# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Baibin Zhou' _publ_contact_author_email 'ZHOU BAI BIN@163.COM' _publ_section_title ; Inorganic-organic Hybrids Constructed from Heteropolymolybdate Anions and Copper-organic Fragments: Syntheses, Structures and ; loop_ _publ_author_name 'Baibin Zhou.' 'Hai-Juan Jin.' 'Zhan-Hua Su.' 'Zhi-Feng Zhao.' # Attachment '1.cif' data_jhj124_0m _database_code_depnum_ccdc_archive 'CCDC 720596' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 Cu Mo5 N8 O23 P2, C12 H13 Cu N8 O, 2(H2 O)' _chemical_formula_sum 'C24 H29 Cu2 Mo5 N16 O26 P2' _chemical_formula_weight 1626.37 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' Cu Cu 0.3201 1.2651 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.28680(10) _cell_length_b 10.7031(2) _cell_length_c 21.5105(3) _cell_angle_alpha 80.7130(10) _cell_angle_beta 84.3760(10) _cell_angle_gamma 84.7330(10) _cell_volume 2319.06(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5211 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 28.17 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 2.329 _exptl_crystal_density_diffrn 2.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1582.0 _exptl_absorpt_coefficient_mu 2.383 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.598 _exptl_absorpt_correction_T_max 0.683 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12697 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8191 _reflns_number_gt 6831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0357P)^2^+0.8134P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8191 _refine_ls_number_parameters 773 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 O1W O 0.9870(3) 0.6012(4) 0.28186(18) 0.0618(11) Uani 1 1 d . . . H1WA H 0.9305 0.5579 0.3052 0.074 Uiso 1 1 d R . . H1WB H 1.0659 0.5948 0.2913 0.074 Uiso 1 1 d R . . O2W O 0.1876(3) 0.3775(4) 0.18996(17) 0.0530(10) Uani 1 1 d . . . H2WA H 0.1994 0.3228 0.2226 0.064 Uiso 1 1 d R . . H2WB H 0.1189 0.3792 0.1707 0.064 Uiso 1 1 d R . . Mo1 Mo 0.37182(3) 0.78599(3) 0.267992(17) 0.02533(10) Uani 1 1 d . . . Mo2 Mo 0.67074(3) 0.78671(3) 0.187070(16) 0.02484(10) Uani 1 1 d . . . Mo3 Mo 0.77245(3) 0.48152(4) 0.168899(19) 0.03119(10) Uani 1 1 d . . . Mo4 Mo 0.57102(3) 0.28315(3) 0.263279(17) 0.02428(9) Uani 1 1 d . . . Mo5 Mo 0.34237(3) 0.45900(3) 0.346724(17) 0.02505(9) Uani 1 1 d . . . Cu1 Cu 0.82148(5) 0.96731(5) 0.04012(2) 0.02888(13) Uani 1 1 d . . . Cu2 Cu 0.17607(5) 0.01690(5) 0.44896(2) 0.02824(13) Uani 1 1 d . . . P1 P 0.63697(10) 0.56093(10) 0.31685(5) 0.0223(2) Uani 1 1 d . . . P2 P 0.43960(10) 0.55602(10) 0.18047(5) 0.0228(2) Uani 1 1 d . . . O3 O 0.4905(3) 0.8555(3) 0.19866(13) 0.0267(6) Uani 1 1 d . . . O4 O 0.4433(2) 0.4579(3) 0.24200(12) 0.0236(6) Uani 1 1 d . . . O5 O 0.5756(2) 0.6000(3) 0.15671(13) 0.0263(6) Uani 1 1 d . . . O6 O 0.5330(3) 0.5211(3) 0.36814(12) 0.0254(6) Uani 1 1 d . . . O7 O 0.7979(3) 0.6460(3) 0.19015(13) 0.0305(7) Uani 1 1 d . . . O8 O 0.5815(2) 0.6787(2) 0.27290(12) 0.0234(6) Uani 1 1 d . . . O9 O 0.3434(3) 0.6664(3) 0.19242(12) 0.0262(6) Uani 1 1 d . . . O10 O 0.4610(3) 0.3074(3) 0.34163(12) 0.0262(6) Uani 1 1 d . . . O11 O 0.6897(3) 0.4547(3) 0.27889(13) 0.0259(6) Uani 1 1 d . . . O12 O 0.6600(3) 0.3451(3) 0.18365(13) 0.0270(6) Uani 1 1 d . . . O13 O 0.6847(3) 0.8463(3) 0.10707(13) 0.0327(7) Uani 1 1 d . . . O14 O 0.3143(3) 0.6379(3) 0.32012(13) 0.0280(7) Uani 1 1 d . . . O15 O 0.7549(3) 0.6013(3) 0.34843(14) 0.0329(7) Uani 1 1 d . . . O16 O 0.4111(3) 0.8662(3) 0.32476(14) 0.0377(8) Uani 1 1 d . . . O17 O 0.2303(3) 0.8686(3) 0.24494(15) 0.0410(8) Uani 1 1 d . . . O18 O 0.2982(3) 0.4419(3) 0.42537(14) 0.0362(7) Uani 1 1 d . . . O19 O 0.7511(3) 0.8837(3) 0.22137(14) 0.0369(7) Uani 1 1 d . . . O20 O 0.3926(3) 0.4871(3) 0.12829(13) 0.0329(7) Uani 1 1 d . . . O21 O 0.6939(3) 0.1877(3) 0.30122(14) 0.0357(7) Uani 1 1 d . . . O22 O 0.3288(3) 0.0846(3) 0.36944(15) 0.0413(8) Uani 1 1 d . . . H22 H 0.2919 0.1189 0.3383 0.062 Uiso 1 1 calc R . . O23 O 0.4792(3) 0.1810(3) 0.23892(14) 0.0381(8) Uani 1 1 d . . . N1 N 0.9709(3) 0.8279(4) 0.05494(16) 0.0305(8) Uani 1 1 d . . . N2 N 0.6881(3) 1.1185(4) 0.02122(17) 0.0320(9) Uani 1 1 d . . . O24 O 0.2095(3) 0.4117(3) 0.31669(14) 0.0365(8) Uani 1 1 d . . . N3 N 0.9047(3) 1.0349(3) 0.10539(17) 0.0307(8) Uani 1 1 d . . . O25 O 0.8001(3) 0.4999(4) 0.08938(16) 0.0523(10) Uani 1 1 d . . . O26 O 0.9154(3) 0.4061(3) 0.19517(18) 0.0478(9) Uani 1 1 d . . . N4 N 0.7559(3) 0.9175(3) -0.03599(16) 0.0298(8) Uani 1 1 d . . . N5 N 0.0501(3) 0.1722(4) 0.43325(17) 0.0329(9) Uani 1 1 d . . . N6 N 0.2792(3) -0.1482(3) 0.47792(16) 0.0298(8) Uani 1 1 d . . . N7 N 0.2699(3) 0.0760(3) 0.51514(16) 0.0303(8) Uani 1 1 d . . . N8 N 0.0579(3) -0.0502(4) 0.39410(17) 0.0324(9) Uani 1 1 d . . . N9 N 0.4077(4) -0.2530(4) 0.54842(18) 0.0349(9) Uani 1 1 d . . . N10 N -0.1075(4) -0.0060(4) 0.33531(19) 0.0370(10) Uani 1 1 d . . . N11 N 0.5353(4) 1.2063(4) -0.0392(2) 0.0402(11) Uani 1 1 d . . . N12 N 1.0393(4) 0.9977(4) 0.18042(19) 0.0368(10) Uani 1 1 d . . . N13 N 1.1241(4) 0.7437(4) 0.1166(2) 0.0382(10) Uani 1 1 d . . . N14 N 0.6250(4) 0.9697(4) -0.11234(18) 0.0346(9) Uani 1 1 d . . . N15 N 0.4169(4) 0.0280(4) 0.58447(19) 0.0380(10) Uani 1 1 d . . . C1 C 0.9971(4) 0.9550(4) 0.1320(2) 0.0294(10) Uani 1 1 d . . . C2 C 0.6657(4) 1.0036(4) -0.0612(2) 0.0293(10) Uani 1 1 d . . . C3 C 0.3477(4) -0.1407(4) 0.52649(19) 0.0280(10) Uani 1 1 d . . . C4 C 1.0343(4) 0.8417(4) 0.1038(2) 0.0317(10) Uani 1 1 d . . . C5 C 0.3788(5) -0.3376(5) 0.5114(2) 0.0383(11) Uani 1 1 d . . . C6 C 0.3833(5) 0.1559(5) 0.5807(2) 0.0417(12) Uani 1 1 d . . . C7 C 0.6277(4) 1.1104(4) -0.0292(2) 0.0299(10) Uani 1 1 d . . . C8 C -0.0325(4) 0.0384(4) 0.3723(2) 0.0312(10) Uani 1 1 d . . . C9 C 0.3472(4) -0.0170(4) 0.54469(19) 0.0291(10) Uani 1 1 d . . . C10 C -0.0654(5) -0.1299(5) 0.3326(2) 0.0391(12) Uani 1 1 d . . . N16 N -0.1078(4) 0.2702(4) 0.3775(2) 0.0403(10) Uani 1 1 d . . . C11 C -0.0345(4) 0.1608(4) 0.3925(2) 0.0324(10) Uani 1 1 d . . . C12 C 0.6927(5) 0.8563(5) -0.1217(2) 0.0382(11) Uani 1 1 d . . . C13 C 0.8885(5) 1.1337(5) 0.1396(2) 0.0389(12) Uani 1 1 d . . . C14 C 0.2994(5) -0.2723(5) 0.4680(2) 0.0355(11) Uani 1 1 d . . . C15 C 0.7724(5) 0.8253(5) -0.0742(2) 0.0366(11) Uani 1 1 d . . . C16 C 0.9716(5) 1.1125(5) 0.1855(2) 0.0388(12) Uani 1 1 d . . . C17 C 0.5360(5) 1.2802(5) 0.0069(2) 0.0435(13) Uani 1 1 d . . . C18 C 0.2924(5) 0.1845(5) 0.5384(2) 0.0400(12) Uani 1 1 d . . . C19 C 0.0365(5) -0.1560(5) 0.3694(2) 0.0394(12) Uani 1 1 d . . . C20 C 1.0231(5) 0.7157(5) 0.0366(3) 0.0425(13) Uani 1 1 d . . . C21 C 0.0280(5) 0.2953(5) 0.4453(2) 0.0410(12) Uani 1 1 d . . . C22 C 0.6300(5) 1.2260(5) 0.0441(3) 0.0417(12) Uani 1 1 d . . . C23 C -0.0702(5) 0.3559(5) 0.4111(3) 0.0427(13) Uani 1 1 d . . . C24 C 1.1181(5) 0.6632(5) 0.0743(3) 0.0472(13) Uani 1 1 d . . . H1 H 0.983(4) 1.161(4) 0.219(2) 0.034(12) Uiso 1 1 d . . . H2 H -0.115(4) 0.438(5) 0.410(2) 0.041(13) Uiso 1 1 d . . . H3 H -0.104(4) -0.176(5) 0.308(2) 0.042(14) Uiso 1 1 d . . . H4 H 0.577(4) 1.025(4) -0.137(2) 0.027(12) Uiso 1 1 d . . . H5 H 0.680(4) 0.819(4) -0.156(2) 0.029(12) Uiso 1 1 d . . . H6 H 0.834(4) 1.204(4) 0.1316(19) 0.022(11) Uiso 1 1 d . . . H7 H 0.397(4) -0.431(4) 0.521(2) 0.030(11) Uiso 1 1 d . . . H8 H 0.081(4) -0.222(4) 0.3740(18) 0.014(11) Uiso 1 1 d . . . H9 H 1.165(4) 0.581(5) 0.074(2) 0.040(13) Uiso 1 1 d . . . H10 H 0.256(4) 0.264(4) 0.5216(18) 0.022(11) Uiso 1 1 d . . . H11 H 1.084(5) 0.961(5) 0.203(3) 0.052(18) Uiso 1 1 d . . . H12 H -0.162(5) 0.285(5) 0.351(2) 0.054(17) Uiso 1 1 d . . . H13 H 1.177(5) 0.735(5) 0.141(2) 0.041(15) Uiso 1 1 d . . . H14 H 0.482(5) 1.357(5) 0.004(2) 0.046(14) Uiso 1 1 d . . . H15 H 0.451(4) -0.273(4) 0.582(2) 0.036(13) Uiso 1 1 d . . . H16 H 0.086(4) 0.332(4) 0.4706(18) 0.019(10) Uiso 1 1 d . . . H17 H 0.490(4) 1.211(4) -0.063(2) 0.024(14) Uiso 1 1 d . . . H18 H 1.003(5) 0.681(5) 0.007(3) 0.059(18) Uiso 1 1 d . . . H19 H 0.658(4) 1.256(4) 0.078(2) 0.035(13) Uiso 1 1 d . . . H20 H 0.267(4) -0.305(4) 0.439(2) 0.039(14) Uiso 1 1 d . . . H21 H 0.830(4) 0.758(5) -0.066(2) 0.040(14) Uiso 1 1 d . . . H25 H 0.463(6) -0.011(6) 0.608(3) 0.07(2) Uiso 1 1 d . . . H23 H -0.167(4) 0.027(5) 0.322(2) 0.031(14) Uiso 1 1 d . . . H24 H 0.417(5) 0.207(5) 0.604(2) 0.053(16) Uiso 1 1 d . . . 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 O1W 0.0333(19) 0.079(3) 0.078(3) -0.024(2) -0.0116(19) -0.003(2) O2W 0.0326(18) 0.070(3) 0.060(2) -0.014(2) -0.0102(16) -0.0087(18) Mo1 0.02418(19) 0.02342(19) 0.02579(19) 0.00225(16) -0.00590(15) 0.00536(15) Mo2 0.02136(18) 0.0264(2) 0.02550(19) 0.00407(16) -0.00783(15) -0.00348(15) Mo3 0.02126(19) 0.0336(2) 0.0391(2) -0.00806(18) -0.00075(16) -0.00154(17) Mo4 0.02419(19) 0.02168(19) 0.0271(2) -0.00199(16) -0.00863(15) 0.00145(15) Mo5 0.02339(19) 0.0250(2) 0.02491(19) 0.00185(16) -0.00383(15) -0.00033(15) Cu1 0.0244(3) 0.0328(3) 0.0277(3) 0.0031(2) -0.0105(2) 0.0019(2) Cu2 0.0243(3) 0.0301(3) 0.0291(3) 0.0005(2) -0.0104(2) 0.0039(2) P1 0.0228(5) 0.0191(5) 0.0249(5) 0.0004(4) -0.0110(4) 0.0013(4) P2 0.0199(5) 0.0270(6) 0.0212(5) 0.0007(5) -0.0081(4) -0.0022(4) O3 0.0249(15) 0.0258(15) 0.0270(15) 0.0051(13) -0.0079(12) 0.0011(12) O4 0.0195(14) 0.0268(15) 0.0221(14) 0.0019(12) -0.0037(11) 0.0023(12) O5 0.0210(14) 0.0287(16) 0.0275(15) 0.0023(13) -0.0036(12) -0.0036(12) O6 0.0275(15) 0.0238(15) 0.0239(14) 0.0013(12) -0.0082(12) 0.0011(12) O7 0.0211(14) 0.0329(17) 0.0374(17) -0.0013(14) -0.0043(13) -0.0065(13) O8 0.0235(14) 0.0197(14) 0.0255(15) 0.0015(12) -0.0074(12) 0.0044(12) O9 0.0224(14) 0.0291(16) 0.0260(15) 0.0025(13) -0.0115(12) 0.0017(12) O10 0.0295(15) 0.0218(15) 0.0264(15) 0.0018(12) -0.0070(12) -0.0015(13) O11 0.0244(15) 0.0226(15) 0.0315(16) -0.0056(13) -0.0083(12) 0.0024(12) O12 0.0239(15) 0.0269(16) 0.0312(16) -0.0081(13) -0.0027(12) -0.0002(13) O13 0.0302(16) 0.0394(18) 0.0269(16) 0.0035(14) -0.0042(13) -0.0076(14) O14 0.0261(15) 0.0245(15) 0.0289(15) 0.0054(13) -0.0024(12) 0.0050(13) O15 0.0328(16) 0.0287(16) 0.0413(18) -0.0071(14) -0.0210(14) -0.0016(14) O16 0.0470(19) 0.0310(17) 0.0340(17) -0.0045(14) -0.0053(15) 0.0030(15) O17 0.0314(17) 0.0410(19) 0.0439(19) 0.0071(16) -0.0047(15) 0.0100(15) O18 0.0403(18) 0.0366(18) 0.0288(16) 0.0024(14) -0.0007(14) -0.0025(15) O19 0.0378(17) 0.0365(18) 0.0380(18) 0.0010(15) -0.0141(14) -0.0117(15) O20 0.0380(17) 0.0333(17) 0.0303(16) -0.0068(14) -0.0130(14) -0.0036(14) O21 0.0355(17) 0.0276(16) 0.0433(18) -0.0010(15) -0.0170(14) 0.0080(14) O22 0.049(2) 0.0364(19) 0.0359(18) 0.0018(16) 0.0002(15) -0.0049(16) O23 0.0445(19) 0.0347(18) 0.0383(18) -0.0088(15) -0.0077(15) -0.0101(15) N1 0.0244(18) 0.035(2) 0.031(2) -0.0001(17) -0.0102(16) 0.0030(17) N2 0.0276(19) 0.036(2) 0.032(2) 0.0009(17) -0.0132(16) 0.0004(17) O24 0.0243(15) 0.046(2) 0.0385(18) -0.0014(16) -0.0033(13) -0.0050(15) N3 0.0255(19) 0.031(2) 0.035(2) -0.0003(17) -0.0096(16) 0.0017(16) O25 0.048(2) 0.065(3) 0.046(2) -0.0137(19) 0.0118(17) -0.0182(19) O26 0.0225(16) 0.046(2) 0.078(3) -0.0205(19) -0.0095(16) 0.0061(15) N4 0.0258(18) 0.035(2) 0.0253(19) 0.0060(17) -0.0090(15) 0.0029(16) N5 0.0279(19) 0.031(2) 0.039(2) -0.0017(18) -0.0091(17) 0.0026(17) N6 0.0303(19) 0.033(2) 0.0249(19) 0.0015(16) -0.0102(16) 0.0015(17) N7 0.0296(19) 0.030(2) 0.032(2) -0.0058(17) -0.0089(16) 0.0029(17) N8 0.0277(19) 0.034(2) 0.034(2) -0.0015(18) -0.0066(16) 0.0020(17) N9 0.036(2) 0.039(2) 0.027(2) 0.0007(18) -0.0106(18) 0.0125(18) N10 0.026(2) 0.048(3) 0.036(2) 0.002(2) -0.0130(19) 0.001(2) N11 0.035(2) 0.047(3) 0.039(2) -0.002(2) -0.022(2) 0.006(2) N12 0.032(2) 0.046(3) 0.032(2) 0.001(2) -0.0139(19) 0.001(2) N13 0.030(2) 0.039(2) 0.042(2) 0.006(2) -0.018(2) 0.0032(19) N14 0.035(2) 0.038(2) 0.030(2) 0.0034(19) -0.0137(18) -0.0002(19) N15 0.033(2) 0.050(3) 0.032(2) -0.004(2) -0.0167(19) 0.003(2) C1 0.022(2) 0.034(3) 0.030(2) 0.005(2) -0.0078(18) -0.0026(19) C2 0.026(2) 0.034(3) 0.027(2) 0.004(2) -0.0074(18) -0.004(2) C3 0.019(2) 0.035(3) 0.027(2) 0.003(2) -0.0050(17) 0.0027(19) C4 0.023(2) 0.035(3) 0.035(2) 0.005(2) -0.0089(19) 0.000(2) C5 0.044(3) 0.032(3) 0.038(3) -0.004(2) -0.009(2) 0.009(2) C6 0.038(3) 0.042(3) 0.047(3) -0.010(3) -0.012(2) -0.001(2) C7 0.023(2) 0.031(2) 0.033(2) 0.004(2) -0.0063(19) 0.0006(19) C8 0.025(2) 0.041(3) 0.026(2) 0.001(2) -0.0064(19) 0.001(2) C9 0.022(2) 0.040(3) 0.024(2) 0.001(2) -0.0036(18) 0.000(2) C10 0.036(3) 0.039(3) 0.044(3) -0.004(2) -0.012(2) -0.006(2) N16 0.028(2) 0.044(3) 0.046(3) 0.005(2) -0.016(2) 0.0057(19) C11 0.023(2) 0.036(3) 0.034(2) 0.005(2) -0.0072(19) 0.005(2) C12 0.041(3) 0.043(3) 0.031(3) -0.006(2) -0.009(2) -0.002(2) C13 0.032(3) 0.036(3) 0.048(3) -0.005(2) -0.013(2) 0.008(2) C14 0.040(3) 0.033(3) 0.033(3) -0.003(2) -0.006(2) 0.000(2) C15 0.034(3) 0.039(3) 0.035(3) 0.000(2) -0.008(2) 0.004(2) C16 0.041(3) 0.042(3) 0.037(3) -0.010(2) -0.012(2) -0.001(2) C17 0.045(3) 0.037(3) 0.047(3) -0.006(3) -0.012(2) 0.012(2) C18 0.040(3) 0.039(3) 0.041(3) -0.002(2) -0.009(2) 0.000(2) C19 0.035(3) 0.038(3) 0.045(3) -0.003(2) -0.014(2) 0.005(2) C20 0.037(3) 0.042(3) 0.050(3) -0.010(3) -0.014(2) 0.005(2) C21 0.031(3) 0.044(3) 0.047(3) -0.005(3) -0.009(2) 0.004(2) C22 0.034(3) 0.046(3) 0.049(3) -0.016(3) -0.016(2) 0.002(2) C23 0.037(3) 0.030(3) 0.058(3) 0.004(3) -0.012(2) 0.006(2) C24 0.045(3) 0.036(3) 0.060(3) -0.004(3) -0.019(3) 0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? Mo1 O16 1.700(3) . ? Mo1 O17 1.706(3) . ? Mo1 O14 1.894(3) . ? Mo1 O3 1.929(3) . ? Mo1 O9 2.281(3) . ? Mo1 O8 2.352(3) . ? Mo2 O19 1.682(3) . ? Mo2 O13 1.733(3) . ? Mo2 O7 1.899(3) . ? Mo2 O3 1.939(3) . ? Mo2 O8 2.182(3) . ? Mo2 O5 2.506(3) . ? Mo3 O25 1.689(3) . ? Mo3 O26 1.712(3) . ? Mo3 O12 1.913(3) . ? Mo3 O7 1.935(3) . ? Mo3 O5 2.303(3) . ? Mo3 O11 2.416(3) . ? Mo4 O23 1.683(3) . ? Mo4 O21 1.733(3) . ? Mo4 O12 1.910(3) . ? Mo4 O10 1.975(3) . ? Mo4 O4 2.197(3) . ? Mo4 O11 2.380(3) . ? Mo5 O18 1.693(3) . ? Mo5 O24 1.717(3) . ? Mo5 O14 1.912(3) . ? Mo5 O10 1.950(3) . ? Mo5 O6 2.240(3) . ? Mo5 O4 2.388(3) . ? Cu1 N3 1.976(4) . ? Cu1 N4 1.996(4) . ? Cu1 N2 2.038(4) . ? Cu1 N1 2.052(3) . ? Cu1 O13 2.251(3) . ? Cu2 N7 2.008(3) . ? Cu2 N6 2.017(3) . ? Cu2 N5 2.017(4) . ? Cu2 N8 2.026(4) . ? Cu2 O22 2.281(3) . ? P1 O6 1.497(3) . ? P1 O11 1.534(3) . ? P1 O8 1.548(3) . ? P1 O15 1.572(3) . ? P2 O9 1.508(3) . ? P2 O5 1.531(3) . ? P2 O4 1.552(3) . ? P2 O20 1.574(3) . ? O22 H22 0.8200 . ? N1 C4 1.324(5) . ? N1 C20 1.371(6) . ? N2 C7 1.320(5) . ? N2 C22 1.387(6) . ? N3 C1 1.327(5) . ? N3 C13 1.371(6) . ? N4 C2 1.336(5) . ? N4 C15 1.373(6) . ? N5 C11 1.320(5) . ? N5 C21 1.377(6) . ? N6 C3 1.333(5) . ? N6 C14 1.373(6) . ? N7 C9 1.333(5) . ? N7 C18 1.382(6) . ? N8 C8 1.328(5) . ? N8 C19 1.369(6) . ? N9 C3 1.337(5) . ? N9 C5 1.368(6) . ? N9 H15 0.87(5) . ? N10 C8 1.327(6) . ? N10 C10 1.365(6) . ? N10 H23 0.73(4) . ? N11 C7 1.339(6) . ? N11 C17 1.365(6) . ? N11 H17 0.71(4) . ? N12 C1 1.328(6) . ? N12 C16 1.372(6) . ? N12 H11 0.75(5) . ? N13 C4 1.344(6) . ? N13 C24 1.361(7) . ? N13 H13 0.78(5) . ? N14 C2 1.328(5) . ? N14 C12 1.376(6) . ? N14 H4 0.87(4) . ? N15 C9 1.340(6) . ? N15 C6 1.372(7) . ? N15 H25 0.77(6) . ? C1 C4 1.446(6) . ? C2 C7 1.433(6) . ? C3 C9 1.439(6) . ? C5 C14 1.363(6) . ? C5 H7 0.99(4) . ? C6 C18 1.348(7) . ? C6 H24 0.91(5) . ? C8 C11 1.444(6) . ? C10 C19 1.357(7) . ? C10 H3 0.91(5) . ? N16 C11 1.345(6) . ? N16 C23 1.358(7) . ? N16 H12 0.82(5) . ? C12 C15 1.353(6) . ? C12 H5 0.92(4) . ? C13 C16 1.348(6) . ? C13 H6 0.90(4) . ? C14 H20 0.88(5) . ? C15 H21 0.90(5) . ? C16 H1 0.97(4) . ? C17 C22 1.346(7) . ? C17 H14 0.94(5) . ? C18 H10 0.93(4) . ? C19 H8 0.81(4) . ? C20 C24 1.355(7) . ? C20 H18 0.84(5) . ? C21 C23 1.361(6) . ? C21 H16 0.99(4) . ? C22 H19 0.93(4) . ? C23 H2 0.95(5) . ? C24 H9 0.97(5) . ? 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 H1WA O1W H1WB 120.0 . . ? H2WA O2W H2WB 120.0 . . ? O16 Mo1 O17 102.03(16) . . ? O16 Mo1 O14 99.27(14) . . ? O17 Mo1 O14 103.92(13) . . ? O16 Mo1 O3 99.45(14) . . ? O17 Mo1 O3 98.72(13) . . ? O14 Mo1 O3 146.74(12) . . ? O16 Mo1 O9 173.20(12) . . ? O17 Mo1 O9 84.64(13) . . ? O14 Mo1 O9 80.16(11) . . ? O3 Mo1 O9 78.03(11) . . ? O16 Mo1 O8 87.24(12) . . ? O17 Mo1 O8 165.90(12) . . ? O14 Mo1 O8 84.75(10) . . ? O3 Mo1 O8 69.00(10) . . ? O9 Mo1 O8 85.96(9) . . ? O19 Mo2 O13 105.28(14) . . ? O19 Mo2 O7 98.83(14) . . ? O13 Mo2 O7 100.95(13) . . ? O19 Mo2 O3 102.22(14) . . ? O13 Mo2 O3 93.18(12) . . ? O7 Mo2 O3 150.52(12) . . ? O19 Mo2 O8 98.10(13) . . ? O13 Mo2 O8 154.86(12) . . ? O7 Mo2 O8 84.17(11) . . ? O3 Mo2 O8 72.67(10) . . ? O19 Mo2 O5 165.44(12) . . ? O13 Mo2 O5 86.45(12) . . ? O7 Mo2 O5 70.00(10) . . ? O3 Mo2 O5 85.39(10) . . ? O8 Mo2 O5 72.07(9) . . ? O25 Mo3 O26 103.85(17) . . ? O25 Mo3 O12 100.75(14) . . ? O26 Mo3 O12 101.41(14) . . ? O25 Mo3 O7 104.40(15) . . ? O26 Mo3 O7 96.55(14) . . ? O12 Mo3 O7 144.44(12) . . ? O25 Mo3 O5 88.64(14) . . ? O26 Mo3 O5 166.18(14) . . ? O12 Mo3 O5 81.67(11) . . ? O7 Mo3 O5 74.27(10) . . ? O25 Mo3 O11 169.07(13) . . ? O26 Mo3 O11 85.83(14) . . ? O12 Mo3 O11 71.94(10) . . ? O7 Mo3 O11 79.12(11) . . ? O5 Mo3 O11 82.33(9) . . ? O23 Mo4 O21 104.72(15) . . ? O23 Mo4 O12 98.64(13) . . ? O21 Mo4 O12 102.16(13) . . ? O23 Mo4 O10 97.34(13) . . ? O21 Mo4 O10 95.19(13) . . ? O12 Mo4 O10 152.51(12) . . ? O23 Mo4 O4 98.75(13) . . ? O21 Mo4 O4 154.80(12) . . ? O12 Mo4 O4 82.97(10) . . ? O10 Mo4 O4 72.58(10) . . ? O23 Mo4 O11 168.51(13) . . ? O21 Mo4 O11 84.92(12) . . ? O12 Mo4 O11 72.84(11) . . ? O10 Mo4 O11 87.83(10) . . ? O4 Mo4 O11 72.94(9) . . ? O18 Mo5 O24 102.97(15) . . ? O18 Mo5 O14 103.32(14) . . ? O24 Mo5 O14 98.61(14) . . ? O18 Mo5 O10 100.96(13) . . ? O24 Mo5 O10 98.81(13) . . ? O14 Mo5 O10 145.94(11) . . ? O18 Mo5 O6 87.30(13) . . ? O24 Mo5 O6 169.62(12) . . ? O14 Mo5 O6 80.19(11) . . ? O10 Mo5 O6 77.46(11) . . ? O18 Mo5 O4 168.52(12) . . ? O24 Mo5 O4 84.18(12) . . ? O14 Mo5 O4 84.20(10) . . ? O10 Mo5 O4 68.76(10) . . ? O6 Mo5 O4 85.45(9) . . ? N3 Cu1 N4 170.56(15) . . ? N3 Cu1 N2 96.30(14) . . ? N4 Cu1 N2 82.23(14) . . ? N3 Cu1 N1 81.42(14) . . ? N4 Cu1 N1 99.08(14) . . ? N2 Cu1 N1 173.86(15) . . ? N3 Cu1 O13 96.62(13) . . ? N4 Cu1 O13 92.81(13) . . ? N2 Cu1 O13 95.91(13) . . ? N1 Cu1 O13 90.02(13) . . ? N7 Cu2 N6 82.02(14) . . ? N7 Cu2 N5 96.72(14) . . ? N6 Cu2 N5 169.77(14) . . ? N7 Cu2 N8 170.38(14) . . ? N6 Cu2 N8 97.89(15) . . ? N5 Cu2 N8 81.65(15) . . ? N7 Cu2 O22 93.18(13) . . ? N6 Cu2 O22 94.80(13) . . ? N5 Cu2 O22 95.41(14) . . ? N8 Cu2 O22 96.41(13) . . ? O6 P1 O11 113.29(16) . . ? O6 P1 O8 108.72(15) . . ? O11 P1 O8 110.84(15) . . ? O6 P1 O15 108.08(16) . . ? O11 P1 O15 107.78(16) . . ? O8 P1 O15 107.96(16) . . ? O9 P2 O5 111.45(16) . . ? O9 P2 O4 108.86(15) . . ? O5 P2 O4 111.82(15) . . ? O9 P2 O20 110.06(16) . . ? O5 P2 O20 107.40(16) . . ? O4 P2 O20 107.15(16) . . ? Mo1 O3 Mo2 121.93(13) . . ? P2 O4 Mo4 129.79(15) . . ? P2 O4 Mo5 132.93(15) . . ? Mo4 O4 Mo5 96.69(9) . . ? P2 O5 Mo3 126.26(16) . . ? P2 O5 Mo2 125.00(15) . . ? Mo3 O5 Mo2 90.19(9) . . ? P1 O6 Mo5 121.72(15) . . ? Mo2 O7 Mo3 125.51(14) . . ? P1 O8 Mo2 130.42(15) . . ? P1 O8 Mo1 132.88(15) . . ? Mo2 O8 Mo1 96.37(9) . . ? P2 O9 Mo1 120.94(14) . . ? Mo5 O10 Mo4 121.67(13) . . ? P1 O11 Mo4 125.49(15) . . ? P1 O11 Mo3 126.33(16) . . ? Mo4 O11 Mo3 90.07(9) . . ? Mo4 O12 Mo3 125.14(14) . . ? Mo2 O13 Cu1 136.73(15) . . ? Mo1 O14 Mo5 148.08(15) . . ? Cu2 O22 H22 109.5 . . ? C4 N1 C20 105.6(4) . . ? C4 N1 Cu1 111.2(3) . . ? C20 N1 Cu1 142.7(3) . . ? C7 N2 C22 105.8(4) . . ? C7 N2 Cu1 111.0(3) . . ? C22 N2 Cu1 143.0(3) . . ? C1 N3 C13 105.3(4) . . ? C1 N3 Cu1 113.5(3) . . ? C13 N3 Cu1 140.5(3) . . ? C2 N4 C15 105.6(4) . . ? C2 N4 Cu1 112.0(3) . . ? C15 N4 Cu1 142.4(3) . . ? C11 N5 C21 105.5(4) . . ? C11 N5 Cu2 112.4(3) . . ? C21 N5 Cu2 141.6(3) . . ? C3 N6 C14 105.5(4) . . ? C3 N6 Cu2 112.1(3) . . ? C14 N6 Cu2 142.3(3) . . ? C9 N7 C18 105.7(4) . . ? C9 N7 Cu2 112.1(3) . . ? C18 N7 Cu2 141.9(3) . . ? C8 N8 C19 105.3(4) . . ? C8 N8 Cu2 111.7(3) . . ? C19 N8 Cu2 143.0(3) . . ? C3 N9 C5 107.0(4) . . ? C3 N9 H15 128(3) . . ? C5 N9 H15 125(3) . . ? C8 N10 C10 108.1(4) . . ? C8 N10 H23 126(4) . . ? C10 N10 H23 125(4) . . ? C7 N11 C17 108.0(4) . . ? C7 N11 H17 124(4) . . ? C17 N11 H17 128(4) . . ? C1 N12 C16 107.3(4) . . ? C1 N12 H11 126(4) . . ? C16 N12 H11 127(4) . . ? C4 N13 C24 107.8(4) . . ? C4 N13 H13 129(4) . . ? C24 N13 H13 123(4) . . ? C2 N14 C12 107.7(4) . . ? C2 N14 H4 119(3) . . ? C12 N14 H4 132(3) . . ? C9 N15 C6 107.9(4) . . ? C9 N15 H25 127(5) . . ? C6 N15 H25 125(5) . . ? N3 C1 N12 111.4(4) . . ? N3 C1 C4 116.5(4) . . ? N12 C1 C4 132.1(4) . . ? N14 C2 N4 111.0(4) . . ? N14 C2 C7 131.8(4) . . ? N4 C2 C7 117.1(4) . . ? N6 C3 N9 111.6(4) . . ? N6 C3 C9 116.4(4) . . ? N9 C3 C9 132.0(4) . . ? N1 C4 N13 110.7(4) . . ? N1 C4 C1 116.4(4) . . ? N13 C4 C1 132.8(4) . . ? C14 C5 N9 106.8(4) . . ? C14 C5 H7 127(2) . . ? N9 C5 H7 125(2) . . ? C18 C6 N15 106.4(5) . . ? C18 C6 H24 130(3) . . ? N15 C6 H24 124(3) . . ? N2 C7 N11 110.6(4) . . ? N2 C7 C2 117.6(4) . . ? N11 C7 C2 131.7(4) . . ? N10 C8 N8 111.1(4) . . ? N10 C8 C11 131.8(4) . . ? N8 C8 C11 117.1(4) . . ? N7 C9 N15 110.6(4) . . ? N7 C9 C3 117.0(4) . . ? N15 C9 C3 132.3(4) . . ? C19 C10 N10 105.7(5) . . ? C19 C10 H3 134(3) . . ? N10 C10 H3 121(3) . . ? C11 N16 C23 107.5(4) . . ? C11 N16 H12 127(4) . . ? C23 N16 H12 126(4) . . ? N5 C11 N16 111.2(4) . . ? N5 C11 C8 116.7(4) . . ? N16 C11 C8 132.0(4) . . ? C15 C12 N14 106.2(4) . . ? C15 C12 H5 133(3) . . ? N14 C12 H5 121(3) . . ? C16 C13 N3 109.6(4) . . ? C16 C13 H6 125(3) . . ? N3 C13 H6 126(3) . . ? C5 C14 N6 109.1(4) . . ? C5 C14 H20 125(3) . . ? N6 C14 H20 126(3) . . ? C12 C15 N4 109.5(4) . . ? C12 C15 H21 131(3) . . ? N4 C15 H21 120(3) . . ? C13 C16 N12 106.3(5) . . ? C13 C16 H1 131(3) . . ? N12 C16 H1 123(3) . . ? C22 C17 N11 106.3(5) . . ? C22 C17 H14 135(3) . . ? N11 C17 H14 118(3) . . ? C6 C18 N7 109.5(5) . . ? C6 C18 H10 129(3) . . ? N7 C18 H10 122(2) . . ? C10 C19 N8 109.8(5) . . ? C10 C19 H8 125(3) . . ? N8 C19 H8 125(3) . . ? C24 C20 N1 109.8(5) . . ? C24 C20 H18 122(4) . . ? N1 C20 H18 128(4) . . ? C23 C21 N5 109.3(5) . . ? C23 C21 H16 128(2) . . ? N5 C21 H16 122(2) . . ? C17 C22 N2 109.2(4) . . ? C17 C22 H19 128(3) . . ? N2 C22 H19 123(3) . . ? N16 C23 C21 106.4(5) . . ? N16 C23 H2 121(3) . . ? C21 C23 H2 132(3) . . ? C20 C24 N13 106.1(5) . . ? C20 C24 H9 127(3) . . ? N13 C24 H9 127(3) . . ? 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 N10 H23 O21 0.73(4) 2.16(5) 2.834(5) 155(5) 1_455 N15 H25 O22 0.77(6) 2.28(6) 2.970(5) 149(6) 2_656 N11 H17 O13 0.71(4) 2.29(4) 2.952(5) 155(5) 2_675 N9 H15 O10 0.87(5) 1.92(5) 2.792(5) 176(4) 2_656 N13 H13 O9 0.78(5) 2.14(5) 2.894(5) 163(5) 1_655 N16 H12 O11 0.82(5) 2.66(5) 3.391(5) 148(5) 1_455 N16 H12 O21 0.82(5) 2.32(5) 3.015(5) 143(5) 1_455 N12 H11 O17 0.75(5) 1.93(5) 2.667(5) 166(6) 1_655 N14 H4 O3 0.87(4) 1.84(5) 2.695(5) 168(4) 2_675 O2W H2WB O26 0.85 2.11 2.782(4) 135.2 1_455 O2W H2WA O24 0.85 2.39 2.841(5) 114.2 . O1W H1WB O24 0.85 2.37 2.985(5) 129.9 1_655 O1W H1WA O15 0.85 2.00 2.661(5) 133.9 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.514 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.099 # Attachment '2.cif' data_jhj1135_0m _database_code_depnum_ccdc_archive 'CCDC 720597' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C18 H20 Cu2 Mo5 N12 O25 P2), C12 H12 Cu N8, 20(H2 O) ; _chemical_formula_sum 'C48 H92 Cu5 Mo10 N32 O70 P4' _chemical_formula_weight 3638.57 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' Cu Cu 0.3201 1.2651 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9385(4) _cell_length_b 12.8328(4) _cell_length_c 19.2691(6) _cell_angle_alpha 78.6160(10) _cell_angle_beta 77.8130(10) _cell_angle_gamma 71.08 _cell_volume 2703.03(15) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9633 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 2.235 _exptl_crystal_density_diffrn 2.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1789.0 _exptl_absorpt_coefficient_mu 2.259 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.537 _exptl_absorpt_correction_T_max 0.608 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19686 _diffrn_reflns_av_R_equivalents 0.0156 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.30 _reflns_number_total 13435 _reflns_number_gt 11101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0401P)^2^+3.8466P] 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 13435 _refine_ls_number_parameters 797 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 O10W O 0.1113(3) 0.5875(3) 0.42481(17) 0.0565(8) Uani 1 1 d . . . H10A H 0.1682 0.6140 0.4036 0.068 Uiso 1 1 d R . . H10B H 0.0419 0.6311 0.4369 0.068 Uiso 1 1 d R . . O1W O 0.9843(4) 0.0926(4) 0.9069(2) 0.0959(15) Uani 1 1 d . . . H1WA H 0.9624 0.0378 0.9315 0.115 Uiso 1 1 d R . . H1WB H 1.0537 0.0971 0.9071 0.115 Uiso 1 1 d R . . O2W O 0.7940(4) 0.8733(4) 0.1757(2) 0.0959(14) Uani 1 1 d . . . H2WA H 0.8613 0.8714 0.1848 0.115 Uiso 1 1 d R . . H2WB H 0.7565 0.9282 0.1483 0.115 Uiso 1 1 d R . . O3W O 0.5126(4) 0.8241(4) 0.5984(3) 0.0909(14) Uani 1 1 d . . . H3WA H 0.5471 0.8590 0.5626 0.109 Uiso 1 1 d R . . H3WB H 0.4950 0.8466 0.6391 0.109 Uiso 1 1 d R . . O4W O 0.4321(4) 0.7128(4) 0.0283(2) 0.0892(13) Uani 1 1 d . . . H4WA H 0.4771 0.7486 0.0345 0.107 Uiso 1 1 d R . . H4WB H 0.3997 0.7304 -0.0093 0.107 Uiso 1 1 d R . . O5W O 0.7360(4) 0.1010(4) 0.0304(2) 0.0919(14) Uani 1 1 d . . . H5WA H 0.6984 0.0805 0.0707 0.110 Uiso 1 1 d R . . H5WB H 0.7402 0.0710 -0.0060 0.110 Uiso 1 1 d R . . O6W O 0.8615(4) 0.6591(4) 0.4608(2) 0.0809(12) Uani 1 1 d . . . H6WA H 0.8669 0.7045 0.4226 0.097 Uiso 1 1 d R . . H6WB H 0.8939 0.6607 0.4957 0.097 Uiso 1 1 d R . . O7W O 0.2922(4) 0.3476(3) 0.4166(2) 0.0754(11) Uani 1 1 d . . . H7WA H 0.3598 0.3553 0.3957 0.091 Uiso 1 1 d R . . H7WB H 0.2324 0.4045 0.4236 0.091 Uiso 1 1 d R . . O8W O 0.5421(4) 1.0030(4) 0.0623(2) 0.0800(12) Uani 1 1 d . . . H8WA H 0.5154 1.0667 0.0762 0.096 Uiso 1 1 d R . . H8WB H 0.5741 0.9968 0.0190 0.096 Uiso 1 1 d R . . O9W O 0.3109(4) 0.5662(3) 0.51360(19) 0.0710(10) Uani 1 1 d . . . H9WA H 0.2461 0.5701 0.5002 0.085 Uiso 1 1 d R . . H9WB H 0.3241 0.5353 0.5555 0.085 Uiso 1 1 d R . . C1 C -0.0618(4) 1.4343(4) 0.3739(2) 0.0497(11) Uani 1 1 d . . . H1 H -0.1142 1.4694 0.4112 0.060 Uiso 1 1 calc R . . C2 C -0.2399(4) 1.1687(4) 0.2000(3) 0.0518(11) Uani 1 1 d . . . H2 H -0.3099 1.1486 0.2174 0.062 Uiso 1 1 calc R . . C3 C 0.1527(4) 1.2093(4) -0.0229(2) 0.0466(10) Uani 1 1 d . . . H3 H 0.1943 1.2016 -0.0691 0.056 Uiso 1 1 calc R . . C4 C 0.1292(4) 1.0972(4) 0.6743(2) 0.0458(10) Uani 1 1 d . . . H4 H 0.1311 1.1472 0.7027 0.055 Uiso 1 1 calc R . . C5 C 0.3367(4) 1.2787(4) 0.1614(3) 0.0490(10) Uani 1 1 d . . . H5 H 0.3704 1.2419 0.1215 0.059 Uiso 1 1 calc R . . C6 C 0.7657(4) 0.4298(4) -0.0006(2) 0.0459(10) Uani 1 1 d . . . H6 H 0.7805 0.4052 -0.0449 0.055 Uiso 1 1 calc R . . C7 C 0.2102(4) 1.3490(3) 0.2503(2) 0.0414(9) Uani 1 1 d . . . C8 C 0.1841(4) 1.2477(3) 0.0286(2) 0.0437(9) Uani 1 1 d . . . H7 H 0.2521 1.2706 0.0239 0.052 Uiso 1 1 calc R . . N1 N 0.3130(4) 1.3688(4) 0.2503(3) 0.0643(13) Uani 1 1 d . . . C9 C 0.2202(4) 1.0459(3) 0.6258(2) 0.0391(9) Uani 1 1 d . . . H8 H 0.2966 1.0547 0.6153 0.047 Uiso 1 1 calc R . . Mo1 Mo 0.24841(2) 0.96191(2) 0.189133(14) 0.02309(6) Uani 1 1 d . . . Mo2 Mo 0.22454(2) 0.69859(2) 0.229482(15) 0.02424(7) Uani 1 1 d . . . Mo3 Mo 0.49831(2) 0.53345(2) 0.303696(15) 0.02450(7) Uani 1 1 d . . . Cu1 Cu 0.23656(3) 0.88319(3) 0.51676(2) 0.02531(9) Uani 1 1 d . . . Mo4 Mo 0.59878(2) 0.71761(2) 0.354140(15) 0.02572(7) Uani 1 1 d . . . Cu2 Cu 1.0000 0.5000 0.0000 0.03139(13) Uani 1 2 d S . . Cu3 Cu 0.06794(4) 1.26316(4) 0.19397(2) 0.03253(10) Uani 1 1 d . . . Mo5 Mo 0.45763(3) 0.97780(2) 0.276072(15) 0.02598(7) Uani 1 1 d . . . P1 P 0.51363(7) 0.75391(7) 0.18389(4) 0.02228(16) Uani 1 1 d . . . P2 P 0.29784(7) 0.79223(6) 0.35711(4) 0.01891(15) Uani 1 1 d . . . O11 O 0.3503(2) 0.57948(18) 0.26679(13) 0.0279(5) Uani 1 1 d . . . O12 O 0.29927(19) 0.90280(17) 0.30663(11) 0.0228(4) Uani 1 1 d . . . O13 O 0.42426(18) 0.70553(17) 0.34382(12) 0.0227(4) Uani 1 1 d . . . O14 O 0.5094(2) 0.87334(19) 0.35796(12) 0.0258(5) Uani 1 1 d . . . O15 O 0.3913(2) 1.00135(19) 0.18972(12) 0.0279(5) Uani 1 1 d . . . O16 O 0.5565(2) 0.80524(19) 0.23470(12) 0.0260(5) Uani 1 1 d . . . O17 O 0.37642(19) 0.79509(18) 0.18823(12) 0.0251(5) Uani 1 1 d . . . O18 O 0.2661(2) 0.8091(2) 0.43457(12) 0.0314(5) Uani 1 1 d . . . O19 O 0.6301(2) 0.57726(19) 0.31984(13) 0.0284(5) Uani 1 1 d . . . O20 O 0.1530(2) 0.86008(18) 0.21317(12) 0.0265(5) Uani 1 1 d . . . O21 O 0.1011(2) 0.6559(2) 0.26290(14) 0.0361(6) Uani 1 1 d . . . O22 O 0.20909(19) 0.74639(18) 0.33572(12) 0.0233(4) Uani 1 1 d . . . O23 O 0.2536(2) 0.6729(2) 0.14233(14) 0.0392(6) Uani 1 1 d . . . O24 O 0.3870(2) 0.9264(2) 0.48846(14) 0.0375(6) Uani 1 1 d . . . H9 H 0.4214 0.9065 0.4496 0.056 Uiso 1 1 calc R . . O25 O 0.1429(2) 1.07332(19) 0.22587(13) 0.0308(5) Uani 1 1 d . . . O26 O 0.5530(2) 0.62870(19) 0.19743(12) 0.0270(5) Uani 1 1 d . . . O27 O 0.5723(2) 0.7873(2) 0.10482(13) 0.0361(6) Uani 1 1 d . . . O28 O 0.5730(2) 0.4194(2) 0.26189(15) 0.0383(6) Uani 1 1 d . . . N2 N 0.0680(2) 0.8749(2) 0.54452(15) 0.0277(6) Uani 1 1 d . . . N3 N 0.1817(3) 0.9789(2) 0.59476(15) 0.0295(6) Uani 1 1 d . . . O29 O 0.2467(2) 0.9939(2) 0.09957(13) 0.0374(6) Uani 1 1 d . . . O30 O 0.4537(2) 0.4759(2) 0.38856(14) 0.0374(6) Uani 1 1 d . . . O31 O 0.3671(2) 1.0861(2) 0.31931(15) 0.0383(6) Uani 1 1 d . . . O32 O 0.5831(2) 1.0177(2) 0.23948(16) 0.0432(7) Uani 1 1 d . . . O33 O 0.7410(2) 0.7289(2) 0.32677(16) 0.0409(6) Uani 1 1 d . . . O34 O 0.5899(2) 0.6762(2) 0.44399(14) 0.0405(6) Uani 1 1 d . . . N4 N -0.1054(3) 0.9237(3) 0.61363(18) 0.0315(6) Uani 1 1 d . . . N5 N 0.0339(3) 1.0607(3) 0.67313(19) 0.0379(8) Uani 1 1 d . . . N6 N -0.0833(3) 1.2309(3) 0.19087(17) 0.0337(7) Uani 1 1 d . . . N7 N 0.9599(3) 0.5359(3) 0.10023(15) 0.0300(6) Uani 1 1 d . . . O35 O 0.3189(3) 0.7284(2) 0.59098(16) 0.0469(7) Uani 1 1 d . . . H10 H 0.3444 0.6747 0.5690 0.070 Uiso 1 1 calc R . . C10 C 0.0060(3) 0.9315(3) 0.59782(17) 0.0263(6) Uani 1 1 d . . . N8 N 0.0139(3) 1.3357(3) 0.28291(18) 0.0367(7) Uani 1 1 d . . . N9 N 0.0983(3) 1.2473(2) 0.08939(17) 0.0343(7) Uani 1 1 d . . . N10 N 0.8431(3) 0.4663(3) 0.02568(16) 0.0342(7) Uani 1 1 d . . . N11 N 0.2206(3) 1.2951(3) 0.19606(19) 0.0392(7) Uani 1 1 d . . . C11 C 0.0685(3) 0.9904(3) 0.62492(18) 0.0275(7) Uani 1 1 d . . . N12 N 0.8210(3) 0.5656(3) 0.19470(16) 0.0316(6) Uani 1 1 d . . . N13 N -0.1739(3) 1.1607(3) 0.1327(2) 0.0471(9) Uani 1 1 d . . . N14 N 0.6813(3) 0.4742(4) 0.1054(2) 0.0530(11) Uani 1 1 d . . . N15 N 0.0478(3) 1.1838(3) 0.00599(19) 0.0445(8) Uani 1 1 d . . . C12 C 0.8508(3) 0.5308(3) 0.13092(18) 0.0279(7) Uani 1 1 d . . . C13 C -0.1164(3) 0.8586(3) 0.5682(2) 0.0352(8) Uani 1 1 d . . . H11 H -0.1843 0.8392 0.5667 0.042 Uiso 1 1 calc R . . N16 N 0.0546(4) 1.4337(3) 0.3510(2) 0.0464(9) Uani 1 1 d . . . C14 C 1.0004(3) 0.5775(3) 0.14751(19) 0.0345(8) Uani 1 1 d . . . H12 H 1.0741 0.5912 0.1403 0.041 Uiso 1 1 calc R . . C15 C 0.7881(3) 0.4912(3) 0.09042(19) 0.0309(7) Uani 1 1 d . . . C16 C -0.0081(3) 0.8285(3) 0.5257(2) 0.0335(8) Uani 1 1 d . . . H13 H 0.0113 0.7837 0.4898 0.040 Uiso 1 1 calc R . . C17 C -0.0808(3) 1.1977(3) 0.1292(2) 0.0351(8) Uani 1 1 d . . . C18 C 0.0185(3) 1.2071(3) 0.0731(2) 0.0348(8) Uani 1 1 d . . . C19 C 0.9151(3) 0.5951(3) 0.2065(2) 0.0340(8) Uani 1 1 d . . . H14 H 0.9197 0.6219 0.2469 0.041 Uiso 1 1 calc R . . C20 C -0.1835(4) 1.2117(3) 0.2362(2) 0.0418(9) Uani 1 1 d . . . H15 H -0.2078 1.2259 0.2834 0.050 Uiso 1 1 calc R . . C21 C 0.0971(4) 1.3741(3) 0.2963(2) 0.0385(9) Uani 1 1 d . . . C22 C -0.0865(4) 1.3738(3) 0.3317(2) 0.0442(9) Uani 1 1 d . . . H16 H -0.1596 1.3603 0.3352 0.053 Uiso 1 1 calc R . . C23 C 0.6655(4) 0.4354(5) 0.0479(3) 0.0594(14) Uani 1 1 d . . . H17 H 0.5987 0.4167 0.0433 0.071 Uiso 1 1 calc R . . C24 C 0.3941(4) 1.3247(5) 0.1947(3) 0.0655(15) Uani 1 1 d . . . H18A H 0.4733 1.3259 0.1822 0.079 Uiso 1 1 calc R . . H19 H -0.154(4) 0.948(3) 0.639(2) 0.025(11) Uiso 1 1 d . . . H20 H 0.761(4) 0.572(3) 0.225(2) 0.037(11) Uiso 1 1 d . . . H21 H -0.025(4) 1.074(4) 0.697(3) 0.049(14) Uiso 1 1 d . . . H22 H 0.084(5) 1.476(5) 0.366(3) 0.073(18) Uiso 1 1 d . . . H23 H -0.013(6) 1.160(5) -0.005(3) 0.09(2) Uiso 1 1 d . . . H24 H 0.633(5) 0.490(5) 0.137(3) 0.070(18) Uiso 1 1 d . . . H25 H -0.186(4) 1.143(4) 0.101(3) 0.047(14) Uiso 1 1 d . . . H26 H 0.307(6) 1.393(6) 0.282(4) 0.09(2) Uiso 1 1 d . . . 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 O10W 0.057(2) 0.060(2) 0.056(2) 0.0008(16) -0.0026(15) -0.0303(17) O1W 0.115(4) 0.098(3) 0.101(3) -0.019(3) -0.065(3) -0.032(3) O2W 0.087(3) 0.120(4) 0.086(3) -0.023(3) -0.009(3) -0.034(3) O3W 0.103(3) 0.100(3) 0.096(3) -0.025(3) -0.056(3) -0.033(3) O4W 0.101(3) 0.131(4) 0.059(2) -0.028(2) -0.018(2) -0.053(3) O5W 0.106(3) 0.129(4) 0.068(3) -0.039(3) -0.012(2) -0.058(3) O6W 0.073(3) 0.106(3) 0.070(3) -0.008(2) -0.028(2) -0.028(2) O7W 0.064(2) 0.083(3) 0.089(3) -0.019(2) -0.019(2) -0.027(2) O8W 0.080(3) 0.113(3) 0.053(2) -0.015(2) 0.0130(19) -0.049(3) O9W 0.090(3) 0.061(2) 0.054(2) -0.0047(17) -0.0014(19) -0.020(2) C1 0.063(3) 0.049(3) 0.038(2) -0.0090(19) 0.000(2) -0.021(2) C2 0.037(2) 0.057(3) 0.069(3) -0.014(2) -0.003(2) -0.025(2) C3 0.048(2) 0.051(2) 0.036(2) -0.0023(18) -0.0020(18) -0.014(2) C4 0.043(2) 0.054(2) 0.052(2) -0.029(2) 0.0068(19) -0.025(2) C5 0.037(2) 0.051(3) 0.064(3) -0.015(2) -0.003(2) -0.0194(19) C6 0.044(2) 0.070(3) 0.037(2) -0.029(2) 0.0027(17) -0.027(2) C7 0.040(2) 0.0329(19) 0.059(3) -0.0090(18) -0.0141(19) -0.0161(17) C8 0.043(2) 0.043(2) 0.044(2) 0.0020(18) -0.0049(18) -0.0160(18) N1 0.048(2) 0.074(3) 0.092(4) -0.041(3) -0.011(2) -0.029(2) C9 0.034(2) 0.045(2) 0.045(2) -0.0182(18) 0.0002(16) -0.0188(17) Mo1 0.02367(14) 0.02248(13) 0.02308(13) -0.00439(10) -0.00496(10) -0.00524(10) Mo2 0.02300(14) 0.02588(14) 0.02870(14) -0.00880(11) -0.00684(11) -0.00911(11) Mo3 0.02152(13) 0.02181(13) 0.03013(15) -0.00568(11) -0.00352(11) -0.00550(10) Cu1 0.02229(19) 0.0316(2) 0.02298(19) -0.01005(16) -0.00070(15) -0.00744(16) Mo4 0.01883(13) 0.03230(15) 0.02892(14) -0.00846(11) -0.00530(10) -0.00804(11) Cu2 0.0293(3) 0.0425(3) 0.0260(3) -0.0124(3) 0.0027(2) -0.0156(3) Cu3 0.0293(2) 0.0323(2) 0.0407(2) -0.00913(18) -0.00755(18) -0.01175(18) Mo5 0.02688(15) 0.02708(14) 0.02878(15) -0.00611(11) -0.00306(11) -0.01398(11) P1 0.0200(4) 0.0264(4) 0.0214(4) -0.0068(3) -0.0003(3) -0.0078(3) P2 0.0165(3) 0.0219(4) 0.0195(4) -0.0059(3) -0.0017(3) -0.0063(3) O11 0.0258(12) 0.0238(11) 0.0375(13) -0.0087(10) -0.0066(10) -0.0083(9) O12 0.0217(11) 0.0227(10) 0.0251(11) -0.0032(9) -0.0045(8) -0.0076(9) O13 0.0162(10) 0.0230(10) 0.0295(11) -0.0074(9) -0.0038(8) -0.0044(8) O14 0.0252(11) 0.0308(12) 0.0257(11) -0.0081(9) -0.0044(9) -0.0115(9) O15 0.0312(12) 0.0286(12) 0.0260(12) -0.0028(9) -0.0026(9) -0.0136(10) O16 0.0239(11) 0.0304(12) 0.0268(11) -0.0084(9) -0.0030(9) -0.0103(9) O17 0.0219(11) 0.0250(11) 0.0301(12) -0.0082(9) -0.0048(9) -0.0060(9) O18 0.0320(13) 0.0416(14) 0.0231(12) -0.0123(10) 0.0002(10) -0.0127(11) O19 0.0204(11) 0.0293(12) 0.0356(13) -0.0079(10) -0.0054(9) -0.0048(9) O20 0.0223(11) 0.0268(11) 0.0324(12) -0.0051(9) -0.0070(9) -0.0077(9) O21 0.0299(13) 0.0423(14) 0.0454(15) -0.0095(12) -0.0101(11) -0.0185(11) O22 0.0187(10) 0.0284(11) 0.0262(11) -0.0083(9) -0.0020(8) -0.0098(9) O23 0.0443(15) 0.0443(15) 0.0373(14) -0.0192(12) -0.0098(12) -0.0144(12) O24 0.0311(13) 0.0508(16) 0.0361(14) -0.0189(12) 0.0055(11) -0.0190(12) O25 0.0301(13) 0.0279(12) 0.0332(13) -0.0065(10) -0.0058(10) -0.0052(10) O26 0.0239(11) 0.0267(11) 0.0288(12) -0.0084(9) -0.0001(9) -0.0053(9) O27 0.0378(14) 0.0466(15) 0.0235(12) -0.0057(11) 0.0049(10) -0.0176(12) O28 0.0356(14) 0.0279(13) 0.0495(16) -0.0127(11) -0.0067(12) -0.0024(11) N2 0.0260(14) 0.0318(15) 0.0255(14) -0.0095(11) -0.0019(11) -0.0067(12) N3 0.0250(14) 0.0362(15) 0.0289(15) -0.0114(12) 0.0000(11) -0.0097(12) O29 0.0443(15) 0.0397(14) 0.0264(12) -0.0025(11) -0.0093(11) -0.0090(12) O30 0.0375(14) 0.0334(13) 0.0398(15) 0.0023(11) -0.0066(11) -0.0126(11) O31 0.0455(16) 0.0309(13) 0.0422(15) -0.0124(11) -0.0053(12) -0.0131(12) O32 0.0382(15) 0.0477(16) 0.0522(17) -0.0023(13) -0.0041(13) -0.0286(13) O33 0.0238(13) 0.0482(16) 0.0573(18) -0.0199(13) -0.0039(12) -0.0136(11) O34 0.0425(15) 0.0459(15) 0.0317(14) -0.0062(12) -0.0139(12) -0.0057(12) N4 0.0232(15) 0.0364(16) 0.0341(16) -0.0125(14) 0.0016(13) -0.0071(13) N5 0.0319(17) 0.0432(18) 0.0426(19) -0.0232(15) 0.0079(15) -0.0151(15) N6 0.0288(15) 0.0328(15) 0.0419(18) -0.0090(13) -0.0061(13) -0.0097(12) N7 0.0253(14) 0.0390(16) 0.0279(14) -0.0112(12) -0.0006(11) -0.0107(12) O35 0.0425(17) 0.0424(16) 0.0484(17) 0.0004(13) -0.0094(13) -0.0054(13) C10 0.0246(16) 0.0265(16) 0.0264(16) -0.0056(13) -0.0011(12) -0.0064(13) N8 0.0385(17) 0.0340(16) 0.0418(18) -0.0078(13) -0.0079(14) -0.0139(14) N9 0.0334(16) 0.0320(15) 0.0394(17) -0.0034(13) -0.0090(13) -0.0109(13) N10 0.0353(17) 0.0438(17) 0.0283(15) -0.0139(13) 0.0026(12) -0.0179(14) N11 0.0350(17) 0.0398(17) 0.049(2) -0.0124(15) -0.0054(14) -0.0162(14) C11 0.0275(17) 0.0293(16) 0.0267(16) -0.0088(13) -0.0006(13) -0.0090(13) N12 0.0246(15) 0.0433(17) 0.0290(15) -0.0128(13) 0.0025(12) -0.0125(13) N13 0.040(2) 0.055(2) 0.058(2) -0.0174(19) -0.0112(18) -0.0222(17) N14 0.0355(19) 0.094(3) 0.045(2) -0.043(2) 0.0143(16) -0.034(2) N15 0.047(2) 0.046(2) 0.0409(19) -0.0063(15) -0.0118(16) -0.0115(17) C12 0.0217(16) 0.0319(17) 0.0303(17) -0.0108(14) -0.0019(13) -0.0060(13) C13 0.0321(19) 0.039(2) 0.040(2) -0.0121(16) -0.0055(15) -0.0140(16) N16 0.058(2) 0.044(2) 0.046(2) -0.0106(16) -0.0110(17) -0.0214(18) C14 0.0259(17) 0.048(2) 0.0341(19) -0.0096(16) -0.0041(14) -0.0154(16) C15 0.0266(17) 0.0375(19) 0.0315(18) -0.0136(15) -0.0014(14) -0.0103(14) C16 0.0316(18) 0.0364(19) 0.0378(19) -0.0152(15) -0.0070(15) -0.0102(15) C17 0.0320(19) 0.0309(18) 0.045(2) -0.0062(16) -0.0102(16) -0.0095(15) C18 0.036(2) 0.0298(18) 0.040(2) -0.0085(15) -0.0111(16) -0.0062(15) C19 0.0271(17) 0.047(2) 0.0315(18) -0.0135(16) -0.0043(14) -0.0115(16) C20 0.034(2) 0.042(2) 0.049(2) -0.0098(18) 0.0008(17) -0.0133(17) C21 0.046(2) 0.0331(19) 0.044(2) -0.0083(16) -0.0140(18) -0.0155(17) C22 0.045(2) 0.044(2) 0.045(2) -0.0075(18) -0.0031(18) -0.0156(19) C23 0.043(2) 0.101(4) 0.056(3) -0.046(3) 0.008(2) -0.040(3) C24 0.041(3) 0.076(4) 0.094(4) -0.033(3) -0.003(3) -0.031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O10W H10A 0.8501 . ? O10W H10B 0.8500 . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8499 . ? O2W H2WA 0.8499 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8501 . ? O4W H4WA 0.8502 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8501 . ? O5W H5WB 0.8499 . ? O6W H6WA 0.8500 . ? O6W H6WB 0.8499 . ? O7W H7WA 0.8500 . ? O7W H7WB 0.8499 . ? O8W H8WA 0.8500 . ? O8W H8WB 0.8500 . ? O9W H9WA 0.8501 . ? O9W H9WB 0.8500 . ? C1 C22 1.362(6) . ? C1 N16 1.365(6) . ? C1 H1 0.9300 . ? C2 C20 1.355(6) . ? C2 N13 1.371(6) . ? C2 H2 0.9300 . ? C3 C8 1.357(6) . ? C3 N15 1.372(6) . ? C3 H3 0.9300 . ? C4 C9 1.355(5) . ? C4 N5 1.368(5) . ? C4 H4 0.9300 . ? C5 C24 1.352(6) . ? C5 N11 1.373(5) . ? C5 H5 0.9300 . ? C6 C23 1.345(6) . ? C6 N10 1.378(5) . ? C6 H6 0.9300 . ? C7 N11 1.326(5) . ? C7 N1 1.332(5) . ? C7 C21 1.428(6) . ? C8 N9 1.384(5) . ? C8 H7 0.9300 . ? N1 C24 1.361(7) . ? N1 H26 0.72(6) . ? C9 N3 1.373(4) . ? C9 H8 0.9300 . ? Mo1 O29 1.696(2) . ? Mo1 O25 1.728(2) . ? Mo1 O20 1.930(2) . ? Mo1 O15 1.933(2) . ? Mo1 O17 2.191(2) . ? Mo1 O12 2.382(2) . ? Mo2 O21 1.694(2) . ? Mo2 O23 1.717(3) . ? Mo2 O11 1.908(2) . ? Mo2 O20 1.957(2) . ? Mo2 O22 2.205(2) . ? Mo2 O17 2.432(2) . ? Mo3 O28 1.703(2) . ? Mo3 O30 1.707(3) . ? Mo3 O11 1.914(2) . ? Mo3 O19 1.933(2) . ? Mo3 O26 2.254(2) . ? Mo3 O13 2.318(2) . ? Cu1 O18 1.917(2) . ? Cu1 O24 1.986(2) . ? Cu1 N3 1.997(3) . ? Cu1 N2 2.003(3) . ? Cu1 O35 2.272(3) . ? Mo4 O34 1.699(3) . ? Mo4 O33 1.713(3) . ? Mo4 O19 1.936(2) . ? Mo4 O14 1.944(2) . ? Mo4 O13 2.191(2) . ? Mo4 O16 2.433(2) . ? Cu2 N7 1.997(3) 2_765 ? Cu2 N7 1.997(3) . ? Cu2 N10 1.998(3) 2_765 ? Cu2 N10 1.998(3) . ? Cu3 N6 1.994(3) . ? Cu3 N8 1.999(3) . ? Cu3 N11 2.003(3) . ? Cu3 N9 2.010(3) . ? Cu3 O25 2.311(2) . ? Mo5 O31 1.702(3) . ? Mo5 O32 1.706(3) . ? Mo5 O15 1.921(2) . ? Mo5 O14 1.926(2) . ? Mo5 O12 2.309(2) . ? Mo5 O16 2.353(2) . ? P1 O26 1.506(2) . ? P1 O16 1.529(2) . ? P1 O17 1.539(2) . ? P1 O27 1.575(2) . ? P2 O18 1.501(2) . ? P2 O22 1.524(2) . ? P2 O12 1.557(2) . ? P2 O13 1.563(2) . ? O24 H9 0.8200 . ? N2 C10 1.325(4) . ? N2 C16 1.374(4) . ? N3 C11 1.327(4) . ? N4 C10 1.332(4) . ? N4 C13 1.375(5) . ? N4 H19 0.71(4) . ? N5 C11 1.332(4) . ? N5 H21 0.75(5) . ? N6 C17 1.331(5) . ? N6 C20 1.385(5) . ? N7 C12 1.329(4) . ? N7 C14 1.376(4) . ? O35 H10 0.8200 . ? C10 C11 1.445(5) . ? N8 C21 1.331(5) . ? N8 C22 1.372(5) . ? N9 C18 1.335(5) . ? N10 C15 1.329(4) . ? N12 C12 1.328(4) . ? N12 C19 1.369(5) . ? N12 H20 0.82(4) . ? N13 C17 1.328(5) . ? N13 H25 0.75(5) . ? N14 C15 1.325(5) . ? N14 C23 1.369(5) . ? N14 H24 0.76(6) . ? N15 C18 1.334(5) . ? N15 H23 0.95(6) . ? C12 C15 1.442(5) . ? C13 C16 1.358(5) . ? C13 H11 0.9300 . ? N16 C21 1.338(5) . ? N16 H22 0.85(6) . ? C14 C19 1.357(5) . ? C14 H12 0.9300 . ? C16 H13 0.9300 . ? C17 C18 1.444(5) . ? C19 H14 0.9300 . ? C20 H15 0.9300 . ? C22 H16 0.9300 . ? C23 H17 0.9300 . ? C24 H18A 0.9300 . ? 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 H10A O10W H10B 120.0 . . ? H1WA O1W H1WB 120.0 . . ? H2WA O2W H2WB 120.0 . . ? H3WA O3W H3WB 120.0 . . ? H4WA O4W H4WB 120.0 . . ? H5WA O5W H5WB 120.0 . . ? H6WA O6W H6WB 120.0 . . ? H7WA O7W H7WB 120.0 . . ? H8WA O8W H8WB 120.0 . . ? H9WA O9W H9WB 120.0 . . ? C22 C1 N16 106.7(4) . . ? C22 C1 H1 126.7 . . ? N16 C1 H1 126.7 . . ? C20 C2 N13 106.7(4) . . ? C20 C2 H2 126.6 . . ? N13 C2 H2 126.6 . . ? C8 C3 N15 107.1(4) . . ? C8 C3 H3 126.4 . . ? N15 C3 H3 126.4 . . ? C9 C4 N5 106.3(3) . . ? C9 C4 H4 126.8 . . ? N5 C4 H4 126.8 . . ? C24 C5 N11 108.9(4) . . ? C24 C5 H5 125.5 . . ? N11 C5 H5 125.5 . . ? C23 C6 N10 109.2(3) . . ? C23 C6 H6 125.4 . . ? N10 C6 H6 125.4 . . ? N11 C7 N1 110.3(4) . . ? N11 C7 C21 117.3(3) . . ? N1 C7 C21 132.4(4) . . ? C3 C8 N9 108.6(4) . . ? C3 C8 H7 125.7 . . ? N9 C8 H7 125.7 . . ? C7 N1 C24 108.2(4) . . ? C7 N1 H26 109(6) . . ? C24 N1 H26 143(6) . . ? C4 C9 N3 109.1(3) . . ? C4 C9 H8 125.4 . . ? N3 C9 H8 125.4 . . ? O29 Mo1 O25 105.01(12) . . ? O29 Mo1 O20 99.85(11) . . ? O25 Mo1 O20 97.67(11) . . ? O29 Mo1 O15 97.29(12) . . ? O25 Mo1 O15 98.74(11) . . ? O20 Mo1 O15 152.27(10) . . ? O29 Mo1 O17 97.61(11) . . ? O25 Mo1 O17 157.02(10) . . ? O20 Mo1 O17 74.16(9) . . ? O15 Mo1 O17 82.11(9) . . ? O29 Mo1 O12 166.86(11) . . ? O25 Mo1 O12 84.90(9) . . ? O20 Mo1 O12 87.10(8) . . ? O15 Mo1 O12 72.31(8) . . ? O17 Mo1 O12 73.42(8) . . ? O21 Mo2 O23 102.05(13) . . ? O21 Mo2 O11 103.24(11) . . ? O23 Mo2 O11 99.39(12) . . ? O21 Mo2 O20 101.09(11) . . ? O23 Mo2 O20 98.80(12) . . ? O11 Mo2 O20 145.67(9) . . ? O21 Mo2 O22 87.12(10) . . ? O23 Mo2 O22 170.68(11) . . ? O11 Mo2 O22 79.91(9) . . ? O20 Mo2 O22 77.50(9) . . ? O21 Mo2 O17 168.67(10) . . ? O23 Mo2 O17 83.92(10) . . ? O11 Mo2 O17 85.05(9) . . ? O20 Mo2 O17 68.25(8) . . ? O22 Mo2 O17 86.76(8) . . ? O28 Mo3 O30 102.49(13) . . ? O28 Mo3 O11 100.25(11) . . ? O30 Mo3 O11 100.10(12) . . ? O28 Mo3 O19 101.24(11) . . ? O30 Mo3 O19 100.02(12) . . ? O11 Mo3 O19 146.47(10) . . ? O28 Mo3 O26 84.20(11) . . ? O30 Mo3 O26 172.97(11) . . ? O11 Mo3 O26 80.60(9) . . ? O19 Mo3 O26 76.31(9) . . ? O28 Mo3 O13 168.02(11) . . ? O30 Mo3 O13 87.94(11) . . ? O11 Mo3 O13 83.45(8) . . ? O19 Mo3 O13 70.76(8) . . ? O26 Mo3 O13 85.18(8) . . ? O18 Cu1 O24 93.48(10) . . ? O18 Cu1 N3 170.04(11) . . ? O24 Cu1 N3 90.56(11) . . ? O18 Cu1 N2 93.04(11) . . ? O24 Cu1 N2 167.66(12) . . ? N3 Cu1 N2 81.41(11) . . ? O18 Cu1 O35 95.67(11) . . ? O24 Cu1 O35 93.75(12) . . ? N3 Cu1 O35 93.15(12) . . ? N2 Cu1 O35 96.03(11) . . ? O34 Mo4 O33 104.54(14) . . ? O34 Mo4 O19 100.95(12) . . ? O33 Mo4 O19 96.26(11) . . ? O34 Mo4 O14 97.33(11) . . ? O33 Mo4 O14 99.88(11) . . ? O19 Mo4 O14 151.68(9) . . ? O34 Mo4 O13 97.19(11) . . ? O33 Mo4 O13 157.51(11) . . ? O19 Mo4 O13 73.64(9) . . ? O14 Mo4 O13 82.80(8) . . ? O34 Mo4 O16 164.74(11) . . ? O33 Mo4 O16 87.77(11) . . ? O19 Mo4 O16 86.37(9) . . ? O14 Mo4 O16 71.26(8) . . ? O13 Mo4 O16 71.84(8) . . ? N7 Cu2 N7 180.0 2_765 . ? N7 Cu2 N10 82.72(12) 2_765 2_765 ? N7 Cu2 N10 97.28(12) . 2_765 ? N7 Cu2 N10 97.29(12) 2_765 . ? N7 Cu2 N10 82.72(12) . . ? N10 Cu2 N10 180.0 2_765 . ? N6 Cu3 N8 98.33(13) . . ? N6 Cu3 N11 179.40(14) . . ? N8 Cu3 N11 82.26(13) . . ? N6 Cu3 N9 82.10(13) . . ? N8 Cu3 N9 159.36(13) . . ? N11 Cu3 N9 97.32(13) . . ? N6 Cu3 O25 85.09(11) . . ? N8 Cu3 O25 108.74(11) . . ? N11 Cu3 O25 94.81(11) . . ? N9 Cu3 O25 91.87(11) . . ? O31 Mo5 O32 103.63(14) . . ? O31 Mo5 O15 103.08(12) . . ? O32 Mo5 O15 98.08(12) . . ? O31 Mo5 O14 98.89(11) . . ? O32 Mo5 O14 101.74(12) . . ? O15 Mo5 O14 145.88(9) . . ? O31 Mo5 O12 86.82(10) . . ? O32 Mo5 O12 168.38(11) . . ? O15 Mo5 O12 74.24(9) . . ? O14 Mo5 O12 81.33(8) . . ? O31 Mo5 O16 167.03(11) . . ? O32 Mo5 O16 88.35(11) . . ? O15 Mo5 O16 79.73(9) . . ? O14 Mo5 O16 73.42(9) . . ? O12 Mo5 O16 81.75(8) . . ? O26 P1 O16 112.47(13) . . ? O26 P1 O17 108.75(13) . . ? O16 P1 O17 112.13(13) . . ? O26 P1 O27 106.25(14) . . ? O16 P1 O27 108.53(14) . . ? O17 P1 O27 108.47(14) . . ? O18 P2 O22 111.44(13) . . ? O18 P2 O12 111.69(13) . . ? O22 P2 O12 107.88(12) . . ? O18 P2 O13 109.81(13) . . ? O22 P2 O13 107.05(12) . . ? O12 P2 O13 108.82(12) . . ? Mo2 O11 Mo3 148.03(13) . . ? P2 O12 Mo5 125.85(12) . . ? P2 O12 Mo1 128.93(12) . . ? Mo5 O12 Mo1 91.62(8) . . ? P2 O13 Mo4 128.78(12) . . ? P2 O13 Mo3 135.35(12) . . ? Mo4 O13 Mo3 95.82(8) . . ? Mo5 O14 Mo4 124.13(11) . . ? Mo5 O15 Mo1 121.61(12) . . ? P1 O16 Mo5 126.20(13) . . ? P1 O16 Mo4 124.88(13) . . ? Mo5 O16 Mo4 91.18(8) . . ? P1 O17 Mo1 131.67(13) . . ? P1 O17 Mo2 131.61(13) . . ? Mo1 O17 Mo2 94.77(8) . . ? P2 O18 Cu1 158.17(17) . . ? Mo3 O19 Mo4 119.78(11) . . ? Mo1 O20 Mo2 122.36(11) . . ? P2 O22 Mo2 124.72(12) . . ? Cu1 O24 H9 109.5 . . ? Mo1 O25 Cu3 137.86(13) . . ? P1 O26 Mo3 122.03(13) . . ? C10 N2 C16 106.5(3) . . ? C10 N2 Cu1 113.3(2) . . ? C16 N2 Cu1 140.2(2) . . ? C11 N3 C9 105.9(3) . . ? C11 N3 Cu1 113.2(2) . . ? C9 N3 Cu1 140.6(3) . . ? C10 N4 C13 107.8(3) . . ? C10 N4 H19 130(3) . . ? C13 N4 H19 123(3) . . ? C11 N5 C4 107.7(3) . . ? C11 N5 H21 125(4) . . ? C4 N5 H21 127(4) . . ? C17 N6 C20 106.3(3) . . ? C17 N6 Cu3 112.0(2) . . ? C20 N6 Cu3 140.4(3) . . ? C12 N7 C14 105.9(3) . . ? C12 N7 Cu2 111.9(2) . . ? C14 N7 Cu2 141.6(2) . . ? Cu1 O35 H10 109.5 . . ? N2 C10 N4 110.7(3) . . ? N2 C10 C11 115.9(3) . . ? N4 C10 C11 133.4(3) . . ? C21 N8 C22 105.7(3) . . ? C21 N8 Cu3 112.0(3) . . ? C22 N8 Cu3 141.6(3) . . ? C18 N9 C8 105.7(3) . . ? C18 N9 Cu3 111.7(3) . . ? C8 N9 Cu3 141.7(3) . . ? C15 N10 C6 105.5(3) . . ? C15 N10 Cu2 111.4(2) . . ? C6 N10 Cu2 142.9(3) . . ? C7 N11 C5 106.2(3) . . ? C7 N11 Cu3 111.7(3) . . ? C5 N11 Cu3 142.1(3) . . ? N3 C11 N5 110.9(3) . . ? N3 C11 C10 116.2(3) . . ? N5 C11 C10 132.9(3) . . ? C12 N12 C19 107.7(3) . . ? C12 N12 H20 132(3) . . ? C19 N12 H20 120(3) . . ? C17 N13 C2 108.0(4) . . ? C17 N13 H25 122(4) . . ? C2 N13 H25 130(4) . . ? C15 N14 C23 107.8(3) . . ? C15 N14 H24 128(4) . . ? C23 N14 H24 124(4) . . ? C18 N15 C3 107.3(4) . . ? C18 N15 H23 109(4) . . ? C3 N15 H23 144(4) . . ? N12 C12 N7 111.0(3) . . ? N12 C12 C15 132.6(3) . . ? N7 C12 C15 116.3(3) . . ? C16 C13 N4 106.3(3) . . ? C16 C13 H11 126.9 . . ? N4 C13 H11 126.9 . . ? C21 N16 C1 107.3(4) . . ? C21 N16 H22 130(4) . . ? C1 N16 H22 121(4) . . ? C19 C14 N7 108.8(3) . . ? C19 C14 H12 125.6 . . ? N7 C14 H12 125.6 . . ? N14 C15 N10 111.0(3) . . ? N14 C15 C12 131.8(3) . . ? N10 C15 C12 117.2(3) . . ? C13 C16 N2 108.8(3) . . ? C13 C16 H13 125.6 . . ? N2 C16 H13 125.6 . . ? N13 C17 N6 110.6(4) . . ? N13 C17 C18 132.7(4) . . ? N6 C17 C18 116.7(3) . . ? N15 C18 N9 111.3(4) . . ? N15 C18 C17 132.6(4) . . ? N9 C18 C17 116.1(3) . . ? C14 C19 N12 106.5(3) . . ? C14 C19 H14 126.8 . . ? N12 C19 H14 126.8 . . ? C2 C20 N6 108.4(4) . . ? C2 C20 H15 125.8 . . ? N6 C20 H15 125.8 . . ? N8 C21 N16 111.2(4) . . ? N8 C21 C7 116.5(3) . . ? N16 C21 C7 132.2(4) . . ? C1 C22 N8 109.1(4) . . ? C1 C22 H16 125.5 . . ? N8 C22 H16 125.5 . . ? C6 C23 N14 106.5(4) . . ? C6 C23 H17 126.8 . . ? N14 C23 H17 126.8 . . ? C5 C24 N1 106.4(4) . . ? C5 C24 H18A 126.8 . . ? N1 C24 H18A 126.8 . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.831 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.101 # Attachment '3.cif' data_jhj127_0m _database_code_depnum_ccdc_archive 'CCDC 720598' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H33 Cu3 Mo5 N18 O24 P2, H2 O' _chemical_formula_sum 'C36 H35 Cu3 Mo5 N18 O25 P2' _chemical_formula_weight 1852.11 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' Cu Cu 0.3201 1.2651 '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' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.8981(5) _cell_length_b 18.8195(7) _cell_length_c 12.6000(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.8650(10) _cell_angle_gamma 90.00 _cell_volume 2713.88(19) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3936 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 23.41 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 2.266 _exptl_crystal_density_diffrn 2.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808.0 _exptl_absorpt_coefficient_mu 2.429 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.712 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19818 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6930 _reflns_number_gt 10346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0235P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(13) _chemical_absolute_configuration ad _refine_ls_number_reflns 6930 _refine_ls_number_parameters 803 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.000 _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 O1W O 0.4190(5) 0.1090(3) 0.9322(6) 0.0572(18) Uani 1 1 d . . . H1WA H 0.4780 0.0902 0.9175 0.069 Uiso 1 1 d R . . H1WB H 0.3942 0.0926 0.9844 0.069 Uiso 1 1 d R . . C1 C 0.2251(7) 0.5527(4) 0.7445(7) 0.035(2) Uani 1 1 d . . . H6 H 0.1864 0.5892 0.6995 0.043 Uiso 1 1 calc R . . C2 C 0.2985(7) 0.5619(4) 0.8457(7) 0.037(2) Uani 1 1 d . . . H5 H 0.3193 0.6046 0.8829 0.045 Uiso 1 1 calc R . . C3 C -0.0522(6) 0.2418(4) -0.2598(6) 0.0269(16) Uani 1 1 d . . . N1 N 0.8365(5) 0.4449(3) -0.0310(5) 0.0284(14) Uani 1 1 d . . . C4 C 0.6026(6) 0.2344(4) -0.2354(6) 0.0315(17) Uani 1 1 d . . . H25 H 0.6410 0.1981 -0.1898 0.038 Uiso 1 1 calc R . . N2 N -0.1576(5) 0.3306(3) 0.3887(6) 0.0352(17) Uani 1 1 d . . . H2 H -0.2289 0.3376 0.3515 0.042 Uiso 1 1 calc R . . C5 C -0.0905(6) 0.3755(4) 0.4610(6) 0.0234(15) Uani 1 1 d . . . C6 C -0.0047(6) 0.3509(4) -0.1782(6) 0.0294(17) Uani 1 1 d . . . H26 H 0.0443 0.3795 -0.1251 0.035 Uiso 1 1 calc R . . C7 C 0.5459(6) 0.3393(4) -0.2994(6) 0.0226(15) Uani 1 1 d . . . C8 C 0.2830(6) 0.4493(4) 0.8034(6) 0.0226(15) Uani 1 1 d . . . N3 N 0.6143(5) 0.3071(3) -0.2111(5) 0.0238(13) Uani 1 1 d . . . C9 C 0.5441(6) 0.4162(4) -0.2951(6) 0.0232(15) Uani 1 1 d . . . C10 C 0.9277(6) 0.4109(4) 0.0348(6) 0.0292(16) Uani 1 1 d . . . N4 N 0.3361(5) 0.4958(3) 0.8827(5) 0.0305(15) Uani 1 1 d . . . H4 H 0.3847 0.4855 0.9450 0.037 Uiso 1 1 calc R . . N5 N 0.4882(5) 0.4645(3) -0.3670(5) 0.0293(15) Uani 1 1 d . . . H5A H 0.4424 0.4563 -0.4315 0.035 Uiso 1 1 calc R . . N6 N 0.4915(5) 0.2934(3) -0.3768(5) 0.0256(14) Uani 1 1 d . . . H6A H 0.4442 0.3039 -0.4397 0.031 Uiso 1 1 calc R . . Mo1 Mo 0.57330(5) 0.40907(3) 0.14035(5) 0.01969(13) Uani 1 1 d . . . Mo2 Mo 0.30986(5) 0.22734(3) 0.32235(5) 0.02104(13) Uani 1 1 d . . . Mo3 Mo 0.53372(5) 0.23793(3) 0.20579(5) 0.02153(13) Uani 1 1 d . . . Mo4 Mo 0.35837(5) 0.50959(3) 0.19396(5) 0.02065(13) Uani 1 1 d . . . Mo5 Mo 0.22966(5) 0.39470(3) 0.36342(5) 0.02007(13) Uani 1 1 d . . . Cu1 Cu 0.12091(7) 0.41653(5) 0.60466(7) 0.02392(19) Uani 1 1 d . . . Cu2 Cu 0.14866(7) 0.22616(5) -0.08215(7) 0.02468(19) Uani 1 1 d . . . Cu3 Cu 0.70027(7) 0.37758(5) -0.09469(8) 0.0259(2) Uani 1 1 d . . . P1 P 0.28298(14) 0.34358(9) 0.10334(15) 0.0167(4) Uani 1 1 d . . . P2 P 0.50947(14) 0.37288(9) 0.37597(15) 0.0183(4) Uani 1 1 d . . . O2 O 0.4488(4) 0.5630(3) 0.2870(5) 0.0343(13) Uani 1 1 d . . . O3 O 0.2216(4) 0.4347(2) 0.4844(4) 0.0250(11) Uani 1 1 d . . . O4 O 0.4871(3) 0.4184(2) 0.2682(4) 0.0182(10) Uani 1 1 d . . . O5 O 0.2685(4) 0.5693(2) 0.1097(4) 0.0326(13) Uani 1 1 d . . . O6 O 0.4204(3) 0.3986(2) 0.4344(3) 0.0190(10) Uani 1 1 d . . . O7 O 0.4084(4) 0.3249(2) 0.1012(4) 0.0182(10) Uani 1 1 d . . . O8 O 0.6278(4) 0.3217(2) 0.2159(4) 0.0205(10) Uani 1 1 d . . . O9 O 0.3841(4) 0.1989(2) 0.2077(4) 0.0216(10) Uani 1 1 d . . . O10 O 0.2613(4) 0.4229(2) 0.0848(4) 0.0199(10) Uani 1 1 d . . . O11 O 0.2630(4) 0.3249(2) 0.2170(4) 0.0210(10) Uani 1 1 d . . . O12 O 0.5754(4) 0.3872(3) 0.0073(4) 0.0271(11) Uani 1 1 d . . . O13 O 0.4814(4) 0.2940(2) 0.3436(4) 0.0193(10) Uani 1 1 d . . . O14 O 0.6300(4) 0.1876(3) 0.2999(5) 0.0340(13) Uani 1 1 d . . . N7 N 0.2240(5) 0.3439(3) 0.7036(5) 0.0280(14) Uani 1 1 d . . . O15 O 0.5412(4) 0.2045(2) 0.0816(4) 0.0299(12) Uani 1 1 d . . . O16 O 0.6331(4) 0.3821(2) 0.4454(4) 0.0251(11) Uani 1 1 d . . . N8 N 0.2153(5) 0.4826(3) 0.7170(5) 0.0269(14) Uani 1 1 d . . . O17 O 0.3791(4) 0.1713(3) 0.4247(4) 0.0312(12) Uani 1 1 d . . . O18 O 0.2678(4) 0.2985(2) 0.4145(4) 0.0243(11) Uani 1 1 d . . . O19 O 0.6970(4) 0.4554(3) 0.1923(4) 0.0349(13) Uani 1 1 d . . . O20 O 0.0861(4) 0.3840(3) 0.2936(4) 0.0263(11) Uani 1 1 d . . . O21 O 0.1787(4) 0.1879(3) 0.2657(5) 0.0347(13) Uani 1 1 d . . . N9 N 0.3605(5) 0.3247(3) 0.8586(5) 0.0278(14) Uani 1 1 d . . . H9 H 0.4116 0.3326 0.9205 0.033 Uiso 1 1 calc R . . O22 O 0.1938(4) 0.3033(2) 0.0143(4) 0.0266(12) Uani 1 1 d . . . O23 O 0.4624(4) 0.4873(2) 0.0987(4) 0.0210(10) Uani 1 1 d . . . N10 N -0.0202(5) 0.4807(3) 0.5610(5) 0.0290(14) Uani 1 1 d . . . O24 O 0.2634(4) 0.4727(2) 0.2819(4) 0.0241(11) Uani 1 1 d . . . O25 O 0.2539(5) 0.1590(3) 0.0129(4) 0.0332(13) Uani 1 1 d . . . H13 H 0.2765 0.1755 0.0754 0.050 Uiso 1 1 calc R . . N11 N 0.0153(5) 0.3486(3) 0.5040(5) 0.0259(14) Uani 1 1 d . . . N12 N 0.0205(5) 0.2825(3) -0.1809(5) 0.0240(13) Uani 1 1 d . . . N13 N 0.0813(5) 0.1492(3) -0.1892(5) 0.0284(14) Uani 1 1 d . . . N14 N 0.8081(5) 0.3083(3) 0.0031(5) 0.0322(15) Uani 1 1 d . . . C11 C 0.2939(6) 0.3728(4) 0.7954(6) 0.0242(15) Uani 1 1 d . . . N15 N 0.9811(5) 0.2887(3) 0.1168(5) 0.0344(16) Uani 1 1 d . . . H15 H 1.0515 0.2956 0.1566 0.041 Uiso 1 1 calc R . . N16 N 1.0242(6) 0.4516(3) 0.0557(6) 0.0380(17) Uani 1 1 d . . . H16 H 1.0926 0.4396 0.0952 0.046 Uiso 1 1 calc R . . C12 C 0.5875(7) 0.5182(4) -0.2183(7) 0.0362(19) Uani 1 1 d . . . H20 H 0.6182 0.5534 -0.1667 0.043 Uiso 1 1 calc R . . C13 C 0.8790(6) 0.5096(4) -0.0505(7) 0.0342(18) Uani 1 1 d . . . H19 H 0.8356 0.5452 -0.0944 0.041 Uiso 1 1 calc R . . C14 C 0.9951(7) 0.5141(4) 0.0043(7) 0.040(2) Uani 1 1 d . . . H18 H 1.0441 0.5528 0.0056 0.048 Uiso 1 1 calc R . . C15 C -0.0192(6) 0.1696(4) -0.2648(6) 0.0282(17) Uani 1 1 d . . . N17 N 0.6071(5) 0.4472(3) -0.2024(5) 0.0275(14) Uani 1 1 d . . . C16 C 0.5169(7) 0.5297(4) -0.3199(7) 0.035(2) Uani 1 1 d . . . H21 H 0.4923 0.5735 -0.3519 0.042 Uiso 1 1 calc R . . C17 C 0.5251(6) 0.2256(4) -0.3378(6) 0.0322(17) Uani 1 1 d . . . H24 H 0.5002 0.1828 -0.3736 0.039 Uiso 1 1 calc R . . C18 C 0.3340(6) 0.2603(4) 0.8083(7) 0.0324(18) Uani 1 1 d . . . H1 H 0.3676 0.2168 0.8339 0.039 Uiso 1 1 calc R . . C19 C 0.8138(7) 0.2375(5) 0.0331(7) 0.043(2) Uani 1 1 d . . . H14 H 0.7543 0.2043 0.0093 0.051 Uiso 1 1 calc R . . N18 N -0.2126(5) 0.4804(3) 0.4857(6) 0.0379(17) Uani 1 1 d . . . H18A H -0.2810 0.4666 0.4487 0.046 Uiso 1 1 calc R . . C20 C 0.9109(6) 0.3376(4) 0.0575(6) 0.0272(17) Uani 1 1 d . . . C21 C -0.1123(6) 0.4457(4) 0.4981(6) 0.0273(17) Uani 1 1 d . . . C22 C 0.0148(6) 0.2824(4) 0.4556(6) 0.0308(18) Uani 1 1 d . . . H7 H 0.0775 0.2510 0.4697 0.037 Uiso 1 1 calc R . . C23 C -0.0918(6) 0.2709(4) 0.3846(7) 0.0343(19) Uani 1 1 d . . . H8 H -0.1157 0.2307 0.3416 0.041 Uiso 1 1 calc R . . C24 C -0.1008(7) 0.3812(5) -0.2509(7) 0.042(2) Uani 1 1 d . . . H27 H -0.1136 0.4298 -0.2471 0.051 Uiso 1 1 calc R . . C25 C 0.2481(6) 0.2723(4) 0.7126(7) 0.0327(18) Uani 1 1 d . . . H2A H 0.2120 0.2377 0.6619 0.039 Uiso 1 1 calc R . . C26 C 0.1149(7) 0.0826(4) -0.1974(7) 0.0351(19) Uani 1 1 d . . . H33 H 0.1840 0.0673 -0.1481 0.042 Uiso 1 1 calc R . . C27 C -0.1536(6) 0.2699(5) -0.3347(6) 0.0334(19) Uani 1 1 d . . . C28 C -0.0864(7) 0.1242(5) -0.3435(7) 0.036(2) Uani 1 1 d . . . C29 C -0.2230(7) 0.2214(6) -0.4155(7) 0.050(2) Uani 1 1 d . . . H29 H -0.2910 0.2377 -0.4652 0.060 Uiso 1 1 calc R . . C30 C -0.0674(7) 0.5423(4) 0.5902(8) 0.044(2) Uani 1 1 d . . . H12 H -0.0251 0.5779 0.6349 0.053 Uiso 1 1 calc R . . C31 C 0.9211(7) 0.2243(5) 0.1034(7) 0.042(2) Uani 1 1 d . . . H34 H 0.9487 0.1811 0.1358 0.051 Uiso 1 1 calc R . . C32 C 0.0543(9) 0.0355(5) -0.2735(8) 0.053(3) Uani 1 1 d . . . H32 H 0.0813 -0.0108 -0.2742 0.063 Uiso 1 1 calc R . . C33 C -0.1752(7) 0.3425(5) -0.3262(7) 0.047(2) Uani 1 1 d . . . H28 H -0.2412 0.3633 -0.3729 0.057 Uiso 1 1 calc R . . C34 C -0.1852(7) 0.5430(5) 0.5438(8) 0.045(2) Uani 1 1 d . . . H11 H -0.2370 0.5788 0.5502 0.054 Uiso 1 1 calc R . . C35 C -0.0461(8) 0.0561(5) -0.3487(8) 0.046(2) Uani 1 1 d . . . H31 H -0.0866 0.0247 -0.4026 0.055 Uiso 1 1 calc R . . C36 C -0.1909(7) 0.1519(6) -0.4204(7) 0.050(3) Uani 1 1 d . . . H30 H -0.2368 0.1221 -0.4738 0.059 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 O1W 0.051(4) 0.048(4) 0.072(5) -0.016(4) 0.017(4) 0.018(3) C1 0.047(5) 0.017(4) 0.037(5) 0.007(4) 0.003(4) -0.004(3) C2 0.044(5) 0.027(4) 0.032(5) -0.009(4) -0.004(4) -0.012(4) C3 0.020(4) 0.041(5) 0.017(4) -0.003(3) 0.001(3) -0.002(3) N1 0.027(3) 0.026(3) 0.032(4) -0.003(3) 0.006(3) 0.001(3) C4 0.033(4) 0.026(4) 0.035(4) 0.004(4) 0.009(4) 0.001(3) N2 0.019(3) 0.036(4) 0.039(4) -0.003(3) -0.011(3) -0.004(3) C5 0.017(3) 0.026(4) 0.025(4) 0.000(3) 0.002(3) -0.002(3) C6 0.031(4) 0.031(4) 0.027(4) 0.001(3) 0.009(4) 0.002(3) C7 0.022(4) 0.023(4) 0.022(4) 0.005(3) 0.006(3) 0.003(3) C8 0.019(4) 0.033(4) 0.013(4) -0.006(3) 0.000(3) -0.009(3) N3 0.027(3) 0.024(3) 0.022(3) 0.002(3) 0.008(3) 0.005(2) C9 0.027(4) 0.022(3) 0.019(4) 0.005(3) 0.004(3) 0.000(3) C10 0.024(4) 0.038(4) 0.023(4) -0.007(4) 0.002(3) 0.001(3) N4 0.031(4) 0.033(4) 0.021(3) 0.000(3) -0.003(3) -0.004(3) N5 0.039(4) 0.019(3) 0.024(4) -0.001(3) -0.002(3) -0.001(3) N6 0.036(4) 0.018(3) 0.018(3) 0.005(3) 0.000(3) 0.001(3) Mo1 0.0173(3) 0.0221(3) 0.0191(3) 0.0018(3) 0.0039(2) -0.0011(2) Mo2 0.0223(3) 0.0179(3) 0.0214(3) 0.0029(3) 0.0036(2) -0.0015(2) Mo3 0.0199(3) 0.0181(3) 0.0247(3) -0.0023(3) 0.0031(2) 0.0019(2) Mo4 0.0227(3) 0.0149(3) 0.0235(3) 0.0001(3) 0.0049(3) -0.0010(2) Mo5 0.0192(3) 0.0222(3) 0.0186(3) 0.0001(3) 0.0048(2) 0.0009(2) Cu1 0.0210(4) 0.0261(5) 0.0214(5) -0.0009(4) 0.0002(4) -0.0014(4) Cu2 0.0231(4) 0.0218(4) 0.0249(5) -0.0048(4) -0.0007(4) -0.0018(4) Cu3 0.0206(4) 0.0298(5) 0.0241(5) 0.0019(4) 0.0007(4) 0.0004(4) P1 0.0157(9) 0.0160(8) 0.0173(9) -0.0018(7) 0.0024(7) 0.0000(6) P2 0.0173(8) 0.0199(9) 0.0157(9) 0.0000(7) 0.0013(7) -0.0011(7) O2 0.038(3) 0.025(3) 0.037(3) -0.008(2) 0.005(3) -0.006(2) O3 0.024(3) 0.026(3) 0.027(3) 0.000(2) 0.009(2) -0.001(2) O4 0.016(2) 0.017(2) 0.020(2) 0.000(2) 0.0021(19) 0.0029(18) O5 0.038(3) 0.023(3) 0.034(3) 0.005(2) 0.003(3) 0.007(2) O6 0.019(2) 0.022(2) 0.016(2) 0.000(2) 0.0048(19) 0.0004(19) O7 0.014(2) 0.022(2) 0.017(3) -0.002(2) 0.0012(19) 0.0016(18) O8 0.015(2) 0.026(2) 0.017(2) -0.003(2) -0.0027(19) -0.0006(18) O9 0.024(3) 0.017(2) 0.019(3) -0.004(2) -0.001(2) -0.0024(19) O10 0.020(2) 0.018(2) 0.021(3) 0.002(2) 0.004(2) 0.0034(18) O11 0.021(2) 0.020(2) 0.024(3) 0.005(2) 0.010(2) 0.0037(19) O12 0.024(2) 0.032(3) 0.026(3) 0.001(2) 0.008(2) 0.005(2) O13 0.020(2) 0.015(2) 0.021(3) -0.001(2) 0.002(2) -0.0027(18) O14 0.035(3) 0.024(3) 0.039(3) 0.000(2) 0.002(3) 0.004(2) N7 0.030(3) 0.023(3) 0.027(4) -0.002(3) 0.002(3) 0.005(3) O15 0.028(3) 0.028(3) 0.033(3) -0.009(2) 0.007(2) 0.004(2) O16 0.017(2) 0.033(3) 0.021(3) -0.002(2) -0.002(2) -0.001(2) N8 0.028(3) 0.030(3) 0.016(3) 0.001(3) -0.004(3) -0.002(3) O17 0.039(3) 0.021(3) 0.031(3) 0.002(2) 0.007(3) 0.004(2) O18 0.029(3) 0.023(3) 0.023(3) 0.007(2) 0.010(2) 0.000(2) O19 0.024(3) 0.035(3) 0.042(4) 0.002(3) 0.003(3) -0.011(2) O20 0.020(2) 0.033(3) 0.024(3) -0.002(2) 0.003(2) -0.003(2) O21 0.029(3) 0.034(3) 0.040(3) 0.001(3) 0.008(3) -0.006(2) N9 0.021(3) 0.037(4) 0.020(3) -0.001(3) -0.004(3) 0.002(3) O22 0.022(3) 0.023(3) 0.028(3) -0.009(2) -0.005(2) -0.001(2) O23 0.026(3) 0.019(2) 0.019(3) 0.005(2) 0.006(2) 0.0005(19) N10 0.021(3) 0.034(4) 0.030(4) -0.002(3) 0.002(3) -0.002(3) O24 0.024(3) 0.025(3) 0.024(3) 0.002(2) 0.009(2) -0.001(2) O25 0.041(3) 0.027(3) 0.024(3) -0.004(2) -0.004(3) 0.002(2) N11 0.017(3) 0.034(3) 0.026(3) -0.009(3) 0.005(3) -0.004(3) N12 0.023(3) 0.027(3) 0.018(3) -0.002(3) -0.001(3) 0.001(2) N13 0.032(4) 0.024(3) 0.027(4) -0.007(3) 0.002(3) -0.002(3) N14 0.023(3) 0.039(4) 0.027(4) 0.003(3) -0.007(3) -0.007(3) C11 0.025(4) 0.026(4) 0.018(4) -0.002(3) -0.001(3) 0.002(3) N15 0.025(3) 0.037(4) 0.030(4) -0.001(3) -0.013(3) 0.004(3) N16 0.027(4) 0.029(4) 0.047(4) -0.003(3) -0.009(3) 0.003(3) C12 0.043(5) 0.024(4) 0.036(5) -0.008(4) 0.001(4) 0.001(3) C13 0.034(4) 0.025(4) 0.039(5) -0.001(4) 0.002(4) 0.004(3) C14 0.028(4) 0.028(4) 0.059(6) -0.008(4) 0.001(4) -0.002(3) C15 0.022(4) 0.032(4) 0.030(4) -0.008(3) 0.006(3) -0.007(3) N17 0.031(4) 0.023(3) 0.026(4) -0.005(3) 0.005(3) 0.001(3) C16 0.055(5) 0.018(4) 0.031(5) 0.001(3) 0.008(4) 0.005(3) C17 0.034(4) 0.030(4) 0.031(4) 0.005(4) 0.006(4) 0.003(4) C18 0.035(4) 0.024(4) 0.038(5) 0.012(4) 0.009(4) 0.007(3) C19 0.040(5) 0.036(5) 0.044(5) 0.018(4) -0.004(4) -0.012(4) N18 0.022(3) 0.028(4) 0.058(5) -0.001(3) 0.002(3) 0.001(3) C20 0.021(4) 0.035(4) 0.022(4) 0.000(3) 0.000(3) 0.005(3) C21 0.027(4) 0.027(4) 0.025(4) 0.004(3) 0.001(3) 0.006(3) C22 0.027(4) 0.031(4) 0.038(5) -0.005(4) 0.013(4) -0.002(3) C23 0.029(4) 0.030(4) 0.040(5) -0.003(4) 0.002(4) -0.004(3) C24 0.054(5) 0.047(5) 0.034(5) 0.009(4) 0.024(4) 0.009(5) C25 0.028(4) 0.034(4) 0.032(5) 0.002(4) 0.001(4) -0.003(3) C26 0.038(5) 0.030(4) 0.030(5) -0.003(4) -0.002(4) 0.001(3) C27 0.021(4) 0.055(5) 0.024(4) 0.009(4) 0.004(3) 0.003(4) C28 0.026(4) 0.051(5) 0.031(5) -0.010(4) 0.008(4) -0.017(4) C29 0.033(5) 0.078(7) 0.036(5) 0.005(5) 0.006(4) -0.009(5) C30 0.035(5) 0.037(5) 0.055(6) -0.010(4) 0.006(4) -0.004(4) C31 0.046(5) 0.034(5) 0.039(5) 0.008(4) -0.002(4) -0.003(4) C32 0.066(7) 0.042(5) 0.056(6) -0.022(5) 0.026(6) -0.025(5) C33 0.034(5) 0.078(7) 0.034(5) 0.018(5) 0.015(4) 0.024(5) C34 0.031(5) 0.037(5) 0.070(7) -0.001(5) 0.018(5) 0.006(4) C35 0.050(6) 0.046(5) 0.045(6) -0.020(5) 0.017(5) -0.031(4) C36 0.038(5) 0.085(7) 0.023(5) -0.020(5) 0.004(4) -0.024(5) _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 O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? C1 C2 1.345(10) . ? C1 N8 1.361(9) . ? C1 H6 0.9300 . ? C2 N4 1.360(9) . ? C2 H5 0.9300 . ? C3 N12 1.362(8) . ? C3 C27 1.416(9) . ? C3 C15 1.420(10) . ? N1 C10 1.334(9) . ? N1 C13 1.367(9) . ? N1 Cu3 2.041(6) . ? C4 C17 1.376(10) . ? C4 N3 1.399(9) . ? C4 H25 0.9300 . ? N2 C5 1.336(9) . ? N2 C23 1.377(9) . ? N2 H2 0.8600 . ? C5 N11 1.327(8) . ? C5 C21 1.448(9) . ? C6 N12 1.323(9) . ? C6 C24 1.378(10) . ? C6 H26 0.9300 . ? C7 N6 1.331(9) . ? C7 N3 1.331(8) . ? C7 C9 1.449(9) . ? C8 N8 1.321(9) . ? C8 N4 1.347(8) . ? C8 C11 1.452(9) . ? N3 Cu3 2.034(6) . ? C9 N5 1.327(8) . ? C9 N17 1.338(9) . ? C10 N16 1.344(9) . ? C10 C20 1.434(10) . ? N4 H4 0.8600 . ? N5 C16 1.364(9) . ? N5 H5A 0.8600 . ? N6 C17 1.386(9) . ? N6 H6A 0.8600 . ? Mo1 O19 1.682(5) . ? Mo1 O12 1.733(5) . ? Mo1 O8 1.921(5) . ? Mo1 O23 1.951(4) . ? Mo1 O4 2.140(4) . ? Mo1 O7 2.464(4) . ? Mo2 O17 1.695(5) . ? Mo2 O21 1.699(5) . ? Mo2 O18 1.926(5) . ? Mo2 O9 1.963(5) . ? Mo2 O11 2.245(4) . ? Mo2 O13 2.348(4) . ? Mo3 O14 1.695(5) . ? Mo3 O15 1.712(5) . ? Mo3 O8 1.918(4) . ? Mo3 O9 1.932(4) . ? Mo3 O13 2.260(4) . ? Mo3 O7 2.359(4) . ? Mo4 O2 1.689(5) . ? Mo4 O5 1.707(5) . ? Mo4 O24 1.917(4) . ? Mo4 O23 1.990(4) . ? Mo4 O10 2.240(4) . ? Mo4 O4 2.320(4) . ? Mo5 O20 1.706(4) . ? Mo5 O3 1.726(5) . ? Mo5 O24 1.895(4) . ? Mo5 O18 1.934(4) . ? Mo5 O6 2.202(4) . ? Mo5 O11 2.384(5) . ? Cu1 N8 1.985(6) . ? Cu1 N11 1.989(6) . ? Cu1 N10 2.019(6) . ? Cu1 N7 2.023(6) . ? Cu1 O3 2.200(5) . ? Cu2 O22 1.876(4) . ? Cu2 O25 1.943(5) . ? Cu2 N12 1.991(6) . ? Cu2 N13 1.992(6) . ? Cu3 N17 1.991(6) . ? Cu3 N14 2.000(6) . ? Cu3 O12 2.222(4) . ? P1 O22 1.519(5) . ? P1 O10 1.523(4) . ? P1 O7 1.541(4) . ? P1 O11 1.555(5) . ? P2 O16 1.502(4) . ? P2 O6 1.525(4) . ? P2 O13 1.552(4) . ? P2 O4 1.566(5) . ? N7 C11 1.341(9) . ? N7 C25 1.376(9) . ? N9 C11 1.317(8) . ? N9 C18 1.365(9) . ? N9 H9 0.8600 . ? N10 C21 1.337(9) . ? N10 C30 1.381(9) . ? O25 H13 0.8200 . ? N11 C22 1.384(9) . ? N13 C26 1.328(9) . ? N13 C15 1.364(9) . ? N14 C20 1.345(9) . ? N14 C19 1.382(10) . ? N15 C20 1.329(9) . ? N15 C31 1.393(10) . ? N15 H15 0.8600 . ? N16 C14 1.343(10) . ? N16 H16 0.8600 . ? C12 C16 1.342(10) . ? C12 N17 1.362(9) . ? C12 H20 0.9300 . ? C13 C14 1.367(10) . ? C13 H19 0.9300 . ? C14 H18 0.9300 . ? C15 C28 1.386(10) . ? C16 H21 0.9300 . ? C17 H24 0.9300 . ? C18 C25 1.370(10) . ? C18 H1 0.9300 . ? C19 C31 1.362(10) . ? C19 H14 0.9300 . ? N18 C21 1.332(9) . ? N18 C34 1.378(10) . ? N18 H18A 0.8600 . ? C22 C23 1.354(9) . ? C22 H7 0.9300 . ? C23 H8 0.9300 . ? C24 C33 1.325(12) . ? C24 H27 0.9300 . ? C25 H2A 0.9300 . ? C26 C32 1.359(11) . ? C26 H33 0.9300 . ? C27 C33 1.399(12) . ? C27 C29 1.447(11) . ? C28 C35 1.375(12) . ? C28 C36 1.448(12) . ? C29 C36 1.368(13) . ? C29 H29 0.9300 . ? C30 C34 1.364(11) . ? C30 H12 0.9300 . ? C31 H34 0.9300 . ? C32 C35 1.362(12) . ? C32 H32 0.9300 . ? C33 H28 0.9300 . ? C34 H11 0.9300 . ? C35 H31 0.9300 . ? C36 H30 0.9300 . ? 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 H1WA O1W H1WB 120.0 . . ? C2 C1 N8 110.7(7) . . ? C2 C1 H6 124.6 . . ? N8 C1 H6 124.6 . . ? C1 C2 N4 105.9(7) . . ? C1 C2 H5 127.0 . . ? N4 C2 H5 127.0 . . ? N12 C3 C27 122.1(7) . . ? N12 C3 C15 116.3(6) . . ? C27 C3 C15 121.6(7) . . ? C10 N1 C13 105.1(6) . . ? C10 N1 Cu3 111.7(5) . . ? C13 N1 Cu3 140.9(5) . . ? C17 C4 N3 108.9(7) . . ? C17 C4 H25 125.5 . . ? N3 C4 H25 125.5 . . ? C5 N2 C23 107.6(6) . . ? C5 N2 H2 126.2 . . ? C23 N2 H2 126.2 . . ? N11 C5 N2 111.0(6) . . ? N11 C5 C21 116.8(6) . . ? N2 C5 C21 132.2(7) . . ? N12 C6 C24 122.6(8) . . ? N12 C6 H26 118.7 . . ? C24 C6 H26 118.7 . . ? N6 C7 N3 112.4(6) . . ? N6 C7 C9 131.8(7) . . ? N3 C7 C9 115.8(7) . . ? N8 C8 N4 111.1(7) . . ? N8 C8 C11 117.2(6) . . ? N4 C8 C11 131.5(7) . . ? C7 N3 C4 105.1(6) . . ? C7 N3 Cu3 112.2(5) . . ? C4 N3 Cu3 142.7(5) . . ? N5 C9 N17 110.8(6) . . ? N5 C9 C7 132.0(7) . . ? N17 C9 C7 117.2(6) . . ? N1 C10 N16 110.8(7) . . ? N1 C10 C20 116.8(6) . . ? N16 C10 C20 131.8(7) . . ? C8 N4 C2 107.2(6) . . ? C8 N4 H4 126.4 . . ? C2 N4 H4 126.4 . . ? C9 N5 C16 107.4(6) . . ? C9 N5 H5A 126.3 . . ? C16 N5 H5A 126.3 . . ? C7 N6 C17 107.6(6) . . ? C7 N6 H6A 126.2 . . ? C17 N6 H6A 126.2 . . ? O19 Mo1 O12 104.9(2) . . ? O19 Mo1 O8 96.3(2) . . ? O12 Mo1 O8 100.6(2) . . ? O19 Mo1 O23 99.7(2) . . ? O12 Mo1 O23 96.1(2) . . ? O8 Mo1 O23 152.97(19) . . ? O19 Mo1 O4 102.3(2) . . ? O12 Mo1 O4 152.15(18) . . ? O8 Mo1 O4 82.15(18) . . ? O23 Mo1 O4 73.28(17) . . ? O19 Mo1 O7 167.3(2) . . ? O12 Mo1 O7 82.82(19) . . ? O8 Mo1 O7 72.05(16) . . ? O23 Mo1 O7 89.32(16) . . ? O4 Mo1 O7 71.60(15) . . ? O17 Mo2 O21 104.3(2) . . ? O17 Mo2 O18 97.3(2) . . ? O21 Mo2 O18 101.4(2) . . ? O17 Mo2 O9 99.6(2) . . ? O21 Mo2 O9 96.7(2) . . ? O18 Mo2 O9 151.28(18) . . ? O17 Mo2 O11 161.7(2) . . ? O21 Mo2 O11 93.3(2) . . ? O18 Mo2 O11 73.99(18) . . ? O9 Mo2 O11 82.95(17) . . ? O17 Mo2 O13 91.1(2) . . ? O21 Mo2 O13 162.0(2) . . ? O18 Mo2 O13 85.47(17) . . ? O9 Mo2 O13 71.19(17) . . ? O11 Mo2 O13 72.43(15) . . ? O14 Mo3 O15 103.9(2) . . ? O14 Mo3 O8 98.2(2) . . ? O15 Mo3 O8 100.8(2) . . ? O14 Mo3 O9 103.2(2) . . ? O15 Mo3 O9 98.6(2) . . ? O8 Mo3 O9 146.62(19) . . ? O14 Mo3 O13 89.9(2) . . ? O15 Mo3 O13 165.56(19) . . ? O8 Mo3 O13 81.00(17) . . ? O9 Mo3 O13 73.73(17) . . ? O14 Mo3 O7 169.0(2) . . ? O15 Mo3 O7 85.82(19) . . ? O8 Mo3 O7 74.63(17) . . ? O9 Mo3 O7 80.05(17) . . ? O13 Mo3 O7 80.84(15) . . ? O2 Mo4 O5 102.2(2) . . ? O2 Mo4 O24 100.3(2) . . ? O5 Mo4 O24 103.3(2) . . ? O2 Mo4 O23 99.3(2) . . ? O5 Mo4 O23 98.7(2) . . ? O24 Mo4 O23 146.56(18) . . ? O2 Mo4 O10 169.5(2) . . ? O5 Mo4 O10 88.1(2) . . ? O24 Mo4 O10 78.72(18) . . ? O23 Mo4 O10 77.15(17) . . ? O2 Mo4 O4 86.3(2) . . ? O5 Mo4 O4 166.0(2) . . ? O24 Mo4 O4 85.83(17) . . ? O23 Mo4 O4 68.66(16) . . ? O10 Mo4 O4 83.22(15) . . ? O20 Mo5 O3 102.6(2) . . ? O20 Mo5 O24 98.2(2) . . ? O3 Mo5 O24 102.3(2) . . ? O20 Mo5 O18 99.9(2) . . ? O3 Mo5 O18 100.3(2) . . ? O24 Mo5 O18 147.12(19) . . ? O20 Mo5 O6 171.54(19) . . ? O3 Mo5 O6 85.78(19) . . ? O24 Mo5 O6 81.16(18) . . ? O18 Mo5 O6 76.96(18) . . ? O20 Mo5 O11 83.74(19) . . ? O3 Mo5 O11 169.91(19) . . ? O24 Mo5 O11 84.40(18) . . ? O18 Mo5 O11 70.63(18) . . ? O6 Mo5 O11 87.80(15) . . ? N8 Cu1 N11 173.5(2) . . ? N8 Cu1 N10 94.9(2) . . ? N11 Cu1 N10 83.0(2) . . ? N8 Cu1 N7 81.6(2) . . ? N11 Cu1 N7 97.5(2) . . ? N10 Cu1 N7 153.0(2) . . ? N8 Cu1 O3 94.9(2) . . ? N11 Cu1 O3 91.7(2) . . ? N10 Cu1 O3 106.8(2) . . ? N7 Cu1 O3 100.2(2) . . ? O22 Cu2 O25 94.7(2) . . ? O22 Cu2 N12 91.5(2) . . ? O25 Cu2 N12 170.4(2) . . ? O22 Cu2 N13 173.0(2) . . ? O25 Cu2 N13 91.0(2) . . ? N12 Cu2 N13 82.3(2) . . ? N17 Cu3 N14 173.1(3) . . ? N17 Cu3 N3 82.0(2) . . ? N14 Cu3 N3 97.5(2) . . ? N17 Cu3 N1 95.4(2) . . ? N14 Cu3 N1 81.7(2) . . ? N3 Cu3 N1 151.3(2) . . ? N17 Cu3 O12 90.3(2) . . ? N14 Cu3 O12 96.6(2) . . ? N3 Cu3 O12 100.8(2) . . ? N1 Cu3 O12 107.9(2) . . ? O22 P1 O10 108.7(3) . . ? O22 P1 O7 111.0(3) . . ? O10 P1 O7 110.2(2) . . ? O22 P1 O11 108.4(3) . . ? O10 P1 O11 107.5(3) . . ? O7 P1 O11 110.9(3) . . ? O16 P2 O6 112.4(3) . . ? O16 P2 O13 111.7(3) . . ? O6 P2 O13 107.7(2) . . ? O16 P2 O4 110.4(3) . . ? O6 P2 O4 105.6(2) . . ? O13 P2 O4 108.8(3) . . ? Mo5 O3 Cu1 135.5(2) . . ? P2 O4 Mo1 127.3(2) . . ? P2 O4 Mo4 133.7(2) . . ? Mo1 O4 Mo4 99.02(17) . . ? P2 O6 Mo5 124.6(2) . . ? P1 O7 Mo3 128.0(3) . . ? P1 O7 Mo1 124.9(2) . . ? Mo3 O7 Mo1 89.26(14) . . ? Mo3 O8 Mo1 124.0(2) . . ? Mo3 O9 Mo2 120.5(2) . . ? P1 O10 Mo4 125.6(3) . . ? P1 O11 Mo2 130.8(3) . . ? P1 O11 Mo5 133.5(2) . . ? Mo2 O11 Mo5 93.45(17) . . ? Mo1 O12 Cu3 140.2(2) . . ? P2 O13 Mo3 124.3(2) . . ? P2 O13 Mo2 131.2(2) . . ? Mo3 O13 Mo2 94.39(16) . . ? C11 N7 C25 105.1(6) . . ? C11 N7 Cu1 112.7(5) . . ? C25 N7 Cu1 142.2(5) . . ? C8 N8 C1 105.0(6) . . ? C8 N8 Cu1 113.0(5) . . ? C1 N8 Cu1 141.3(5) . . ? Mo2 O18 Mo5 121.8(2) . . ? C11 N9 C18 107.7(6) . . ? C11 N9 H9 126.1 . . ? C18 N9 H9 126.1 . . ? P1 O22 Cu2 152.0(3) . . ? Mo1 O23 Mo4 118.9(2) . . ? C21 N10 C30 104.1(6) . . ? C21 N10 Cu1 110.7(5) . . ? C30 N10 Cu1 142.9(6) . . ? Mo5 O24 Mo4 147.1(3) . . ? Cu2 O25 H13 109.5 . . ? C5 N11 C22 105.9(6) . . ? C5 N11 Cu1 112.2(5) . . ? C22 N11 Cu1 141.7(5) . . ? C6 N12 C3 117.6(6) . . ? C6 N12 Cu2 130.0(5) . . ? C3 N12 Cu2 112.4(5) . . ? C26 N13 C15 115.8(6) . . ? C26 N13 Cu2 131.7(5) . . ? C15 N13 Cu2 112.5(5) . . ? C20 N14 C19 106.7(6) . . ? C20 N14 Cu3 112.7(5) . . ? C19 N14 Cu3 140.6(5) . . ? N9 C11 N7 111.8(6) . . ? N9 C11 C8 133.5(7) . . ? N7 C11 C8 114.6(6) . . ? C20 N15 C31 108.1(6) . . ? C20 N15 H15 125.9 . . ? C31 N15 H15 125.9 . . ? C14 N16 C10 108.1(7) . . ? C14 N16 H16 126.0 . . ? C10 N16 H16 126.0 . . ? C16 C12 N17 109.6(7) . . ? C16 C12 H20 125.2 . . ? N17 C12 H20 125.2 . . ? N1 C13 C14 109.7(7) . . ? N1 C13 H19 125.2 . . ? C14 C13 H19 125.2 . . ? N16 C14 C13 106.3(7) . . ? N16 C14 H18 126.8 . . ? C13 C14 H18 126.8 . . ? N13 C15 C28 123.4(7) . . ? N13 C15 C3 116.0(6) . . ? C28 C15 C3 120.6(7) . . ? C9 N17 C12 105.4(6) . . ? C9 N17 Cu3 112.5(5) . . ? C12 N17 Cu3 141.9(5) . . ? C12 C16 N5 106.7(7) . . ? C12 C16 H21 126.6 . . ? N5 C16 H21 126.6 . . ? C4 C17 N6 106.0(7) . . ? C4 C17 H24 127.0 . . ? N6 C17 H24 127.0 . . ? N9 C18 C25 106.6(6) . . ? N9 C18 H1 126.7 . . ? C25 C18 H1 126.7 . . ? C31 C19 N14 108.6(7) . . ? C31 C19 H14 125.7 . . ? N14 C19 H14 125.7 . . ? C21 N18 C34 106.4(7) . . ? C21 N18 H18A 126.8 . . ? C34 N18 H18A 126.8 . . ? N15 C20 N14 110.3(7) . . ? N15 C20 C10 132.7(7) . . ? N14 C20 C10 116.8(7) . . ? N18 C21 N10 113.0(7) . . ? N18 C21 C5 130.1(7) . . ? N10 C21 C5 116.8(6) . . ? C23 C22 N11 109.0(7) . . ? C23 C22 H7 125.5 . . ? N11 C22 H7 125.5 . . ? C22 C23 N2 106.5(7) . . ? C22 C23 H8 126.8 . . ? N2 C23 H8 126.8 . . ? C33 C24 C6 121.2(8) . . ? C33 C24 H27 119.4 . . ? C6 C24 H27 119.4 . . ? C18 C25 N7 108.8(7) . . ? C18 C25 H2A 125.6 . . ? N7 C25 H2A 125.6 . . ? N13 C26 C32 123.9(8) . . ? N13 C26 H33 118.1 . . ? C32 C26 H33 118.1 . . ? C33 C27 C3 117.1(8) . . ? C33 C27 C29 126.1(8) . . ? C3 C27 C29 116.8(8) . . ? C35 C28 C15 117.8(8) . . ? C35 C28 C36 123.4(8) . . ? C15 C28 C36 118.6(8) . . ? C36 C29 C27 121.5(8) . . ? C36 C29 H29 119.3 . . ? C27 C29 H29 119.3 . . ? C34 C30 N10 109.9(7) . . ? C34 C30 H12 125.1 . . ? N10 C30 H12 125.1 . . ? C19 C31 N15 106.3(7) . . ? C19 C31 H34 126.9 . . ? N15 C31 H34 126.9 . . ? C26 C32 C35 120.0(9) . . ? C26 C32 H32 120.0 . . ? C35 C32 H32 120.0 . . ? C24 C33 C27 119.4(8) . . ? C24 C33 H28 120.3 . . ? C27 C33 H28 120.3 . . ? C30 C34 N18 106.5(7) . . ? C30 C34 H11 126.7 . . ? N18 C34 H11 126.7 . . ? C32 C35 C28 118.9(8) . . ? C32 C35 H31 120.6 . . ? C28 C35 H31 120.6 . . ? C29 C36 C28 120.9(8) . . ? C29 C36 H30 119.6 . . ? C28 C36 H30 119.6 . . ? 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 N16 H16 O10 0.86 2.07 2.796(8) 141.6 1_655 N15 H15 O11 0.86 2.48 3.316(7) 162.8 1_655 N15 H15 O20 0.86 2.35 2.867(8) 118.8 1_655 O25 H13 O9 0.82 1.86 2.628(7) 156.4 . N9 H9 O7 0.86 2.29 2.952(8) 133.7 1_556 N9 H9 O12 0.86 2.21 2.968(7) 146.8 1_556 N6 H6A O18 0.86 2.38 3.191(7) 156.5 1_554 N6 H6A O6 0.86 2.35 3.033(7) 136.3 1_554 N5 H5A O3 0.86 2.58 3.261(8) 136.7 1_554 N5 H5A O6 0.86 1.96 2.710(7) 144.4 1_554 N4 H4 O23 0.86 1.90 2.730(7) 160.5 1_556 N2 H2 O16 0.86 2.42 2.938(8) 119.1 1_455 N2 H2 O8 0.86 2.08 2.872(7) 153.0 1_455 O1W H1WB O25 0.85 2.19 2.622(8) 111.1 1_556 O1W H1WA O23 0.85 2.09 2.773(7) 136.8 2_646 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.830 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.140 # Attachment '4.cif' data_jhj126_0m _database_code_depnum_ccdc_archive 'CCDC 720601' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H14 Cu2 Mg Mo5 N8 O25 P2, 2(H2 O), 2(O) ' _chemical_formula_sum 'C12 H18 Cu2 Mg Mo5 N8 O29 P2' _chemical_formula_weight 1431.39 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' Mg Mg 0.0486 0.0363 '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' Cu Cu 0.3201 1.2651 '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 C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 20.7624(7) _cell_length_b 11.4376(4) _cell_length_c 16.7341(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.6620(10) _cell_angle_gamma 90.00 _cell_volume 3877.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3270 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 25.95 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 2.452 _exptl_crystal_density_diffrn 2.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752.0 _exptl_absorpt_coefficient_mu 2.847 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.540 _exptl_absorpt_correction_T_max 0.634 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14259 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4816 _reflns_number_gt 3528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0537P)^2^+19.6288P] 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 4816 _refine_ls_number_parameters 279 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.083 _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 O3W O 0.0474(3) 0.3441(5) 0.8889(4) 0.0675(18) Uani 1 1 d . . . H3WA H 0.0101 0.3108 0.8740 0.081 Uiso 1 1 d R . . H3WB H 0.0569 0.3809 0.9341 0.081 Uiso 1 1 d R . . Mo1 Mo 1.07907(3) -0.10755(4) 0.21859(3) 0.02164(14) Uani 1 1 d . . . Mo2 Mo 1.0000 0.34939(6) 0.2500 0.02458(18) Uani 1 2 d S . . Mo3 Mo 1.09799(3) 0.17059(5) 0.16452(3) 0.02382(14) Uani 1 1 d . . . Cu1 Cu 0.88888(4) 0.23945(6) -0.02636(5) 0.02444(18) Uani 1 1 d . . . P1 P 0.93872(7) 0.09153(13) 0.14721(9) 0.0198(3) Uani 1 1 d . . . Mg1 Mg 1.0000 0.0000 0.0000 0.0270(7) Uani 1 2 d S . . O4 O 1.0000 -0.1584(5) 0.2500 0.0226(12) Uani 1 2 d S . . O5 O 1.01397(18) 0.0613(3) 0.1686(2) 0.0205(8) Uani 1 1 d . . . O6 O 1.0336(2) 0.2972(4) 0.1593(3) 0.0264(9) Uani 1 1 d . . . O7 O 0.90326(19) -0.0189(3) 0.1641(2) 0.0229(9) Uani 1 1 d . . . O8 O 0.9204(2) 0.1256(4) 0.0576(3) 0.0294(10) Uani 1 1 d . . . O9 O 1.13553(19) 0.0231(3) 0.2027(2) 0.0235(9) Uani 1 1 d . . . O10 O 1.0585(2) -0.1488(4) 0.1164(3) 0.0272(9) Uani 1 1 d . . . O11 O 1.0900(2) 0.1575(4) 0.0611(3) 0.0347(11) Uani 1 1 d . . . O12 O 1.1691(2) 0.2485(4) 0.1991(3) 0.0332(11) Uani 1 1 d . . . O13 O 0.9398(2) 0.4409(4) 0.1995(3) 0.0366(11) Uani 1 1 d . . . O14 O 0.9244(2) 0.1936(4) 0.2026(2) 0.0246(9) Uani 1 1 d . . . N3 N 0.8005(3) 0.1646(4) -0.0555(3) 0.0287(12) Uani 1 1 d . . . O15 O 0.9660(2) 0.3443(4) 0.0056(3) 0.0358(11) Uani 1 1 d . . . H15 H 0.9849 0.3307 0.0530 0.054 Uiso 1 1 calc R . . O16 O 1.1353(2) -0.2099(4) 0.2597(3) 0.0348(11) Uani 1 1 d . . . N4 N 0.8435(3) 0.3586(4) -0.1047(3) 0.0288(12) Uani 1 1 d . . . C1 C 0.7558(3) 0.2262(6) -0.1069(4) 0.0291(14) Uani 1 1 d . . . C2 C 0.7798(3) 0.3343(5) -0.1353(4) 0.0288(14) Uani 1 1 d . . . N1 N 0.6965(3) 0.1737(5) -0.1223(3) 0.0335(13) Uani 1 1 d . . . H1 H 0.6607 0.1988 -0.1539 0.040 Uiso 1 1 calc R . . N2 N 0.7519(3) 0.4179(5) -0.1867(4) 0.0422(16) Uani 1 1 d . . . H2 H 0.7112 0.4208 -0.2125 0.051 Uiso 1 1 calc R . . C3 C 0.8566(4) 0.4606(6) -0.1399(5) 0.0439(19) Uani 1 1 d . . . H3 H 0.8973 0.4981 -0.1306 0.053 Uiso 1 1 calc R . . C4 C 0.7683(4) 0.0668(7) -0.0371(5) 0.0414(18) Uani 1 1 d . . . H4 H 0.7871 0.0065 -0.0025 0.050 Uiso 1 1 calc R . . C5 C 0.8002(4) 0.4988(7) -0.1908(5) 0.058(3) Uani 1 1 d . . . H5 H 0.7953 0.5664 -0.2224 0.070 Uiso 1 1 calc R . . C6 C 0.7042(4) 0.0727(7) -0.0780(5) 0.0409(18) Uani 1 1 d . . . H6 H 0.6715 0.0179 -0.0760 0.049 Uiso 1 1 calc R . . O1W O 0.7815(8) 0.7594(10) 0.0564(8) 0.080(4) Uani 0.50 1 d PU . . O2W O 0.7088(6) 0.7615(11) 0.0227(11) 0.076(4) Uani 0.50 1 d PU . . 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 O3W 0.077(5) 0.062(4) 0.066(4) -0.004(3) 0.022(4) -0.029(3) Mo1 0.0228(3) 0.0214(3) 0.0211(3) -0.0019(2) 0.0058(2) 0.00141(19) Mo2 0.0250(4) 0.0216(4) 0.0263(4) 0.000 0.0037(3) 0.000 Mo3 0.0205(3) 0.0269(3) 0.0245(3) 0.0011(2) 0.0059(2) -0.0032(2) Cu1 0.0226(4) 0.0252(4) 0.0242(4) 0.0034(3) 0.0021(3) 0.0004(3) P1 0.0177(7) 0.0234(8) 0.0178(7) 0.0026(6) 0.0026(6) 0.0001(6) Mg1 0.0288(16) 0.0322(16) 0.0204(15) -0.0056(12) 0.0063(12) 0.0061(13) O4 0.024(3) 0.019(3) 0.025(3) 0.000 0.008(2) 0.000 O5 0.016(2) 0.022(2) 0.023(2) -0.0001(17) 0.0045(16) -0.0006(15) O6 0.028(2) 0.022(2) 0.029(2) 0.0064(18) 0.0071(18) -0.0004(17) O7 0.022(2) 0.025(2) 0.021(2) 0.0017(17) 0.0023(17) -0.0041(16) O8 0.030(2) 0.034(2) 0.021(2) 0.0070(19) 0.0010(18) -0.0031(19) O9 0.018(2) 0.028(2) 0.026(2) -0.0019(18) 0.0065(17) -0.0015(16) O10 0.031(2) 0.028(2) 0.025(2) -0.0050(18) 0.0117(19) 0.0001(18) O11 0.028(2) 0.049(3) 0.030(3) 0.005(2) 0.012(2) 0.000(2) O12 0.030(3) 0.030(2) 0.039(3) 0.001(2) 0.005(2) -0.0069(19) O13 0.036(3) 0.031(2) 0.042(3) 0.004(2) 0.007(2) 0.008(2) O14 0.023(2) 0.027(2) 0.024(2) -0.0020(18) 0.0068(17) 0.0030(17) N3 0.025(3) 0.029(3) 0.030(3) 0.008(2) 0.001(2) 0.001(2) O15 0.032(3) 0.037(3) 0.031(3) 0.007(2) -0.008(2) -0.005(2) O16 0.035(3) 0.032(2) 0.037(3) 0.000(2) 0.006(2) 0.012(2) N4 0.026(3) 0.025(3) 0.034(3) 0.004(2) 0.003(2) -0.001(2) C1 0.027(3) 0.028(3) 0.029(3) 0.003(3) 0.001(3) -0.001(3) C2 0.028(3) 0.026(3) 0.030(3) 0.001(3) -0.001(3) 0.002(2) N1 0.024(3) 0.040(3) 0.033(3) 0.004(3) -0.003(2) -0.006(2) N2 0.037(3) 0.028(3) 0.051(4) 0.007(3) -0.013(3) -0.004(3) C3 0.040(4) 0.032(4) 0.053(5) 0.014(3) -0.006(4) -0.011(3) C4 0.034(4) 0.038(4) 0.049(5) 0.014(3) 0.004(3) -0.005(3) C5 0.063(6) 0.031(4) 0.065(6) 0.018(4) -0.021(4) -0.017(4) C6 0.036(4) 0.040(4) 0.044(4) 0.013(3) 0.004(3) -0.012(3) O1W 0.117(8) 0.039(5) 0.054(6) 0.009(5) -0.050(6) -0.027(6) O2W 0.062(6) 0.059(6) 0.138(9) 0.015(6) 0.091(6) 0.032(5) _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 O3W H3WA 0.8500 . ? O3W H3WB 0.8501 . ? Mo1 O16 1.689(4) . ? Mo1 O10 1.734(4) . ? Mo1 O4 1.9204(17) . ? Mo1 O9 1.953(4) . ? Mo1 O7 2.168(4) 2_755 ? Mo1 O5 2.400(4) . ? Mo2 O13 1.706(4) 2_755 ? Mo2 O13 1.706(4) . ? Mo2 O6 1.901(4) . ? Mo2 O6 1.901(4) 2_755 ? Mo2 O14 2.392(4) 2_755 ? Mo2 O14 2.392(4) . ? Mo3 O11 1.708(5) . ? Mo3 O12 1.712(4) . ? Mo3 O9 1.909(4) . ? Mo3 O6 1.959(4) . ? Mo3 O5 2.159(4) . ? Mo3 O14 2.384(4) 2_755 ? Cu1 O8 1.923(4) . ? Cu1 O15 1.978(4) . ? Cu1 N4 1.980(5) . ? Cu1 N3 1.986(5) . ? Cu1 O10 2.295(4) 5_755 ? P1 O8 1.514(4) . ? P1 O7 1.520(4) . ? P1 O14 1.559(4) . ? P1 O5 1.563(4) . ? Mg1 O8 2.534(5) 5_755 ? Mg1 O8 2.534(5) . ? Mg1 O11 2.635(5) . ? Mg1 O11 2.635(5) 5_755 ? Mg1 O10 2.670(4) . ? Mg1 O10 2.670(4) 5_755 ? Mg1 P1 3.1871(16) 5_755 ? O4 Mo1 1.9204(17) 2_755 ? O7 Mo1 2.168(4) 2_755 ? O10 Cu1 2.295(4) 5_755 ? O14 Mo3 2.384(4) 2_755 ? N3 C1 1.323(8) . ? N3 C4 1.373(8) . ? O15 H15 0.8200 . ? N4 C2 1.339(8) . ? N4 C3 1.361(8) . ? C1 N1 1.343(8) . ? C1 C2 1.452(9) . ? C2 N2 1.331(8) . ? N1 C6 1.363(9) . ? N1 H1 0.8600 . ? N2 C5 1.378(9) . ? N2 H2 0.8600 . ? C3 C5 1.360(10) . ? C3 H3 0.9300 . ? C4 C6 1.358(10) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? O1W O2W 1.403(18) 7_665 ? O2W O1W 1.403(18) 7_665 ? 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 H3WA O3W H3WB 120.0 . . ? O16 Mo1 O10 102.3(2) . . ? O16 Mo1 O4 103.5(2) . . ? O10 Mo1 O4 98.42(15) . . ? O16 Mo1 O9 101.8(2) . . ? O10 Mo1 O9 95.73(19) . . ? O4 Mo1 O9 147.53(19) . . ? O16 Mo1 O7 89.45(19) . 2_755 ? O10 Mo1 O7 167.42(18) . 2_755 ? O4 Mo1 O7 83.05(14) . 2_755 ? O9 Mo1 O7 77.17(16) . 2_755 ? O16 Mo1 O5 170.26(19) . . ? O10 Mo1 O5 82.92(17) . . ? O4 Mo1 O5 83.64(16) . . ? O9 Mo1 O5 69.27(15) . . ? O7 Mo1 O5 84.84(14) 2_755 . ? O13 Mo2 O13 104.3(3) 2_755 . ? O13 Mo2 O6 103.3(2) 2_755 . ? O13 Mo2 O6 98.9(2) . . ? O13 Mo2 O6 98.9(2) 2_755 2_755 ? O13 Mo2 O6 103.3(2) . 2_755 ? O6 Mo2 O6 143.4(2) . 2_755 ? O13 Mo2 O14 86.38(19) 2_755 2_755 ? O13 Mo2 O14 167.91(19) . 2_755 ? O6 Mo2 O14 72.64(16) . 2_755 ? O6 Mo2 O14 80.23(16) 2_755 2_755 ? O13 Mo2 O14 167.91(19) 2_755 . ? O13 Mo2 O14 86.38(19) . . ? O6 Mo2 O14 80.23(16) . . ? O6 Mo2 O14 72.64(16) 2_755 . ? O14 Mo2 O14 83.69(19) 2_755 . ? O11 Mo3 O12 105.9(2) . . ? O11 Mo3 O9 101.7(2) . . ? O12 Mo3 O9 95.05(19) . . ? O11 Mo3 O6 96.1(2) . . ? O12 Mo3 O6 99.2(2) . . ? O9 Mo3 O6 153.19(17) . . ? O11 Mo3 O5 94.67(19) . . ? O12 Mo3 O5 158.88(19) . . ? O9 Mo3 O5 75.58(16) . . ? O6 Mo3 O5 83.20(16) . . ? O11 Mo3 O14 163.52(18) . 2_755 ? O12 Mo3 O14 87.54(19) . 2_755 ? O9 Mo3 O14 86.21(16) . 2_755 ? O6 Mo3 O14 71.91(16) . 2_755 ? O5 Mo3 O14 73.16(14) . 2_755 ? O8 Cu1 O15 95.00(18) . . ? O8 Cu1 N4 170.5(2) . . ? O15 Cu1 N4 90.0(2) . . ? O8 Cu1 N3 92.05(19) . . ? O15 Cu1 N3 167.7(2) . . ? N4 Cu1 N3 81.6(2) . . ? O8 Cu1 O10 92.25(18) . 5_755 ? O15 Cu1 O10 88.70(19) . 5_755 ? N4 Cu1 O10 95.9(2) . 5_755 ? N3 Cu1 O10 101.1(2) . 5_755 ? O8 P1 O7 111.8(2) . . ? O8 P1 O14 110.9(2) . . ? O7 P1 O14 110.4(2) . . ? O8 P1 O5 107.7(2) . . ? O7 P1 O5 105.9(2) . . ? O14 P1 O5 109.9(2) . . ? O8 Mg1 O8 180.0 5_755 . ? O8 Mg1 O11 93.98(14) 5_755 . ? O8 Mg1 O11 86.02(14) . . ? O8 Mg1 O11 86.02(14) 5_755 5_755 ? O8 Mg1 O11 93.98(14) . 5_755 ? O11 Mg1 O11 180.0 . 5_755 ? O8 Mg1 O10 71.73(13) 5_755 . ? O8 Mg1 O10 108.27(13) . . ? O11 Mg1 O10 88.97(13) . . ? O11 Mg1 O10 91.03(13) 5_755 . ? O8 Mg1 O10 108.27(13) 5_755 5_755 ? O8 Mg1 O10 71.73(13) . 5_755 ? O11 Mg1 O10 91.03(13) . 5_755 ? O11 Mg1 O10 88.97(13) 5_755 5_755 ? O10 Mg1 O10 180.0 . 5_755 ? O8 Mg1 P1 27.82(9) 5_755 5_755 ? O8 Mg1 P1 152.18(9) . 5_755 ? O11 Mg1 P1 98.94(10) . 5_755 ? O11 Mg1 P1 81.06(10) 5_755 5_755 ? O10 Mg1 P1 99.21(9) . 5_755 ? O10 Mg1 P1 80.79(9) 5_755 5_755 ? Mo1 O4 Mo1 144.7(3) 2_755 . ? P1 O5 Mo3 129.7(2) . . ? P1 O5 Mo1 135.7(2) . . ? Mo3 O5 Mo1 94.57(14) . . ? Mo2 O6 Mo3 124.3(2) . . ? P1 O7 Mo1 124.4(2) . 2_755 ? P1 O8 Cu1 150.4(3) . . ? P1 O8 Mg1 100.8(2) . . ? Cu1 O8 Mg1 104.58(19) . . ? Mo3 O9 Mo1 120.6(2) . . ? Mo1 O10 Cu1 136.1(2) . 5_755 ? Mo1 O10 Mg1 121.4(2) . . ? Cu1 O10 Mg1 90.83(14) 5_755 . ? Mo3 O11 Mg1 110.9(2) . . ? P1 O14 Mo3 125.0(2) . 2_755 ? P1 O14 Mo2 124.0(2) . . ? Mo3 O14 Mo2 91.18(14) 2_755 . ? C1 N3 C4 105.8(5) . . ? C1 N3 Cu1 114.2(4) . . ? C4 N3 Cu1 140.0(4) . . ? Cu1 O15 H15 109.5 . . ? C2 N4 C3 106.6(5) . . ? C2 N4 Cu1 113.4(4) . . ? C3 N4 Cu1 140.0(5) . . ? N3 C1 N1 111.7(6) . . ? N3 C1 C2 115.1(6) . . ? N1 C1 C2 133.2(6) . . ? N2 C2 N4 110.6(6) . . ? N2 C2 C1 133.7(6) . . ? N4 C2 C1 115.7(5) . . ? C1 N1 C6 106.3(5) . . ? C1 N1 H1 126.8 . . ? C6 N1 H1 126.8 . . ? C2 N2 C5 107.2(6) . . ? C2 N2 H2 126.4 . . ? C5 N2 H2 126.4 . . ? C5 C3 N4 108.7(6) . . ? C5 C3 H3 125.6 . . ? N4 C3 H3 125.6 . . ? C6 C4 N3 108.6(6) . . ? C6 C4 H4 125.7 . . ? N3 C4 H4 125.7 . . ? C3 C5 N2 106.8(6) . . ? C3 C5 H5 126.6 . . ? N2 C5 H5 126.6 . . ? C4 C6 N1 107.6(6) . . ? C4 C6 H6 126.2 . . ? N1 C6 H6 126.2 . . ? 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 O15 H15 O6 0.82 1.88 2.701(6) 176.0 . O3W H3WA O10 0.85 2.36 3.122(7) 148.8 5_656 N1 H1 O14 0.86 2.16 2.988(7) 161.0 7_655 N1 H1 O12 0.86 2.58 3.049(7) 115.8 8_455 N1 H1 O13 0.86 2.61 3.129(7) 120.2 7_655 N2 H2 O9 0.86 1.98 2.785(7) 155.5 8_455 N2 H2 O12 0.86 2.48 2.964(7) 116.6 8_455 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.789 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.170