0.081(5) 0.078(5) -0.009(4) -0.019(4) 0.018(4) C6 0.088(5) 0.078(5) 0.072(4) 0.002(4) -0.016(4) 0.010(4) C7 0.218(12) 0.147(9) 0.062(5) -0.017(6) -0.017(6) 0.071(8) C8 0.095(6) 0.076(5) 0.107(6) 0.007(5) -0.027(5) 0.008(4) C9 0.091(5) 0.073(5) 0.103(6) 0.012(4) -0.019(5) -0.006(4) C10 0.088(5) 0.080(5) 0.093(6) 0.008(4) -0.009(4) 0.002(4) C11 0.092(5) 0.064(4) 0.092(5) 0.002(4) -0.013(4) 0.010(4) C12 0.082(5) 0.078(5) 0.102(6) -0.005(4) -0.011(4) 0.018(4) C13 0.080(5) 0.084(5) 0.108(6) -0.013(5) -0.014(5) 0.017(4) C14 0.119(8) 0.128(8) 0.141(9) -0.023(7) 0.034(7) 0.004(7) C111 0.069(4) 0.053(3) 0.076(4) -0.005(3) -0.011(3) -0.015(3) C112 0.089(4) 0.069(4) 0.079(4) -0.001(3) -0.010(4) -0.025(4) C113 0.136(7) 0.091(6) 0.118(7) -0.019(5) 0.015(6) -0.065(5) C114 0.113(7) 0.298(19) 0.33(2) -0.129(17) 0.070(12) -0.090(10) C121 0.075(4) 0.047(3) 0.077(4) -0.010(3) -0.012(3) -0.013(3) C122 0.075(4) 0.056(4) 0.086(5) -0.013(3) -0.013(4) -0.007(3) C123 0.099(5) 0.064(4) 0.065(4) -0.006(3) -0.009(4) -0.003(4) C124 0.112(6) 0.099(6) 0.089(6) -0.017(5) -0.011(5) 0.017(5) C131 0.098(5) 0.054(3) 0.061(4) -0.004(3) -0.014(4) -0.015(3) C132 0.125(6) 0.069(4) 0.066(4) -0.011(4) -0.008(4) -0.013(4) C133 0.160(9) 0.147(9) 0.075(6) -0.009(6) -0.013(6) -0.045(8) C134 0.222(14) 0.289(18) 0.087(7) -0.043(9) 0.006(8) -0.114(14) C141 0.071(4) 0.052(3) 0.079(4) -0.003(3) -0.007(3) -0.011(3) C142 0.069(4) 0.083(5) 0.113(6) -0.018(4) -0.002(4) -0.011(4) C143 0.069(5) 0.087(6) 0.180(9) -0.042(6) -0.007(5) -0.014(4) C144 0.086(6) 0.127(8) 0.273(16) -0.070(9) 0.037(8) -0.037(6) C211 0.106(7) 0.259(14) 0.099(7) -0.019(8) -0.020(6) -0.073(9) C212 0.179(13) 0.35(2) 0.093(8) -0.015(11) -0.021(8) -0.112(14) C213 0.151(13) 0.57(4) 0.114(11) -0.124(17) 0.010(10) -0.109(19) C214 0.28(3) 0.70(6) 0.197(19) -0.19(3) -0.142(19) 0.17(3) C221 0.079(6) 0.209(12) 0.133(9) 0.014(8) -0.031(6) -0.039(7) C222 0.098(7) 0.155(10) 0.172(11) 0.004(8) -0.047(7) -0.013(7) C223 0.142(10) 0.173(12) 0.223(15) 0.038(11) -0.093(10) -0.052(10) C224 0.246(19) 0.26(2) 0.31(2) 0.062(18) -0.159(18) -0.115(17) C231 0.082(6) 0.172(10) 0.122(8) 0.009(7) -0.032(6) -0.031(6) C232 0.084(7) 0.167(11) 0.168(11) -0.003(9) -0.008(7) 0.013(7) C233 0.136(10) 0.160(12) 0.152(11) -0.011(9) -0.033(9) 0.013(9) C234 0.105(8) 0.220(15) 0.174(13) -0.037(12) -0.014(8) 0.011(9) C241 0.077(6) 0.385(13) 0.178(11) 0.130(12) -0.055(7) -0.083(8) C242 0.212(10) 0.437(16) 0.254(15) 0.170(14) -0.108(11) -0.201(9) C243 0.351 0.429 0.362 0.234 -0.219 -0.217 C244 0.32(2) 0.40(3) 0.35(2) 0.219(18) -0.20(2) -0.16(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.728(5) . ? Mo1 O10 1.926(4) . ? Mo1 O9 1.929(4) . ? Mo1 O8 1.946(4) . ? Mo1 O7 1.954(4) . ? Mo1 O1 2.226(3) . ? Mo2 O2 1.686(5) . ? Mo2 O12 1.895(5) . ? Mo2 O7 1.897(4) . ? Mo2 O15 1.941(4) . ? Mo2 O11 1.949(5) . ? Mo2 O1 2.311(3) . ? Mo3 O3 1.690(5) . ? Mo3 O8 1.882(4) . ? Mo3 O11 1.901(5) . ? Mo3 O16 1.936(4) . ? Mo3 O13 1.943(5) . ? Mo3 O1 2.317(3) . ? Mo4 O4 1.685(4) . ? Mo4 O14 1.896(4) . ? Mo4 O9 1.910(4) . ? Mo4 O17 1.916(4) . ? Mo4 O12 1.942(4) . ? Mo4 O1 2.327(3) . ? Mo5 O5 1.687(5) . ? Mo5 O13 1.908(5) . ? Mo5 O10 1.912(4) . ? Mo5 O18 1.925(4) . ? Mo5 O14 1.941(5) . ? Mo5 O1 2.327(3) . ? Mo6 O6 1.680(4) . ? Mo6 O15 1.887(4) . ? Mo6 O16 1.900(4) . ? Mo6 O18 1.915(4) . ? Mo6 O17 1.933(4) . ? Mo6 O1 2.356(3) . ? O19 C2 1.363(8) . ? O19 C7 1.438(10) . ? O20 C9 1.378(9) . ? O20 C14 1.383(10) . ? N1 C1 1.366(8) . ? N2 C8 1.402(9) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 C131 1.506(7) . ? N3 C141 1.513(8) . ? N3 C111 1.523(7) . ? N3 C121 1.527(7) . ? N4 C211 1.518(11) . ? N4 C241 1.518(12) . ? N4 C231 1.524(12) . ? N4 C221 1.530(12) . ? C1 C6 1.394(9) . ? C1 C2 1.406(10) . ? C2 C3 1.383(9) . ? C3 C4 1.419(10) . ? C3 H3 0.9300 . ? C4 C5 1.386(10) . ? C4 C11 1.484(9) . ? C5 C6 1.377(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.375(11) . ? C8 C13 1.379(11) . ? C9 C10 1.398(10) . ? C10 C11 1.407(10) . ? C10 H10 0.9300 . ? C11 C12 1.391(10) . ? C12 C13 1.381(10) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C111 C112 1.498(8) . ? C111 H11A 0.9700 . ? C111 H11B 0.9700 . ? C112 C113 1.508(8) . ? C112 H11C 0.9700 . ? C112 H11D 0.9700 . ? C113 C114 1.443(10) . ? C113 H11E 0.9700 . ? C113 H11F 0.9700 . ? C114 H11G 0.9600 . ? C114 H11H 0.9600 . ? C114 H11I 0.9600 . ? C121 C122 1.489(7) . ? C121 H12A 0.9700 . ? C121 H12B 0.9700 . ? C122 C123 1.518(8) . ? C122 H12C 0.9700 . ? C122 H12D 0.9700 . ? C123 C124 1.493(9) . ? C123 H12E 0.9700 . ? C123 H12F 0.9700 . ? C124 H12G 0.9600 . ? C124 H12H 0.9600 . ? C124 H12I 0.9600 . ? C131 C132 1.526(8) . ? C131 H13A 0.9700 . ? C131 H13B 0.9700 . ? C132 C133 1.522(9) . ? C132 H13C 0.9700 . ? C132 H13D 0.9700 . ? C133 C134 1.476(10) . ? C133 H13E 0.9700 . ? C133 H13F 0.9700 . ? C134 H13G 0.9600 . ? C134 H13H 0.9600 . ? C134 H13I 0.9600 . ? C141 C142 1.513(8) . ? C141 H14D 0.9700 . ? C141 H14E 0.9700 . ? C142 C143 1.508(9) . ? C142 H14F 0.9700 . ? C142 H14G 0.9700 . ? C143 C144 1.477(9) . ? C143 H14H 0.9700 . ? C143 H14I 0.9700 . ? C144 H14J 0.9600 . ? C144 H14K 0.9600 . ? C144 H14L 0.9600 . ? C211 C212 1.504(11) . ? C211 H21A 0.9700 . ? C211 H21B 0.9700 . ? C212 C213 1.501(11) . ? C212 H21C 0.9700 . ? C212 H21D 0.9700 . ? C213 C214 1.463(12) . ? C213 H21E 0.9700 . ? C213 H21F 0.9700 . ? C214 H21G 0.9600 . ? C214 H21H 0.9600 . ? C214 H21I 0.9600 . ? C221 C222 1.504(10) . ? C221 H22A 0.9700 . ? C221 H22B 0.9700 . ? C222 C223 1.505(11) . ? C222 H22C 0.9700 . ? C222 H22D 0.9700 . ? C223 C224 1.465(11) . ? C223 H22E 0.9700 . ? C223 H22F 0.9700 . ? C224 H22G 0.9600 . ? C224 H22H 0.9600 . ? C224 H22I 0.9600 . ? C231 C232 1.510(10) . ? C231 H23A 0.9700 . ? C231 H23B 0.9700 . ? C232 C233 1.531(11) . ? C232 H23C 0.9700 . ? C232 H23D 0.9700 . ? C233 C234 1.459(11) . ? C233 H23E 0.9700 . ? C233 H23F 0.9700 . ? C234 H23G 0.9600 . ? C234 H23H 0.9600 . ? C234 H23I 0.9600 . ? C241 C242 1.516(12) . ? C241 H24A 0.9700 . ? C241 H24B 0.9700 . ? C242 C243 1.568(13) . ? C242 H24C 0.9700 . ? C242 H24D 0.9700 . ? C243 C244 1.457(12) . ? C243 H24E 0.9700 . ? C243 H24F 0.9700 . ? C244 H24G 0.9600 . ? C244 H24H 0.9600 . ? C244 H24I 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 O10 102.2(2) . . ? N1 Mo1 O9 102.0(2) . . ? O10 Mo1 O9 88.46(19) . . ? N1 Mo1 O8 102.4(2) . . ? O10 Mo1 O8 87.6(2) . . ? O9 Mo1 O8 155.58(17) . . ? N1 Mo1 O7 101.9(2) . . ? O10 Mo1 O7 155.88(17) . . ? O9 Mo1 O7 86.62(19) . . ? O8 Mo1 O7 87.2(2) . . ? N1 Mo1 O1 179.5(2) . . ? O10 Mo1 O1 78.16(15) . . ? O9 Mo1 O1 78.25(14) . . ? O8 Mo1 O1 77.35(15) . . ? O7 Mo1 O1 77.72(15) . . ? O2 Mo2 O12 104.0(3) . . ? O2 Mo2 O7 104.3(2) . . ? O12 Mo2 O7 88.02(19) . . ? O2 Mo2 O15 102.3(2) . . ? O12 Mo2 O15 86.95(19) . . ? O7 Mo2 O15 153.33(17) . . ? O2 Mo2 O11 103.2(3) . . ? O12 Mo2 O11 152.57(19) . . ? O7 Mo2 O11 87.9(2) . . ? O15 Mo2 O11 84.64(19) . . ? O2 Mo2 O1 178.6(2) . . ? O12 Mo2 O1 76.90(15) . . ? O7 Mo2 O1 76.71(15) . . ? O15 Mo2 O1 76.63(14) . . ? O11 Mo2 O1 75.77(16) . . ? O3 Mo3 O8 104.5(2) . . ? O3 Mo3 O11 103.7(3) . . ? O8 Mo3 O11 88.6(2) . . ? O3 Mo3 O16 102.6(2) . . ? O8 Mo3 O16 152.87(18) . . ? O11 Mo3 O16 85.95(19) . . ? O3 Mo3 O13 103.4(3) . . ? O8 Mo3 O13 87.7(2) . . ? O11 Mo3 O13 152.73(19) . . ? O16 Mo3 O13 85.16(19) . . ? O3 Mo3 O1 179.2(2) . . ? O8 Mo3 O1 76.30(15) . . ? O11 Mo3 O1 76.48(16) . . ? O16 Mo3 O1 76.58(15) . . ? O13 Mo3 O1 76.39(16) . . ? O4 Mo4 O14 103.6(2) . . ? O4 Mo4 O9 104.5(2) . . ? O14 Mo4 O9 87.97(18) . . ? O4 Mo4 O17 102.2(2) . . ? O14 Mo4 O17 87.57(19) . . ? O9 Mo4 O17 153.27(17) . . ? O4 Mo4 O12 103.7(2) . . ? O14 Mo4 O12 152.65(18) . . ? O9 Mo4 O12 86.07(18) . . ? O17 Mo4 O12 85.90(19) . . ? O4 Mo4 O1 179.2(2) . . ? O14 Mo4 O1 76.99(15) . . ? O9 Mo4 O1 76.10(14) . . ? O17 Mo4 O1 77.21(15) . . ? O12 Mo4 O1 75.66(16) . . ? O5 Mo5 O13 104.0(3) . . ? O5 Mo5 O10 103.5(2) . . ? O13 Mo5 O10 87.8(2) . . ? O5 Mo5 O18 103.6(2) . . ? O13 Mo5 O18 87.1(2) . . ? O10 Mo5 O18 152.87(17) . . ? O5 Mo5 O14 103.1(3) . . ? O13 Mo5 O14 152.93(18) . . ? O10 Mo5 O14 86.06(18) . . ? O18 Mo5 O14 86.45(19) . . ? O5 Mo5 O1 179.0(2) . . ? O13 Mo5 O1 76.78(16) . . ? O10 Mo5 O1 75.90(15) . . ? O18 Mo5 O1 76.99(14) . . ? O14 Mo5 O1 76.15(15) . . ? O6 Mo6 O15 104.5(2) . . ? O6 Mo6 O16 104.2(2) . . ? O15 Mo6 O16 87.5(2) . . ? O6 Mo6 O18 102.6(2) . . ? O15 Mo6 O18 152.92(17) . . ? O16 Mo6 O18 86.7(2) . . ? O6 Mo6 O17 103.4(2) . . ? O15 Mo6 O17 87.1(2) . . ? O16 Mo6 O17 152.42(18) . . ? O18 Mo6 O17 85.9(2) . . ? O6 Mo6 O1 178.96(18) . . ? O15 Mo6 O1 76.48(15) . . ? O16 Mo6 O1 76.25(15) . . ? O18 Mo6 O1 76.45(14) . . ? O17 Mo6 O1 76.18(15) . . ? Mo1 O1 Mo2 91.08(12) . . ? Mo1 O1 Mo3 90.85(12) . . ? Mo2 O1 Mo3 90.52(12) . . ? Mo1 O1 Mo4 90.60(12) . . ? Mo2 O1 Mo4 90.00(13) . . ? Mo3 O1 Mo4 178.45(16) . . ? Mo1 O1 Mo5 90.73(12) . . ? Mo2 O1 Mo5 178.14(16) . . ? Mo3 O1 Mo5 89.91(13) . . ? Mo4 O1 Mo5 89.52(11) . . ? Mo1 O1 Mo6 179.70(18) . . ? Mo2 O1 Mo6 89.16(12) . . ? Mo3 O1 Mo6 89.33(12) . . ? Mo4 O1 Mo6 89.21(12) . . ? Mo5 O1 Mo6 89.03(11) . . ? Mo2 O7 Mo1 114.48(19) . . ? Mo3 O8 Mo1 115.5(2) . . ? Mo4 O9 Mo1 114.99(19) . . ? Mo5 O10 Mo1 115.22(19) . . ? Mo3 O11 Mo2 117.2(2) . . ? Mo2 O12 Mo4 117.4(2) . . ? Mo5 O13 Mo3 116.9(2) . . ? Mo4 O14 Mo5 117.31(19) . . ? Mo6 O15 Mo2 117.7(2) . . ? Mo6 O16 Mo3 117.8(2) . . ? Mo4 O17 Mo6 117.4(2) . . ? Mo6 O18 Mo5 117.51(19) . . ? C2 O19 C7 116.9(6) . . ? C9 O20 C14 116.8(7) . . ? C1 N1 Mo1 176.7(5) . . ? C8 N2 H2A 120.0 . . ? C8 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C131 N3 C141 112.0(5) . . ? C131 N3 C111 108.8(5) . . ? C141 N3 C111 108.7(4) . . ? C131 N3 C121 107.8(4) . . ? C141 N3 C121 108.9(5) . . ? C111 N3 C121 110.6(4) . . ? C211 N4 C241 111.8(8) . . ? C211 N4 C231 105.6(6) . . ? C241 N4 C231 111.7(10) . . ? C211 N4 C221 109.5(9) . . ? C241 N4 C221 106.2(7) . . ? C231 N4 C221 112.1(8) . . ? N1 C1 C6 119.9(6) . . ? N1 C1 C2 121.2(6) . . ? C6 C1 C2 118.8(6) . . ? O19 C2 C3 124.7(7) . . ? O19 C2 C1 115.6(6) . . ? C3 C2 C1 119.7(7) . . ? C2 C3 C4 120.6(7) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 118.9(7) . . ? C5 C4 C11 120.9(7) . . ? C3 C4 C11 120.2(7) . . ? C6 C5 C4 120.1(7) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 121.6(7) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? O19 C7 H7A 109.5 . . ? O19 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O19 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 118.3(8) . . ? C9 C8 N2 118.8(8) . . ? C13 C8 N2 122.9(8) . . ? C8 C9 O20 114.7(7) . . ? C8 C9 C10 121.8(8) . . ? O20 C9 C10 123.5(8) . . ? C9 C10 C11 118.7(7) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 119.4(7) . . ? C12 C11 C4 120.6(7) . . ? C10 C11 C4 120.0(7) . . ? C13 C12 C11 119.7(8) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C8 C13 C12 122.0(8) . . ? C8 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? O20 C14 H14A 109.5 . . ? O20 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O20 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C112 C111 N3 117.1(5) . . ? C112 C111 H11A 108.0 . . ? N3 C111 H11A 108.0 . . ? C112 C111 H11B 108.0 . . ? N3 C111 H11B 108.0 . . ? H11A C111 H11B 107.3 . . ? C111 C112 C113 110.9(6) . . ? C111 C112 H11C 109.5 . . ? C113 C112 H11C 109.5 . . ? C111 C112 H11D 109.5 . . ? C113 C112 H11D 109.5 . . ? H11C C112 H11D 108.1 . . ? C114 C113 C112 112.6(7) . . ? C114 C113 H11E 109.1 . . ? C112 C113 H11E 109.1 . . ? C114 C113 H11F 109.1 . . ? C112 C113 H11F 109.1 . . ? H11E C113 H11F 107.8 . . ? C113 C114 H11G 109.5 . . ? C113 C114 H11H 109.5 . . ? H11G C114 H11H 109.5 . . ? C113 C114 H11I 109.5 . . ? H11G C114 H11I 109.5 . . ? H11H C114 H11I 109.5 . . ? C122 C121 N3 116.6(5) . . ? C122 C121 H12A 108.1 . . ? N3 C121 H12A 108.1 . . ? C122 C121 H12B 108.1 . . ? N3 C121 H12B 108.1 . . ? H12A C121 H12B 107.3 . . ? C121 C122 C123 110.7(5) . . ? C121 C122 H12C 109.5 . . ? C123 C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? C123 C122 H12D 109.5 . . ? H12C C122 H12D 108.1 . . ? C124 C123 C122 112.1(6) . . ? C124 C123 H12E 109.2 . . ? C122 C123 H12E 109.2 . . ? C124 C123 H12F 109.2 . . ? C122 C123 H12F 109.2 . . ? H12E C123 H12F 107.9 . . ? C123 C124 H12G 109.5 . . ? C123 C124 H12H 109.5 . . ? H12G C124 H12H 109.5 . . ? C123 C124 H12I 109.5 . . ? H12G C124 H12I 109.5 . . ? H12H C124 H12I 109.5 . . ? N3 C131 C132 115.1(5) . . ? N3 C131 H13A 108.5 . . ? C132 C131 H13A 108.5 . . ? N3 C131 H13B 108.5 . . ? C132 C131 H13B 108.5 . . ? H13A C131 H13B 107.5 . . ? C133 C132 C131 110.1(6) . . ? C133 C132 H13C 109.6 . . ? C131 C132 H13C 109.6 . . ? C133 C132 H13D 109.6 . . ? C131 C132 H13D 109.6 . . ? H13C C132 H13D 108.1 . . ? C134 C133 C132 111.6(9) . . ? C134 C133 H13E 109.3 . . ? C132 C133 H13E 109.3 . . ? C134 C133 H13F 109.3 . . ? C132 C133 H13F 109.3 . . ? H13E C133 H13F 108.0 . . ? C133 C134 H13G 109.5 . . ? C133 C134 H13H 109.5 . . ? H13G C134 H13H 109.5 . . ? C133 C134 H13I 109.5 . . ? H13G C134 H13I 109.5 . . ? H13H C134 H13I 109.5 . . ? C142 C141 N3 115.5(5) . . ? C142 C141 H14D 108.4 . . ? N3 C141 H14D 108.4 . . ? C142 C141 H14E 108.4 . . ? N3 C141 H14E 108.4 . . ? H14D C141 H14E 107.5 . . ? C143 C142 C141 111.0(6) . . ? C143 C142 H14F 109.4 . . ? C141 C142 H14F 109.4 . . ? C143 C142 H14G 109.4 . . ? C141 C142 H14G 109.4 . . ? H14F C142 H14G 108.0 . . ? C144 C143 C142 112.9(8) . . ? C144 C143 H14H 109.0 . . ? C142 C143 H14H 109.0 . . ? C144 C143 H14I 109.0 . . ? C142 C143 H14I 109.0 . . ? H14H C143 H14I 107.8 . . ? C143 C144 H14J 109.5 . . ? C143 C144 H14K 109.5 . . ? H14J C144 H14K 109.5 . . ? C143 C144 H14L 109.5 . . ? H14J C144 H14L 109.5 . . ? H14K C144 H14L 109.5 . . ? C212 C211 N4 116.1(8) . . ? C212 C211 H21A 108.3 . . ? N4 C211 H21A 108.3 . . ? C212 C211 H21B 108.3 . . ? N4 C211 H21B 108.3 . . ? H21A C211 H21B 107.4 . . ? C213 C212 C211 111.2(10) . . ? C213 C212 H21C 109.4 . . ? C211 C212 H21C 109.4 . . ? C213 C212 H21D 109.4 . . ? C211 C212 H21D 109.4 . . ? H21C C212 H21D 108.0 . . ? C214 C213 C212 114.9(15) . . ? C214 C213 H21E 108.6 . . ? C212 C213 H21E 108.6 . . ? C214 C213 H21F 108.6 . . ? C212 C213 H21F 108.6 . . ? H21E C213 H21F 107.5 . . ? C213 C214 H21G 109.5 . . ? C213 C214 H21H 109.5 . . ? H21G C214 H21H 109.5 . . ? C213 C214 H21I 109.5 . . ? H21G C214 H21I 109.5 . . ? H21H C214 H21I 109.5 . . ? C222 C221 N4 115.4(8) . . ? C222 C221 H22A 108.4 . . ? N4 C221 H22A 108.4 . . ? C222 C221 H22B 108.4 . . ? N4 C221 H22B 108.4 . . ? H22A C221 H22B 107.5 . . ? C221 C222 C223 110.9(9) . . ? C221 C222 H22C 109.5 . . ? C223 C222 H22C 109.5 . . ? C221 C222 H22D 109.5 . . ? C223 C222 H22D 109.4 . . ? H22C C222 H22D 108.0 . . ? C224 C223 C222 116.8(10) . . ? C224 C223 H22E 108.1 . . ? C222 C223 H22E 108.1 . . ? C224 C223 H22F 108.1 . . ? C222 C223 H22F 108.1 . . ? H22E C223 H22F 107.3 . . ? C223 C224 H22G 109.5 . . ? C223 C224 H22H 109.5 . . ? H22G C224 H22H 109.5 . . ? C223 C224 H22I 109.5 . . ? H22G C224 H22I 109.5 . . ? H22H C224 H22I 109.5 . . ? C232 C231 N4 117.5(8) . . ? C232 C231 H23A 107.9 . . ? N4 C231 H23A 107.9 . . ? C232 C231 H23B 107.9 . . ? N4 C231 H23B 107.9 . . ? H23A C231 H23B 107.2 . . ? C231 C232 C233 110.9(9) . . ? C231 C232 H23C 109.5 . . ? C233 C232 H23C 109.5 . . ? C231 C232 H23D 109.5 . . ? C233 C232 H23D 109.5 . . ? H23C C232 H23D 108.0 . . ? C234 C233 C232 110.2(11) . . ? C234 C233 H23E 109.6 . . ? C232 C233 H23E 109.6 . . ? C234 C233 H23F 109.6 . . ? C232 C233 H23F 109.6 . . ? H23E C233 H23F 108.1 . . ? C233 C234 H23G 109.5 . . ? C233 C234 H23H 109.5 . . ? H23G C234 H23H 109.5 . . ? C233 C234 H23I 109.5 . . ? H23G C234 H23I 109.5 . . ? H23H C234 H23I 109.5 . . ? C242 C241 N4 114.6(9) . . ? C242 C241 H24A 108.6 . . ? N4 C241 H24A 108.6 . . ? C242 C241 H24B 108.6 . . ? N4 C241 H24B 108.6 . . ? H24A C241 H24B 107.6 . . ? C241 C242 C243 111.7(11) . . ? C241 C242 H24C 109.3 . . ? C243 C242 H24C 109.3 . . ? C241 C242 H24D 109.3 . . ? C243 C242 H24D 109.3 . . ? H24C C242 H24D 107.9 . . ? C244 C243 C242 110.9(16) . . ? C244 C243 H24E 109.5 . . ? C242 C243 H24E 109.5 . . ? C244 C243 H24F 109.5 . . ? C242 C243 H24F 109.5 . . ? H24E C243 H24F 108.1 . . ? C243 C244 H24G 109.5 . . ? C243 C244 H24H 109.5 . . ? H24G C244 H24H 109.5 . . ? C243 C244 H24I 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.094 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.105 # Attachment '- MebiPh.CIF' data_MebiPh _database_code_depnum_ccdc_archive 'CCDC 810528' #TrackingRef '- MebiPh.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H89 Mo6 N5 O18' _chemical_formula_weight 1599.88 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.867(3) _cell_length_b 17.653(4) _cell_length_c 21.675(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.34(3) _cell_angle_gamma 90.00 _cell_volume 6454(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 33317 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4480 _exptl_absorpt_correction_T_max 0.7960 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean '100x100 micron' _diffrn_reflns_number 43505 _diffrn_reflns_av_R_equivalents 0.1131 _diffrn_reflns_av_sigmaI/netI 0.0978 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10661 _reflns_number_gt 6627 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku RAPID AUTO Ver2.30' _computing_cell_refinement 'Rigaku RAPID AUTO Ver2.30' _computing_data_reduction 'Rigaku RAPID AUTO Ver2.30' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0060P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00179(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10661 _refine_ls_number_parameters 690 _refine_ls_number_restraints 213 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.1809 _refine_ls_wR_factor_gt 0.1668 _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_restrained_S_all 1.218 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.24919(5) 0.87136(4) 0.85466(4) 0.0701(3) Uani 1 1 d . . . Mo2 Mo 0.20448(6) 1.04608(5) 0.88598(4) 0.0834(3) Uani 1 1 d . . . Mo3 Mo 0.12424(5) 0.95991(5) 0.76529(5) 0.0848(3) Uani 1 1 d . . . Mo4 Mo 0.38346(5) 1.00100(5) 0.83478(4) 0.0723(3) Uani 1 1 d . . . Mo5 Mo 0.30209(5) 0.91506(5) 0.71370(4) 0.0777(3) Uani 1 1 d . . . Mo6 Mo 0.25848(5) 1.09383(5) 0.74448(4) 0.0735(3) Uani 1 1 d . . . O1 O 0.2540(3) 0.9786(3) 0.8011(2) 0.0634(15) Uani 1 1 d . . . O2 O 0.1717(5) 1.0941(4) 0.9481(3) 0.114(3) Uani 1 1 d . . . O3 O 0.0303(4) 0.9475(5) 0.7398(4) 0.118(3) Uani 1 1 d . . . O4 O 0.4779(4) 1.0176(4) 0.8589(3) 0.099(2) Uani 1 1 d . . . O5 O 0.3362(5) 0.8702(4) 0.6503(3) 0.108(2) Uani 1 1 d . . . O6 O 0.2590(3) 1.1760(4) 0.7045(3) 0.0886(19) Uani 1 1 d . . . O7 O 0.2123(4) 0.9430(3) 0.9150(3) 0.0780(17) Uani 1 1 d . . . O8 O 0.1430(3) 0.8732(3) 0.8149(3) 0.0833(18) Uani 1 1 d . . . O9 O 0.3583(3) 0.9063(3) 0.8718(3) 0.0739(16) Uani 1 1 d . . . O10 O 0.2902(4) 0.8371(3) 0.7728(3) 0.0784(17) Uani 1 1 d . . . O11 O 0.1105(4) 1.0160(4) 0.8419(3) 0.0878(19) Uani 1 1 d . . . O12 O 0.3190(4) 1.0493(3) 0.8964(3) 0.0832(19) Uani 1 1 d . . . O13 O 0.1880(4) 0.9133(4) 0.7022(3) 0.0871(19) Uani 1 1 d . . . O14 O 0.3973(3) 0.9468(3) 0.7568(3) 0.0751(17) Uani 1 1 d . . . O15 O 0.2187(4) 1.1232(3) 0.8253(3) 0.0856(19) Uani 1 1 d . . . O16 O 0.1525(4) 1.0558(3) 0.7296(3) 0.0853(19) Uani 1 1 d . . . O17 O 0.3615(3) 1.0889(3) 0.7837(3) 0.0750(17) Uani 1 1 d . . . O18 O 0.2949(4) 1.0198(3) 0.6872(3) 0.0756(17) Uani 1 1 d . . . N1 N 0.2455(4) 0.7846(4) 0.8924(3) 0.071(2) Uani 1 1 d . . . N2 N 0.2411(5) 0.2407(5) 1.0165(5) 0.124(4) Uani 1 1 d . . . H2A H 0.2552 0.2252 1.0526 0.148 Uiso 1 1 calc R . . H2B H 0.2255 0.2086 0.9891 0.148 Uiso 1 1 calc R . . N3 N 0.5069(4) 0.3014(5) 0.1602(4) 0.083(2) Uani 1 1 d . . . N4 N 0.0282(5) 0.2773(6) 0.1280(4) 0.110(3) Uani 1 1 d . . . N5 N 0.3299(9) 1.1056(8) 0.0794(7) 0.163(5) Uani 1 1 d . . . C1 C 0.2417(5) 0.7095(5) 0.9133(5) 0.075(3) Uani 1 1 d . . . C2 C 0.2498(6) 0.6895(6) 0.9773(5) 0.081(3) Uani 1 1 d . . . C3 C 0.2483(6) 0.6128(5) 0.9924(5) 0.084(3) Uani 1 1 d . . . H3A H 0.2534 0.5994 1.0338 0.100 Uiso 1 1 calc R . . C4 C 0.2395(5) 0.5552(5) 0.9493(5) 0.072(2) Uani 1 1 d . . . C5 C 0.2299(5) 0.5756(5) 0.8867(5) 0.080(3) Uani 1 1 d . . . H5A H 0.2220 0.5384 0.8568 0.096 Uiso 1 1 calc R . . C6 C 0.2323(6) 0.6519(6) 0.8699(5) 0.087(3) Uani 1 1 d . . . H6A H 0.2275 0.6648 0.8284 0.104 Uiso 1 1 calc R . . C7 C 0.2605(6) 0.7507(6) 1.0264(5) 0.106(4) Uani 1 1 d . . . H7A H 0.2588 0.7997 1.0072 0.159 Uiso 1 1 calc R . . H7B H 0.3107 0.7440 1.0467 0.159 Uiso 1 1 calc R . . H7C H 0.2187 0.7469 1.0561 0.159 Uiso 1 1 calc R . . C8 C 0.2400(6) 0.4744(5) 0.9684(5) 0.079(3) Uani 1 1 d . . . C9 C 0.2127(6) 0.4179(5) 0.9254(5) 0.092(3) Uani 1 1 d . . . H9A H 0.1936 0.4326 0.8869 0.111 Uiso 1 1 calc R . . C10 C 0.2147(7) 0.3386(6) 0.9418(6) 0.098(3) Uani 1 1 d . . . C11 C 0.2433(7) 0.3180(6) 1.0024(6) 0.095(3) Uani 1 1 d . . . C12 C 0.2668(6) 0.3719(6) 1.0425(5) 0.088(3) Uani 1 1 d . . . H12A H 0.2843 0.3576 1.0816 0.105 Uiso 1 1 calc R . . C13 C 0.2656(5) 0.4488(6) 1.0271(5) 0.082(3) Uani 1 1 d . . . H13A H 0.2821 0.4842 1.0562 0.098 Uiso 1 1 calc R . . C14 C 0.1868(10) 0.2813(7) 0.8943(6) 0.171(7) Uani 1 1 d . . . H14A H 0.1591 0.3070 0.8616 0.256 Uiso 1 1 calc R . . H14B H 0.1519 0.2456 0.9135 0.256 Uiso 1 1 calc R . . H14C H 0.2318 0.2551 0.8777 0.256 Uiso 1 1 calc R . . C15 C 0.3666(13) 0.9756(9) 0.0319(8) 0.231(11) Uani 1 1 d . . . H15A H 0.3190 0.9474 0.0237 0.347 Uiso 1 1 calc R . . H15B H 0.3990 0.9483 0.0609 0.347 Uiso 1 1 calc R . . H15C H 0.3953 0.9827 -0.0058 0.347 Uiso 1 1 calc R . . C16 C 0.3462(11) 1.0489(10) 0.0576(7) 0.133(5) Uani 1 1 d . . . C111 C 0.4738(6) 0.3813(5) 0.1470(4) 0.081(3) Uani 1 1 d D . . H11D H 0.4266 0.3762 0.1216 0.098 Uiso 1 1 calc R . . H11E H 0.4580 0.4039 0.1858 0.098 Uiso 1 1 calc R . . C112 C 0.5309(6) 0.4356(5) 0.1148(5) 0.096(3) Uani 1 1 d D . . H11F H 0.5781 0.4427 0.1399 0.115 Uiso 1 1 calc R . . H11G H 0.5467 0.4146 0.0754 0.115 Uiso 1 1 calc R . . C113 C 0.4897(7) 0.5109(5) 0.1049(5) 0.108(4) Uani 1 1 d D . . H11H H 0.4750 0.5314 0.1448 0.129 Uiso 1 1 calc R . . H11I H 0.4412 0.5023 0.0817 0.129 Uiso 1 1 calc R . . C114 C 0.5389(8) 0.5694(7) 0.0712(6) 0.146(5) Uani 1 1 d D . . H11A H 0.5091 0.6155 0.0671 0.219 Uiso 1 1 calc R . . H11B H 0.5521 0.5507 0.0310 0.219 Uiso 1 1 calc R . . H11C H 0.5867 0.5792 0.0941 0.219 Uiso 1 1 calc R . . C121 C 0.5352(6) 0.2626(6) 0.1015(5) 0.092(3) Uani 1 1 d D . . H12E H 0.5555 0.2129 0.1123 0.110 Uiso 1 1 calc R . . H12F H 0.5789 0.2916 0.0847 0.110 Uiso 1 1 calc R . . C122 C 0.4721(6) 0.2531(6) 0.0511(4) 0.093(3) Uani 1 1 d D . . H12G H 0.4288 0.2226 0.0668 0.112 Uiso 1 1 calc R . . H12H H 0.4510 0.3024 0.0400 0.112 Uiso 1 1 calc R . . C123 C 0.5062(8) 0.2155(8) -0.0055(5) 0.145(5) Uani 1 1 d D . . H12I H 0.5300 0.1677 0.0066 0.174 Uiso 1 1 calc R . . H12J H 0.5479 0.2474 -0.0218 0.174 Uiso 1 1 calc R . . C124 C 0.4455(8) 0.2006(8) -0.0565(6) 0.148(5) Uani 1 1 d D . . H12B H 0.4704 0.1740 -0.0898 0.221 Uiso 1 1 calc R . . H12C H 0.4248 0.2479 -0.0713 0.221 Uiso 1 1 calc R . . H12D H 0.4029 0.1705 -0.0405 0.221 Uiso 1 1 calc R . . C131 C 0.4384(6) 0.2568(5) 0.1909(5) 0.092(3) Uani 1 1 d DU . . H13E H 0.4225 0.2846 0.2274 0.111 Uiso 1 1 calc R . . H13F H 0.3937 0.2572 0.1626 0.111 Uiso 1 1 calc R . . C132 C 0.4532(7) 0.1748(6) 0.2101(6) 0.128(4) Uani 1 1 d DU . . H13G H 0.5026 0.1707 0.2329 0.153 Uiso 1 1 calc R . . H13H H 0.4564 0.1425 0.1739 0.153 Uiso 1 1 calc R . . C133 C 0.3810(8) 0.1499(8) 0.2520(8) 0.203(7) Uani 1 1 d DU . . H13I H 0.3854 0.1731 0.2925 0.244 Uiso 1 1 calc R . . H13J H 0.3312 0.1656 0.2334 0.244 Uiso 1 1 calc R . . C134 C 0.3840(13) 0.0641(8) 0.2577(12) 0.323(14) Uani 1 1 d DU . . H13B H 0.3367 0.0463 0.2774 0.484 Uiso 1 1 calc R . . H13C H 0.4294 0.0497 0.2818 0.484 Uiso 1 1 calc R . . H13D H 0.3876 0.0420 0.2173 0.484 Uiso 1 1 calc R . . C141 C 0.5790(6) 0.3057(6) 0.2036(5) 0.108(4) Uani 1 1 d DU . . H14G H 0.5997 0.2549 0.2092 0.130 Uiso 1 1 calc R . . H14H H 0.6198 0.3353 0.1835 0.130 Uiso 1 1 calc R . . C142 C 0.5640(8) 0.3398(9) 0.2670(6) 0.152(5) Uani 1 1 d DU . . H14I H 0.5177 0.3158 0.2848 0.182 Uiso 1 1 calc R . . H14J H 0.5525 0.3933 0.2623 0.182 Uiso 1 1 calc R . . C143 C 0.6343(11) 0.3305(9) 0.3117(7) 0.203(8) Uani 1 1 d DU . . H14K H 0.6146 0.3246 0.3533 0.244 Uiso 1 1 calc R . . H14L H 0.6635 0.2850 0.3011 0.244 Uiso 1 1 calc R . . C144 C 0.6881(13) 0.3966(14) 0.3092(12) 0.347(16) Uani 1 1 d DU . . H14D H 0.7316 0.3890 0.3373 0.382 Uiso 1 1 calc R . . H14E H 0.6596 0.4415 0.3207 0.382 Uiso 1 1 calc R . . H14F H 0.7080 0.4022 0.2680 0.382 Uiso 1 1 calc R . . C211 C -0.0263(6) 0.2850(7) 0.1825(5) 0.113(4) Uani 1 1 d D . . H21D H -0.0500 0.2359 0.1904 0.135 Uiso 1 1 calc R . . H21E H -0.0689 0.3193 0.1711 0.135 Uiso 1 1 calc R . . C212 C 0.0106(8) 0.3133(9) 0.2423(5) 0.157(6) Uani 1 1 d D . . H21F H 0.0446 0.2740 0.2591 0.188 Uiso 1 1 calc R . . H21G H 0.0435 0.3570 0.2334 0.188 Uiso 1 1 calc R . . C213 C -0.0500(10) 0.3350(9) 0.2901(7) 0.193(8) Uani 1 1 d D . . H21H H -0.0816 0.3767 0.2744 0.231 Uiso 1 1 calc R . . H21I H -0.0227 0.3524 0.3269 0.231 Uiso 1 1 calc R . . C214 C -0.1047(10) 0.2702(10) 0.3071(8) 0.212(9) Uani 1 1 d D . . H21A H -0.1430 0.2876 0.3364 0.318 Uiso 1 1 calc R . . H21B H -0.0741 0.2298 0.3249 0.318 Uiso 1 1 calc R . . H21C H -0.1314 0.2523 0.2707 0.318 Uiso 1 1 calc R . . C221 C 0.0667(7) 0.3526(7) 0.1097(6) 0.121(4) Uani 1 1 d D . . H22D H 0.0930 0.3451 0.0705 0.146 Uiso 1 1 calc R . . H22E H 0.1075 0.3641 0.1399 0.146 Uiso 1 1 calc R . . C222 C 0.0129(7) 0.4235(7) 0.1034(6) 0.132(5) Uani 1 1 d D . . H22F H -0.0294 0.4134 0.0740 0.158 Uiso 1 1 calc R . . H22G H -0.0109 0.4351 0.1429 0.158 Uiso 1 1 calc R . . C223 C 0.0621(8) 0.4910(7) 0.0815(7) 0.142(5) Uani 1 1 d D . . H22H H 0.1078 0.4962 0.1085 0.171 Uiso 1 1 calc R . . H22I H 0.0815 0.4801 0.0404 0.171 Uiso 1 1 calc R . . C224 C 0.0190(10) 0.5651(8) 0.0797(7) 0.172(6) Uani 1 1 d D . . H22A H 0.0550 0.6045 0.0677 0.258 Uiso 1 1 calc R . . H22B H -0.0017 0.5762 0.1199 0.258 Uiso 1 1 calc R . . H22C H -0.0238 0.5622 0.0505 0.258 Uiso 1 1 calc R . . C231 C -0.0206(7) 0.2453(8) 0.0749(5) 0.133(5) Uani 1 1 d D . . H23D H -0.0649 0.2792 0.0673 0.159 Uiso 1 1 calc R . . H23E H -0.0424 0.1970 0.0877 0.159 Uiso 1 1 calc R . . C232 C 0.0230(8) 0.2336(9) 0.0143(5) 0.147(5) Uani 1 1 d D . . H23F H 0.0705 0.2039 0.0215 0.177 Uiso 1 1 calc R . . H23G H 0.0387 0.2822 -0.0025 0.177 Uiso 1 1 calc R . . C233 C -0.0309(10) 0.1925(12) -0.0320(6) 0.236(12) Uani 1 1 d D . . H23H H -0.0785 0.2225 -0.0381 0.283 Uiso 1 1 calc R . . H23I H -0.0038 0.1897 -0.0713 0.283 Uiso 1 1 calc R . . C234 C -0.0550(13) 0.1129(11) -0.0130(10) 0.254(12) Uani 1 1 d D . . H23A H -0.0903 0.0921 -0.0435 0.381 Uiso 1 1 calc R . . H23B H -0.0813 0.1148 0.0261 0.381 Uiso 1 1 calc R . . H23C H -0.0087 0.0816 -0.0097 0.381 Uiso 1 1 calc R . . C241 C 0.0985(7) 0.2230(8) 0.1401(7) 0.152(5) Uani 1 1 d DU . . H24D H 0.1303 0.2436 0.1736 0.182 Uiso 1 1 calc R . . H24E H 0.1315 0.2222 0.1036 0.182 Uiso 1 1 calc R . . C242 C 0.0765(7) 0.1403(8) 0.1566(8) 0.175(6) Uani 1 1 d DU . . H24F H 0.0368 0.1392 0.1889 0.210 Uiso 1 1 calc R . . H24G H 0.0558 0.1139 0.1207 0.210 Uiso 1 1 calc R . . C243 C 0.1537(9) 0.1036(9) 0.1790(10) 0.253(9) Uani 1 1 d DU . . H24H H 0.1925 0.1067 0.1462 0.304 Uiso 1 1 calc R . . H24I H 0.1740 0.1324 0.2138 0.304 Uiso 1 1 calc R . . C244 C 0.1454(10) 0.0228(9) 0.1979(11) 0.262 Uani 1 1 d DU . . H24A H 0.1968 0.0024 0.2075 0.392 Uiso 1 1 calc R . . H24B H 0.1220 -0.0056 0.1647 0.392 Uiso 1 1 calc R . . H24C H 0.1122 0.0196 0.2336 0.392 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 0.0669(5) 0.0613(5) 0.0821(6) 0.0101(4) -0.0017(4) -0.0015(4) Mo2 0.0889(7) 0.0715(6) 0.0901(7) -0.0039(5) 0.0208(5) 0.0060(5) Mo3 0.0574(5) 0.0881(7) 0.1086(8) 0.0228(5) -0.0131(5) -0.0104(4) Mo4 0.0595(5) 0.0769(6) 0.0805(6) 0.0042(4) -0.0085(4) -0.0077(4) Mo5 0.0803(6) 0.0778(6) 0.0749(6) -0.0081(4) 0.0016(5) -0.0016(5) Mo6 0.0620(5) 0.0666(5) 0.0918(7) 0.0158(4) -0.0003(4) -0.0016(4) O1 0.050(3) 0.068(3) 0.073(4) -0.013(3) 0.004(3) -0.006(3) O2 0.134(7) 0.098(5) 0.111(6) -0.019(4) 0.036(5) 0.011(5) O3 0.052(4) 0.159(7) 0.142(7) 0.042(5) -0.027(4) -0.026(4) O4 0.058(4) 0.128(6) 0.111(5) 0.015(4) -0.025(4) -0.028(4) O5 0.127(6) 0.100(5) 0.097(5) -0.020(4) 0.008(5) 0.007(5) O6 0.063(4) 0.088(4) 0.114(5) 0.023(4) -0.009(4) 0.004(3) O7 0.087(4) 0.068(4) 0.079(4) 0.002(3) 0.012(3) -0.003(3) O8 0.064(4) 0.076(4) 0.109(5) 0.010(4) -0.010(3) -0.017(3) O9 0.073(4) 0.067(4) 0.082(4) 0.008(3) -0.011(3) -0.005(3) O10 0.080(4) 0.056(3) 0.099(5) -0.001(3) -0.002(4) 0.011(3) O11 0.063(4) 0.093(5) 0.107(5) 0.008(4) 0.002(4) 0.009(3) O12 0.084(5) 0.086(4) 0.080(4) -0.011(3) 0.005(3) -0.023(4) O13 0.074(4) 0.098(5) 0.089(5) 0.006(4) -0.020(3) -0.022(4) O14 0.058(4) 0.081(4) 0.087(4) -0.003(3) 0.002(3) 0.010(3) O15 0.085(5) 0.058(4) 0.114(5) 0.009(3) 0.016(4) 0.006(3) O16 0.071(4) 0.078(4) 0.107(5) 0.027(4) -0.007(4) -0.006(3) O17 0.059(4) 0.072(4) 0.094(5) 0.004(3) -0.006(3) -0.017(3) O18 0.080(4) 0.077(4) 0.069(4) 0.007(3) -0.006(3) 0.002(3) N1 0.054(4) 0.062(4) 0.098(6) 0.012(4) -0.008(4) 0.001(4) N2 0.130(9) 0.079(6) 0.163(10) 0.018(6) 0.020(7) -0.010(6) N3 0.062(5) 0.093(6) 0.092(6) -0.009(5) 0.001(4) 0.011(4) N4 0.071(6) 0.156(9) 0.102(7) 0.013(6) -0.009(5) -0.033(6) N5 0.186(14) 0.139(12) 0.165(13) 0.005(10) 0.006(10) 0.004(11) C1 0.068(6) 0.071(6) 0.086(7) 0.004(5) 0.005(5) 0.004(5) C2 0.076(7) 0.080(7) 0.087(7) -0.001(6) -0.005(5) -0.003(5) C3 0.104(8) 0.070(6) 0.077(7) 0.009(5) -0.005(6) 0.002(6) C4 0.060(6) 0.064(6) 0.092(7) 0.001(5) 0.005(5) -0.001(4) C5 0.078(7) 0.070(6) 0.091(8) 0.001(5) -0.003(5) 0.003(5) C6 0.089(7) 0.097(8) 0.075(7) 0.004(6) 0.004(5) 0.006(6) C7 0.105(9) 0.094(8) 0.119(9) -0.021(7) -0.025(7) -0.005(7) C8 0.080(7) 0.065(6) 0.094(8) 0.001(5) 0.009(6) -0.005(5) C9 0.105(8) 0.070(6) 0.103(8) -0.007(6) 0.010(6) -0.010(6) C10 0.108(9) 0.069(7) 0.116(10) -0.011(7) 0.016(7) -0.013(6) C11 0.085(8) 0.075(8) 0.126(10) 0.015(7) 0.020(7) 0.000(6) C12 0.080(7) 0.070(6) 0.114(9) 0.026(6) -0.007(6) 0.003(6) C13 0.065(6) 0.096(8) 0.085(7) 0.008(6) -0.001(5) 0.009(5) C14 0.27(2) 0.085(9) 0.161(13) -0.040(9) 0.012(13) -0.059(11) C15 0.39(3) 0.140(14) 0.164(16) -0.028(12) -0.128(17) 0.092(17) C16 0.161(15) 0.142(14) 0.097(11) 0.025(10) -0.033(10) 0.004(12) C111 0.075(6) 0.076(6) 0.093(7) -0.002(5) 0.006(5) 0.018(5) C112 0.086(8) 0.093(8) 0.107(9) -0.012(6) 0.003(6) 0.011(6) C113 0.114(10) 0.098(8) 0.111(9) -0.009(7) 0.011(7) -0.003(7) C114 0.172(14) 0.126(10) 0.140(12) 0.010(9) 0.020(10) -0.026(10) C121 0.072(7) 0.091(7) 0.112(9) -0.020(6) 0.016(6) 0.010(6) C122 0.093(8) 0.090(7) 0.097(8) -0.015(6) 0.015(6) 0.008(6) C123 0.144(13) 0.151(13) 0.139(12) -0.059(10) 0.011(10) 0.009(10) C124 0.154(14) 0.160(13) 0.129(12) -0.037(10) 0.016(10) -0.023(11) C131 0.067(6) 0.110(7) 0.100(8) 0.008(6) 0.015(5) 0.006(6) C132 0.114(9) 0.106(8) 0.162(12) -0.007(8) -0.032(8) 0.022(7) C133 0.124(11) 0.161(12) 0.32(2) 0.142(13) -0.050(11) -0.043(10) C134 0.28(3) 0.184(14) 0.51(4) 0.09(2) 0.01(3) -0.038(17) C141 0.062(6) 0.114(9) 0.147(9) -0.018(7) -0.019(6) 0.018(6) C142 0.129(11) 0.191(13) 0.137(10) -0.024(10) -0.023(8) 0.039(10) C143 0.222(18) 0.180(15) 0.207(14) -0.053(13) -0.104(13) 0.049(13) C144 0.22(2) 0.40(3) 0.42(4) -0.06(3) -0.07(2) -0.09(2) C211 0.084(8) 0.149(11) 0.106(9) 0.014(8) 0.018(7) -0.011(7) C212 0.158(14) 0.231(17) 0.082(9) -0.010(10) 0.001(9) -0.097(12) C213 0.23(2) 0.25(2) 0.105(12) -0.021(13) 0.021(13) -0.073(17) C214 0.23(2) 0.24(2) 0.169(17) -0.024(15) 0.064(15) -0.056(17) C221 0.082(8) 0.157(12) 0.124(10) 0.012(9) -0.025(7) -0.031(9) C222 0.101(10) 0.161(13) 0.133(11) 0.003(10) -0.018(8) -0.036(10) C223 0.126(12) 0.173(14) 0.129(12) 0.025(11) -0.009(9) -0.047(11) C224 0.204(19) 0.160(14) 0.151(14) 0.023(12) -0.045(12) 0.004(13) C231 0.092(9) 0.211(15) 0.094(9) -0.031(9) -0.003(7) -0.029(9) C232 0.120(12) 0.227(17) 0.095(10) -0.016(10) 0.006(9) 0.008(11) C233 0.121(14) 0.48(4) 0.109(13) -0.089(19) -0.015(10) -0.029(19) C234 0.28(3) 0.22(2) 0.27(3) -0.003(19) 0.08(2) -0.080(19) C241 0.081(9) 0.201(12) 0.173(13) 0.069(11) 0.000(9) -0.013(9) C242 0.094(9) 0.192(12) 0.240(16) 0.046(12) 0.024(11) -0.013(8) C243 0.123(12) 0.217(12) 0.42(2) 0.068(16) 0.059(15) 0.072(11) C244 0.120 0.246 0.420 0.067 0.072 0.070 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N1 1.737(7) . ? Mo1 O7 1.926(6) . ? Mo1 O9 1.974(6) . ? Mo1 O8 1.983(6) . ? Mo1 O10 2.001(6) . ? Mo1 O1 2.222(5) . ? Mo2 O2 1.687(6) . ? Mo2 O15 1.910(6) . ? Mo2 O11 1.921(7) . ? Mo2 O7 1.929(6) . ? Mo2 O12 1.945(6) . ? Mo2 O1 2.349(5) . ? Mo3 O3 1.689(6) . ? Mo3 O8 1.897(6) . ? Mo3 O16 1.923(6) . ? Mo3 O13 1.930(7) . ? Mo3 O11 1.948(7) . ? Mo3 O1 2.342(5) . ? Mo4 O4 1.699(6) . ? Mo4 O9 1.903(5) . ? Mo4 O12 1.927(6) . ? Mo4 O17 1.939(6) . ? Mo4 O14 1.957(6) . ? Mo4 O1 2.331(5) . ? Mo5 O5 1.690(6) . ? Mo5 O10 1.892(6) . ? Mo5 O14 1.936(6) . ? Mo5 O13 1.939(6) . ? Mo5 O18 1.940(6) . ? Mo5 O1 2.350(5) . ? Mo6 O6 1.690(6) . ? Mo6 O18 1.907(6) . ? Mo6 O17 1.933(6) . ? Mo6 O16 1.935(6) . ? Mo6 O15 1.949(6) . ? Mo6 O1 2.378(5) . ? N1 C1 1.404(10) . ? N2 C11 1.401(12) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 C121 1.525(10) . ? N3 C141 1.535(12) . ? N3 C111 1.542(11) . ? N3 C131 1.550(10) . ? N4 C211 1.507(12) . ? N4 C231 1.521(13) . ? N4 C221 1.533(13) . ? N4 C241 1.547(14) . ? N5 C16 1.143(17) . ? C1 C6 1.393(12) . ? C1 C2 1.438(12) . ? C2 C3 1.394(12) . ? C2 C7 1.526(12) . ? C3 C4 1.389(12) . ? C3 H3A 0.9300 . ? C4 C5 1.412(12) . ? C4 C8 1.486(12) . ? C5 C6 1.397(12) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C13 1.415(13) . ? C8 C9 1.437(13) . ? C9 C10 1.445(13) . ? C9 H9A 0.9300 . ? C10 C11 1.443(15) . ? C10 C14 1.515(15) . ? C11 C12 1.348(14) . ? C12 C13 1.398(12) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.450(19) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C111 C112 1.530(10) . ? C111 H11D 0.9700 . ? C111 H11E 0.9700 . ? C112 C113 1.515(10) . ? C112 H11F 0.9700 . ? C112 H11G 0.9700 . ? C113 C114 1.516(10) . ? C113 H11H 0.9700 . ? C113 H11I 0.9700 . ? C114 H11A 0.9600 . ? C114 H11B 0.9600 . ? C114 H11C 0.9600 . ? C121 C122 1.529(10) . ? C121 H12E 0.9700 . ? C121 H12F 0.9700 . ? C122 C123 1.512(10) . ? C122 H12G 0.9700 . ? C122 H12H 0.9700 . ? C123 C124 1.525(11) . ? C123 H12I 0.9700 . ? C123 H12J 0.9700 . ? C124 H12B 0.9600 . ? C124 H12C 0.9600 . ? C124 H12D 0.9600 . ? C131 C132 1.527(10) . ? C131 H13E 0.9700 . ? C131 H13F 0.9700 . ? C132 C133 1.587(12) . ? C132 H13G 0.9700 . ? C132 H13H 0.9700 . ? C133 C134 1.521(8) . ? C133 H13I 0.9700 . ? C133 H13J 0.9700 . ? C134 H13B 0.9600 . ? C134 H13C 0.9600 . ? C134 H13D 0.9600 . ? C141 C142 1.523(11) . ? C141 H14G 0.9700 . ? C141 H14H 0.9700 . ? C142 C143 1.534(12) . ? C142 H14I 0.9700 . ? C142 H14J 0.9700 . ? C143 C144 1.480(8) . ? C143 H14K 0.9700 . ? C143 H14L 0.9700 . ? C144 H14D 0.9600 . ? C144 H14E 0.9600 . ? C144 H14F 0.9600 . ? C211 C212 1.518(11) . ? C211 H21D 0.9700 . ? C211 H21E 0.9700 . ? C212 C213 1.509(12) . ? C212 H21F 0.9700 . ? C212 H21G 0.9700 . ? C213 C214 1.515(8) . ? C213 H21H 0.9700 . ? C213 H21I 0.9700 . ? C214 H21A 0.9600 . ? C214 H21B 0.9600 . ? C214 H21C 0.9600 . ? C221 C222 1.551(11) . ? C221 H22D 0.9700 . ? C221 H22E 0.9700 . ? C222 C223 1.529(11) . ? C222 H22F 0.9700 . ? C222 H22G 0.9700 . ? C223 C224 1.497(12) . ? C223 H22H 0.9700 . ? C223 H22I 0.9700 . ? C224 H22A 0.9600 . ? C224 H22B 0.9600 . ? C224 H22C 0.9600 . ? C231 C232 1.524(11) . ? C231 H23D 0.9700 . ? C231 H23E 0.9700 . ? C232 C233 1.532(12) . ? C232 H23F 0.9700 . ? C232 H23G 0.9700 . ? C233 C234 1.520(14) . ? C233 H23H 0.9700 . ? C233 H23I 0.9700 . ? C234 H23A 0.9600 . ? C234 H23B 0.9600 . ? C234 H23C 0.9600 . ? C241 C242 1.549(12) . ? C241 H24D 0.9700 . ? C241 H24E 0.9700 . ? C242 C243 1.530(13) . ? C242 H24F 0.9700 . ? C242 H24G 0.9700 . ? C243 C244 1.491(8) . ? C243 H24H 0.9700 . ? C243 H24I 0.9700 . ? C244 H24A 0.9600 . ? C244 H24B 0.9600 . ? C244 H24C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mo1 O7 104.3(3) . . ? N1 Mo1 O9 102.9(3) . . ? O7 Mo1 O9 88.4(3) . . ? N1 Mo1 O8 100.6(3) . . ? O7 Mo1 O8 89.4(3) . . ? O9 Mo1 O8 156.2(2) . . ? N1 Mo1 O10 99.5(3) . . ? O7 Mo1 O10 156.3(2) . . ? O9 Mo1 O10 86.2(2) . . ? O8 Mo1 O10 86.4(3) . . ? N1 Mo1 O1 176.6(3) . . ? O7 Mo1 O1 78.9(2) . . ? O9 Mo1 O1 78.2(2) . . ? O8 Mo1 O1 78.2(2) . . ? O10 Mo1 O1 77.3(2) . . ? O2 Mo2 O15 103.6(3) . . ? O2 Mo2 O11 105.2(3) . . ? O15 Mo2 O11 87.8(3) . . ? O2 Mo2 O7 103.6(3) . . ? O15 Mo2 O7 152.7(2) . . ? O11 Mo2 O7 87.4(3) . . ? O2 Mo2 O12 102.8(3) . . ? O15 Mo2 O12 86.0(3) . . ? O11 Mo2 O12 151.9(3) . . ? O7 Mo2 O12 85.7(3) . . ? O2 Mo2 O1 178.1(3) . . ? O15 Mo2 O1 77.0(2) . . ? O11 Mo2 O1 76.5(2) . . ? O7 Mo2 O1 75.7(2) . . ? O12 Mo2 O1 75.4(2) . . ? O3 Mo3 O8 103.5(3) . . ? O3 Mo3 O16 102.5(3) . . ? O8 Mo3 O16 153.9(3) . . ? O3 Mo3 O13 103.8(3) . . ? O8 Mo3 O13 88.1(3) . . ? O16 Mo3 O13 87.1(3) . . ? O3 Mo3 O11 103.2(3) . . ? O8 Mo3 O11 86.9(3) . . ? O16 Mo3 O11 85.8(3) . . ? O13 Mo3 O11 152.9(3) . . ? O3 Mo3 O1 179.3(3) . . ? O8 Mo3 O1 76.9(2) . . ? O16 Mo3 O1 77.1(2) . . ? O13 Mo3 O1 76.8(2) . . ? O11 Mo3 O1 76.2(2) . . ? O4 Mo4 O9 103.5(3) . . ? O4 Mo4 O12 104.0(3) . . ? O9 Mo4 O12 88.2(2) . . ? O4 Mo4 O17 102.3(3) . . ? O9 Mo4 O17 154.2(2) . . ? O12 Mo4 O17 86.3(3) . . ? O4 Mo4 O14 103.5(3) . . ? O9 Mo4 O14 87.9(2) . . ? O12 Mo4 O14 152.4(3) . . ? O17 Mo4 O14 85.5(2) . . ? O4 Mo4 O1 179.7(3) . . ? O9 Mo4 O1 76.8(2) . . ? O12 Mo4 O1 76.2(2) . . ? O17 Mo4 O1 77.4(2) . . ? O14 Mo4 O1 76.3(2) . . ? O5 Mo5 O10 104.3(3) . . ? O5 Mo5 O14 104.1(3) . . ? O10 Mo5 O14 88.5(3) . . ? O5 Mo5 O13 103.3(3) . . ? O10 Mo5 O13 88.1(3) . . ? O14 Mo5 O13 152.4(3) . . ? O5 Mo5 O18 103.1(3) . . ? O10 Mo5 O18 152.5(2) . . ? O14 Mo5 O18 85.3(3) . . ? O13 Mo5 O18 85.2(3) . . ? O5 Mo5 O1 179.3(3) . . ? O10 Mo5 O1 76.2(2) . . ? O14 Mo5 O1 76.2(2) . . ? O13 Mo5 O1 76.4(2) . . ? O18 Mo5 O1 76.3(2) . . ? O6 Mo6 O18 104.6(3) . . ? O6 Mo6 O17 104.9(3) . . ? O18 Mo6 O17 87.9(3) . . ? O6 Mo6 O16 102.7(3) . . ? O18 Mo6 O16 87.4(3) . . ? O17 Mo6 O16 152.3(2) . . ? O6 Mo6 O15 103.6(3) . . ? O18 Mo6 O15 151.8(2) . . ? O17 Mo6 O15 86.0(3) . . ? O16 Mo6 O15 85.4(3) . . ? O6 Mo6 O1 178.4(2) . . ? O18 Mo6 O1 76.2(2) . . ? O17 Mo6 O1 76.4(2) . . ? O16 Mo6 O1 76.0(2) . . ? O15 Mo6 O1 75.6(2) . . ? Mo1 O1 Mo4 91.1(2) . . ? Mo1 O1 Mo3 90.93(17) . . ? Mo4 O1 Mo3 178.0(3) . . ? Mo1 O1 Mo2 90.52(18) . . ? Mo4 O1 Mo2 90.34(18) . . ? Mo3 O1 Mo2 89.70(16) . . ? Mo1 O1 Mo5 91.64(18) . . ? Mo4 O1 Mo5 90.36(16) . . ? Mo3 O1 Mo5 89.51(18) . . ? Mo2 O1 Mo5 177.7(3) . . ? Mo1 O1 Mo6 179.5(3) . . ? Mo4 O1 Mo6 89.08(17) . . ? Mo3 O1 Mo6 88.93(19) . . ? Mo2 O1 Mo6 89.01(18) . . ? Mo5 O1 Mo6 88.83(18) . . ? Mo1 O7 Mo2 114.8(3) . . ? Mo3 O8 Mo1 114.0(3) . . ? Mo4 O9 Mo1 113.9(3) . . ? Mo5 O10 Mo1 114.8(3) . . ? Mo2 O11 Mo3 117.6(3) . . ? Mo4 O12 Mo2 118.1(3) . . ? Mo3 O13 Mo5 117.3(3) . . ? Mo5 O14 Mo4 117.1(3) . . ? Mo2 O15 Mo6 118.3(3) . . ? Mo3 O16 Mo6 118.0(3) . . ? Mo6 O17 Mo4 117.1(3) . . ? Mo6 O18 Mo5 118.7(3) . . ? C1 N1 Mo1 170.8(7) . . ? C11 N2 H2A 120.0 . . ? C11 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C121 N3 C141 106.4(7) . . ? C121 N3 C111 111.8(7) . . ? C141 N3 C111 110.7(8) . . ? C121 N3 C131 111.5(7) . . ? C141 N3 C131 110.6(8) . . ? C111 N3 C131 105.9(6) . . ? C211 N4 C231 107.3(8) . . ? C211 N4 C221 112.7(10) . . ? C231 N4 C221 110.7(10) . . ? C211 N4 C241 113.2(9) . . ? C231 N4 C241 108.0(11) . . ? C221 N4 C241 104.9(8) . . ? C6 C1 N1 118.4(9) . . ? C6 C1 C2 118.9(9) . . ? N1 C1 C2 122.6(9) . . ? C3 C2 C1 117.6(9) . . ? C3 C2 C7 121.8(10) . . ? C1 C2 C7 120.6(9) . . ? C4 C3 C2 123.7(9) . . ? C4 C3 H3A 118.1 . . ? C2 C3 H3A 118.1 . . ? C3 C4 C5 118.1(9) . . ? C3 C4 C8 121.0(9) . . ? C5 C4 C8 120.9(9) . . ? C6 C5 C4 119.6(9) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C1 C6 C5 122.0(10) . . ? C1 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 117.2(9) . . ? C13 C8 C4 123.9(10) . . ? C9 C8 C4 118.9(10) . . ? C8 C9 C10 120.4(11) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 118.3(10) . . ? C11 C10 C14 123.4(11) . . ? C9 C10 C14 118.3(12) . . ? C12 C11 N2 123.7(12) . . ? C12 C11 C10 120.4(10) . . ? N2 C11 C10 115.8(12) . . ? C11 C12 C13 121.8(11) . . ? C11 C12 H12A 119.1 . . ? C13 C12 H12A 119.1 . . ? C12 C13 C8 121.9(10) . . ? C12 C13 H13A 119.0 . . ? C8 C13 H13A 119.0 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N5 C16 C15 178.0(18) . . ? C112 C111 N3 115.5(7) . . ? C112 C111 H11D 108.4 . . ? N3 C111 H11D 108.4 . . ? C112 C111 H11E 108.4 . . ? N3 C111 H11E 108.4 . . ? H11D C111 H11E 107.5 . . ? C113 C112 C111 109.0(8) . . ? C113 C112 H11F 109.9 . . ? C111 C112 H11F 109.9 . . ? C113 C112 H11G 109.9 . . ? C111 C112 H11G 109.9 . . ? H11F C112 H11G 108.3 . . ? C112 C113 C114 114.4(9) . . ? C112 C113 H11H 108.6 . . ? C114 C113 H11H 108.6 . . ? C112 C113 H11I 108.6 . . ? C114 C113 H11I 108.6 . . ? H11H C113 H11I 107.6 . . ? C113 C114 H11A 109.5 . . ? C113 C114 H11B 109.5 . . ? H11A C114 H11B 109.5 . . ? C113 C114 H11C 109.5 . . ? H11A C114 H11C 109.5 . . ? H11B C114 H11C 109.5 . . ? N3 C121 C122 115.1(7) . . ? N3 C121 H12E 108.5 . . ? C122 C121 H12E 108.5 . . ? N3 C121 H12F 108.5 . . ? C122 C121 H12F 108.5 . . ? H12E C121 H12F 107.5 . . ? C123 C122 C121 111.2(8) . . ? C123 C122 H12G 109.4 . . ? C121 C122 H12G 109.4 . . ? C123 C122 H12H 109.4 . . ? C121 C122 H12H 109.4 . . ? H12G C122 H12H 108.0 . . ? C122 C123 C124 114.0(10) . . ? C122 C123 H12I 108.7 . . ? C124 C123 H12I 108.7 . . ? C122 C123 H12J 108.7 . . ? C124 C123 H12J 108.7 . . ? H12I C123 H12J 107.6 . . ? C123 C124 H12B 109.5 . . ? C123 C124 H12C 109.5 . . ? H12B C124 H12C 109.5 . . ? C123 C124 H12D 109.5 . . ? H12B C124 H12D 109.5 . . ? H12C C124 H12D 109.5 . . ? C132 C131 N3 118.5(8) . . ? C132 C131 H13E 107.7 . . ? N3 C131 H13E 107.7 . . ? C132 C131 H13F 107.7 . . ? N3 C131 H13F 107.7 . . ? H13E C131 H13F 107.1 . . ? C131 C132 C133 107.1(9) . . ? C131 C132 H13G 110.3 . . ? C133 C132 H13G 110.3 . . ? C131 C132 H13H 110.3 . . ? C133 C132 H13H 110.3 . . ? H13G C132 H13H 108.6 . . ? C134 C133 C132 107.2(12) . . ? C134 C133 H13I 110.3 . . ? C132 C133 H13I 110.3 . . ? C134 C133 H13J 110.3 . . ? C132 C133 H13J 110.3 . . ? H13I C133 H13J 108.5 . . ? C133 C134 H13B 109.5 . . ? C133 C134 H13C 109.5 . . ? H13B C134 H13C 109.5 . . ? C133 C134 H13D 109.5 . . ? H13B C134 H13D 109.5 . . ? H13C C134 H13D 109.5 . . ? C142 C141 N3 115.9(8) . . ? C142 C141 H14G 108.3 . . ? N3 C141 H14G 108.3 . . ? C142 C141 H14H 108.3 . . ? N3 C141 H14H 108.3 . . ? H14G C141 H14H 107.4 . . ? C141 C142 C143 113.3(11) . . ? C141 C142 H14I 108.9 . . ? C143 C142 H14I 108.9 . . ? C141 C142 H14J 108.9 . . ? C143 C142 H14J 108.9 . . ? H14I C142 H14J 107.7 . . ? C144 C143 C142 111.4(14) . . ? C144 C143 H14K 109.4 . . ? C142 C143 H14K 109.4 . . ? C144 C143 H14L 109.4 . . ? C142 C143 H14L 109.4 . . ? H14K C143 H14L 108.0 . . ? C143 C144 H14D 109.5 . . ? C143 C144 H14E 109.5 . . ? H14D C144 H14E 109.5 . . ? C143 C144 H14F 109.5 . . ? H14D C144 H14F 109.5 . . ? H14E C144 H14F 109.5 . . ? N4 C211 C212 116.7(9) . . ? N4 C211 H21D 108.1 . . ? C212 C211 H21D 108.1 . . ? N4 C211 H21E 108.1 . . ? C212 C211 H21E 108.1 . . ? H21D C211 H21E 107.3 . . ? C213 C212 C211 113.2(11) . . ? C213 C212 H21F 108.9 . . ? C211 C212 H21F 108.9 . . ? C213 C212 H21G 108.9 . . ? C211 C212 H21G 108.9 . . ? H21F C212 H21G 107.8 . . ? C212 C213 C214 113.0(12) . . ? C212 C213 H21H 109.0 . . ? C214 C213 H21H 109.0 . . ? C212 C213 H21I 109.0 . . ? C214 C213 H21I 109.0 . . ? H21H C213 H21I 107.8 . . ? C213 C214 H21A 109.5 . . ? C213 C214 H21B 109.5 . . ? H21A C214 H21B 109.5 . . ? C213 C214 H21C 109.5 . . ? H21A C214 H21C 109.5 . . ? H21B C214 H21C 109.5 . . ? N4 C221 C222 118.3(10) . . ? N4 C221 H22D 107.7 . . ? C222 C221 H22D 107.7 . . ? N4 C221 H22E 107.7 . . ? C222 C221 H22E 107.7 . . ? H22D C221 H22E 107.1 . . ? C223 C222 C221 109.7(10) . . ? C223 C222 H22F 109.7 . . ? C221 C222 H22F 109.7 . . ? C223 C222 H22G 109.7 . . ? C221 C222 H22G 109.7 . . ? H22F C222 H22G 108.2 . . ? C224 C223 C222 115.2(12) . . ? C224 C223 H22H 108.5 . . ? C222 C223 H22H 108.5 . . ? C224 C223 H22I 108.5 . . ? C222 C223 H22I 108.5 . . ? H22H C223 H22I 107.5 . . ? C223 C224 H22A 109.5 . . ? C223 C224 H22B 109.5 . . ? H22A C224 H22B 109.5 . . ? C223 C224 H22C 109.5 . . ? H22A C224 H22C 109.5 . . ? H22B C224 H22C 109.5 . . ? N4 C231 C232 116.2(10) . . ? N4 C231 H23D 108.2 . . ? C232 C231 H23D 108.2 . . ? N4 C231 H23E 108.2 . . ? C232 C231 H23E 108.2 . . ? H23D C231 H23E 107.4 . . ? C231 C232 C233 109.9(10) . . ? C231 C232 H23F 109.7 . . ? C233 C232 H23F 109.7 . . ? C231 C232 H23G 109.7 . . ? C233 C232 H23G 109.7 . . ? H23F C232 H23G 108.2 . . ? C234 C233 C232 114.8(15) . . ? C234 C233 H23H 108.6 . . ? C232 C233 H23H 108.6 . . ? C234 C233 H23I 108.6 . . ? C232 C233 H23I 108.6 . . ? H23H C233 H23I 107.6 . . ? C233 C234 H23A 109.5 . . ? C233 C234 H23B 109.5 . . ? H23A C234 H23B 109.5 . . ? C233 C234 H23C 109.5 . . ? H23A C234 H23C 109.5 . . ? H23B C234 H23C 109.5 . . ? N4 C241 C242 116.0(10) . . ? N4 C241 H24D 108.3 . . ? C242 C241 H24D 108.3 . . ? N4 C241 H24E 108.3 . . ? C242 C241 H24E 108.3 . . ? H24D C241 H24E 107.4 . . ? C243 C242 C241 105.5(11) . . ? C243 C242 H24F 110.6 . . ? C241 C242 H24F 110.6 . . ? C243 C242 H24G 110.6 . . ? C241 C242 H24G 110.6 . . ? H24F C242 H24G 108.8 . . ? C244 C243 C242 114.3(13) . . ? C244 C243 H24H 108.7 . . ? C242 C243 H24H 108.7 . . ? C244 C243 H24I 108.7 . . ? C242 C243 H24I 108.7 . . ? H24H C243 H24I 107.6 . . ? C243 C244 H24A 109.5 . . ? C243 C244 H24B 109.5 . . ? H24A C244 H24B 109.5 . . ? C243 C244 H24C 109.5 . . ? H24A C244 H24C 109.5 . . ? H24B C244 H24C 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 N2 H2A N5 0.86 2.52 3.125(17) 127.6 1_546 N2 H2B O2 0.86 2.39 3.200(12) 158.3 1_545 _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.046 _refine_diff_density_min -1.496 _refine_diff_density_rms 0.144