data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_address X.-M.Zhang ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; H.-S.Wu ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; F.-Q.Zhang ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; "Alexander Prikhod'ko" ; Anorganisch-Chemisches Institut University Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; 'Shigemasa Kuwata' ; Anorganisch-Chemisches Institut University Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; 'Peter Comba' ; Anorganisch-Chemisches Institut University Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; _publ_contact_author_name 'Prof Peter Comba' _publ_contact_author_address ; Institute of Inorganic Chemistry University of Heidelberg INF 270 Heidelberg D-69120 GERMANY ; _publ_contact_author_email PETER.COMBA@ACI.UNI-HEIDELBERG.DE _publ_section_title ; The three-electron heteropoly blue [P6Mo18O73] 11- with a basket-shaped skeleton ; data_mo _database_code_depnum_ccdc_archive 'CCDC 237041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H96 K Mo18 N10 O86 P6' _chemical_formula_weight 3925.01 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' P P 0.1023 0.0942 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.375(4) _cell_length_b 20.003(3) _cell_length_c 19.700(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.261(2) _cell_angle_gamma 90.00 _cell_volume 9940(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1664 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7596 _exptl_absorpt_coefficient_mu 2.451 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6399 _exptl_absorpt_correction_T_max 0.6399 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22863 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10380 _reflns_number_gt 9529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Water molecules were located from Fourier map. A check with PLATON did not turn up any extra solvent accessible voids larger than 40 cubic \%A. The large peaks Q1 in the difference Fourier is localized at position with Q1-O5w, Q1-O7w and Q1-O8w distances 1.956, 2.354 and 2.227 \%A, respectively. This is an artifact of the poor quality of the crystal. The O5w, O7w and O8w were refined with occupancy of 0.5. Hydrogen atoms of organic group were placed at calculated positions in the riding model approximation. Eight hydrogen atoms of water moleucles were located from Fourier map; the other hydrogen atoms of water molecules could not be placed in sensible positions even by the HYDROGEN (Nardelli, 1999) option in the WinGX (Farrugia, 1999) suite. ; _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^)+(0.0360P)^2^+69.8878P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10380 _refine_ls_number_parameters 695 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 0.310818(15) 0.22021(2) 0.34296(2) 0.01638(9) Uani 1 1 d . . . Mo2 Mo 0.290658(15) 0.22134(2) 0.16325(2) 0.01490(9) Uani 1 1 d . . . Mo3 Mo 0.426090(15) -0.010497(19) 0.24796(2) 0.01465(9) Uani 1 1 d . . . Mo4 Mo 0.296446(15) 0.07739(2) 0.25154(2) 0.01584(9) Uani 1 1 d . . . Mo5 Mo 0.306252(17) 0.36667(2) 0.25349(2) 0.01890(10) Uani 1 1 d . . . Mo6 Mo 0.418578(17) 0.418442(19) 0.16604(2) 0.01826(10) Uani 1 1 d . . . Mo7 Mo 0.565236(17) 0.41814(2) 0.16286(2) 0.01877(10) Uani 1 1 d . . . Mo8 Mo 0.409004(15) 0.254341(19) 0.078084(19) 0.01351(9) Uani 1 1 d . . . Mo9 Mo 0.554534(15) 0.253488(19) 0.07678(2) 0.01440(9) Uani 1 1 d . . . P1 P 0.41816(4) 0.26735(6) 0.25067(6) 0.0121(2) Uani 1 1 d . . . P2 P 0.38105(4) 0.10262(6) 0.12993(6) 0.0127(2) Uani 1 1 d . . . P3 P 0.40541(4) 0.10133(6) 0.37192(6) 0.0146(2) Uani 1 1 d . . . K1 K 0.5000 0.14134(6) 0.2500 0.0119(3) Uani 1 2 d S . . O1 O 0.27755(12) 0.17702(16) 0.25375(16) 0.0170(7) Uani 1 1 d . . . O2 O 0.35633(12) 0.13570(16) 0.32920(16) 0.0169(7) Uani 1 1 d . . . O3 O 0.35618(12) 0.26602(16) 0.25301(16) 0.0173(7) Uani 1 1 d . . . O4 O 0.36548(13) 0.25139(16) 0.39742(16) 0.0184(7) Uani 1 1 d . . . O5 O 0.27085(13) 0.1862(2) 0.39676(18) 0.0262(8) Uani 1 1 d . . . O6 O 0.27623(13) 0.29819(18) 0.32007(17) 0.0221(7) Uani 1 1 d . . . O7 O 0.23953(13) 0.18940(17) 0.11160(17) 0.0222(7) Uani 1 1 d . . . O8 O 0.26298(13) 0.29886(17) 0.18962(16) 0.0199(7) Uani 1 1 d . . . O9 O 0.33451(12) 0.25333(15) 0.10691(16) 0.0171(7) Uani 1 1 d . . . O10 O 0.33923(12) 0.13607(15) 0.17298(16) 0.0151(6) Uani 1 1 d . . . O11 O 0.44150(12) 0.07653(15) 0.32035(16) 0.0157(7) Uani 1 1 d . . . O12 O 0.42835(12) 0.08119(15) 0.17983(16) 0.0155(6) Uani 1 1 d . . . O13 O 0.41572(13) -0.06025(17) 0.17710(17) 0.0215(7) Uani 1 1 d . . . O14 O 0.42450(13) -0.06679(17) 0.31230(17) 0.0223(7) Uani 1 1 d . . . O15 O 0.5000 0.0032(2) 0.2500 0.0185(10) Uani 1 2 d S . . O16 O 0.25092(13) 0.05558(18) 0.18467(18) 0.0230(7) Uani 1 1 d . . . O17 O 0.35175(12) 0.01931(16) 0.24823(16) 0.0171(7) Uani 1 1 d . . . O18 O 0.26605(13) 0.05413(18) 0.32036(18) 0.0249(8) Uani 1 1 d . . . O19 O 0.25432(14) 0.41955(18) 0.25579(18) 0.0277(8) Uani 1 1 d . . . O20 O 0.35475(13) 0.39426(17) 0.32046(17) 0.0224(7) Uani 1 1 d . . . O21 O 0.33983(13) 0.39505(16) 0.18356(17) 0.0207(7) Uani 1 1 d . . . O22 O 0.39659(15) 0.48058(17) 0.11142(18) 0.0270(8) Uani 1 1 d . . . O23 O 0.41948(14) 0.46578(16) 0.25159(17) 0.0218(7) Uani 1 1 d . . . O24 O 0.43399(13) 0.34189(16) 0.25005(16) 0.0175(7) Uani 1 1 d . . . O25 O 0.41485(13) 0.34405(16) 0.10705(16) 0.0183(7) Uani 1 1 d . . . O26 O 0.49138(13) 0.42637(16) 0.16579(16) 0.0207(7) Uani 1 1 d . . . O27 O 0.57443(14) 0.47965(17) 0.10738(18) 0.0256(8) Uani 1 1 d . . . O28 O 0.55508(13) 0.34355(16) 0.10512(16) 0.0187(7) Uani 1 1 d . . . O29 O 0.39886(12) 0.15513(15) 0.08003(16) 0.0151(6) Uani 1 1 d . . . O30 O 0.38725(13) 0.26554(16) -0.00552(16) 0.0193(7) Uani 1 1 d . . . O31 O 0.48113(12) 0.24703(16) 0.07157(16) 0.0167(7) Uani 1 1 d . . . O32 O 0.43207(12) 0.23142(15) 0.18746(16) 0.0150(6) Uani 1 1 d . . . O33 O 0.44631(12) 0.23136(15) 0.31248(16) 0.0145(6) Uani 1 1 d . . . O34 O 0.43606(12) 0.15350(16) 0.41892(16) 0.0162(7) Uani 1 1 d . . . O35 O 0.56017(13) 0.26372(17) -0.00706(17) 0.0213(7) Uani 1 1 d . . . O36 O 0.35670(12) 0.04450(16) 0.08866(16) 0.0168(7) Uani 1 1 d . . . O37 O 0.38719(12) 0.04686(17) 0.41665(17) 0.0212(7) Uani 1 1 d . . . N1 N 0.19709(16) 0.4869(2) 0.0366(2) 0.0245(9) Uani 1 1 d . . . H1A H 0.1805 0.4741 -0.0040 0.029 Uiso 1 1 calc R . . H1E H 0.1728 0.5059 0.0606 0.029 Uiso 1 1 calc R . . N2 N 0.30336(17) 0.4474(2) 0.0242(2) 0.0284(10) Uani 1 1 d . . . H2A H 0.3199 0.4602 0.0648 0.034 Uiso 1 1 calc R . . H2C H 0.3277 0.4287 0.0001 0.034 Uiso 1 1 calc R . . N3 N 0.11402(19) 0.1956(2) 0.2847(2) 0.0314(10) Uani 1 1 d . . . H3C H 0.0796 0.2066 0.2841 0.038 Uiso 1 1 calc R . . H3D H 0.1157 0.1526 0.2716 0.038 Uiso 1 1 calc R . . N4 N 0.16835(17) 0.3146(2) 0.3296(2) 0.0263(10) Uani 1 1 d . . . H4B H 0.1690 0.3576 0.3432 0.032 Uiso 1 1 calc R . . H4C H 0.2021 0.3010 0.3288 0.032 Uiso 1 1 calc R . . N5 N 0.45346(16) 0.0147(2) 0.5325(2) 0.0215(9) Uani 1 1 d . . . H5A H 0.4350 0.0122 0.5689 0.026 Uiso 1 1 calc R . . H5D H 0.4335 0.0367 0.4991 0.026 Uiso 1 1 calc R . . C1 C 0.3236(3) 0.5585(3) -0.0209(4) 0.0434(16) Uani 1 1 d . . . H1B H 0.3503 0.5390 -0.0458 0.065 Uiso 1 1 calc R . . H1C H 0.3394 0.5722 0.0234 0.065 Uiso 1 1 calc R . . H1D H 0.3084 0.5966 -0.0453 0.065 Uiso 1 1 calc R . . C2 C 0.2806(2) 0.5074(3) -0.0131(3) 0.0295(12) Uani 1 1 d . . . H2B H 0.2648 0.4938 -0.0586 0.035 Uiso 1 1 calc R . . C3 C 0.2380(2) 0.5367(3) 0.0253(3) 0.0257(11) Uani 1 1 d . . . H3A H 0.2538 0.5535 0.0690 0.031 Uiso 1 1 calc R . . H3B H 0.2216 0.5740 -0.0003 0.031 Uiso 1 1 calc R . . C4 C 0.2195(2) 0.4265(3) 0.0742(3) 0.0246(11) Uani 1 1 d . . . H4A H 0.2355 0.4403 0.1196 0.029 Uiso 1 1 calc R . . C5 C 0.2621(2) 0.3964(3) 0.0356(3) 0.0249(11) Uani 1 1 d . . . H5B H 0.2786 0.3591 0.0614 0.030 Uiso 1 1 calc R . . H5C H 0.2462 0.3795 -0.0081 0.030 Uiso 1 1 calc R . . C6 C 0.1755(2) 0.3770(3) 0.0826(3) 0.0293(12) Uani 1 1 d . . . H6A H 0.1494 0.3977 0.1076 0.044 Uiso 1 1 calc R . . H6B H 0.1899 0.3386 0.1071 0.044 Uiso 1 1 calc R . . H6C H 0.1592 0.3635 0.0384 0.044 Uiso 1 1 calc R . . C7 C 0.1070(6) 0.2327(4) 0.1661(4) 0.120(5) Uani 1 1 d . . . H7A H 0.1067 0.1869 0.1515 0.180 Uiso 1 1 calc R . . H7B H 0.1229 0.2599 0.1338 0.180 Uiso 1 1 calc R . . H7C H 0.0714 0.2474 0.1692 0.180 Uiso 1 1 calc R . . C8 C 0.1386(3) 0.2386(3) 0.2347(3) 0.0456(17) Uani 1 1 d . . . H8A H 0.1749 0.2233 0.2314 0.055 Uiso 1 1 calc R . . C9 C 0.1403(3) 0.2022(3) 0.3560(3) 0.0401(15) Uani 1 1 d . . . H9A H 0.1761 0.1845 0.3582 0.048 Uiso 1 1 calc R . . H9B H 0.1210 0.1759 0.3864 0.048 Uiso 1 1 calc R . . C10 C 0.1426(2) 0.2733(3) 0.3795(3) 0.0330(13) Uani 1 1 d . . . H10A H 0.1063 0.2895 0.3812 0.040 Uiso 1 1 calc R . . C11 C 0.1401(3) 0.3099(3) 0.2595(3) 0.0405(16) Uani 1 1 d . . . H11A H 0.1579 0.3375 0.2287 0.049 Uiso 1 1 calc R . . H11B H 0.1041 0.3264 0.2597 0.049 Uiso 1 1 calc R . . C12 C 0.1730(3) 0.2809(4) 0.4500(3) 0.0502(19) Uani 1 1 d . . . H12A H 0.1733 0.3271 0.4633 0.075 Uiso 1 1 calc R . . H12B H 0.2087 0.2656 0.4489 0.075 Uiso 1 1 calc R . . H12C H 0.1561 0.2548 0.4824 0.075 Uiso 1 1 calc R . . C13 C 0.4922(2) 0.1230(3) 0.5749(3) 0.0292(12) Uani 1 1 d . . . H13A H 0.4720 0.1209 0.6133 0.044 Uiso 1 1 calc R . . H13B H 0.4723 0.1467 0.5382 0.044 Uiso 1 1 calc R . . H13C H 0.5250 0.1460 0.5878 0.044 Uiso 1 1 calc R . . C14 C 0.50367(19) 0.0527(3) 0.5516(2) 0.0221(10) Uani 1 1 d . . . H14A H 0.5243 0.0293 0.5894 0.027 Uiso 1 1 calc R . . C15 C 0.46439(19) -0.0538(2) 0.5088(3) 0.0221(10) Uani 1 1 d . . . H15A H 0.4311 -0.0767 0.4961 0.027 Uiso 1 1 calc R . . H15B H 0.4837 -0.0785 0.5459 0.027 Uiso 1 1 calc R . . O1W O 0.5141(2) 0.5728(3) 0.0116(2) 0.0589(14) Uani 1 1 d . . . H1WA H 0.4998 0.5828 -0.0287 0.071 Uiso 1 1 d R . . H1WB H 0.4935 0.5856 0.0410 0.071 Uiso 1 1 d R . . O2W O -0.0341(4) 0.1040(4) 0.1269(5) 0.140(3) Uani 1 1 d . . . H2WA H -0.0199 0.0872 0.1641 0.168 Uiso 1 1 d R . . O3W O 0.37641(18) 0.3983(2) -0.0539(3) 0.0505(13) Uani 1 1 d . . . H3WA H 0.3735 0.3559 -0.0480 0.061 Uiso 1 1 d R . . H3WB H 0.3825 0.4177 -0.0912 0.061 Uiso 1 1 d R . . O4W O 0.19762(14) 0.43622(18) 0.37301(18) 0.0268(8) Uani 1 1 d . . . H4WA H 0.1746 0.4677 0.3728 0.032 Uiso 1 1 d R . . O5W O 0.0331(6) 0.0968(9) 0.2151(19) 0.29(2) Uani 0.50 1 d P . . O6W O 0.3546(2) 0.5746(3) 0.2645(6) 0.170(5) Uani 1 1 d . . . H6WA H 0.3793 0.5519 0.2871 0.204 Uiso 1 1 d R . . H6WB H 0.3195 0.5754 0.2804 0.204 Uiso 1 1 d R . . O7W O 0.0212(5) 0.2919(9) 0.2518(11) 0.127(6) Uani 0.50 1 d P . . O8W O -0.0203(6) 0.2174(9) 0.1449(8) 0.114(6) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01295(19) 0.0243(2) 0.0120(2) 0.00028(15) 0.00191(15) 0.00424(15) Mo2 0.01443(19) 0.0182(2) 0.01188(19) 0.00021(15) 0.00063(15) 0.00359(15) Mo3 0.01489(19) 0.01302(18) 0.0153(2) 0.00086(14) -0.00164(15) -0.00141(14) Mo4 0.01234(18) 0.0207(2) 0.0144(2) 0.00227(15) 0.00139(15) -0.00234(15) Mo5 0.0213(2) 0.0196(2) 0.0151(2) -0.00268(15) -0.00139(16) 0.00870(16) Mo6 0.0275(2) 0.01258(19) 0.0136(2) 0.00084(14) -0.00277(16) 0.00030(16) Mo7 0.0266(2) 0.01454(19) 0.0140(2) 0.00273(15) -0.00310(16) -0.00566(16) Mo8 0.01666(19) 0.01356(19) 0.01025(19) 0.00054(14) 0.00113(15) -0.00115(14) Mo9 0.01576(19) 0.01695(19) 0.01047(19) 0.00032(14) 0.00129(15) -0.00307(15) P1 0.0153(5) 0.0118(5) 0.0091(5) 0.0002(4) 0.0010(4) 0.0017(4) P2 0.0128(5) 0.0129(5) 0.0123(5) 0.0006(4) 0.0017(4) 0.0002(4) P3 0.0123(5) 0.0174(6) 0.0138(6) 0.0028(4) 0.0006(4) -0.0006(4) K1 0.0106(6) 0.0125(6) 0.0127(6) 0.000 0.0016(5) 0.000 O1 0.0151(15) 0.0228(17) 0.0129(16) 0.0002(13) 0.0010(12) 0.0048(13) O2 0.0124(15) 0.0211(17) 0.0170(17) 0.0017(13) 0.0008(13) 0.0004(13) O3 0.0170(16) 0.0182(16) 0.0164(17) 0.0003(13) -0.0001(13) 0.0026(13) O4 0.0177(16) 0.0228(17) 0.0147(17) -0.0002(13) 0.0025(13) 0.0052(13) O5 0.0156(17) 0.043(2) 0.0202(19) 0.0008(16) 0.0043(14) -0.0007(15) O6 0.0178(17) 0.0300(19) 0.0178(17) -0.0021(14) -0.0006(13) 0.0092(14) O7 0.0195(17) 0.0265(18) 0.0205(18) -0.0009(14) 0.0009(14) 0.0016(14) O8 0.0197(17) 0.0249(18) 0.0142(17) -0.0023(13) -0.0018(13) 0.0084(14) O9 0.0187(16) 0.0164(16) 0.0161(17) 0.0023(12) 0.0015(13) 0.0035(13) O10 0.0125(15) 0.0180(16) 0.0149(16) 0.0018(12) 0.0020(12) 0.0016(12) O11 0.0129(15) 0.0172(16) 0.0166(16) 0.0009(12) 0.0003(12) -0.0020(12) O12 0.0133(15) 0.0182(16) 0.0149(16) 0.0006(12) 0.0013(12) 0.0003(12) O13 0.0219(17) 0.0196(17) 0.0221(18) -0.0020(14) -0.0017(14) 0.0010(14) O14 0.0216(17) 0.0226(18) 0.0212(18) 0.0046(14) -0.0041(14) -0.0038(14) O15 0.011(2) 0.022(2) 0.021(2) 0.000 -0.0037(18) 0.000 O16 0.0166(16) 0.0279(19) 0.0233(19) 0.0016(15) -0.0031(14) -0.0035(14) O17 0.0137(15) 0.0195(16) 0.0177(17) 0.0012(13) 0.0003(13) -0.0016(13) O18 0.0219(18) 0.033(2) 0.0214(19) 0.0044(15) 0.0073(14) -0.0064(15) O19 0.0283(19) 0.031(2) 0.0226(19) -0.0065(15) -0.0017(15) 0.0158(16) O20 0.0240(18) 0.0240(18) 0.0183(18) -0.0056(14) -0.0012(14) 0.0070(14) O21 0.0245(18) 0.0185(17) 0.0182(17) -0.0022(13) -0.0018(14) 0.0060(14) O22 0.042(2) 0.0172(17) 0.0193(18) 0.0049(14) -0.0069(16) -0.0002(15) O23 0.0305(19) 0.0137(16) 0.0192(18) -0.0016(13) -0.0054(14) 0.0000(14) O24 0.0230(17) 0.0142(16) 0.0149(16) 0.0009(12) 0.0008(13) 0.0020(13) O25 0.0235(17) 0.0154(16) 0.0158(17) -0.0016(13) 0.0011(13) -0.0024(13) O26 0.0280(19) 0.0183(17) 0.0152(17) -0.0004(13) 0.0001(14) -0.0031(14) O27 0.032(2) 0.0212(18) 0.0217(19) 0.0074(14) -0.0049(15) -0.0069(15) O28 0.0226(17) 0.0168(16) 0.0157(17) 0.0014(13) -0.0030(13) -0.0046(13) O29 0.0169(16) 0.0150(15) 0.0139(16) -0.0005(12) 0.0039(12) -0.0011(12) O30 0.0261(18) 0.0195(16) 0.0122(16) 0.0021(13) 0.0021(14) -0.0023(14) O31 0.0161(16) 0.0184(16) 0.0162(17) -0.0007(13) 0.0040(13) -0.0031(13) O32 0.0174(16) 0.0153(15) 0.0127(16) -0.0008(12) 0.0037(13) 0.0001(12) O33 0.0168(16) 0.0154(15) 0.0116(15) 0.0013(12) 0.0021(12) 0.0000(12) O34 0.0175(16) 0.0177(16) 0.0132(16) 0.0025(12) 0.0007(12) 0.0012(13) O35 0.0227(17) 0.0267(18) 0.0142(17) 0.0035(14) 0.0015(14) -0.0048(14) O36 0.0188(16) 0.0161(16) 0.0149(16) -0.0002(13) -0.0007(13) -0.0018(13) O37 0.0162(16) 0.0279(19) 0.0190(18) 0.0089(14) 0.0002(13) -0.0039(14) N1 0.023(2) 0.032(2) 0.018(2) -0.0074(18) -0.0031(17) 0.0086(18) N2 0.023(2) 0.036(3) 0.026(2) 0.000(2) 0.0037(18) 0.0101(19) N3 0.032(3) 0.036(3) 0.026(2) 0.000(2) 0.002(2) -0.001(2) N4 0.028(2) 0.027(2) 0.025(2) -0.0034(18) 0.0051(18) 0.0063(19) N5 0.018(2) 0.027(2) 0.019(2) 0.0085(17) 0.0013(16) -0.0008(17) C1 0.042(4) 0.044(4) 0.047(4) 0.013(3) 0.018(3) 0.005(3) C2 0.034(3) 0.035(3) 0.020(3) 0.006(2) 0.002(2) 0.008(2) C3 0.030(3) 0.027(3) 0.020(3) -0.003(2) 0.000(2) 0.009(2) C4 0.026(3) 0.030(3) 0.016(2) 0.003(2) -0.002(2) 0.006(2) C5 0.028(3) 0.028(3) 0.018(3) -0.001(2) -0.002(2) 0.011(2) C6 0.023(3) 0.035(3) 0.028(3) 0.002(2) -0.003(2) 0.002(2) C7 0.284(17) 0.053(5) 0.018(4) -0.003(3) -0.011(6) -0.059(8) C8 0.089(5) 0.023(3) 0.028(3) -0.003(2) 0.019(3) -0.002(3) C9 0.040(3) 0.055(4) 0.023(3) 0.014(3) -0.008(3) -0.015(3) C10 0.024(3) 0.058(4) 0.019(3) -0.002(3) 0.008(2) -0.006(3) C11 0.079(5) 0.022(3) 0.019(3) 0.001(2) -0.001(3) -0.001(3) C12 0.041(4) 0.088(6) 0.020(3) 0.001(3) 0.000(3) -0.028(4) C13 0.036(3) 0.026(3) 0.025(3) 0.002(2) 0.002(2) -0.001(2) C14 0.022(2) 0.028(3) 0.016(2) 0.007(2) -0.0031(19) -0.001(2) C15 0.020(2) 0.023(3) 0.023(3) 0.007(2) 0.002(2) -0.0030(19) O1W 0.066(3) 0.069(4) 0.037(3) 0.008(2) -0.014(2) 0.009(3) O2W 0.168(9) 0.091(6) 0.171(9) 0.007(6) 0.062(7) -0.002(6) O3W 0.062(3) 0.028(2) 0.069(3) 0.014(2) 0.043(3) 0.010(2) O4W 0.0296(19) 0.0248(18) 0.0242(19) -0.0051(15) -0.0046(15) 0.0123(15) O5W 0.076(10) 0.104(13) 0.67(6) -0.24(2) -0.12(2) 0.056(9) O6W 0.031(3) 0.025(3) 0.453(17) 0.034(6) 0.021(6) 0.006(2) O7W 0.079(11) 0.154(15) 0.145(15) -0.034(14) -0.005(13) 0.027(9) O8W 0.070(9) 0.158(16) 0.112(13) -0.040(11) 0.007(8) 0.017(9) _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 O5 1.688(3) . ? Mo1 O4 1.772(3) . ? Mo1 O6 1.822(3) . ? Mo1 O1 2.055(3) . ? Mo1 O2 2.082(3) . ? Mo1 O3 2.398(3) . ? Mo2 O7 1.685(3) . ? Mo2 O9 1.774(3) . ? Mo2 O8 1.802(3) . ? Mo2 O1 2.050(3) . ? Mo2 O10 2.101(3) . ? Mo2 O3 2.460(3) . ? Mo3 O14 1.699(3) . ? Mo3 O13 1.711(3) . ? Mo3 O15 1.8916(8) . ? Mo3 O17 1.979(3) . ? Mo3 O11 2.257(3) . ? Mo3 O12 2.277(3) . ? Mo3 K1 3.5675(12) . ? Mo4 O18 1.696(3) . ? Mo4 O16 1.711(3) . ? Mo4 O17 1.828(3) . ? Mo4 O1 2.052(3) . ? Mo4 O10 2.306(3) . ? Mo4 O2 2.346(3) . ? Mo5 O19 1.694(3) . ? Mo5 O21 1.789(3) . ? Mo5 O20 1.790(3) . ? Mo5 O8 2.080(3) . ? Mo5 O6 2.096(4) . ? Mo5 O3 2.379(3) . ? Mo6 O22 1.698(3) . ? Mo6 O26 1.855(3) . ? Mo6 O25 1.884(3) . ? Mo6 O23 1.931(3) . ? Mo6 O21 2.117(3) . ? Mo6 O24 2.257(3) . ? Mo7 O27 1.679(3) . ? Mo7 O28 1.877(3) . ? Mo7 O26 1.889(3) . ? Mo7 O23 1.938(3) 2_655 ? Mo7 O20 2.077(3) 2_655 ? Mo7 O24 2.294(3) 2_655 ? Mo8 O30 1.694(3) . ? Mo8 O31 1.854(3) . ? Mo8 O25 1.884(3) . ? Mo8 O29 2.002(3) . ? Mo8 O9 2.032(3) . ? Mo8 O32 2.218(3) . ? Mo9 O35 1.686(3) . ? Mo9 O31 1.859(3) . ? Mo9 O28 1.886(3) . ? Mo9 O34 2.015(3) 2_655 ? Mo9 O4 2.038(3) 2_655 ? Mo9 O33 2.229(3) 2_655 ? P1 O32 1.513(3) . ? P1 O33 1.524(3) . ? P1 O24 1.545(3) . ? P1 O3 1.579(3) . ? P1 K1 3.2669(15) . ? P2 O36 1.512(3) . ? P2 O12 1.527(3) . ? P2 O29 1.540(3) . ? P2 O10 1.578(3) . ? P2 K1 3.7078(12) . ? P3 O37 1.505(3) . ? P3 O11 1.523(3) . ? P3 O34 1.547(3) . ? P3 O2 1.582(3) . ? P3 K1 3.6643(13) . ? K1 O12 2.473(3) . ? K1 O12 2.473(3) 2_655 ? K1 O11 2.501(3) . ? K1 O11 2.501(3) 2_655 ? K1 O33 2.642(3) 2_655 ? K1 O33 2.642(3) . ? K1 O32 2.697(3) 2_655 ? K1 O32 2.697(3) . ? K1 O15 2.763(5) . ? K1 P1 3.2670(15) 2_655 ? O4 Mo9 2.038(3) 2_655 ? O15 Mo3 1.8916(8) 2_655 ? O20 Mo7 2.077(3) 2_655 ? O23 Mo7 1.938(3) 2_655 ? O24 Mo7 2.294(3) 2_655 ? O33 Mo9 2.229(3) 2_655 ? O34 Mo9 2.015(3) 2_655 ? N1 C3 1.473(7) . ? N1 C4 1.495(6) . ? N1 H1A 0.9000 . ? N1 H1E 0.9000 . ? N2 C2 1.491(7) . ? N2 C5 1.496(7) . ? N2 H2A 0.9000 . ? N2 H2C 0.9000 . ? N3 C9 1.493(7) . ? N3 C8 1.494(8) . ? N3 H3C 0.9000 . ? N3 H3D 0.9000 . ? N4 C11 1.487(7) . ? N4 C10 1.490(7) . ? N4 H4B 0.9000 . ? N4 H4C 0.9000 . ? N5 C15 1.484(6) . ? N5 C14 1.496(6) . ? N5 H5A 0.9000 . ? N5 H5D 0.9000 . ? C1 C2 1.514(8) . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C2 C3 1.504(7) . ? C2 H2B 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.514(7) . ? C4 C6 1.515(7) . ? C4 H4A 0.9800 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.498(11) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C11 1.507(8) . ? C8 H8A 0.9800 . ? C9 C10 1.494(9) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C12 1.521(8) . ? C10 H10A 0.9800 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.518(7) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.512(7) 5_656 ? C14 H14A 0.9800 . ? C15 C14 1.512(7) 5_656 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? O1W H1WA 0.8600 . ? O1W H1WB 0.8600 . ? O2W H2WA 0.8500 . ? O3W H3WA 0.8600 . ? O3W H3WB 0.8601 . ? O4W H4WA 0.8601 . ? O6W H6WA 0.8591 . ? O6W H6WB 0.9739 . ? O7W O7W 1.07(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mo1 O4 104.23(16) . . ? O5 Mo1 O6 101.18(17) . . ? O4 Mo1 O6 99.94(15) . . ? O5 Mo1 O1 98.56(15) . . ? O4 Mo1 O1 152.52(14) . . ? O6 Mo1 O1 90.37(14) . . ? O5 Mo1 O2 97.74(16) . . ? O4 Mo1 O2 87.47(13) . . ? O6 Mo1 O2 157.23(14) . . ? O1 Mo1 O2 74.29(12) . . ? O5 Mo1 O3 171.04(14) . . ? O4 Mo1 O3 84.59(13) . . ? O6 Mo1 O3 75.35(13) . . ? O1 Mo1 O3 73.40(12) . . ? O2 Mo1 O3 84.05(12) . . ? O7 Mo2 O9 104.66(16) . . ? O7 Mo2 O8 101.64(15) . . ? O9 Mo2 O8 99.25(15) . . ? O7 Mo2 O1 100.01(15) . . ? O9 Mo2 O1 150.69(13) . . ? O8 Mo2 O1 90.92(14) . . ? O7 Mo2 O10 98.78(14) . . ? O9 Mo2 O10 87.03(13) . . ? O8 Mo2 O10 156.28(13) . . ? O1 Mo2 O10 73.67(12) . . ? O7 Mo2 O3 170.98(14) . . ? O9 Mo2 O3 84.13(13) . . ? O8 Mo2 O3 74.58(12) . . ? O1 Mo2 O3 72.12(12) . . ? O10 Mo2 O3 83.43(11) . . ? O14 Mo3 O13 102.07(17) . . ? O14 Mo3 O15 100.64(14) . . ? O13 Mo3 O15 99.54(14) . . ? O14 Mo3 O17 95.60(15) . . ? O13 Mo3 O17 96.63(14) . . ? O15 Mo3 O17 154.08(17) . . ? O14 Mo3 O11 93.23(14) . . ? O13 Mo3 O11 164.69(14) . . ? O15 Mo3 O11 76.80(13) . . ? O17 Mo3 O11 82.27(12) . . ? O14 Mo3 O12 167.85(14) . . ? O13 Mo3 O12 89.95(14) . . ? O15 Mo3 O12 78.87(13) . . ? O17 Mo3 O12 81.03(12) . . ? O11 Mo3 O12 74.78(11) . . ? O14 Mo3 K1 127.66(11) . . ? O13 Mo3 K1 122.56(12) . . ? O15 Mo3 K1 50.01(14) . . ? O17 Mo3 K1 104.10(9) . . ? O11 Mo3 K1 44.08(8) . . ? O12 Mo3 K1 43.44(8) . . ? O18 Mo4 O16 102.57(17) . . ? O18 Mo4 O17 105.78(16) . . ? O16 Mo4 O17 105.49(16) . . ? O18 Mo4 O1 97.00(16) . . ? O16 Mo4 O1 97.14(15) . . ? O17 Mo4 O1 143.13(13) . . ? O18 Mo4 O10 164.65(15) . . ? O16 Mo4 O10 86.61(14) . . ? O17 Mo4 O10 83.12(13) . . ? O1 Mo4 O10 69.38(12) . . ? O18 Mo4 O2 86.20(14) . . ? O16 Mo4 O2 164.51(14) . . ? O17 Mo4 O2 83.92(13) . . ? O1 Mo4 O2 68.86(12) . . ? O10 Mo4 O2 82.28(11) . . ? O19 Mo5 O21 105.04(17) . . ? O19 Mo5 O20 105.19(16) . . ? O21 Mo5 O20 97.05(16) . . ? O19 Mo5 O8 93.58(15) . . ? O21 Mo5 O8 90.31(14) . . ? O20 Mo5 O8 157.18(14) . . ? O19 Mo5 O6 93.12(16) . . ? O21 Mo5 O6 157.66(14) . . ? O20 Mo5 O6 90.45(15) . . ? O8 Mo5 O6 75.43(13) . . ? O19 Mo5 O3 160.81(16) . . ? O21 Mo5 O3 88.11(13) . . ? O20 Mo5 O3 86.57(13) . . ? O8 Mo5 O3 72.06(12) . . ? O6 Mo5 O3 71.31(12) . . ? O22 Mo6 O26 101.20(17) . . ? O22 Mo6 O25 101.33(15) . . ? O26 Mo6 O25 92.81(14) . . ? O22 Mo6 O23 99.55(16) . . ? O26 Mo6 O23 92.48(14) . . ? O25 Mo6 O23 157.01(14) . . ? O22 Mo6 O21 90.82(16) . . ? O26 Mo6 O21 167.83(13) . . ? O25 Mo6 O21 86.63(13) . . ? O23 Mo6 O21 83.55(14) . . ? O22 Mo6 O24 168.48(16) . . ? O26 Mo6 O24 88.11(13) . . ? O25 Mo6 O24 84.80(13) . . ? O23 Mo6 O24 73.03(13) . . ? O21 Mo6 O24 79.73(12) . . ? O27 Mo7 O28 101.99(16) . . ? O27 Mo7 O26 99.49(16) . . ? O28 Mo7 O26 90.96(14) . . ? O27 Mo7 O23 100.19(16) . 2_655 ? O28 Mo7 O23 156.79(14) . 2_655 ? O26 Mo7 O23 92.04(14) . 2_655 ? O27 Mo7 O20 93.94(16) . 2_655 ? O28 Mo7 O20 88.88(14) . 2_655 ? O26 Mo7 O20 166.30(14) . 2_655 ? O23 Mo7 O20 82.88(14) 2_655 2_655 ? O27 Mo7 O24 169.63(14) . 2_655 ? O28 Mo7 O24 85.07(13) . 2_655 ? O26 Mo7 O24 87.86(13) . 2_655 ? O23 Mo7 O24 72.06(12) 2_655 2_655 ? O20 Mo7 O24 78.47(12) 2_655 2_655 ? O30 Mo8 O31 99.36(15) . . ? O30 Mo8 O25 100.09(15) . . ? O31 Mo8 O25 92.89(14) . . ? O30 Mo8 O29 96.93(14) . . ? O31 Mo8 O29 93.04(13) . . ? O25 Mo8 O29 160.80(13) . . ? O30 Mo8 O9 93.36(15) . . ? O31 Mo8 O9 166.82(13) . . ? O25 Mo8 O9 88.27(13) . . ? O29 Mo8 O9 81.91(12) . . ? O30 Mo8 O32 174.44(14) . . ? O31 Mo8 O32 83.86(13) . . ? O25 Mo8 O32 84.20(13) . . ? O29 Mo8 O32 78.31(12) . . ? O9 Mo8 O32 83.19(12) . . ? O35 Mo9 O31 98.39(15) . . ? O35 Mo9 O28 100.11(15) . . ? O31 Mo9 O28 93.31(14) . . ? O35 Mo9 O34 98.01(15) . 2_655 ? O31 Mo9 O34 92.68(13) . 2_655 ? O28 Mo9 O34 159.86(13) . 2_655 ? O35 Mo9 O4 93.34(15) . 2_655 ? O31 Mo9 O4 167.67(13) . 2_655 ? O28 Mo9 O4 88.33(13) . 2_655 ? O34 Mo9 O4 81.89(13) 2_655 2_655 ? O35 Mo9 O33 173.81(14) . 2_655 ? O31 Mo9 O33 85.62(13) . 2_655 ? O28 Mo9 O33 84.28(13) . 2_655 ? O34 Mo9 O33 77.02(12) 2_655 2_655 ? O4 Mo9 O33 82.38(12) 2_655 2_655 ? O32 P1 O33 107.59(18) . . ? O32 P1 O24 111.59(18) . . ? O33 P1 O24 111.27(18) . . ? O32 P1 O3 109.80(18) . . ? O33 P1 O3 110.51(18) . . ? O24 P1 O3 106.09(18) . . ? O32 P1 K1 54.87(12) . . ? O33 P1 K1 52.83(12) . . ? O24 P1 K1 125.37(13) . . ? O3 P1 K1 128.53(13) . . ? O36 P2 O12 112.13(18) . . ? O36 P2 O29 108.20(18) . . ? O12 P2 O29 109.74(18) . . ? O36 P2 O10 110.85(18) . . ? O12 P2 O10 107.49(17) . . ? O29 P2 O10 108.38(17) . . ? O36 P2 K1 139.49(13) . . ? O12 P2 K1 28.39(12) . . ? O29 P2 K1 89.41(12) . . ? O10 P2 K1 96.72(12) . . ? O37 P3 O11 113.58(19) . . ? O37 P3 O34 107.71(19) . . ? O11 P3 O34 108.63(18) . . ? O37 P3 O2 110.58(18) . . ? O11 P3 O2 106.41(18) . . ? O34 P3 O2 109.90(18) . . ? O37 P3 K1 143.77(15) . . ? O11 P3 K1 31.73(12) . . ? O34 P3 K1 85.56(13) . . ? O2 P3 K1 95.19(13) . . ? O12 K1 O12 121.78(15) . 2_655 ? O12 K1 O11 67.23(10) . . ? O12 K1 O11 83.26(10) 2_655 . ? O12 K1 O11 83.26(10) . 2_655 ? O12 K1 O11 67.23(10) 2_655 2_655 ? O11 K1 O11 117.55(15) . 2_655 ? O12 K1 O33 117.15(10) . 2_655 ? O12 K1 O33 101.94(10) 2_655 2_655 ? O11 K1 O33 168.24(11) . 2_655 ? O11 K1 O33 74.20(10) 2_655 2_655 ? O12 K1 O33 101.94(10) . . ? O12 K1 O33 117.15(10) 2_655 . ? O11 K1 O33 74.20(10) . . ? O11 K1 O33 168.24(11) 2_655 . ? O33 K1 O33 94.06(14) 2_655 . ? O12 K1 O32 167.10(11) . 2_655 ? O12 K1 O32 71.06(10) 2_655 2_655 ? O11 K1 O32 118.79(10) . 2_655 ? O11 K1 O32 102.19(10) 2_655 2_655 ? O33 K1 O32 54.62(10) 2_655 2_655 ? O33 K1 O32 70.62(10) . 2_655 ? O12 K1 O32 71.06(10) . . ? O12 K1 O32 167.10(11) 2_655 . ? O11 K1 O32 102.19(10) . . ? O11 K1 O32 118.79(10) 2_655 . ? O33 K1 O32 70.62(10) 2_655 . ? O33 K1 O32 54.62(10) . . ? O32 K1 O32 96.15(14) 2_655 . ? O12 K1 O15 60.89(8) . . ? O12 K1 O15 60.89(8) 2_655 . ? O11 K1 O15 58.77(8) . . ? O11 K1 O15 58.77(8) 2_655 . ? O33 K1 O15 132.97(7) 2_655 . ? O33 K1 O15 132.97(7) . . ? O32 K1 O15 131.92(7) 2_655 . ? O32 K1 O15 131.92(7) . . ? O12 K1 P1 87.06(7) . . ? O12 K1 P1 143.33(8) 2_655 . ? O11 K1 P1 88.95(7) . . ? O11 K1 P1 144.91(8) 2_655 . ? O33 K1 P1 80.58(8) 2_655 . ? O33 K1 P1 27.36(7) . . ? O32 K1 P1 81.81(8) 2_655 . ? O32 K1 P1 27.30(7) . . ? O15 K1 P1 140.50(3) . . ? O12 K1 P1 143.33(8) . 2_655 ? O12 K1 P1 87.06(7) 2_655 2_655 ? O11 K1 P1 144.91(8) . 2_655 ? O11 K1 P1 88.95(7) 2_655 2_655 ? O33 K1 P1 27.36(7) 2_655 2_655 ? O33 K1 P1 80.58(8) . 2_655 ? O32 K1 P1 27.30(7) 2_655 2_655 ? O32 K1 P1 81.81(8) . 2_655 ? O15 K1 P1 140.50(3) . 2_655 ? P1 K1 P1 79.01(5) . 2_655 ? O12 K1 Mo3 39.28(7) . . ? O12 K1 Mo3 86.88(8) 2_655 . ? O11 K1 Mo3 38.90(7) . . ? O11 K1 Mo3 84.00(8) 2_655 . ? O33 K1 Mo3 150.72(7) 2_655 . ? O33 K1 Mo3 106.76(7) . . ? O32 K1 Mo3 152.01(7) 2_655 . ? O32 K1 Mo3 104.75(7) . . ? O15 K1 Mo3 31.642(14) . . ? P1 K1 Mo3 108.86(2) . . ? P1 K1 Mo3 172.08(3) 2_655 . ? Mo2 O1 Mo4 109.94(14) . . ? Mo2 O1 Mo1 118.12(16) . . ? Mo4 O1 Mo1 110.57(14) . . ? P3 O2 Mo1 134.38(19) . . ? P3 O2 Mo4 123.17(18) . . ? Mo1 O2 Mo4 99.19(12) . . ? P1 O3 Mo5 121.23(17) . . ? P1 O3 Mo1 126.02(17) . . ? Mo5 O3 Mo1 91.24(11) . . ? P1 O3 Mo2 125.64(18) . . ? Mo5 O3 Mo2 89.53(10) . . ? Mo1 O3 Mo2 92.93(11) . . ? Mo1 O4 Mo9 148.29(19) . 2_655 ? Mo1 O6 Mo5 121.07(17) . . ? Mo2 O8 Mo5 122.61(16) . . ? Mo2 O9 Mo8 147.58(18) . . ? P2 O10 Mo2 135.86(19) . . ? P2 O10 Mo4 122.56(17) . . ? Mo2 O10 Mo4 99.21(12) . . ? P3 O11 Mo3 126.67(17) . . ? P3 O11 K1 129.59(18) . . ? Mo3 O11 K1 97.01(12) . . ? P2 O12 Mo3 122.47(17) . . ? P2 O12 K1 134.53(18) . . ? Mo3 O12 K1 97.27(11) . . ? Mo3 O15 Mo3 163.3(3) . 2_655 ? Mo3 O15 K1 98.35(14) . . ? Mo3 O15 K1 98.35(14) 2_655 . ? Mo4 O17 Mo3 157.99(19) . . ? Mo5 O20 Mo7 140.27(19) . 2_655 ? Mo5 O21 Mo6 137.12(17) . . ? Mo6 O23 Mo7 120.00(17) . 2_655 ? P1 O24 Mo6 129.51(18) . . ? P1 O24 Mo7 128.09(18) . 2_655 ? Mo6 O24 Mo7 94.82(12) . 2_655 ? Mo8 O25 Mo6 159.42(19) . . ? Mo6 O26 Mo7 170.0(2) . . ? Mo7 O28 Mo9 159.24(19) . . ? P2 O29 Mo8 137.37(19) . . ? Mo8 O31 Mo9 168.91(19) . . ? P1 O32 Mo8 129.87(18) . . ? P1 O32 K1 97.83(15) . . ? Mo8 O32 K1 132.04(13) . . ? P1 O33 Mo9 129.40(18) . 2_655 ? P1 O33 K1 99.81(15) . . ? Mo9 O33 K1 130.69(13) 2_655 . ? P3 O34 Mo9 138.08(19) . 2_655 ? C3 N1 C4 112.6(4) . . ? C3 N1 H1A 109.1 . . ? C4 N1 H1A 109.1 . . ? C3 N1 H1E 109.1 . . ? C4 N1 H1E 109.1 . . ? H1A N1 H1E 107.8 . . ? C2 N2 C5 112.6(4) . . ? C2 N2 H2A 109.1 . . ? C5 N2 H2A 109.1 . . ? C2 N2 H2C 109.1 . . ? C5 N2 H2C 109.1 . . ? H2A N2 H2C 107.8 . . ? C9 N3 C8 113.1(5) . . ? C9 N3 H3C 109.0 . . ? C8 N3 H3C 109.0 . . ? C9 N3 H3D 109.0 . . ? C8 N3 H3D 109.0 . . ? H3C N3 H3D 107.8 . . ? C11 N4 C10 112.1(4) . . ? C11 N4 H4B 109.2 . . ? C10 N4 H4B 109.2 . . ? C11 N4 H4C 109.2 . . ? C10 N4 H4C 109.2 . . ? H4B N4 H4C 107.9 . . ? C15 N5 C14 111.4(4) . . ? C15 N5 H5A 109.3 . . ? C14 N5 H5A 109.3 . . ? C15 N5 H5D 109.3 . . ? C14 N5 H5D 109.3 . . ? H5A N5 H5D 108.0 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N2 C2 C3 109.0(4) . . ? N2 C2 C1 110.4(5) . . ? C3 C2 C1 110.8(5) . . ? N2 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? N1 C3 C2 111.7(4) . . ? N1 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? N1 C4 C5 109.1(4) . . ? N1 C4 C6 109.6(4) . . ? C5 C4 C6 111.7(4) . . ? N1 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? C6 C4 H4A 108.8 . . ? N2 C5 C4 110.7(4) . . ? N2 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? C4 C5 H5C 109.5 . . ? H5B C5 H5C 108.1 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C7 109.2(7) . . ? N3 C8 C11 109.2(5) . . ? C7 C8 C11 111.0(6) . . ? N3 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? C11 C8 H8A 109.1 . . ? N3 C9 C10 112.0(5) . . ? N3 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? N3 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? N4 C10 C9 109.1(5) . . ? N4 C10 C12 109.4(5) . . ? C9 C10 C12 112.2(6) . . ? N4 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C12 C10 H10A 108.7 . . ? N4 C11 C8 110.7(5) . . ? N4 C11 H11A 109.5 . . ? C8 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 C15 108.9(4) . 5_656 ? N5 C14 C13 111.1(4) . . ? C15 C14 C13 111.2(4) 5_656 . ? N5 C14 H14A 108.5 . . ? C15 C14 H14A 108.5 5_656 . ? C13 C14 H14A 108.5 . . ? N5 C15 C14 111.6(4) . 5_656 ? N5 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 5_656 . ? N5 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 5_656 . ? H15A C15 H15B 108.0 . . ? H1WA O1W H1WB 108.9 . . ? H3WA O3W H3WB 125.7 . . ? H6WA O6W H6WB 118.8 . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 3.309 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.137