# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Hai Fu' _publ_contact_author_email fuh170@nenu.edu.cn loop_ _publ_author_name 'Hai Fu' 'Chao Qin' 'Yang-Guang Li' 'Ying Lu' 'En-Bo Wang' data_1 _database_code_depnum_ccdc_archive 'CCDC 832445' #TrackingRef '- compound-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 Cu4 Mo8 N18 O26' _chemical_formula_weight 2158.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.469(3) _cell_length_b 13.905(3) _cell_length_c 18.135(4) _cell_angle_alpha 88.61(3) _cell_angle_beta 70.12(3) _cell_angle_gamma 73.73(3) _cell_volume 2829.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0.371 _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2076 _exptl_absorpt_coefficient_mu 3.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.519 _exptl_absorpt_process_details ? _exptl_special_details ; Higashi, T. (1995) A program for absorption correction. RIGAKU corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18597 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.1026 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9239 _reflns_number_gt 5909 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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. During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree. The highest residual peak and the deepest hole are both close to the heavy metal centers and featureless. ; _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^)+(0.1028P)^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 SHELXL _refine_ls_number_reflns 9239 _refine_ls_number_parameters 819 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1937 _refine_ls_wR_factor_gt 0.1604 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -1.51493(10) -0.39065(8) 0.05602(7) 0.0214(3) Uani 1 1 d . . . Mo2 Mo -1.75435(10) -0.41827(8) 0.04116(7) 0.0240(3) Uani 1 1 d . . . Mo3 Mo -1.77907(10) -0.91558(8) -0.49121(7) 0.0259(3) Uani 1 1 d . . . Mo4 Mo -1.50303(10) -0.87188(8) -0.47200(7) 0.0260(3) Uani 1 1 d . . . Mo5 Mo -1.63090(11) -0.41985(9) -0.14913(7) 0.0272(3) Uani 1 1 d . . . Mo6 Mo -1.38803(10) -0.39627(8) -0.13197(7) 0.0245(3) Uani 1 1 d . . . Mo7 Mo -1.71773(10) -1.00741(9) -0.33279(7) 0.0282(3) Uani 1 1 d . . . Mo8 Mo -1.56265(12) -0.90862(10) -0.66413(8) 0.0386(4) Uani 1 1 d . . . Cu1 Cu -1.46432(19) -0.28521(17) -0.77490(12) 0.0493(5) Uani 1 1 d . . . Cu2 Cu -2.37756(18) -0.95043(16) -0.15770(15) 0.0548(6) Uani 1 1 d . . . Cu3 Cu -1.62981(17) -0.54376(15) -0.34318(14) 0.0463(5) Uani 1 1 d . . . Cu4 Cu -1.98483(19) -0.76625(14) -0.27841(14) 0.0450(5) Uani 1 1 d . . . O26 O -1.5380(11) -0.8074(9) -0.7090(7) 0.062(4) Uani 1 1 d . . . O25 O -1.6586(8) -0.4301(6) 0.1105(5) 0.0223(19) Uani 1 1 d . . . O24 O -1.4643(8) -0.4326(7) -0.1958(6) 0.031(2) Uani 1 1 d . . . O23 O -1.4590(8) -0.4128(6) 0.1333(5) 0.027(2) Uani 1 1 d . . . O22 O -1.4446(9) -0.2708(7) -0.1190(6) 0.038(3) Uani 1 1 d . . . O21 O -1.8052(8) -0.2921(7) 0.0494(6) 0.038(3) Uani 1 1 d . . . O20 O -1.5575(8) -0.4275(6) -0.0407(5) 0.024(2) Uani 1 1 d . . . O19 O -1.3626(7) -0.4137(6) -0.0277(5) 0.024(2) Uani 1 1 d . . . O18 O -1.6870(10) -0.2936(7) -0.1429(7) 0.045(3) Uani 1 1 d . . . O17 O -1.7518(8) -0.4494(6) -0.0612(5) 0.025(2) Uani 1 1 d . . . O16 O -1.5685(9) -0.2637(6) 0.0617(6) 0.035(2) Uani 1 1 d . . . O15 O -1.2454(9) -0.4190(7) -0.1954(6) 0.035(2) Uani 1 1 d . . . O14 O -1.8214(9) -0.9008(7) -0.2802(6) 0.037(3) Uani 1 1 d . . . O13 O -1.6854(9) -0.8485(7) -0.5689(6) 0.035(2) Uani 1 1 d . . . O12 O -1.8839(9) -0.8164(7) -0.4294(6) 0.038(3) Uani 1 1 d . . . O11 O -1.8537(9) -0.9548(7) -0.5416(6) 0.034(2) Uani 1 1 d . . . O10 O -1.7764(8) -1.0157(6) -0.4155(6) 0.028(2) Uani 1 1 d . . . O9 O -1.6432(8) -0.8983(7) -0.4308(6) 0.032(2) Uani 1 1 d . . . O8 O -1.8728(9) -0.4574(8) 0.0965(7) 0.042(3) Uani 1 1 d . . . O7 O -1.4002(8) -0.9566(7) -0.4376(5) 0.032(2) Uani 1 1 d . . . O6 O -1.6586(10) -0.4612(9) -0.2293(7) 0.050(3) Uani 1 1 d . . . O5 O -1.4524(9) -0.8871(8) -0.5791(6) 0.042(3) Uani 1 1 d . . . O4 O -1.4129(9) -1.0046(8) -0.6966(6) 0.041(3) Uani 1 1 d . . . O3 O -1.7543(10) -1.1029(8) -0.2823(6) 0.044(3) Uani 1 1 d . . . O2 O -1.5221(10) -0.7517(7) -0.4413(7) 0.047(3) Uani 1 1 d . . . O1 O -1.6296(11) -0.9603(11) -0.7120(8) 0.073(4) Uani 1 1 d . . . C1 C -2.1934(12) -0.8428(10) -0.2079(9) 0.030(3) Uani 1 1 d . . . H1A H -2.2421 -0.7826 -0.1761 0.036 Uiso 1 1 calc R . . C2 C -2.0474(12) -0.9483(9) -0.2911(9) 0.033(3) Uani 1 1 d . . . H2A H -1.9731 -0.9781 -0.3314 0.039 Uiso 1 1 calc R . . C3 C -2.1209(12) -1.1003(9) -0.2700(9) 0.028(3) Uani 1 1 d . . . H3A H -2.0523 -1.1310 -0.3181 0.034 Uiso 1 1 calc R . . H3B H -2.1940 -1.1061 -0.2775 0.034 Uiso 1 1 calc R . . C4 C -2.1043(12) -1.1578(9) -0.1984(8) 0.027(3) Uani 1 1 d . . . C5 C -2.1820(13) -1.2119(10) -0.1598(9) 0.034(3) Uani 1 1 d . . . H5A H -2.2481 -1.2108 -0.1749 0.041 Uiso 1 1 calc R . . C6 C -2.0140(13) -1.1567(10) -0.1711(9) 0.033(3) Uani 1 1 d . . . H6A H -1.9623 -1.1172 -0.1951 0.039 Uiso 1 1 calc R . . C8 C -2.1624(12) -1.2676(9) -0.0989(7) 0.026(3) Uani 1 1 d . . . H8A H -2.2130 -1.3078 -0.0747 0.032 Uiso 1 1 calc R . . C7 C -1.9976(13) -1.2110(9) -0.1109(8) 0.029(3) Uiso 1 1 d . . . H7A H -1.9328 -1.2106 -0.0947 0.035 Uiso 1 1 calc R . . C9 C -2.0717(12) -1.2663(10) -0.0728(8) 0.029(3) Uani 1 1 d . . . C10 C -2.0511(14) -1.3290(13) -0.0070(10) 0.048(5) Uani 1 1 d . . . H10A H -2.0408 -1.4001 -0.0213 0.058 Uiso 1 1 calc R . . H10B H -1.9767 -1.3250 -0.0006 0.058 Uiso 1 1 calc R . . C11 C -2.2634(17) -1.2032(11) 0.1658(9) 0.041(4) Uani 1 1 d . . . H11A H -2.2967 -1.1509 0.2069 0.049 Uiso 1 1 calc R . . C12 C -2.2384(13) -1.3320(10) 0.0976(9) 0.034(3) Uani 1 1 d . . . H12A H -2.2483 -1.3901 0.0774 0.041 Uiso 1 1 calc R . . C13 C -1.4386(14) -0.4468(11) -0.3761(10) 0.041(4) Uani 1 1 d . . . H13A H -1.4755 -0.4015 -0.3303 0.049 Uiso 1 1 calc R . . C14 C -1.4020(12) -0.5596(10) -0.4664(9) 0.032(3) Uani 1 1 d . . . H14A H -1.4113 -0.6112 -0.4950 0.038 Uiso 1 1 calc R . . C15 C -1.2524(15) -0.3930(12) -0.4395(13) 0.055(5) Uani 1 1 d . . . H15A H -1.2708 -0.3602 -0.3870 0.067 Uiso 1 1 calc R . . H15B H -1.2676 -0.3393 -0.4747 0.067 Uiso 1 1 calc R . . C16 C -1.1222(14) -0.4510(11) -0.4708(9) 0.037(3) Uiso 1 1 d . . . C17 C -1.0522(14) -0.4284(10) -0.5400(9) 0.035(3) Uani 1 1 d . . . H17A H -1.0865 -0.3785 -0.5687 0.042 Uiso 1 1 calc R . . C18 C -1.0702(15) -0.5227(11) -0.4299(10) 0.043(4) Uani 1 1 d . . . H18A H -1.1177 -0.5391 -0.3808 0.052 Uiso 1 1 calc R . . C19 C -2.5761(13) -1.0374(12) -0.1072(10) 0.041(4) Uani 1 1 d . . . H19A H -2.5454 -1.0857 -0.1509 0.049 Uiso 1 1 calc R . . C20 C -2.6048(14) -0.9160(11) -0.0274(10) 0.044(4) Uani 1 1 d . . . H20A H -2.5954 -0.8594 -0.0046 0.053 Uiso 1 1 calc R . . C21 C -2.7506(15) -1.0961(11) -0.0265(12) 0.058(6) Uani 1 1 d . . . H21A H -2.7433 -1.1290 0.0213 0.070 Uiso 1 1 calc R . . H21B H -2.7211 -1.1496 -0.0697 0.070 Uiso 1 1 calc R . . C22 C -2.8798(14) -1.0451(9) -0.0120(9) 0.033(3) Uani 1 1 d . . . C23 C -2.9151(14) -0.9910(11) -0.0687(9) 0.036(3) Uani 1 1 d . . . H23A H -2.8563 -0.9846 -0.1167 0.043 Uiso 1 1 calc R . . C24 C -3.0351(13) -0.9455(10) -0.0572(9) 0.033(3) Uani 1 1 d . . . H24A H -3.0577 -0.9085 -0.0970 0.050 Uiso 1 1 calc R . . C25 C -1.9659(13) -0.5645(10) -0.2568(8) 0.029(3) Uani 1 1 d . . . H25A H -2.0489 -0.5355 -0.2302 0.034 Uiso 1 1 calc R . . C26 C -1.7995(13) -0.6656(9) -0.3181(9) 0.035(4) Uani 1 1 d . . . H26A H -1.7401 -0.7248 -0.3456 0.042 Uiso 1 1 calc R . . C27 C -1.9043(14) -0.4084(10) -0.2560(8) 0.034(3) Uani 1 1 d . . . H27A H -1.8435 -0.4016 -0.2344 0.040 Uiso 1 1 calc R . . H27B H -1.9837 -0.3800 -0.2152 0.040 Uiso 1 1 calc R . . C28 C -1.8958(12) -0.3491(8) -0.3279(7) 0.020(3) Uani 1 1 d . . . C29 C -1.9775(12) -0.3397(10) -0.3648(8) 0.031(3) Uani 1 1 d . . . H29A H -2.0399 -0.3702 -0.3450 0.037 Uiso 1 1 calc R . . C30 C -1.8094(12) -0.2992(9) -0.3558(8) 0.029(3) Uani 1 1 d . . . H30A H -1.7537 -0.3045 -0.3298 0.035 Uiso 1 1 calc R . . C31 C -1.9687(14) -0.2838(9) -0.4333(9) 0.036(4) Uani 1 1 d . . . H31A H -2.0239 -0.2795 -0.4595 0.044 Uiso 1 1 calc R . . C32 C -1.8015(13) -0.2432(10) -0.4185(10) 0.037(4) Uani 1 1 d . . . H32A H -1.7430 -0.2082 -0.4345 0.045 Uiso 1 1 calc R . . C33 C -1.8817(13) -0.2369(10) -0.4610(9) 0.036(4) Uani 1 1 d . . . C34 C -1.8749(15) -0.1801(11) -0.5334(9) 0.040(4) Uani 1 1 d . . . H34A H -1.9501 -0.1694 -0.5439 0.048 Uiso 1 1 calc R . . H34B H -1.8665 -0.1133 -0.5237 0.048 Uiso 1 1 calc R . . C35 C -1.6793(14) -0.2086(11) -0.6411(10) 0.039(4) Uani 1 1 d . . . H35A H -1.6579 -0.1519 -0.6292 0.046 Uiso 1 1 calc R . . C36 C -1.6827(14) -0.3405(10) -0.6957(8) 0.035(4) Uani 1 1 d . . . H36A H -1.6599 -0.3971 -0.7318 0.042 Uiso 1 1 calc R . . N1 N -2.0853(11) -0.8532(8) -0.2584(7) 0.034(3) Uani 1 1 d . . . N2 N -2.2272(10) -0.9265(8) -0.2064(7) 0.030(3) Uani 1 1 d . . . N3 N -2.1302(9) -0.9933(8) -0.2582(6) 0.024(2) Uani 1 1 d . . . N4 N -2.1493(11) -1.2962(9) 0.0677(7) 0.032(3) Uani 1 1 d . . . N5 N -2.1642(14) -1.2125(11) 0.1088(9) 0.050(4) Uani 1 1 d . . . N6 N -2.3142(11) -1.2735(9) 0.1616(8) 0.038(3) Uani 1 1 d . . . N7 N -1.4817(11) -0.5149(9) -0.3963(8) 0.040(3) Uani 1 1 d . . . N8 N -1.3100(12) -0.5237(10) -0.4907(9) 0.047(3) Uani 1 1 d . . . N9 N -1.3331(11) -0.4538(8) -0.4325(7) 0.035(3) Uani 1 1 d . . . N10 N -2.5255(11) -0.9662(9) -0.0978(8) 0.041(3) Uani 1 1 d . . . N11 N -2.6938(12) -0.9526(10) 0.0055(8) 0.045(3) Uani 1 1 d . . . N12 N -2.6735(11) -1.0295(8) -0.0470(8) 0.034(3) Uani 1 1 d . . . N13 N -1.9154(10) -0.6613(8) -0.2816(7) 0.031(3) Uani 1 1 d . . . N14 N -1.7769(9) -0.5791(8) -0.3118(7) 0.028(3) Uani 1 1 d . . . N15 N -1.8865(10) -0.5139(8) -0.2738(6) 0.024(2) Uani 1 1 d . . . N16 N -1.6146(11) -0.2766(9) -0.7011(7) 0.037(3) Uani 1 1 d . . . N17 N -1.7802(13) -0.3157(9) -0.6370(8) 0.045(3) Uani 1 1 d . . . N18 N -1.7786(11) -0.2313(8) -0.6001(7) 0.032(3) Uani 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 Mo1 0.0166(6) 0.0225(6) 0.0231(6) -0.0037(4) -0.0040(5) -0.0058(4) Mo2 0.0173(6) 0.0276(6) 0.0249(7) -0.0007(4) -0.0061(5) -0.0042(5) Mo3 0.0198(6) 0.0265(6) 0.0302(7) -0.0003(4) -0.0063(5) -0.0077(5) Mo4 0.0174(6) 0.0218(6) 0.0358(7) -0.0011(4) -0.0044(5) -0.0068(5) Mo5 0.0209(6) 0.0385(7) 0.0240(7) 0.0023(5) -0.0097(5) -0.0091(5) Mo6 0.0223(6) 0.0288(6) 0.0249(7) 0.0038(4) -0.0083(5) -0.0114(5) Mo7 0.0177(6) 0.0339(6) 0.0314(7) 0.0003(5) -0.0048(5) -0.0093(5) Mo8 0.0247(7) 0.0504(8) 0.0345(8) -0.0017(6) -0.0088(6) -0.0026(6) Cu1 0.0364(12) 0.0706(14) 0.0352(12) -0.0013(9) -0.0010(9) -0.0203(10) Cu2 0.0245(11) 0.0588(13) 0.0698(16) 0.0172(11) -0.0002(10) -0.0156(10) Cu3 0.0252(10) 0.0499(11) 0.0611(15) 0.0078(9) -0.0059(9) -0.0186(9) Cu4 0.0399(12) 0.0358(10) 0.0642(15) 0.0118(9) -0.0134(10) -0.0249(9) O26 0.060(8) 0.070(8) 0.037(7) 0.022(6) -0.002(6) -0.008(7) O25 0.017(5) 0.031(5) 0.020(5) 0.003(3) -0.008(4) -0.008(4) O24 0.030(6) 0.036(5) 0.032(6) 0.001(4) -0.019(5) -0.009(4) O23 0.028(5) 0.034(5) 0.018(5) -0.002(4) -0.006(4) -0.009(4) O22 0.041(6) 0.032(5) 0.042(7) 0.002(4) -0.018(5) -0.008(5) O21 0.022(5) 0.040(6) 0.033(6) -0.006(4) 0.004(4) 0.002(4) O20 0.019(5) 0.024(4) 0.025(5) 0.001(3) -0.005(4) -0.002(4) O19 0.010(4) 0.037(5) 0.023(5) 0.002(4) -0.001(4) -0.008(4) O18 0.048(7) 0.032(6) 0.049(7) 0.007(5) -0.018(6) 0.000(5) O17 0.024(5) 0.034(5) 0.023(5) -0.002(4) -0.006(4) -0.018(4) O16 0.026(5) 0.019(5) 0.048(7) -0.003(4) -0.003(5) -0.001(4) O15 0.030(6) 0.043(6) 0.033(6) 0.003(4) -0.013(5) -0.010(5) O14 0.033(6) 0.048(6) 0.031(6) -0.013(4) -0.013(5) -0.008(5) O13 0.032(6) 0.029(5) 0.040(6) 0.008(4) -0.013(5) -0.002(4) O12 0.039(6) 0.034(5) 0.043(7) -0.007(4) -0.023(5) 0.000(5) O11 0.029(6) 0.041(5) 0.036(6) 0.003(4) -0.016(5) -0.012(4) O10 0.016(5) 0.029(5) 0.037(6) 0.003(4) -0.011(4) -0.003(4) O9 0.025(5) 0.041(5) 0.039(6) 0.010(4) -0.014(5) -0.020(4) O8 0.020(5) 0.051(6) 0.053(7) 0.008(5) -0.006(5) -0.017(5) O7 0.021(5) 0.044(6) 0.025(6) 0.001(4) -0.002(4) -0.007(4) O6 0.037(7) 0.082(8) 0.035(7) -0.006(6) -0.014(5) -0.022(6) O5 0.025(6) 0.045(6) 0.047(7) 0.008(5) -0.018(5) 0.007(5) O4 0.022(5) 0.053(6) 0.042(7) -0.005(5) -0.006(5) -0.010(5) O3 0.041(7) 0.067(7) 0.035(7) 0.015(5) -0.014(5) -0.033(6) O2 0.048(7) 0.039(6) 0.049(7) -0.014(5) -0.008(6) -0.015(5) O1 0.041(8) 0.104(11) 0.070(10) -0.034(8) -0.030(7) 0.000(7) C1 0.023(7) 0.024(7) 0.038(9) 0.006(5) -0.005(6) -0.006(6) C2 0.019(7) 0.023(7) 0.046(9) 0.009(6) -0.002(6) -0.003(6) C3 0.022(7) 0.021(6) 0.044(9) 0.001(5) -0.012(6) -0.008(6) C4 0.019(7) 0.027(7) 0.036(9) -0.004(5) -0.008(6) -0.012(6) C5 0.023(8) 0.040(8) 0.032(9) -0.003(6) 0.000(6) -0.007(6) C6 0.027(8) 0.030(7) 0.048(10) -0.003(6) -0.013(7) -0.020(6) C8 0.029(8) 0.029(7) 0.016(7) 0.007(5) -0.003(6) -0.008(6) C9 0.022(7) 0.028(7) 0.034(9) -0.003(5) -0.011(6) 0.001(6) C10 0.025(8) 0.055(10) 0.045(10) 0.019(8) -0.003(7) 0.004(7) C11 0.074(13) 0.044(9) 0.021(8) 0.006(6) -0.020(8) -0.039(9) C12 0.030(8) 0.036(8) 0.048(10) 0.014(6) -0.011(7) -0.029(7) C13 0.038(9) 0.050(9) 0.045(10) -0.007(7) -0.018(8) -0.023(8) C14 0.025(8) 0.038(8) 0.044(10) 0.009(6) -0.022(7) -0.015(6) C15 0.033(10) 0.040(9) 0.096(16) -0.010(9) -0.015(10) -0.023(8) C17 0.043(9) 0.036(8) 0.038(9) 0.005(6) -0.018(7) -0.025(7) C18 0.048(11) 0.050(9) 0.044(10) 0.014(7) -0.014(8) -0.037(8) C19 0.025(8) 0.049(9) 0.040(10) -0.005(7) -0.009(7) 0.000(7) C20 0.032(9) 0.049(9) 0.053(11) -0.014(7) -0.001(8) -0.029(8) C21 0.038(10) 0.020(8) 0.095(15) 0.012(8) 0.007(10) -0.013(7) C22 0.039(9) 0.015(6) 0.056(11) 0.003(6) -0.020(8) -0.020(6) C23 0.035(9) 0.051(9) 0.036(9) 0.011(7) -0.014(7) -0.035(7) C24 0.034(8) 0.028(7) 0.036(9) 0.010(6) -0.007(7) -0.012(6) C25 0.031(8) 0.041(8) 0.015(7) 0.005(5) -0.006(6) -0.016(7) C26 0.036(9) 0.012(6) 0.051(10) -0.010(5) -0.009(7) -0.005(6) C27 0.047(9) 0.033(7) 0.011(7) -0.006(5) -0.002(6) -0.007(7) C28 0.027(7) 0.018(6) 0.021(7) -0.003(5) -0.007(6) -0.014(5) C29 0.025(8) 0.037(7) 0.028(8) -0.004(6) 0.002(6) -0.021(6) C30 0.022(7) 0.028(7) 0.034(9) -0.021(6) -0.010(6) -0.001(6) C31 0.049(10) 0.022(7) 0.036(9) -0.009(6) -0.016(7) -0.005(7) C32 0.024(8) 0.022(7) 0.060(11) 0.002(6) -0.003(7) -0.012(6) C33 0.022(7) 0.028(7) 0.042(9) -0.008(6) 0.010(6) -0.005(6) C34 0.045(10) 0.036(8) 0.027(9) 0.006(6) -0.002(7) -0.009(7) C35 0.035(9) 0.042(9) 0.051(11) 0.013(7) -0.022(8) -0.021(7) C36 0.045(10) 0.034(8) 0.022(8) -0.002(6) -0.015(7) -0.002(7) N1 0.034(7) 0.024(6) 0.033(7) 0.009(5) 0.003(6) -0.009(5) N2 0.018(6) 0.041(7) 0.026(7) 0.008(5) -0.001(5) -0.011(5) N3 0.012(6) 0.036(6) 0.024(6) 0.007(5) -0.001(5) -0.013(5) N4 0.036(7) 0.041(7) 0.031(7) 0.007(5) -0.018(6) -0.026(6) N5 0.068(11) 0.066(9) 0.047(10) 0.017(7) -0.032(8) -0.051(8) N6 0.037(8) 0.040(7) 0.036(8) 0.000(5) -0.009(6) -0.015(6) N7 0.020(6) 0.051(8) 0.046(9) 0.011(6) -0.002(6) -0.018(6) N8 0.039(8) 0.049(8) 0.051(9) 0.003(6) -0.011(7) -0.016(7) N9 0.032(7) 0.029(6) 0.034(7) -0.010(5) 0.006(6) -0.013(5) N10 0.030(7) 0.044(7) 0.040(8) 0.001(6) -0.002(6) -0.008(6) N11 0.035(8) 0.061(8) 0.037(8) -0.005(6) -0.001(6) -0.024(7) N12 0.027(7) 0.021(6) 0.046(8) 0.000(5) -0.002(6) -0.009(5) N13 0.025(6) 0.030(6) 0.034(7) 0.000(5) -0.001(5) -0.013(5) N14 0.011(5) 0.033(6) 0.042(8) 0.004(5) -0.012(5) -0.006(5) N15 0.021(6) 0.030(6) 0.017(6) -0.001(4) -0.003(5) -0.004(5) N16 0.036(7) 0.047(7) 0.030(7) 0.006(5) -0.011(6) -0.017(6) N17 0.052(9) 0.030(7) 0.051(9) 0.006(6) -0.007(7) -0.024(6) N18 0.027(7) 0.025(6) 0.036(7) 0.007(5) -0.003(5) -0.004(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 Mo1 O16 1.696(8) . ? Mo1 O23 1.752(9) . ? Mo1 O19 1.933(9) . ? Mo1 O25 1.951(9) . ? Mo1 O20 2.109(9) . ? Mo1 O20 2.423(8) 2_245 ? Mo1 Mo2 3.2136(18) . ? Mo2 O21 1.682(9) . ? Mo2 O8 1.703(10) . ? Mo2 O17 1.905(9) . ? Mo2 O25 1.984(8) . ? Mo2 O19 2.350(8) 2_245 ? Mo2 O20 2.367(9) . ? Mo3 O11 1.698(10) . ? Mo3 O12 1.714(9) . ? Mo3 O13 1.909(10) . ? Mo3 O10 1.933(9) . ? Mo3 O9 2.373(10) . ? Mo3 O7 2.397(9) 2_234 ? Mo4 O2 1.701(10) . ? Mo4 O7 1.756(9) . ? Mo4 O9 1.790(10) . ? Mo4 O5 1.824(11) . ? Mo5 O18 1.689(9) . ? Mo5 O6 1.749(11) . ? Mo5 O17 1.913(9) . ? Mo5 O24 1.915(10) . ? Mo5 O23 2.341(9) 2_245 ? Mo5 O20 2.424(9) . ? Mo6 O22 1.677(9) . ? Mo6 O15 1.702(10) . ? Mo6 O24 1.884(9) . ? Mo6 O19 2.020(9) . ? Mo6 O20 2.344(9) . ? Mo6 O25 2.375(8) 2_245 ? Mo7 O3 1.676(11) . ? Mo7 O14 1.713(9) . ? Mo7 O10 1.897(9) . ? Mo7 O4 1.927(11) 2_234 ? Mo7 O5 2.296(10) 2_234 ? Mo7 O9 2.421(10) . ? Mo8 O26 1.660(12) . ? Mo8 O1 1.681(13) . ? Mo8 O4 1.873(10) . ? Mo8 O13 1.892(10) . ? Mo8 O5 2.460(11) . ? Cu1 N16 1.870(13) . ? Cu1 N6 1.885(13) 1_664 ? Cu1 O23 2.434(9) 1_554 ? Cu2 N10 1.866(14) . ? Cu2 N2 1.902(12) . ? Cu3 N7 1.920(12) . ? Cu3 N14 1.927(11) . ? Cu3 O6 2.256(11) . ? Cu4 N13 1.885(12) . ? Cu4 N1 1.918(12) . ? Cu4 O14 2.340(10) . ? O25 Mo6 2.375(8) 2_245 ? O23 Mo5 2.341(9) 2_245 ? O23 Cu1 2.434(9) 1_556 ? O20 Mo1 2.423(8) 2_245 ? O19 Mo2 2.350(8) 2_245 ? O7 Mo3 2.397(9) 2_234 ? O5 Mo7 2.296(10) 2_234 ? O4 Mo7 1.927(11) 2_234 ? C1 N1 1.317(18) . ? C1 N2 1.341(17) . ? C1 H1A 0.9500 . ? C2 N3 1.318(17) . ? C2 N1 1.350(17) . ? C2 H2A 0.9500 . ? C3 N3 1.475(16) . ? C3 C4 1.552(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C6 1.379(19) . ? C4 C5 1.38(2) . ? C5 C8 1.383(19) . ? C5 H5A 0.9500 . ? C6 C7 1.35(2) . ? C6 H6A 0.9500 . ? C8 C9 1.371(19) . ? C8 H8A 0.9500 . ? C7 C9 1.36(2) . ? C7 H7A 0.9500 . ? C9 C10 1.51(2) . ? C10 N4 1.460(19) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N5 1.29(2) . ? C11 N6 1.322(19) . ? C11 H11A 0.9500 . ? C12 N4 1.290(18) . ? C12 N6 1.330(19) . ? C12 H12A 0.9500 . ? C13 N7 1.325(19) . ? C13 N9 1.34(2) . ? C13 H13A 0.9500 . ? C14 N8 1.31(2) . ? C14 N7 1.351(19) . ? C14 H14A 0.9500 . ? C15 N9 1.458(19) . ? C15 C16 1.51(2) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.35(2) . ? C16 C18 1.38(2) . ? C17 C18 1.40(2) 2_344 ? C17 H17A 0.9500 . ? C18 C17 1.40(2) 2_344 ? C18 H18A 0.9500 . ? C19 N12 1.31(2) . ? C19 N10 1.36(2) . ? C19 H19A 0.9500 . ? C20 N11 1.30(2) . ? C20 N10 1.376(19) . ? C20 H20A 0.9500 . ? C21 N12 1.469(19) . ? C21 C22 1.50(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C24 1.37(2) 2_/35 ? C22 C23 1.38(2) . ? C23 C24 1.40(2) . ? C23 H23A 0.9500 . ? C24 C22 1.37(2) 2_/35 ? C24 H24A 0.9500 . ? C25 N15 1.320(18) . ? C25 N13 1.330(17) . ? C25 H25A 0.9500 . ? C26 N14 1.325(17) . ? C26 N13 1.354(18) . ? C26 H26A 0.9500 . ? C27 N15 1.449(16) . ? C27 C28 1.515(18) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.372(19) . ? C28 C30 1.390(19) . ? C29 C31 1.44(2) . ? C29 H29A 0.9500 . ? C30 C32 1.35(2) . ? C30 H30A 0.9500 . ? C31 C33 1.36(2) . ? C31 H31A 0.9500 . ? C32 C33 1.44(2) . ? C32 H32A 0.9500 . ? C33 C34 1.51(2) . ? C34 N18 1.409(18) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N16 1.32(2) . ? C35 N18 1.329(19) . ? C35 H35A 0.9500 . ? C36 N17 1.28(2) . ? C36 N16 1.37(2) . ? C36 H36A 0.9500 . ? N2 N3 1.360(15) . ? N4 N5 1.331(17) . ? N6 Cu1 1.885(13) 1_446 ? N8 N9 1.352(17) . ? N11 N12 1.359(17) . ? N14 N15 1.364(14) . ? N17 N18 1.374(17) . ? 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 O16 Mo1 O23 103.6(5) . . ? O16 Mo1 O19 101.4(4) . . ? O23 Mo1 O19 96.5(4) . . ? O16 Mo1 O25 102.2(4) . . ? O23 Mo1 O25 94.9(4) . . ? O19 Mo1 O25 150.5(4) . . ? O16 Mo1 O20 99.5(4) . . ? O23 Mo1 O20 156.9(4) . . ? O19 Mo1 O20 79.2(4) . . ? O25 Mo1 O20 79.7(4) . . ? O16 Mo1 O20 176.3(4) . 2_245 ? O23 Mo1 O20 80.1(4) . 2_245 ? O19 Mo1 O20 78.0(3) . 2_245 ? O25 Mo1 O20 77.3(3) . 2_245 ? O20 Mo1 O20 76.7(3) . 2_245 ? O16 Mo1 Mo2 91.8(4) . . ? O23 Mo1 Mo2 130.5(3) . . ? O19 Mo1 Mo2 126.5(3) . . ? O25 Mo1 Mo2 35.6(2) . . ? O20 Mo1 Mo2 47.4(2) . . ? O20 Mo1 Mo2 85.7(2) 2_245 . ? O21 Mo2 O8 105.2(5) . . ? O21 Mo2 O17 101.6(4) . . ? O8 Mo2 O17 99.7(5) . . ? O21 Mo2 O25 96.9(4) . . ? O8 Mo2 O25 103.2(5) . . ? O17 Mo2 O25 145.6(4) . . ? O21 Mo2 O19 165.2(4) . 2_245 ? O8 Mo2 O19 87.4(4) . 2_245 ? O17 Mo2 O19 83.6(3) . 2_245 ? O25 Mo2 O19 72.2(3) . 2_245 ? O21 Mo2 O20 95.7(4) . . ? O8 Mo2 O20 159.2(4) . . ? O17 Mo2 O20 76.6(3) . . ? O25 Mo2 O20 72.9(3) . . ? O19 Mo2 O20 71.9(3) 2_245 . ? O21 Mo2 Mo1 86.5(4) . . ? O8 Mo2 Mo1 138.1(4) . . ? O17 Mo2 Mo1 117.6(3) . . ? O25 Mo2 Mo1 34.9(3) . . ? O19 Mo2 Mo1 78.9(2) 2_245 . ? O20 Mo2 Mo1 41.0(2) . . ? O11 Mo3 O12 104.2(5) . . ? O11 Mo3 O13 101.6(5) . . ? O12 Mo3 O13 101.7(5) . . ? O11 Mo3 O10 100.5(4) . . ? O12 Mo3 O10 98.5(4) . . ? O13 Mo3 O10 145.2(4) . . ? O11 Mo3 O9 166.7(4) . . ? O12 Mo3 O9 88.4(4) . . ? O13 Mo3 O9 79.5(4) . . ? O10 Mo3 O9 73.0(4) . . ? O11 Mo3 O7 90.5(4) . 2_234 ? O12 Mo3 O7 165.3(4) . 2_234 ? O13 Mo3 O7 74.5(4) . 2_234 ? O10 Mo3 O7 78.8(3) . 2_234 ? O9 Mo3 O7 76.9(3) . 2_234 ? O2 Mo4 O7 110.5(5) . . ? O2 Mo4 O9 108.0(5) . . ? O7 Mo4 O9 108.0(4) . . ? O2 Mo4 O5 110.4(5) . . ? O7 Mo4 O5 110.0(4) . . ? O9 Mo4 O5 109.9(5) . . ? O18 Mo5 O6 104.1(6) . . ? O18 Mo5 O17 99.2(5) . . ? O6 Mo5 O17 102.6(5) . . ? O18 Mo5 O24 99.9(5) . . ? O6 Mo5 O24 100.5(5) . . ? O17 Mo5 O24 145.2(4) . . ? O18 Mo5 O23 166.9(4) . 2_245 ? O6 Mo5 O23 89.0(5) . 2_245 ? O17 Mo5 O23 77.8(3) . 2_245 ? O24 Mo5 O23 76.9(4) . 2_245 ? O18 Mo5 O20 96.8(4) . . ? O6 Mo5 O20 159.1(4) . . ? O17 Mo5 O20 75.0(3) . . ? O24 Mo5 O20 74.2(3) . . ? O23 Mo5 O20 70.1(3) 2_245 . ? O22 Mo6 O15 105.8(5) . . ? O22 Mo6 O24 102.8(4) . . ? O15 Mo6 O24 102.1(5) . . ? O22 Mo6 O19 95.9(4) . . ? O15 Mo6 O19 101.3(4) . . ? O24 Mo6 O19 144.7(4) . . ? O22 Mo6 O20 94.7(4) . . ? O15 Mo6 O20 159.1(4) . . ? O24 Mo6 O20 76.7(4) . . ? O19 Mo6 O20 72.0(3) . . ? O22 Mo6 O25 163.2(4) . 2_245 ? O15 Mo6 O25 87.6(4) . 2_245 ? O24 Mo6 O25 83.8(3) . 2_245 ? O19 Mo6 O25 71.1(3) . 2_245 ? O20 Mo6 O25 71.5(3) . 2_245 ? O3 Mo7 O14 105.4(6) . . ? O3 Mo7 O10 100.0(5) . . ? O14 Mo7 O10 99.8(4) . . ? O3 Mo7 O4 102.4(5) . 2_234 ? O14 Mo7 O4 97.2(4) . 2_234 ? O10 Mo7 O4 147.0(4) . 2_234 ? O3 Mo7 O5 92.4(5) . 2_234 ? O14 Mo7 O5 161.5(5) . 2_234 ? O10 Mo7 O5 81.8(4) . 2_234 ? O4 Mo7 O5 73.4(4) 2_234 2_234 ? O3 Mo7 O9 166.9(5) . . ? O14 Mo7 O9 86.7(4) . . ? O10 Mo7 O9 72.4(4) . . ? O4 Mo7 O9 80.7(4) 2_234 . ? O5 Mo7 O9 76.2(4) 2_234 . ? O26 Mo8 O1 107.3(7) . . ? O26 Mo8 O4 104.5(6) . . ? O1 Mo8 O4 99.1(5) . . ? O26 Mo8 O13 100.7(5) . . ? O1 Mo8 O13 104.5(6) . . ? O4 Mo8 O13 138.3(4) . . ? O26 Mo8 O5 90.2(6) . . ? O1 Mo8 O5 161.6(6) . . ? O4 Mo8 O5 70.3(4) . . ? O13 Mo8 O5 76.9(4) . . ? N16 Cu1 N6 169.6(6) . 1_664 ? N16 Cu1 O23 97.6(5) . 1_554 ? N6 Cu1 O23 92.7(4) 1_664 1_554 ? N10 Cu2 N2 172.5(6) . . ? N7 Cu3 N14 168.0(6) . . ? N7 Cu3 O6 93.1(5) . . ? N14 Cu3 O6 98.4(5) . . ? N13 Cu4 N1 167.4(5) . . ? N13 Cu4 O14 98.3(4) . . ? N1 Cu4 O14 91.1(4) . . ? Mo1 O25 Mo2 109.5(4) . . ? Mo1 O25 Mo6 111.3(4) . 2_245 ? Mo2 O25 Mo6 103.2(4) . 2_245 ? Mo6 O24 Mo5 117.8(5) . . ? Mo1 O23 Mo5 117.1(4) . 2_245 ? Mo1 O23 Cu1 126.0(4) . 1_556 ? Mo5 O23 Cu1 116.9(4) 2_245 1_556 ? Mo1 O20 Mo6 92.7(3) . . ? Mo1 O20 Mo2 91.6(3) . . ? Mo6 O20 Mo2 164.8(4) . . ? Mo1 O20 Mo1 103.3(3) . 2_245 ? Mo6 O20 Mo1 97.4(3) . 2_245 ? Mo2 O20 Mo1 95.9(3) . 2_245 ? Mo1 O20 Mo5 164.1(4) . . ? Mo6 O20 Mo5 86.0(3) . . ? Mo2 O20 Mo5 85.9(3) . . ? Mo1 O20 Mo5 92.6(3) 2_245 . ? Mo1 O19 Mo6 109.4(4) . . ? Mo1 O19 Mo2 111.9(4) . 2_245 ? Mo6 O19 Mo2 103.0(4) . 2_245 ? Mo2 O17 Mo5 117.5(4) . . ? Mo7 O14 Cu4 145.0(5) . . ? Mo8 O13 Mo3 126.3(5) . . ? Mo7 O10 Mo3 122.1(5) . . ? Mo4 O9 Mo3 130.3(5) . . ? Mo4 O9 Mo7 134.0(5) . . ? Mo3 O9 Mo7 88.7(3) . . ? Mo4 O7 Mo3 129.9(5) . 2_234 ? Mo5 O6 Cu3 160.8(6) . . ? Mo4 O5 Mo7 130.2(4) . 2_234 ? Mo4 O5 Mo8 128.9(5) . . ? Mo7 O5 Mo8 89.2(4) 2_234 . ? Mo8 O4 Mo7 123.2(6) . 2_234 ? N1 C1 N2 112.5(12) . . ? N1 C1 H1A 123.7 . . ? N2 C1 H1A 123.7 . . ? N3 C2 N1 109.0(12) . . ? N3 C2 H2A 125.5 . . ? N1 C2 H2A 125.5 . . ? N3 C3 C4 110.9(11) . . ? N3 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C6 C4 C5 118.1(14) . . ? C6 C4 C3 122.0(13) . . ? C5 C4 C3 119.8(13) . . ? C8 C5 C4 119.4(14) . . ? C8 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C7 C6 C4 121.2(14) . . ? C7 C6 H6A 119.4 . . ? C4 C6 H6A 119.4 . . ? C9 C8 C5 121.7(14) . . ? C9 C8 H8A 119.1 . . ? C5 C8 H8A 119.1 . . ? C6 C7 C9 121.7(14) . . ? C6 C7 H7A 119.2 . . ? C9 C7 H7A 119.2 . . ? C7 C9 C8 117.7(13) . . ? C7 C9 C10 121.5(13) . . ? C8 C9 C10 120.7(14) . . ? N4 C10 C9 112.4(11) . . ? N4 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? N4 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? N5 C11 N6 113.5(14) . . ? N5 C11 H11A 123.3 . . ? N6 C11 H11A 123.3 . . ? N4 C12 N6 108.3(13) . . ? N4 C12 H12A 125.9 . . ? N6 C12 H12A 125.9 . . ? N7 C13 N9 107.3(13) . . ? N7 C13 H13A 126.4 . . ? N9 C13 H13A 126.4 . . ? N8 C14 N7 112.4(14) . . ? N8 C14 H14A 123.8 . . ? N7 C14 H14A 123.8 . . ? N9 C15 C16 114.4(12) . . ? N9 C15 H15A 108.7 . . ? C16 C15 H15A 108.7 . . ? N9 C15 H15B 108.7 . . ? C16 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C18 118.4(15) . . ? C17 C16 C15 118.9(15) . . ? C18 C16 C15 122.6(16) . . ? C16 C17 C18 121.1(14) . 2_344 ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 2_344 . ? C16 C18 C17 120.5(15) . 2_344 ? C16 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 2_344 . ? N12 C19 N10 109.8(14) . . ? N12 C19 H19A 125.1 . . ? N10 C19 H19A 125.1 . . ? N11 C20 N10 114.3(13) . . ? N11 C20 H20A 122.8 . . ? N10 C20 H20A 122.8 . . ? N12 C21 C22 114.9(11) . . ? N12 C21 H21A 108.6 . . ? C22 C21 H21A 108.6 . . ? N12 C21 H21B 108.6 . . ? C22 C21 H21B 108.6 . . ? H21A C21 H21B 107.5 . . ? C24 C22 C23 119.1(14) 2_/35 . ? C24 C22 C21 120.1(14) 2_/35 . ? C23 C22 C21 120.7(15) . . ? C22 C23 C24 121.6(14) . . ? C22 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? C22 C24 C23 119.3(14) 2_/35 . ? C22 C24 H24A 120.4 2_/35 . ? C23 C24 H24A 120.4 . . ? N15 C25 N13 111.7(12) . . ? N15 C25 H25A 124.2 . . ? N13 C25 H25A 124.2 . . ? N14 C26 N13 113.4(11) . . ? N14 C26 H26A 123.3 . . ? N13 C26 H26A 123.3 . . ? N15 C27 C28 112.1(10) . . ? N15 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? N15 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C29 C28 C30 118.5(12) . . ? C29 C28 C27 120.4(13) . . ? C30 C28 C27 121.1(12) . . ? C28 C29 C31 120.1(13) . . ? C28 C29 H29A 119.9 . . ? C31 C29 H29A 119.9 . . ? C32 C30 C28 122.6(13) . . ? C32 C30 H30A 118.7 . . ? C28 C30 H30A 118.7 . . ? C33 C31 C29 120.6(15) . . ? C33 C31 H31A 119.7 . . ? C29 C31 H31A 119.7 . . ? C30 C32 C33 120.0(14) . . ? C30 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C31 C33 C32 118.0(15) . . ? C31 C33 C34 118.9(15) . . ? C32 C33 C34 123.1(14) . . ? N18 C34 C33 112.3(12) . . ? N18 C34 H34A 109.1 . . ? C33 C34 H34A 109.1 . . ? N18 C34 H34B 109.1 . . ? C33 C34 H34B 109.1 . . ? H34A C34 H34B 107.9 . . ? N16 C35 N18 109.9(13) . . ? N16 C35 H35A 125.0 . . ? N18 C35 H35A 125.0 . . ? N17 C36 N16 112.9(13) . . ? N17 C36 H36A 123.6 . . ? N16 C36 H36A 123.6 . . ? C1 N1 C2 105.2(12) . . ? C1 N1 Cu4 131.4(10) . . ? C2 N1 Cu4 123.1(10) . . ? C1 N2 N3 103.8(11) . . ? C1 N2 Cu2 131.3(9) . . ? N3 N2 Cu2 124.5(9) . . ? C2 N3 N2 109.4(11) . . ? C2 N3 C3 127.1(11) . . ? N2 N3 C3 123.4(11) . . ? C12 N4 N5 111.0(13) . . ? C12 N4 C10 127.6(14) . . ? N5 N4 C10 120.8(14) . . ? C11 N5 N4 103.3(13) . . ? C11 N6 C12 104.0(13) . . ? C11 N6 Cu1 129.1(11) . 1_446 ? C12 N6 Cu1 126.8(10) . 1_446 ? C13 N7 C14 106.0(13) . . ? C13 N7 Cu3 129.1(12) . . ? C14 N7 Cu3 124.8(11) . . ? C14 N8 N9 103.7(13) . . ? C13 N9 N8 110.6(13) . . ? C13 N9 C15 128.8(13) . . ? N8 N9 C15 120.4(13) . . ? C19 N10 C20 101.9(13) . . ? C19 N10 Cu2 129.1(11) . . ? C20 N10 Cu2 128.6(11) . . ? C20 N11 N12 103.0(12) . . ? C19 N12 N11 111.0(13) . . ? C19 N12 C21 129.6(14) . . ? N11 N12 C21 119.1(13) . . ? C25 N13 C26 102.6(11) . . ? C25 N13 Cu4 130.2(10) . . ? C26 N13 Cu4 126.9(9) . . ? C26 N14 N15 103.8(11) . . ? C26 N14 Cu3 131.7(9) . . ? N15 N14 Cu3 124.4(9) . . ? C25 N15 N14 108.3(11) . . ? C25 N15 C27 129.0(12) . . ? N14 N15 C27 122.7(12) . . ? C35 N16 C36 103.9(13) . . ? C35 N16 Cu1 128.2(11) . . ? C36 N16 Cu1 128.0(10) . . ? C36 N17 N18 105.2(13) . . ? C35 N18 N17 108.1(12) . . ? C35 N18 C34 130.3(13) . . ? N17 N18 C34 121.5(13) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.187 _refine_diff_density_min -1.049 _refine_diff_density_rms 0.255 # Attachment '- compound-2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 832446' #TrackingRef '- compound-2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H64 Cu5 Mo7 N24 O32' _chemical_formula_weight 2478.51 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.357(2) _cell_length_b 12.884(3) _cell_length_c 15.307(3) _cell_angle_alpha 112.97(3) _cell_angle_beta 98.94(3) _cell_angle_gamma 101.66(3) _cell_volume 1778.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0.433 _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1215 _exptl_absorpt_coefficient_mu 2.755 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4420 _exptl_absorpt_correction_T_max 0.5450 _exptl_absorpt_process_details ? _exptl_special_details ; Higashi, T. (1995) A program for absorption correction. RIGAKU corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13877 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6159 _reflns_number_gt 5050 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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. During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree. In the structure, The Cu2 and two trizole ligands coordinated with Cu2 center are disordered in two parts with the occupancies of 50%. The Mo4 and Cu3 centers also show the site- occupancies disorder. The restrained commands 'AFIX 59' and 'DELU' were used to fix all the disordered trizole 5-member rings. Furthermore, the restrained command 'isor' was used to retrain some non-H atoms with NPD or ADP problems. These atoms are as follows: o12 o13 c14 mo4 cu3 N5 > C12, N10 > C20, N5A > C12A, and N10A > C20A. All these restrained command led to a high restraint value of 229. They are as follow: ISOR 0.003 MO4 CU3 ISOR 0.005 O2 O13 ISOR 0.01 C14 to avoid the ADP NPD problems DFIX 1.75 0.01 MO4 O2 CU3 O2 DFIX 1.75 0.01 MO4 O13 CU3 O13 to define the Mo-O and Cu-O distance EXYZ Mo4 Cu3 EADP Mo4 Cu3 Mo4 and Cu3 were 50% disorder DFIX 2.0 0.01 N5 Cu2 N10 Cu2 DFIX 2.0 0.01 N5A Cu2A N10A Cu2A to define the Cu-N distance ISOR 0.006 CU2 CU2A ISOR 0.01 N5 C11 N4 N6 C12 N10 C19 N11 N12 C20 ISOR 0.01 N5A C11a N4a N6a C12A N10A C19a N11a N12a C20A to avoid the ADP NPD problems DELU N5 C11 N4 N6 C12 to refine the five member-ring DELU N10 C19 N11 N12 C20 to refine the five member-ring ISOR 0.005 O1W ISOR 0.01 O2W O3W to avoid the ADP NPD problems DELU N5A C11a N4a N6a C12A to refine the five member-ring DELU N10A C19a N11a N12a C20A to refine the five member-ring REM PART 3 SIMU 0.01 0.02 3.0 O4W O5W to refine the two water molecule And the orders AFIX 43 and AFIX 23 AFIX 0 were used to define all the H atoms. The highest residual peak and the deepest hole are both close to the heavy metal centers and featureless. ; _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^)+(0.0556P)^2^+37.5634P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method shelxl _refine_ls_extinction_coef ? _refine_ls_number_reflns 6159 _refine_ls_number_parameters 595 _refine_ls_number_restraints 229 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.1868 _refine_ls_wR_factor_gt 0.1786 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.145 _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 Mo1 Mo 0.08943(10) 0.93187(8) 0.41585(7) 0.0273(3) Uani 1 1 d . . . Mo2 Mo 0.26257(11) 1.16635(10) 0.60789(9) 0.0417(3) Uani 1 1 d . . . Mo3 Mo -0.01297(13) 0.80516(9) 0.54540(8) 0.0420(3) Uani 1 1 d . . . Mo4 Mo 0.16250(15) 1.04209(10) 0.74387(9) 0.0436(4) Uani 0.50 1 d PDU . 1 Cu3 Cu 0.16250(15) 1.04209(10) 0.74387(9) 0.0436(4) Uani 0.50 1 d PDU . 2 O1 O 0.0211(12) 0.8926(8) 0.6815(7) 0.061(3) Uani 1 1 d . . . O2 O 0.1611(15) 1.0955(11) 0.8665(6) 0.089(4) Uani 1 1 d DU . . O3 O -0.0486(8) 0.8011(6) 0.4125(5) 0.0332(18) Uani 1 1 d . . . O4 O 0.3315(11) 1.3101(9) 0.6325(9) 0.072(3) Uani 1 1 d . . . O5 O 0.1751(9) 1.0990(7) 0.4654(6) 0.040(2) Uani 1 1 d . . . O6 O 0.2287(11) 0.8817(10) 0.4154(8) 0.063(3) Uani 1 1 d . . . O7 O 0.2397(10) 1.1812(7) 0.7312(6) 0.050(2) Uani 1 1 d . . . O8 O 0.0979(8) 0.9923(6) 0.5673(5) 0.0295(17) Uani 1 1 d . . . O9 O 0.0261(11) 0.9036(8) 0.2946(7) 0.052(2) Uani 1 1 d . . . O10 O 0.1288(12) 0.7588(8) 0.5347(8) 0.069(4) Uani 1 1 d . . . O11 O -0.1346(13) 0.6826(8) 0.5251(8) 0.075(4) Uani 1 1 d . . . O12 O 0.3941(11) 1.1063(10) 0.5980(9) 0.072(3) Uani 1 1 d . . . O13 O 0.3019(9) 0.9866(9) 0.7361(8) 0.069(3) Uani 1 1 d DU . . Cu1 Cu 0.15366(16) 0.55815(15) -0.50667(11) 0.0419(4) Uani 1 1 d . . . N1 N 0.2574(9) 0.6175(8) -0.3759(7) 0.030(2) Uani 1 1 d . . . N2 N 0.3870(10) 0.7391(8) -0.2320(7) 0.029(2) Uani 1 1 d . . . N3 N 0.3989(10) 0.6312(8) -0.2437(7) 0.034(2) Uani 1 1 d . . . N7 N 0.0596(10) 0.4899(9) -0.6400(7) 0.036(2) Uani 1 1 d . . . N8 N -0.0594(11) 0.4550(11) -0.7821(8) 0.044(3) Uani 1 1 d . . . N9 N -0.0253(16) 0.3567(10) -0.7964(8) 0.064(4) Uani 1 1 d . . . C1 C 0.3039(12) 0.7297(10) -0.3102(8) 0.031(2) Uani 1 1 d . . . H1 H 0.2805 0.7933 -0.3187 0.037 Uiso 1 1 calc R . . C2 C 0.3179(11) 0.5623(10) -0.3307(8) 0.032(3) Uani 1 1 d . . . H2 H 0.3027 0.4794 -0.3600 0.039 Uiso 1 1 calc R . . C3 C 0.4652(12) 0.8457(10) -0.1432(8) 0.035(3) Uani 1 1 d . . . H3A H 0.4597 0.9157 -0.1541 0.042 Uiso 1 1 calc R . . H3B H 0.5623 0.8471 -0.1299 0.042 Uiso 1 1 calc R . . C4 C 0.4137(12) 0.8523(9) -0.0556(8) 0.031(3) Uani 1 1 d . . . C5 C 0.3002(12) 0.8893(11) -0.0402(9) 0.040(3) Uani 1 1 d . . . H5 H 0.2496 0.9076 -0.0868 0.048 Uiso 1 1 calc R . . C6 C 0.4853(13) 0.8250(10) 0.0135(9) 0.038(3) Uani 1 1 d . . . H6 H 0.5638 0.7997 0.0028 0.045 Uiso 1 1 calc R . . C7 C 0.4448(14) 0.8339(11) 0.0960(9) 0.044(3) Uani 1 1 d . . . H7 H 0.4937 0.8135 0.1417 0.053 Uiso 1 1 calc R . . C8 C 0.2603(13) 0.8997(12) 0.0465(12) 0.051(4) Uani 1 1 d . . . H8 H 0.1824 0.9256 0.0586 0.062 Uiso 1 1 calc R . . C9 C 0.3330(14) 0.8726(11) 0.1128(9) 0.043(3) Uani 1 1 d . . . C10 C 0.2925(19) 0.8907(13) 0.2078(12) 0.063(4) Uani 1 1 d . . . H10A H 0.1933 0.8534 0.1927 0.076 Uiso 0.50 1 calc PR A 1 H10B H 0.3414 0.8521 0.2410 0.076 Uiso 0.50 1 calc PR A 1 H10C H 0.1919 0.8710 0.1949 0.076 Uiso 0.50 1 calc PR A 2 H10D H 0.3231 0.8372 0.2329 0.076 Uiso 0.50 1 calc PR A 2 C13 C -0.0106(13) 0.5342(12) -0.6887(8) 0.037(3) Uani 1 1 d . . . H13 H -0.0240 0.6100 -0.6616 0.044 Uiso 1 1 calc R . . C14 C 0.0468(17) 0.3806(12) -0.7088(10) 0.051(4) Uani 1 1 d U . . H14 H 0.0862 0.3265 -0.6950 0.061 Uiso 1 1 calc R . . C15 C -0.1476(13) 0.4648(16) -0.8624(11) 0.056(4) Uani 1 1 d . . . H15A H -0.1852 0.5318 -0.8343 0.067 Uiso 1 1 calc R . . H15B H -0.2251 0.3921 -0.8983 0.067 Uiso 1 1 calc R . . C16 C -0.0697(13) 0.4830(13) -0.9331(10) 0.044(3) Uani 1 1 d . . . C17 C -0.0416(14) 0.3894(13) -1.0035(10) 0.048(4) Uani 1 1 d . . . H17 H -0.0696 0.3131 -1.0061 0.058 Uiso 1 1 calc R . . C18 C 0.0265(14) 0.4059(12) -1.0698(9) 0.047(3) Uani 1 1 d . . . H18 H 0.0441 0.3407 -1.1179 0.056 Uiso 1 1 calc R . . C21 C 0.6688(19) 1.5863(14) 0.8959(12) 0.072(5) Uani 1 1 d . . . H21A H 0.6348 1.6489 0.8869 0.087 Uiso 0.50 1 calc PR B 1 H21B H 0.7621 1.6249 0.9402 0.087 Uiso 0.50 1 calc PR B 1 H21C H 0.6268 1.6366 0.8727 0.087 Uiso 0.50 1 calc PR B 2 H21D H 0.7602 1.6347 0.9406 0.087 Uiso 0.50 1 calc PR B 2 C22 C 0.5815(15) 1.5398(12) 0.9492(10) 0.051(4) Uani 1 1 d . . . C23 C 0.4672(16) 1.4458(13) 0.8990(11) 0.057(4) Uani 1 1 d . . . H23 H 0.4429 1.4090 0.8292 0.069 Uiso 1 1 calc R C . C24 C 0.3872(16) 1.4042(13) 0.9484(11) 0.057(4) Uani 1 1 d . . . H24 H 0.3101 1.3369 0.9127 0.068 Uiso 1 1 calc R . . Cu2 Cu 0.5260(6) 1.3321(5) 0.5080(4) 0.0784(15) Uani 0.50 1 d PDU C 1 N5 N 0.424(2) 1.1908(13) 0.3867(12) 0.047(5) Uani 0.50 1 d PGDU C 1 C11 C 0.427(2) 1.0809(18) 0.3539(15) 0.052(6) Uani 0.50 1 d PGU C 1 H11 H 0.4907 1.0523 0.3825 0.063 Uiso 0.50 1 calc PR C 1 N4 N 0.326(3) 1.0175(18) 0.274(2) 0.048(7) Uani 0.50 1 d PGU C 1 N6 N 0.260(2) 1.088(2) 0.2582(18) 0.067(7) Uani 0.50 1 d PGU C 1 C12 C 0.321(2) 1.1953(15) 0.3276(17) 0.056(6) Uani 0.50 1 d PGU C 1 H12 H 0.2948 1.2639 0.3339 0.067 Uiso 0.50 1 calc PR C 1 N10 N 0.6335(19) 1.3922(17) 0.6461(9) 0.049(5) Uani 0.50 1 d PGDU C 1 C19 C 0.629(2) 1.4943(17) 0.7103(13) 0.044(6) Uani 0.50 1 d PGU C 1 H19 H 0.5931 1.5496 0.6953 0.053 Uiso 0.50 1 calc PR C 1 N11 N 0.682(3) 1.5063(18) 0.7988(14) 0.041(6) Uani 0.50 1 d PGU C 1 N12 N 0.719(3) 1.412(2) 0.7894(16) 0.067(7) Uani 0.50 1 d PGU C 1 C20 C 0.689(3) 1.3411(17) 0.6950(13) 0.066(7) Uani 0.50 1 d PGU C 1 H20 H 0.7057 1.2665 0.6670 0.079 Uiso 0.50 1 calc PR C 1 O1W O 0.5000 1.5000 0.5000 0.044(3) Uani 1 2 d SU . 1 O2W O 0.6171(19) 1.2275(16) 0.5322(13) 0.032(4) Uani 0.50 1 d PU C 1 O3W O 0.2345(9) 1.3367(7) 0.3562(7) 0.040(2) Uani 1 1 d U D 1 Cu2A Cu 0.5781(6) 1.2825(7) 0.5352(4) 0.0831(18) Uani 0.50 1 d PDU C 2 N5A N 0.471(2) 1.1602(16) 0.4058(10) 0.053(5) Uani 0.50 1 d PGDU C 2 C11A C 0.449(2) 1.049(2) 0.3590(17) 0.062(7) Uani 0.50 1 d PGU C 2 H11A H 0.4971 1.0026 0.3785 0.075 Uiso 0.50 1 calc PR C 2 N4A N 0.353(3) 1.0112(18) 0.2812(19) 0.045(6) Uani 0.50 1 d PGU C 2 N6A N 0.314(2) 1.0990(19) 0.2800(16) 0.049(5) Uani 0.50 1 d PGU C 2 C12A C 0.387(2) 1.1911(14) 0.3570(16) 0.050(6) Uani 0.50 1 d PGU . 2 H12A H 0.3805 1.2688 0.3748 0.060 Uiso 0.50 1 calc PR C 2 N10A N 0.668(2) 1.3710(16) 0.6766(8) 0.049(5) Uani 0.50 1 d PGDU C 2 C19A C 0.629(2) 1.4618(19) 0.7259(13) 0.048(6) Uani 0.50 1 d PGU C 2 H19A H 0.5735 1.4975 0.6986 0.058 Uiso 0.50 1 calc PR C 2 N11A N 0.681(3) 1.4952(18) 0.8190(14) 0.039(6) Uani 0.50 1 d PGU C 2 N12A N 0.751(2) 1.4250(18) 0.8274(13) 0.052(6) Uani 0.50 1 d PGU C 2 C20A C 0.743(2) 1.3483(15) 0.7394(12) 0.044(5) Uani 0.50 1 d PGU C 2 H20A H 0.7853 1.2865 0.7237 0.053 Uiso 0.50 1 calc PR C 2 O4W O 0.4358(13) 1.4859(11) 0.4693(10) 0.013(3) Uiso 0.50 1 d PU . 2 O5W O 0.6079(16) 1.6558(14) 0.5627(12) 0.035(3) Uiso 0.50 1 d PU . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0335(5) 0.0242(5) 0.0241(5) 0.0049(4) 0.0136(4) 0.0150(4) Mo2 0.0362(6) 0.0319(6) 0.0443(7) 0.0149(5) -0.0075(5) 0.0006(5) Mo3 0.0648(8) 0.0207(5) 0.0275(6) 0.0100(4) -0.0106(5) 0.0040(5) Mo4 0.0728(9) 0.0208(6) 0.0199(6) 0.0072(5) -0.0171(6) 0.0036(6) Cu3 0.0728(9) 0.0208(6) 0.0199(6) 0.0072(5) -0.0171(6) 0.0036(6) O1 0.104(9) 0.039(5) 0.029(5) 0.020(4) -0.003(5) 0.005(5) O2 0.104(6) 0.082(6) 0.079(6) 0.042(4) 0.009(4) 0.021(4) O3 0.046(5) 0.024(4) 0.023(4) 0.006(3) -0.002(3) 0.013(4) O4 0.066(7) 0.046(6) 0.073(8) 0.024(6) -0.020(6) -0.014(5) O5 0.043(5) 0.037(5) 0.034(5) 0.016(4) 0.009(4) 0.000(4) O6 0.057(6) 0.073(7) 0.065(7) 0.020(6) 0.027(5) 0.046(6) O7 0.066(6) 0.030(4) 0.027(5) 0.002(4) -0.021(4) 0.006(4) O8 0.037(4) 0.020(4) 0.025(4) 0.006(3) 0.000(3) 0.009(3) O9 0.076(7) 0.047(5) 0.032(5) 0.010(4) 0.022(5) 0.020(5) O10 0.094(8) 0.037(5) 0.056(7) 0.011(5) -0.029(6) 0.032(5) O11 0.112(9) 0.037(5) 0.046(6) 0.024(5) -0.024(6) -0.019(6) O12 0.044(6) 0.065(7) 0.089(9) 0.027(6) 0.000(6) 0.008(5) O13 0.074(5) 0.057(5) 0.068(5) 0.028(4) -0.007(4) 0.023(4) Cu1 0.0373(8) 0.0602(10) 0.0223(8) 0.0183(7) 0.0017(6) 0.0055(7) N1 0.034(5) 0.028(5) 0.027(5) 0.010(4) 0.006(4) 0.011(4) N2 0.035(5) 0.026(5) 0.025(5) 0.011(4) 0.007(4) 0.006(4) N3 0.040(6) 0.030(5) 0.031(5) 0.016(4) 0.005(4) 0.009(4) N7 0.038(5) 0.043(6) 0.027(5) 0.020(5) 0.007(4) 0.006(5) N8 0.039(6) 0.067(8) 0.030(6) 0.033(6) 0.003(5) 0.008(5) N9 0.116(12) 0.040(7) 0.029(6) 0.020(5) 0.007(7) 0.007(7) C1 0.041(6) 0.033(6) 0.027(6) 0.018(5) 0.009(5) 0.014(5) C2 0.033(6) 0.033(6) 0.031(6) 0.013(5) 0.007(5) 0.012(5) C3 0.038(6) 0.027(6) 0.029(6) 0.011(5) 0.002(5) -0.002(5) C4 0.039(6) 0.019(5) 0.027(6) 0.007(5) 0.008(5) -0.005(5) C5 0.035(7) 0.043(7) 0.030(7) 0.008(6) 0.004(5) 0.003(6) C6 0.045(7) 0.029(6) 0.028(6) 0.003(5) 0.004(5) 0.010(5) C7 0.057(8) 0.033(7) 0.031(7) 0.009(5) 0.004(6) 0.004(6) C8 0.025(6) 0.036(7) 0.077(11) 0.011(7) 0.019(7) 0.000(6) C9 0.057(8) 0.027(6) 0.029(7) 0.004(5) 0.009(6) -0.005(6) C10 0.092(12) 0.042(8) 0.064(10) 0.024(8) 0.043(9) 0.016(8) C13 0.047(7) 0.047(7) 0.026(6) 0.023(6) 0.016(5) 0.012(6) C14 0.085(8) 0.046(6) 0.035(6) 0.030(5) 0.019(6) 0.019(6) C15 0.033(7) 0.092(12) 0.047(8) 0.046(9) -0.004(6) 0.004(7) C16 0.039(7) 0.063(9) 0.034(7) 0.036(7) -0.001(5) 0.000(6) C17 0.053(8) 0.051(8) 0.033(7) 0.030(7) -0.009(6) -0.008(7) C18 0.058(8) 0.046(8) 0.028(7) 0.019(6) -0.004(6) 0.004(7) C21 0.085(12) 0.045(9) 0.045(9) -0.009(7) -0.023(9) 0.020(9) C22 0.057(9) 0.042(8) 0.042(8) 0.009(6) -0.005(7) 0.023(7) C23 0.066(10) 0.043(8) 0.035(8) -0.002(6) -0.016(7) 0.022(7) C24 0.059(9) 0.042(8) 0.045(9) 0.006(7) -0.015(7) 0.013(7) Cu2 0.077(3) 0.073(3) 0.056(3) 0.004(2) 0.036(2) -0.002(2) N5 0.058(9) 0.040(7) 0.042(9) 0.011(7) 0.032(7) 0.009(7) C11 0.053(10) 0.046(9) 0.052(10) 0.010(8) 0.025(7) 0.015(8) N4 0.053(11) 0.042(8) 0.046(10) 0.018(7) 0.019(7) 0.006(7) N6 0.065(11) 0.060(9) 0.067(10) 0.016(7) 0.017(7) 0.024(8) C12 0.063(11) 0.047(8) 0.059(11) 0.016(7) 0.030(7) 0.020(8) N10 0.041(9) 0.048(9) 0.048(8) 0.010(6) 0.020(7) 0.008(7) C19 0.044(10) 0.047(9) 0.037(9) 0.015(7) 0.008(7) 0.012(8) N11 0.034(10) 0.045(9) 0.036(8) 0.014(6) -0.008(7) 0.016(8) N12 0.069(12) 0.065(10) 0.069(9) 0.024(8) 0.015(8) 0.036(9) C20 0.067(12) 0.054(10) 0.074(10) 0.020(7) 0.024(9) 0.024(9) O1W 0.047(5) 0.045(5) 0.046(5) 0.023(4) 0.019(4) 0.011(4) O2W 0.040(8) 0.028(7) 0.020(7) 0.007(6) 0.000(6) 0.006(6) O3W 0.042(4) 0.039(4) 0.048(5) 0.024(4) 0.018(4) 0.015(4) Cu2A 0.069(3) 0.104(4) 0.046(3) 0.012(3) 0.023(2) 0.001(3) N5A 0.043(9) 0.066(9) 0.038(9) 0.014(7) 0.013(6) 0.006(8) C11A 0.060(11) 0.071(9) 0.061(11) 0.028(8) 0.015(7) 0.034(9) N4A 0.043(10) 0.046(8) 0.043(9) 0.013(7) 0.020(7) 0.013(8) N6A 0.045(9) 0.051(9) 0.047(9) 0.017(7) 0.014(6) 0.017(7) C12A 0.052(11) 0.048(8) 0.051(10) 0.019(7) 0.023(8) 0.015(8) N10A 0.048(10) 0.053(9) 0.043(7) 0.021(7) 0.009(7) 0.008(7) C19A 0.052(11) 0.053(10) 0.045(9) 0.030(8) 0.010(7) 0.014(8) N11A 0.042(10) 0.039(9) 0.040(8) 0.024(7) 0.005(7) 0.012(7) N12A 0.055(10) 0.054(9) 0.046(7) 0.021(7) 0.005(7) 0.026(8) C20A 0.046(10) 0.040(9) 0.043(9) 0.017(6) 0.009(7) 0.010(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O6 1.695(9) . ? Mo1 O9 1.734(9) . ? Mo1 O5 1.934(8) . ? Mo1 O3 1.954(8) . ? Mo1 O8 2.118(8) . ? Mo1 O8 2.348(8) 2_576 ? Mo1 Mo3 3.1942(17) . ? Mo1 Mo2 3.197(2) . ? Mo2 O12 1.696(11) . ? Mo2 O4 1.708(10) . ? Mo2 O7 1.879(10) . ? Mo2 O5 1.980(8) . ? Mo2 O8 2.315(7) . ? Mo2 O3 2.334(8) 2_576 ? Mo3 O11 1.694(10) . ? Mo3 O10 1.701(12) . ? Mo3 O1 1.874(9) . ? Mo3 O3 1.989(8) . ? Mo3 O5 2.299(9) 2_576 ? Mo3 O8 2.318(7) . ? Mo4 O2 1.732(7) . ? Mo4 O13 1.736(7) . ? Mo4 O7 1.905(10) . ? Mo4 O1 1.938(10) . ? Mo4 O9 2.273(11) 2_576 ? Mo4 O8 2.465(8) . ? O3 Mo2 2.334(8) 2_576 ? O5 Mo3 2.299(9) 2_576 ? O8 Mo1 2.348(8) 2_576 ? O9 Cu3 2.273(11) 2_576 ? O9 Mo4 2.273(11) 2_576 ? Cu1 N7 1.877(10) . ? Cu1 N1 1.885(9) . ? N1 C1 1.329(15) . ? N1 C2 1.345(14) . ? N2 C1 1.308(14) . ? N2 N3 1.364(13) . ? N2 C3 1.464(14) . ? N3 C2 1.301(15) . ? N7 C13 1.320(15) . ? N7 C14 1.353(17) . ? N8 N9 1.329(17) . ? N8 C13 1.329(16) . ? N8 C15 1.477(15) . ? N9 C14 1.313(18) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C4 1.497(16) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.375(17) . ? C4 C6 1.394(17) . ? C5 C8 1.416(19) . ? C5 H5 0.9500 . ? C6 C7 1.362(18) . ? C6 H6 0.9500 . ? C7 C9 1.37(2) . ? C7 H7 0.9500 . ? C8 C9 1.37(2) . ? C8 H8 0.9500 . ? C9 C10 1.520(19) . ? C10 N4A 1.45(2) . ? C10 N4 1.48(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 H10C 0.9900 . ? C10 H10D 0.9900 . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.507(18) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.39(2) . ? C16 C18 1.392(18) 2_563 ? C17 C18 1.379(19) . ? C17 H17 0.9500 . ? C18 C16 1.392(18) 2_563 ? C18 H18 0.9500 . ? C21 N11A 1.34(2) . ? C21 N11 1.49(3) . ? C21 C22 1.49(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 H21C 0.9900 . ? C21 H21D 0.9900 . ? C22 C23 1.37(2) . ? C22 C24 1.40(2) 2_687 ? C23 C24 1.37(2) . ? C23 H23 0.9500 . ? C24 C22 1.40(2) 2_687 ? C24 H24 0.9500 . ? Cu2 O2W 1.908(19) . ? Cu2 N5 1.963(10) . ? Cu2 N10 1.988(10) . ? Cu2 O1W 2.280(7) . ? N5 C11 1.313(13) . ? N5 C12 1.313(13) . ? C11 N4 1.313(13) . ? C11 H11 0.9500 . ? N4 N6 1.313(13) . ? N6 C12 1.313(13) . ? C12 H12 0.9500 . ? N10 C20 1.316(13) . ? N10 C19 1.316(13) . ? C19 N11 1.316(13) . ? C19 H19 0.9500 . ? N11 N12 1.316(13) . ? N12 C20 1.316(13) . ? C20 H20 0.9500 . ? O1W Cu2 2.280(7) 2_686 ? Cu2A N5A 1.953(10) . ? Cu2A N10A 1.968(10) . ? N5A C11A 1.279(12) . ? N5A C12A 1.279(12) . ? C11A N4A 1.279(12) . ? C11A H11A 0.9500 . ? N4A N6A 1.279(12) . ? N6A C12A 1.279(12) . ? C12A O5W 1.86(2) 2_686 ? C12A H12A 0.9500 . ? N10A C19A 1.302(12) . ? N10A C20A 1.302(12) . ? C19A N11A 1.302(12) . ? C19A H19A 0.9500 . ? N11A N12A 1.302(12) . ? N12A C20A 1.302(12) . ? C20A H20A 0.9500 . ? O4W O4W 1.39(3) 2_686 ? O4W O5W 1.64(2) 2_686 ? O5W O4W 1.64(2) 2_686 ? O5W C12A 1.86(9) 2_686 ? 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 O6 Mo1 O9 104.4(5) . . ? O6 Mo1 O5 100.5(5) . . ? O9 Mo1 O5 97.2(4) . . ? O6 Mo1 O3 101.8(5) . . ? O9 Mo1 O3 95.5(4) . . ? O5 Mo1 O3 150.6(4) . . ? O6 Mo1 O8 98.7(4) . . ? O9 Mo1 O8 156.9(4) . . ? O5 Mo1 O8 78.4(3) . . ? O3 Mo1 O8 79.5(3) . . ? O6 Mo1 O8 174.6(4) . 2_576 ? O9 Mo1 O8 81.0(4) . 2_576 ? O5 Mo1 O8 78.1(3) . 2_576 ? O3 Mo1 O8 77.8(3) . 2_576 ? O8 Mo1 O8 75.9(3) . 2_576 ? O6 Mo1 Mo3 91.1(4) . . ? O9 Mo1 Mo3 131.8(3) . . ? O5 Mo1 Mo3 124.8(3) . . ? O3 Mo1 Mo3 36.3(2) . . ? O8 Mo1 Mo3 46.5(2) . . ? O8 Mo1 Mo3 85.47(19) 2_576 . ? O6 Mo1 Mo2 89.4(4) . . ? O9 Mo1 Mo2 132.9(3) . . ? O5 Mo1 Mo2 35.7(2) . . ? O3 Mo1 Mo2 125.9(2) . . ? O8 Mo1 Mo2 46.4(2) . . ? O8 Mo1 Mo2 86.55(18) 2_576 . ? Mo3 Mo1 Mo2 91.67(4) . . ? O12 Mo2 O4 105.1(6) . . ? O12 Mo2 O7 102.1(5) . . ? O4 Mo2 O7 101.3(5) . . ? O12 Mo2 O5 96.9(5) . . ? O4 Mo2 O5 100.4(5) . . ? O7 Mo2 O5 146.1(4) . . ? O12 Mo2 O8 95.4(4) . . ? O4 Mo2 O8 159.1(5) . . ? O7 Mo2 O8 77.6(3) . . ? O5 Mo2 O8 72.8(3) . . ? O12 Mo2 O3 164.5(4) . 2_576 ? O4 Mo2 O3 87.5(5) . 2_576 ? O7 Mo2 O3 83.8(4) . 2_576 ? O5 Mo2 O3 71.5(3) . 2_576 ? O8 Mo2 O3 71.6(3) . 2_576 ? O12 Mo2 Mo1 85.7(4) . . ? O4 Mo2 Mo1 135.2(4) . . ? O7 Mo2 Mo1 119.0(3) . . ? O5 Mo2 Mo1 34.8(2) . . ? O8 Mo2 Mo1 41.45(19) . . ? O3 Mo2 Mo1 78.89(19) 2_576 . ? O11 Mo3 O10 103.5(6) . . ? O11 Mo3 O1 101.3(5) . . ? O10 Mo3 O1 102.6(5) . . ? O11 Mo3 O3 100.8(4) . . ? O10 Mo3 O3 93.9(5) . . ? O1 Mo3 O3 148.3(4) . . ? O11 Mo3 O5 91.0(5) . 2_576 ? O10 Mo3 O5 161.6(5) . 2_576 ? O1 Mo3 O5 85.1(4) . 2_576 ? O3 Mo3 O5 72.1(3) . 2_576 ? O11 Mo3 O8 163.1(5) . . ? O10 Mo3 O8 92.9(4) . . ? O1 Mo3 O8 78.2(3) . . ? O3 Mo3 O8 74.1(3) . . ? O5 Mo3 O8 72.1(3) 2_576 . ? O11 Mo3 Mo1 136.2(3) . . ? O10 Mo3 Mo1 82.9(4) . . ? O1 Mo3 Mo1 119.7(3) . . ? O3 Mo3 Mo1 35.5(2) . . ? O5 Mo3 Mo1 78.8(2) 2_576 . ? O8 Mo3 Mo1 41.51(19) . . ? O2 Mo4 O13 105.5(6) . . ? O2 Mo4 O7 103.0(5) . . ? O13 Mo4 O7 97.4(5) . . ? O2 Mo4 O1 103.9(6) . . ? O13 Mo4 O1 97.6(5) . . ? O7 Mo4 O1 144.3(4) . . ? O2 Mo4 O9 91.5(5) . 2_576 ? O13 Mo4 O9 162.9(4) . 2_576 ? O7 Mo4 O9 78.3(4) . 2_576 ? O1 Mo4 O9 78.0(4) . 2_576 ? O2 Mo4 O8 160.6(5) . . ? O13 Mo4 O8 93.8(4) . . ? O7 Mo4 O8 73.4(3) . . ? O1 Mo4 O8 73.5(3) . . ? O9 Mo4 O8 69.1(3) 2_576 . ? Mo3 O1 Mo4 117.7(5) . . ? Mo1 O3 Mo3 108.2(4) . . ? Mo1 O3 Mo2 110.0(3) . 2_576 ? Mo3 O3 Mo2 103.0(4) . 2_576 ? Mo1 O5 Mo2 109.5(4) . . ? Mo1 O5 Mo3 110.4(4) . 2_576 ? Mo2 O5 Mo3 104.6(4) . 2_576 ? Mo2 O7 Mo4 118.4(4) . . ? Mo1 O8 Mo2 92.2(3) . . ? Mo1 O8 Mo3 92.0(3) . . ? Mo2 O8 Mo3 163.4(4) . . ? Mo1 O8 Mo1 104.1(3) . 2_576 ? Mo2 O8 Mo1 98.0(3) . 2_576 ? Mo3 O8 Mo1 96.5(3) . 2_576 ? Mo1 O8 Mo4 164.4(4) . . ? Mo2 O8 Mo4 85.6(2) . . ? Mo3 O8 Mo4 86.0(3) . . ? Mo1 O8 Mo4 91.6(3) 2_576 . ? Mo1 O9 Cu3 118.3(5) . 2_576 ? Mo1 O9 Mo4 118.3(5) . 2_576 ? Cu3 O9 Mo4 0.00(4) 2_576 2_576 ? N7 Cu1 N1 175.0(4) . . ? C1 N1 C2 103.1(9) . . ? C1 N1 Cu1 126.8(8) . . ? C2 N1 Cu1 129.5(8) . . ? C1 N2 N3 110.4(9) . . ? C1 N2 C3 128.6(10) . . ? N3 N2 C3 121.0(9) . . ? C2 N3 N2 102.2(9) . . ? C13 N7 C14 103.7(11) . . ? C13 N7 Cu1 129.2(9) . . ? C14 N7 Cu1 127.1(9) . . ? N9 N8 C13 111.2(10) . . ? N9 N8 C15 121.2(12) . . ? C13 N8 C15 127.5(13) . . ? C14 N9 N8 102.9(11) . . ? N2 C1 N1 109.6(10) . . ? N2 C1 H1 125.2 . . ? N1 C1 H1 125.2 . . ? N3 C2 N1 114.7(10) . . ? N3 C2 H2 122.6 . . ? N1 C2 H2 122.6 . . ? N2 C3 C4 112.0(9) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C6 119.5(11) . . ? C5 C4 C3 121.1(11) . . ? C6 C4 C3 119.4(11) . . ? C4 C5 C8 118.6(12) . . ? C4 C5 H5 120.7 . . ? C8 C5 H5 120.7 . . ? C7 C6 C4 121.3(12) . . ? C7 C6 H6 119.3 . . ? C4 C6 H6 119.3 . . ? C6 C7 C9 119.6(13) . . ? C6 C7 H7 120.2 . . ? C9 C7 H7 120.2 . . ? C9 C8 C5 120.4(13) . . ? C9 C8 H8 119.8 . . ? C5 C8 H8 119.8 . . ? C8 C9 C7 120.6(13) . . ? C8 C9 C10 119.3(14) . . ? C7 C9 C10 120.0(14) . . ? N4A C10 N4 12.5(15) . . ? N4A C10 C9 110.9(17) . . ? N4 C10 C9 111.2(17) . . ? N4A C10 H10A 119.8 . . ? N4 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? N4A C10 H10B 98.4 . . ? N4 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N4A C10 H10C 109.5 . . ? N4 C10 H10C 98.2 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 12.7 . . ? H10B C10 H10C 118.7 . . ? N4A C10 H10D 109.5 . . ? N4 C10 H10D 119.6 . . ? C9 C10 H10D 109.5 . . ? H10A C10 H10D 96.6 . . ? H10B C10 H10D 12.6 . . ? H10C C10 H10D 108.0 . . ? N7 C13 N8 108.6(12) . . ? N7 C13 H13 125.7 . . ? N8 C13 H13 125.7 . . ? N9 C14 N7 113.6(13) . . ? N9 C14 H14 123.2 . . ? N7 C14 H14 123.2 . . ? N8 C15 C16 111.5(11) . . ? N8 C15 H15A 109.3 . . ? C16 C15 H15A 109.3 . . ? N8 C15 H15B 109.3 . . ? C16 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C18 118.6(12) . 2_563 ? C17 C16 C15 120.9(13) . . ? C18 C16 C15 120.5(15) 2_563 . ? C18 C17 C16 120.7(12) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C16 120.7(14) . 2_563 ? C17 C18 H18 119.6 . . ? C16 C18 H18 119.6 2_563 . ? N11A C21 N11 14.7(14) . . ? N11A C21 C22 108.8(17) . . ? N11 C21 C22 120.6(16) . . ? N11A C21 H21A 121.1 . . ? N11 C21 H21A 107.2 . . ? C22 C21 H21A 107.2 . . ? N11A C21 H21B 105.0 . . ? N11 C21 H21B 107.2 . . ? C22 C21 H21B 107.2 . . ? H21A C21 H21B 106.8 . . ? N11A C21 H21C 109.9 . . ? N11 C21 H21C 96.5 . . ? C22 C21 H21C 109.9 . . ? H21A C21 H21C 11.8 . . ? H21B C21 H21C 115.7 . . ? N11A C21 H21D 109.9 . . ? N11 C21 H21D 110.4 . . ? C22 C21 H21D 109.9 . . ? H21A C21 H21D 99.3 . . ? H21B C21 H21D 7.5 . . ? H21C C21 H21D 108.3 . . ? C23 C22 C24 118.9(16) . 2_687 ? C23 C22 C21 121.1(14) . . ? C24 C22 C21 119.9(14) 2_687 . ? C22 C23 C24 120.7(15) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C22 120.3(14) . 2_687 ? C23 C24 H24 119.9 . . ? C22 C24 H24 119.9 2_687 . ? O2W Cu2 N5 83.2(9) . . ? O2W Cu2 N10 65.5(8) . . ? N5 Cu2 N10 145.2(10) . . ? O2W Cu2 O1W 158.4(6) . . ? N5 Cu2 O1W 112.0(8) . . ? N10 Cu2 O1W 102.3(6) . . ? C11 N5 C12 108.0 . . ? C11 N5 Cu2 132.1(14) . . ? C12 N5 Cu2 119.4(14) . . ? N5 C11 N4 108.0 . . ? N5 C11 H11 126.0 . . ? N4 C11 H11 126.0 . . ? C11 N4 N6 108.0 . . ? C11 N4 C10 128.1(17) . . ? N6 N4 C10 123.7(17) . . ? C12 N6 N4 108.0 . . ? N6 C12 N5 108.0 . . ? N6 C12 H12 126.0 . . ? N5 C12 H12 126.0 . . ? C20 N10 C19 108.0 . . ? C20 N10 Cu2 132.7(12) . . ? C19 N10 Cu2 117.7(12) . . ? N11 C19 N10 108.0 . . ? N11 C19 H19 126.0 . . ? N10 C19 H19 126.0 . . ? N12 N11 C19 108.0 . . ? N12 N11 C21 119.6(16) . . ? C19 N11 C21 130.0(16) . . ? C20 N12 N11 108.0 . . ? N10 C20 N12 108.0 . . ? N10 C20 H20 126.0 . . ? N12 C20 H20 126.0 . . ? Cu2 O1W Cu2 180 . 2_686 ? N5A Cu2A N10A 164.1(11) . . ? C11A N5A C12A 108.0 . . ? C11A N5A Cu2A 135.8(15) . . ? C12A N5A Cu2A 115.6(15) . . ? N5A C11A N4A 108.0 . . ? N5A C11A H11A 126.0 . . ? N4A C11A H11A 126.0 . . ? N6A N4A C11A 108.0 . . ? N6A N4A C10 124.8(18) . . ? C11A N4A C10 127.2(18) . . ? N4A N6A C12A 108.0 . . ? N5A C12A N6A 108.0 . . ? N5A C12A O5W 107.6(15) . 2_686 ? N6A C12A O5W 142.4(15) . 2_686 ? N5A C12A H12A 126.0 . . ? N6A C12A H12A 126.0 . . ? O5W C12A H12A 21.2 2_686 . ? C19A N10A C20A 108.0 . . ? C19A N10A Cu2A 117.1(13) . . ? C20A N10A Cu2A 133.6(12) . . ? N10A C19A N11A 108.0 . . ? N10A C19A H19A 126.0 . . ? N11A C19A H19A 126.0 . . ? C19A N11A N12A 108.0 . . ? C19A N11A C21 128.3(16) . . ? N12A N11A C21 123.7(17) . . ? C20A N12A N11A 108.0 . . ? N10A C20A N12A 108.0 . . ? N10A C20A H20A 126.0 . . ? N12A C20A H20A 126.0 . . ? O4W O4W O5W 97.5(13) 2_686 2_686 ? O4W O5W C12A 152(6) 2_686 2_686 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.319 _refine_diff_density_min -1.395 _refine_diff_density_rms 0.187 # Attachment '- compound-3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 832447' #TrackingRef '- compound-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H60 Cu3 Mo8 N30 O26' _chemical_formula_weight 2575.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.583(3) _cell_length_b 13.642(3) _cell_length_c 14.263(3) _cell_angle_alpha 105.78(3) _cell_angle_beta 114.65(3) _cell_angle_gamma 101.16(3) _cell_volume 2005.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0.53 _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1261 _exptl_absorpt_coefficient_mu 2.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_T_max 0.646 _exptl_absorpt_process_details ? _exptl_special_details ; Higashi, T. (1995) A program for absorption correction. RIGAKU corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15088 _diffrn_reflns_av_R_equivalents 0.1264 _diffrn_reflns_av_sigmaI/netI 0.1823 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6927 _reflns_number_gt 3689 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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. During the refinement, the command 'omit -3 50' was used to omit the weak reflections above 50 degree. The restrained commands 'AFIX 59' and 'AFIX 69' were used to fix all the disordered 5-member and 6-member rings. Furthermore, the restrained command 'isor' was used to retrain some non-H atoms with NPD or ADP problems. These atoms are as follows: N12 N11 C24 N7 C23 C14 and C25. And the commond EADP was used to the atoms C2 C29 C28 C27 C26 and C30. All these restrained command led to a high restraint value of 53. they are as follow: DFIX 2.0 cu2 n7 cu2 n13 to define the Cu-N distance DFIX 1.4 n14 c27 DFIX 2.8 c27 c30 to define the N-C and the C-C distance DFIX 1.4 c32 c29 c29 c28 c28 c30 c30 c27 c30 c31 c31 c33 c33 c32 to define the C-C distance of the organic ligand eadp C2 C29 C28 C27 C26 C30 to refine the C2 C29 C28 C27 C26 C30 atoms isor 0.001 N12 N11 C24 N7 C23 C14 C25 to avoid the ADP and NPD problems The order afix 59 and Afix 0 were used to define the five member-ring N10 N11 C24 N12 C23 and N13 C25 N14 N15 C26 and N16 N17 C36 N18 C35. The order AFIX 69 and AFIX 0 were used to define the six member-ring C29 C28 C30 C31 C32 C33. And the orders AFIX 43, AFIX 23 and AFIX 0 were used to define all the H atoms. The highest residual peak and the deepest hole are both close to the heavy metal centers and featureless. ; _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^)+(0.0000P)^2^+6.6573P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method shelxl _refine_ls_extinction_coef ? _refine_ls_number_reflns 6927 _refine_ls_number_parameters 516 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.1317 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.235 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 1.16338(10) -1.46140(10) -0.40574(9) 0.0261(3) Uani 1 1 d . . . Mo2 Mo 0.95541(12) -1.34525(10) -0.35285(10) 0.0314(3) Uani 1 1 d . . . Mo3 Mo 0.84878(11) -1.78864(10) -0.59456(10) 0.0294(3) Uani 1 1 d . . . Mo4 Mo 0.97341(11) -1.59044(10) -0.34816(9) 0.0292(3) Uani 1 1 d . . . Cu1 Cu 1.0000 -2.0000 -0.5000 0.0285(6) Uani 1 2 d S . . O13 O 0.9542(9) -1.8478(8) -0.5390(7) 0.034(2) Uani 1 1 d . . . O12 O 1.0856(9) -1.6412(8) -0.2917(8) 0.042(3) Uani 1 1 d . . . O11 O 1.2646(9) -1.5200(8) -0.3486(8) 0.040(3) Uani 1 1 d . . . O10 O 1.1093(9) -1.2329(7) -0.2962(7) 0.029(2) Uani 1 1 d . . . O9 O 0.8497(9) -1.2928(8) -0.4234(8) 0.043(3) Uani 1 1 d . . . O8 O 0.9980(8) -1.6020(7) -0.5032(7) 0.028(2) Uani 1 1 d . . . O7 O 1.0882(8) -1.4457(7) -0.3108(7) 0.026(2) Uani 1 1 d . . . O6 O 0.8542(8) -1.5012(8) -0.4461(7) 0.030(2) Uani 1 1 d . . . O5 O 0.8395(8) -1.7194(8) -0.4640(7) 0.032(2) Uani 1 1 d . . . O4 O 0.9222(11) -1.5584(8) -0.2552(8) 0.045(3) Uani 1 1 d . . . O3 O 1.2527(8) -1.3250(7) -0.3519(7) 0.028(2) Uani 1 1 d . . . O2 O 0.7107(9) -1.8925(9) -0.6749(8) 0.049(3) Uani 1 1 d . . . O1 O 0.9514(11) -1.3301(9) -0.2340(8) 0.048(3) Uani 1 1 d . . . N1 N 1.1673(12) -1.8876(9) -0.3752(9) 0.035(3) Uani 1 1 d . . . N2 N 1.3384(11) -1.7447(9) -0.2675(9) 0.034(3) Uani 1 1 d . . . N3 N 1.3496(12) -1.8118(11) -0.2107(10) 0.044(4) Uani 1 1 d . . . N4 N 0.9366(11) -1.9790(10) -0.3907(9) 0.033(3) Uani 1 1 d . . . N5 N 0.8573(12) -1.9938(10) -0.2844(10) 0.037(3) Uani 1 1 d . . . N6 N 0.8944(16) -1.8845(13) -0.2642(11) 0.062(5) Uani 1 1 d . . . N7 N 1.6982(18) -0.3692(17) 0.8420(13) 0.091(6) Uani 1 1 d DU . . N8 N 1.6920(15) -0.3084(12) 0.9325(13) 0.059(4) Uani 1 1 d . . . C1 C 1.2478(15) -1.8946(12) -0.2765(11) 0.045(5) Uani 1 1 d . . . H1A H 1.2295 -1.9546 -0.2594 0.054 Uiso 1 1 calc R . . C2 C 1.2300(16) -1.7913(15) -0.3629(14) 0.053(3) Uiso 1 1 d . . . H2A H 1.2019 -1.7599 -0.4146 0.064 Uiso 1 1 calc R . . C3 C 1.4407(14) -1.6433(12) -0.2193(11) 0.042(4) Uani 1 1 d . . . H3A H 1.4207 -1.6066 -0.2704 0.050 Uiso 1 1 calc R . . H3B H 1.5151 -1.6592 -0.2116 0.050 Uiso 1 1 calc R . . C5 C 1.5849(14) -1.5409(12) -0.0135(12) 0.042(4) Uani 1 1 d . . . H5A H 1.6423 -1.5702 -0.0232 0.050 Uiso 1 1 calc R . . C4 C 1.4684(14) -1.5673(11) -0.1050(11) 0.034(4) Uani 1 1 d . . . C6 C 1.3848(15) -1.5277(15) -0.0902(13) 0.050(5) Uani 1 1 d . . . H6A H 1.3058 -1.5470 -0.1510 0.060 Uiso 1 1 calc R . . C7 C 0.9386(18) -1.8790(14) -0.3321(13) 0.052(5) Uani 1 1 d . . . H7A H 0.9678 -1.8153 -0.3398 0.062 Uiso 1 1 calc R . . C8 C 0.8837(14) -2.0417(13) -0.3569(12) 0.041(4) Uani 1 1 d . . . H8A H 0.8665 -2.1164 -0.3838 0.049 Uiso 1 1 calc R . . C9 C 0.8069(15) -2.0299(14) -0.2195(11) 0.046(4) Uani 1 1 d . . . H9A H 0.7555 -2.1064 -0.2610 0.055 Uiso 1 1 calc R . . H9B H 0.7541 -1.9897 -0.2095 0.055 Uiso 1 1 calc R . . C10 C 0.9089(17) -2.0139(12) -0.1051(12) 0.045(4) Uani 1 1 d . . . C11 C 0.9763(16) -1.9113(14) -0.0228(13) 0.050(4) Uani 1 1 d . . . H11A H 0.9621 -1.8509 -0.0364 0.060 Uiso 1 1 calc R . . C12 C 1.0684(16) -1.8999(12) 0.0839(13) 0.046(4) Uani 1 1 d . . . H12A H 1.1145 -1.8308 0.1408 0.055 Uiso 1 1 calc R . . C15 C 1.6226(14) -0.1462(13) 0.9423(11) 0.039(4) Uani 1 1 d . . . C16 C 1.7359(15) -0.0664(14) 1.0311(13) 0.048(5) Uani 1 1 d . . . H16A H 1.7988 -0.0862 1.0760 0.058 Uiso 1 1 calc R . . C17 C 1.5343(15) -0.1149(13) 0.8752(13) 0.051(5) Uani 1 1 d . . . H17A H 1.4599 -0.1677 0.8150 0.061 Uiso 1 1 calc R . . C18 C 1.5524(15) -0.0083(14) 0.8942(15) 0.060(6) Uani 1 1 d . . . H18A H 1.4909 0.0106 0.8463 0.072 Uiso 1 1 calc R . . C19 C 1.7534(15) 0.0431(13) 1.0514(13) 0.047(4) Uani 1 1 d . . . H19A H 1.8281 0.0963 1.1110 0.056 Uiso 1 1 calc R . . C20 C 1.5936(16) -0.2665(14) 0.9270(14) 0.049(4) Uani 1 1 d . . . H20A H 1.5751 -0.2749 0.9845 0.059 Uiso 1 1 calc R . . H20B H 1.5191 -0.3104 0.8547 0.059 Uiso 1 1 calc R . . C21 C 1.6627(14) 0.0733(12) 0.9852(11) 0.038(4) Uani 1 1 d . . . C22 C 1.6744(18) 0.1905(16) 1.0114(15) 0.061(5) Uiso 1 1 d . . . H22A H 1.5913 0.1939 0.9765 0.073 Uiso 1 1 calc R . . H22B H 1.7113 0.2279 1.0920 0.073 Uiso 1 1 calc R . . N10 N 1.7485(10) 0.2486(9) 0.9750(9) 0.045(4) Uani 1 1 d G . . N11 N 1.7270(13) 0.2154(11) 0.8702(10) 0.099(6) Uani 1 1 d GU . . C24 C 1.8042(15) 0.2915(13) 0.8641(12) 0.124(10) Uani 1 1 d GU . . H24A H 1.8089 0.2891 0.8002 0.149 Uiso 1 1 calc R . . N12 N 1.8734(13) 0.3717(11) 0.9651(12) 0.076(5) Uani 1 1 d GU . . C23 C 1.8390(11) 0.3452(10) 1.0337(9) 0.076(6) Uani 1 1 d GU . . H23A H 1.8725 0.3870 1.1095 0.091 Uiso 1 1 calc R . . N9 N 1.848(2) -0.367(2) 0.991(2) 0.123(8) Uiso 1 1 d . . . C13 C 1.800(3) -0.395(2) 0.888(2) 0.109(9) Uiso 1 1 d . . . H13A H 1.8317 -0.4312 0.8461 0.130 Uiso 1 1 calc R . . C14 C 1.788(3) -0.312(2) 1.029(2) 0.109(9) Uani 1 1 d U . . H14A H 1.8045 -0.2818 1.1028 0.131 Uiso 1 1 calc R . . Cu2 Cu 1.6009(5) -0.4021(4) 0.6955(4) 0.0645(14) Uani 0.50 1 d PD . . Cu3 Cu 2.0265(6) 0.4635(5) 0.9801(6) 0.095(2) Uani 0.50 1 d P . . C27 C 1.365(3) -0.235(2) 0.391(3) 0.053(3) Uiso 0.50 1 d PD . . H27A H 1.2805 -0.2589 0.3776 0.064 Uiso 0.50 1 calc PR . . H27B H 1.3625 -0.2534 0.3191 0.064 Uiso 0.50 1 calc PR . . C34 C 1.537(4) 0.175(3) 0.431(3) 0.067(11) Uiso 0.50 1 d P . . H34A H 1.4784 0.1466 0.3522 0.081 Uiso 0.50 1 d PR . . H34B H 1.6197 0.1956 0.4417 0.081 Uiso 0.50 1 d PR . . N13 N 1.538(2) -0.346(2) 0.5751(19) 0.081 Uiso 0.50 1 d PGD . . C25 C 1.456(3) -0.294(2) 0.551(2) 0.085(13) Uani 0.50 1 d PGU . . H25A H 1.4187 -0.2685 0.5942 0.102 Uiso 0.50 1 d PR . . N14 N 1.437(3) -0.283(2) 0.455(2) 0.102 Uiso 0.50 1 d PGD . . N15 N 1.506(3) -0.329(2) 0.420(2) 0.102 Uiso 0.50 1 d PG . . C26 C 1.569(2) -0.368(2) 0.494(2) 0.053(3) Uiso 0.50 1 d PG . . H26A H 1.6253 -0.4048 0.4904 0.064 Uiso 0.50 1 d PR . . C29 C 1.423(2) -0.027(2) 0.531(2) 0.053(3) Uiso 0.50 1 d PGD . . H29A H 1.3874 -0.0370 0.5765 0.064 Uiso 0.50 1 d PR . . C28 C 1.429(2) -0.1134(17) 0.460(2) 0.053(3) Uiso 0.50 1 d PGD . . C30 C 1.481(2) -0.0978(17) 0.3956(18) 0.053(3) Uiso 0.50 1 d PGD . . H30A H 1.4853 -0.1584 0.3463 0.064 Uiso 0.50 1 d PR . . C31 C 1.527(2) 0.005(2) 0.4016(19) 0.080(13) Uiso 0.50 1 d PGD . . H31A H 1.5631 0.0155 0.3566 0.096 Uiso 0.50 1 d PR . . C33 C 1.521(3) 0.0914(17) 0.472(2) 0.054(9) Uiso 0.50 1 d PGD . . C32 C 1.469(3) 0.076(2) 0.537(2) 0.100(16) Uiso 0.50 1 d PGD . . H32A H 1.4646 0.1363 0.5859 0.120 Uiso 0.50 1 d PR . . N16 N 1.519(2) 0.2687(19) 0.488(2) 0.072(10) Uiso 0.50 1 d PG . . N17 N 1.404(2) 0.276(2) 0.4572(19) 0.060(8) Uiso 0.50 1 d PG . . C36 C 1.420(2) 0.378(2) 0.521(2) 0.16(3) Uiso 0.50 1 d PG . . H36A H 1.3551 0.4053 0.5171 0.195 Uiso 0.50 1 d PR . . N18 N 1.544(2) 0.4326(19) 0.5905(18) 0.052(7) Uiso 0.50 1 d PG . . C35 C 1.605(2) 0.365(2) 0.5700(19) 0.056(9) Uiso 0.50 1 d PG . . H35A H 1.6936 0.3828 0.6071 0.067 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0235(6) 0.0229(7) 0.0282(6) 0.0101(5) 0.0092(5) 0.0091(5) Mo2 0.0384(7) 0.0237(7) 0.0354(7) 0.0107(5) 0.0204(6) 0.0140(6) Mo3 0.0274(6) 0.0236(7) 0.0293(7) 0.0086(5) 0.0093(6) 0.0070(5) Mo4 0.0327(7) 0.0256(7) 0.0277(6) 0.0113(5) 0.0136(5) 0.0093(5) Cu1 0.0339(13) 0.0242(13) 0.0249(12) 0.0077(10) 0.0149(10) 0.0081(10) O13 0.033(5) 0.034(6) 0.034(5) 0.012(4) 0.015(4) 0.014(4) O12 0.043(6) 0.032(6) 0.050(6) 0.017(5) 0.023(5) 0.014(5) O11 0.035(5) 0.036(6) 0.051(6) 0.020(5) 0.017(5) 0.021(5) O10 0.038(5) 0.022(5) 0.020(4) 0.002(4) 0.010(4) 0.012(4) O9 0.047(6) 0.021(6) 0.055(7) 0.013(5) 0.019(5) 0.016(5) O8 0.025(5) 0.030(6) 0.022(4) 0.005(4) 0.010(4) 0.012(4) O7 0.035(5) 0.012(5) 0.032(5) 0.011(4) 0.017(4) 0.005(4) O6 0.027(5) 0.034(6) 0.029(5) 0.013(4) 0.015(4) 0.010(4) O5 0.032(5) 0.031(6) 0.036(5) 0.017(4) 0.015(4) 0.014(4) O4 0.074(8) 0.016(5) 0.055(6) 0.010(5) 0.045(6) 0.011(5) O3 0.028(5) 0.012(5) 0.038(5) 0.008(4) 0.015(4) 0.004(4) O2 0.031(6) 0.063(8) 0.029(5) 0.013(5) 0.004(5) 0.003(5) O1 0.067(7) 0.051(7) 0.031(5) 0.015(5) 0.030(5) 0.023(6) N1 0.053(8) 0.022(7) 0.031(6) 0.013(5) 0.021(6) 0.008(6) N2 0.035(6) 0.028(7) 0.030(6) 0.016(5) 0.008(5) 0.011(5) N3 0.046(8) 0.039(8) 0.034(7) 0.014(6) 0.011(6) 0.008(6) N4 0.037(7) 0.036(7) 0.030(6) 0.011(5) 0.023(5) 0.012(6) N5 0.061(8) 0.026(7) 0.049(7) 0.020(6) 0.044(7) 0.019(6) N6 0.101(13) 0.067(11) 0.053(9) 0.035(8) 0.055(9) 0.045(10) N7 0.091(6) 0.091(6) 0.091(6) 0.036(3) 0.046(3) 0.031(2) N8 0.068(10) 0.033(8) 0.078(10) 0.008(7) 0.049(9) 0.010(7) C1 0.066(11) 0.028(9) 0.030(8) 0.018(7) 0.011(8) 0.018(8) C3 0.043(9) 0.036(9) 0.030(8) 0.018(7) 0.006(7) 0.003(7) C5 0.040(9) 0.025(8) 0.052(9) 0.014(7) 0.016(8) 0.012(7) C4 0.047(9) 0.014(7) 0.025(7) 0.004(6) 0.011(7) -0.002(6) C6 0.036(9) 0.061(12) 0.036(9) 0.010(8) 0.008(8) 0.018(8) C7 0.086(13) 0.038(10) 0.045(9) 0.023(8) 0.041(9) 0.021(9) C8 0.051(10) 0.031(9) 0.046(9) 0.013(7) 0.032(8) 0.013(7) C9 0.060(10) 0.048(11) 0.023(7) 0.011(7) 0.022(7) 0.008(8) C10 0.091(13) 0.020(8) 0.050(9) 0.016(7) 0.059(9) 0.014(8) C11 0.070(11) 0.037(10) 0.058(10) 0.017(8) 0.046(9) 0.021(9) C12 0.072(11) 0.020(8) 0.045(9) 0.009(7) 0.036(9) 0.006(8) C15 0.037(8) 0.050(11) 0.026(7) 0.010(7) 0.018(7) 0.008(7) C16 0.037(9) 0.061(12) 0.043(9) 0.027(8) 0.013(7) 0.015(8) C17 0.044(9) 0.037(10) 0.040(9) 0.011(7) 0.002(8) 0.002(8) C18 0.035(9) 0.043(11) 0.071(12) 0.024(9) 0.003(9) 0.007(8) C19 0.047(9) 0.031(9) 0.051(10) 0.008(7) 0.022(8) 0.010(7) C20 0.052(10) 0.046(11) 0.058(10) 0.023(8) 0.033(9) 0.018(8) C21 0.041(8) 0.029(9) 0.036(8) 0.008(6) 0.019(7) 0.008(7) N10 0.046(8) 0.024(7) 0.043(7) 0.009(6) 0.013(6) 0.000(6) N11 0.099(6) 0.099(6) 0.099(6) 0.039(3) 0.050(3) 0.034(2) C24 0.124(10) 0.124(10) 0.124(10) 0.049(4) 0.062(5) 0.043(4) N12 0.075(5) 0.076(5) 0.076(5) 0.031(2) 0.037(3) 0.026(2) C23 0.076(6) 0.076(6) 0.076(6) 0.030(3) 0.037(3) 0.026(2) C14 0.109(9) 0.109(9) 0.109(9) 0.043(4) 0.055(4) 0.038(3) Cu2 0.066(3) 0.065(3) 0.061(3) 0.022(2) 0.035(2) 0.017(2) Cu3 0.083(4) 0.055(4) 0.148(5) 0.038(4) 0.071(4) 0.002(3) C25 0.085(13) 0.085(13) 0.085(13) 0.034(5) 0.042(6) 0.030(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 Mo1 O11 1.676(9) . ? Mo1 O3 1.735(8) . ? Mo1 O6 1.937(9) 2_724 ? Mo1 O7 1.940(10) . ? Mo1 O8 2.129(9) . ? Mo1 O8 2.376(9) 2_724 ? Mo1 Mo4 3.207(2) . ? Mo1 Mo2 3.207(3) 2_724 ? Mo2 O1 1.675(10) . ? Mo2 O9 1.714(10) . ? Mo2 O10 1.904(9) . ? Mo2 O6 1.979(9) . ? Mo2 O8 2.334(9) 2_724 ? Mo2 O7 2.351(9) . ? Mo2 Mo1 3.207(3) 2_724 ? Mo3 O2 1.686(10) . ? Mo3 O13 1.710(10) . ? Mo3 O5 1.909(10) . ? Mo3 O10 1.915(9) 2_724 ? Mo3 O3 2.283(9) 2_724 ? Mo3 O8 2.452(9) . ? Mo4 O12 1.690(10) . ? Mo4 O4 1.694(11) . ? Mo4 O5 1.901(9) . ? Mo4 O7 1.987(8) . ? Mo4 O8 2.325(9) . ? Mo4 O6 2.360(9) . ? Cu1 N4 2.008(12) 2_714 ? Cu1 N4 2.008(12) . ? Cu1 N1 2.023(11) . ? Cu1 N1 2.023(11) 2_714 ? Cu1 O13 2.403(10) . ? Cu1 O13 2.403(10) 2_714 ? O10 Mo3 1.915(9) 2_724 ? O8 Mo2 2.334(9) 2_724 ? O8 Mo1 2.376(9) 2_724 ? O6 Mo1 1.937(9) 2_724 ? O3 Mo3 2.283(9) 2_724 ? N1 C2 1.32(2) . ? N1 C1 1.392(16) . ? N2 C2 1.327(18) . ? N2 N3 1.367(15) . ? N2 C3 1.449(17) . ? N3 C1 1.288(18) . ? N4 C8 1.295(18) . ? N4 C7 1.38(2) . ? N5 C8 1.27(2) . ? N5 N6 1.382(19) . ? N5 C9 1.455(18) . ? N6 C7 1.31(2) . ? N7 C13 1.34(3) . ? N7 N8 1.37(2) . ? N7 Cu2 1.792(15) . ? N8 C14 1.42(3) . ? N8 C20 1.44(2) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.52(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.36(2) 2_825 ? C5 C4 1.387(19) . ? C5 H5A 0.9300 . ? C4 C6 1.34(2) . ? C6 C5 1.36(2) 2_825 ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C9 C10 1.52(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C12 1.34(2) 2_715 ? C10 C11 1.37(2) . ? C11 C12 1.42(2) . ? C11 H11A 0.9300 . ? C12 C10 1.34(2) 2_715 ? C12 H12A 0.9300 . ? C15 C17 1.36(2) . ? C15 C16 1.40(2) . ? C15 C20 1.54(2) . ? C16 C19 1.40(2) . ? C16 H16A 0.9300 . ? C17 C18 1.36(2) . ? C17 H17A 0.9300 . ? C18 C21 1.40(2) . ? C18 H18A 0.9300 . ? C19 C21 1.36(2) . ? C19 H19A 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.50(2) . ? C22 N10 1.45(2) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? N10 C23 1.326(9) . ? N10 N11 1.326(9) . ? N11 C24 1.326(9) . ? C24 N12 1.326(9) . ? C24 H24A 0.9300 . ? N12 C23 1.326(9) . ? N12 Cu3 1.975(14) . ? N12 Cu3 2.092(14) 2_967 ? C23 H23A 0.9300 . ? N9 C13 1.24(3) . ? N9 C14 1.34(4) . ? N9 Cu3 2.23(3) 2_957 ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? Cu2 N13 1.990(18) . ? Cu2 N18 2.12(19) 1_545 ? Cu3 Cu3 1.423(14) 2_967 ? Cu3 N12 2.09(4) 2_967 ? Cu3 N9 2.23(3) 2_957 ? C27 N14 1.39(2) . ? C27 C28 1.52(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C34 C33 1.43(4) . ? C34 N16 1.43(5) . ? C34 C25 1.56(13) 2_856 ? C34 N14 1.73(16) 2_856 ? C34 C28 1.89(5) 2_856 ? C34 H34A 0.9601 . ? C34 H34B 0.9600 . ? N13 C26 1.342(17) . ? N13 C25 1.343(17) . ? N13 N17 1.38(16) 2_856 ? N13 C36 1.6(2) 2_856 ? N13 N16 1.65(3) 2_856 ? C25 N16 0.84(3) 2_856 ? C25 N14 1.342(17) . ? C25 C35 1.48(15) 2_856 ? C25 C34 1.56(5) 2_856 ? C25 N17 1.77(18) 2_856 ? C25 H25A 0.9604 . ? N14 N16 0.72(3) 2_856 ? N14 C35 1.03(13) 2_856 ? N14 N15 1.343(17) . ? N14 C34 1.73(5) 2_856 ? N14 N17 1.83(15) 2_856 ? N15 C26 1.343(17) . ? N15 N18 1.38(15) 2_856 ? N15 C36 1.38(16) 2_856 ? N15 C35 1.48(18) 2_856 ? N15 N17 1.49(15) 2_856 ? N15 N16 1.54(4) 2_856 ? C26 C36 0.3(2) 2_856 ? C26 N17 1.15(13) 2_856 ? C26 N18 1.33(17) 2_856 ? C26 N16 1.93(4) 2_856 ? C26 C35 2.00(17) 2_856 ? C26 H26A 0.9603 . ? C29 C31 0.83(5) 2_856 ? C29 C33 1.24(5) 2_856 ? C29 C32 1.368(8) . ? C29 C28 1.368(8) . ? C29 C30 1.62(6) 2_856 ? C29 H29A 0.9601 . ? C28 C33 0.83(5) 2_856 ? C28 C32 1.26(4) 2_856 ? C28 C30 1.368(8) . ? C28 C31 1.89(5) 2_856 ? C28 C34 1.89(4) 2_856 ? C30 C32 0.83(5) 2_856 ? C30 C31 1.368(8) . ? C30 C29 1.62(4) 2_856 ? C30 C33 1.87(4) 2_856 ? C30 H30A 0.9552 . ? C31 C29 0.83(2) 2_856 ? C31 C33 1.368(8) . ? C31 C32 1.58(4) 2_856 ? C31 C28 1.89(5) 2_856 ? C31 H31A 0.9551 . ? C33 C28 0.83(5) 2_856 ? C33 C29 1.24(4) 2_856 ? C33 C32 1.368(8) . ? C33 C30 1.87(6) 2_856 ? C32 C30 0.83(6) 2_856 ? C32 C28 1.26(6) 2_856 ? C32 C31 1.58(6) 2_856 ? C32 H32A 0.9552 . ? N16 N14 0.72(16) 2_856 ? N16 C25 0.84(16) 2_856 ? N16 C35 1.356(18) . ? N16 N17 1.356(18) . ? N16 N15 1.54(17) 2_856 ? N16 N13 1.65(3) 2_856 ? N16 C26 1.93(16) 2_856 ? N17 C26 1.15(16) 2_856 ? N17 C36 1.356(18) . ? N17 N13 1.38(3) 2_856 ? N17 N15 1.49(18) 2_856 ? N17 C25 1.77(18) 2_856 ? N17 N14 1.83(16) 2_856 ? C36 C26 0.3(2) 2_856 ? C36 N18 1.356(18) . ? C36 N15 1.38(14) 2_856 ? C36 N13 1.65(4) 2_856 ? C36 H36A 0.9528 . ? N18 C26 1.3(2) 2_856 ? N18 C35 1.355(18) . ? N18 N15 1.38(13) 2_856 ? N18 Cu2 2.12(2) 1_565 ? C35 N14 1.03(12) 2_856 ? C35 N15 1.48(19) 2_856 ? C35 C25 1.48(18) 2_856 ? C35 C26 2.00(19) 2_856 ? C35 H35A 0.9529 . ? 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 O11 Mo1 O3 105.0(4) . . ? O11 Mo1 O6 101.6(5) . 2_724 ? O3 Mo1 O6 96.7(4) . 2_724 ? O11 Mo1 O7 101.0(5) . . ? O3 Mo1 O7 96.7(4) . . ? O6 Mo1 O7 149.6(4) 2_724 . ? O11 Mo1 O8 98.5(4) . . ? O3 Mo1 O8 156.5(4) . . ? O6 Mo1 O8 78.4(4) 2_724 . ? O7 Mo1 O8 78.4(4) . . ? O11 Mo1 O8 173.5(4) . 2_724 ? O3 Mo1 O8 81.5(4) . 2_724 ? O6 Mo1 O8 77.5(4) 2_724 2_724 ? O7 Mo1 O8 77.7(3) . 2_724 ? O8 Mo1 O8 75.0(4) . 2_724 ? O11 Mo1 Mo4 89.5(4) . . ? O3 Mo1 Mo4 132.5(3) . . ? O6 Mo1 Mo4 124.8(3) 2_724 . ? O7 Mo1 Mo4 35.8(2) . . ? O8 Mo1 Mo4 46.4(2) . . ? O8 Mo1 Mo4 85.8(2) 2_724 . ? O11 Mo1 Mo2 90.1(4) . 2_724 ? O3 Mo1 Mo2 132.1(3) . 2_724 ? O6 Mo1 Mo2 35.4(3) 2_724 2_724 ? O7 Mo1 Mo2 125.1(2) . 2_724 ? O8 Mo1 Mo2 46.7(3) . 2_724 ? O8 Mo1 Mo2 85.5(2) 2_724 2_724 ? Mo4 Mo1 Mo2 91.79(6) . 2_724 ? O1 Mo2 O9 105.9(6) . . ? O1 Mo2 O10 100.4(5) . . ? O9 Mo2 O10 101.4(4) . . ? O1 Mo2 O6 101.7(5) . . ? O9 Mo2 O6 97.7(4) . . ? O10 Mo2 O6 145.4(4) . . ? O1 Mo2 O8 161.3(5) . 2_724 ? O9 Mo2 O8 92.7(5) . 2_724 ? O10 Mo2 O8 77.7(3) . 2_724 ? O6 Mo2 O8 72.8(3) . 2_724 ? O1 Mo2 O7 90.0(5) . . ? O9 Mo2 O7 162.8(4) . . ? O10 Mo2 O7 81.8(3) . . ? O6 Mo2 O7 72.0(3) . . ? O8 Mo2 O7 71.3(3) 2_724 . ? O1 Mo2 Mo1 136.2(4) . 2_724 ? O9 Mo2 Mo1 84.7(3) . 2_724 ? O10 Mo2 Mo1 119.3(3) . 2_724 ? O6 Mo2 Mo1 34.6(3) . 2_724 ? O8 Mo2 Mo1 41.6(2) 2_724 2_724 ? O7 Mo2 Mo1 79.1(2) . 2_724 ? O2 Mo3 O13 104.3(5) . . ? O2 Mo3 O5 102.2(5) . . ? O13 Mo3 O5 98.6(4) . . ? O2 Mo3 O10 102.3(4) . 2_724 ? O13 Mo3 O10 98.5(5) . 2_724 ? O5 Mo3 O10 145.5(4) . 2_724 ? O2 Mo3 O3 88.6(5) . 2_724 ? O13 Mo3 O3 167.0(4) . 2_724 ? O5 Mo3 O3 79.1(4) . 2_724 ? O10 Mo3 O3 77.6(4) 2_724 2_724 ? O2 Mo3 O8 158.8(5) . . ? O13 Mo3 O8 96.8(4) . . ? O5 Mo3 O8 73.8(4) . . ? O10 Mo3 O8 74.6(3) 2_724 . ? O3 Mo3 O8 70.2(3) 2_724 . ? O12 Mo4 O4 105.4(5) . . ? O12 Mo4 O5 101.2(4) . . ? O4 Mo4 O5 101.3(5) . . ? O12 Mo4 O7 96.4(4) . . ? O4 Mo4 O7 101.4(4) . . ? O5 Mo4 O7 146.2(4) . . ? O12 Mo4 O8 94.9(4) . . ? O4 Mo4 O8 159.5(4) . . ? O5 Mo4 O8 77.0(4) . . ? O7 Mo4 O8 72.9(3) . . ? O12 Mo4 O6 163.5(4) . . ? O4 Mo4 O6 88.5(4) . . ? O5 Mo4 O6 84.3(3) . . ? O7 Mo4 O6 71.7(3) . . ? O8 Mo4 O6 71.0(3) . . ? O12 Mo4 Mo1 85.0(4) . . ? O4 Mo4 Mo1 136.2(3) . . ? O5 Mo4 Mo1 118.6(3) . . ? O7 Mo4 Mo1 34.8(3) . . ? O8 Mo4 Mo1 41.6(2) . . ? O6 Mo4 Mo1 78.8(2) . . ? N4 Cu1 N4 180. 2_714 . ? N4 Cu1 N1 91.3(5) 2_714 . ? N4 Cu1 N1 88.7(5) . . ? N4 Cu1 N1 88.7(5) 2_714 2_714 ? N4 Cu1 N1 91.3(5) . 2_714 ? N1 Cu1 N1 180. . 2_714 ? N4 Cu1 O13 88.7(4) 2_714 . ? N4 Cu1 O13 91.3(4) . . ? N1 Cu1 O13 84.7(4) . . ? N1 Cu1 O13 95.3(4) 2_714 . ? N4 Cu1 O13 91.3(4) 2_714 2_714 ? N4 Cu1 O13 88.7(4) . 2_714 ? N1 Cu1 O13 95.3(4) . 2_714 ? N1 Cu1 O13 84.7(4) 2_714 2_714 ? O13 Cu1 O13 180. . 2_714 ? Mo3 O13 Cu1 150.5(5) . . ? Mo2 O10 Mo3 116.2(4) . 2_724 ? Mo1 O8 Mo4 92.0(3) . . ? Mo1 O8 Mo2 91.8(3) . 2_724 ? Mo4 O8 Mo2 162.7(4) . 2_724 ? Mo1 O8 Mo1 105.0(4) . 2_724 ? Mo4 O8 Mo1 97.9(4) . 2_724 ? Mo2 O8 Mo1 97.4(3) 2_724 2_724 ? Mo1 O8 Mo3 164.0(4) . . ? Mo4 O8 Mo3 86.5(3) . . ? Mo2 O8 Mo3 85.3(3) 2_724 . ? Mo1 O8 Mo3 91.0(3) 2_724 . ? Mo1 O7 Mo4 109.5(4) . . ? Mo1 O7 Mo2 110.8(4) . . ? Mo4 O7 Mo2 103.4(4) . . ? Mo1 O6 Mo2 110.0(4) 2_724 . ? Mo1 O6 Mo4 110.8(5) 2_724 . ? Mo2 O6 Mo4 103.4(3) . . ? Mo4 O5 Mo3 118.4(5) . . ? Mo1 O3 Mo3 117.3(4) . 2_724 ? C2 N1 C1 101.3(12) . . ? C2 N1 Cu1 131.6(10) . . ? C1 N1 Cu1 127.1(10) . . ? C2 N2 N3 109.2(12) . . ? C2 N2 C3 132.3(13) . . ? N3 N2 C3 118.5(11) . . ? C1 N3 N2 103.1(11) . . ? C8 N4 C7 101.6(14) . . ? C8 N4 Cu1 135.6(12) . . ? C7 N4 Cu1 122.7(11) . . ? C8 N5 N6 107.3(13) . . ? C8 N5 C9 133.5(14) . . ? N6 N5 C9 119.1(13) . . ? C7 N6 N5 103.9(14) . . ? C13 N7 N8 104.4(18) . . ? C13 N7 Cu2 126(2) . . ? N8 N7 Cu2 129.5(17) . . ? N7 N8 C14 107(2) . . ? N7 N8 C20 125.7(17) . . ? C14 N8 C20 127(2) . . ? N3 C1 N1 114.9(13) . . ? N3 C1 H1A 122.5 . . ? N1 C1 H1A 122.5 . . ? N1 C2 N2 111.5(14) . . ? N1 C2 H2A 124.3 . . ? N2 C2 H2A 124.3 . . ? N2 C3 C4 113.2(13) . . ? N2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.8 . . ? C6 C5 C4 120.0(16) 2_825 . ? C6 C5 H5A 120.0 2_825 . ? C4 C5 H5A 120.0 . . ? C6 C4 C5 119.8(14) . . ? C6 C4 C3 122.6(13) . . ? C5 C4 C3 117.6(16) . . ? C4 C6 C5 120.1(14) . 2_825 ? C4 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 2_825 . ? N6 C7 N4 112.0(15) . . ? N6 C7 H7A 124.0 . . ? N4 C7 H7A 124.0 . . ? N5 C8 N4 115.2(15) . . ? N5 C8 H8A 122.4 . . ? N4 C8 H8A 122.4 . . ? N5 C9 C10 112.3(13) . . ? N5 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N5 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C12 C10 C11 120.0(16) 2_715 . ? C12 C10 C9 120.3(14) 2_715 . ? C11 C10 C9 119.7(15) . . ? C10 C11 C12 118.0(16) . . ? C10 C11 H11A 121.0 . . ? C12 C11 H11A 121.0 . . ? C10 C12 C11 122.0(15) 2_715 . ? C10 C12 H12A 119.0 2_715 . ? C11 C12 H12A 119.0 . . ? C17 C15 C16 118.9(16) . . ? C17 C15 C20 120.2(13) . . ? C16 C15 C20 120.6(14) . . ? C19 C16 C15 119.4(15) . . ? C19 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C18 C17 C15 121.5(14) . . ? C18 C17 H17A 119.3 . . ? C15 C17 H17A 119.3 . . ? C17 C18 C21 120.7(15) . . ? C17 C18 H18A 119.7 . . ? C21 C18 H18A 119.7 . . ? C21 C19 C16 120.9(14) . . ? C21 C19 H19A 119.5 . . ? C16 C19 H19A 119.5 . . ? N8 C20 C15 115.2(14) . . ? N8 C20 H20A 108.5 . . ? C15 C20 H20A 108.5 . . ? N8 C20 H20B 108.5 . . ? C15 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C19 C21 C18 118.5(15) . . ? C19 C21 C22 121.9(13) . . ? C18 C21 C22 119.5(15) . . ? N10 C22 C21 115.3(16) . . ? N10 C22 H22A 108.5 . . ? C21 C22 H22A 108.5 . . ? N10 C22 H22B 108.5 . . ? C21 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C23 N10 N11 108.0 . . ? C23 N10 C22 128.0(12) . . ? N11 N10 C22 123.7(11) . . ? C24 N11 N10 108.0 . . ? N12 C24 N11 108.0 . . ? N12 C24 H24A 126.0 . . ? N11 C24 H24A 126.0 . . ? C24 N12 C23 108.0 . . ? C24 N12 Cu3 111.2(9) . . ? C23 N12 Cu3 136.4(9) . . ? C24 N12 Cu3 132.7(9) . 2_967 ? C23 N12 Cu3 115.9(9) . 2_967 ? Cu3 N12 Cu3 40.8(4) . 2_967 ? N10 C23 N12 108.0 . . ? N10 C23 H23A 126.0 . . ? N12 C23 H23A 126.0 . . ? C13 N9 C14 110(3) . . ? C13 N9 Cu3 100(2) . 2_957 ? C14 N9 Cu3 147(2) . 2_957 ? N9 C13 N7 113(3) . . ? N9 C13 H13A 123.3 . . ? N7 C13 H13A 123.3 . . ? N9 C14 N8 105(3) . . ? N9 C14 H14A 127.5 . . ? N8 C14 H14A 127.5 . . ? N7 Cu2 N13 146.8(11) . . ? N7 Cu2 N18 114(6) . 1_545 ? N13 Cu2 N18 98(6) . 1_545 ? Cu3 Cu3 N12 74.0(7) 2_967 . ? Cu3 Cu3 N12 65.2(15) 2_967 2_967 ? N12 Cu3 N12 139.2(11) . 2_967 ? Cu3 Cu3 N9 151.0(10) 2_967 2_957 ? N12 Cu3 N9 103.8(8) . 2_957 ? N12 Cu3 N9 111.7(15) 2_967 2_957 ? N14 C27 C28 105(2) . . ? N14 C27 H27A 110.7 . . ? C28 C27 H27A 110.7 . . ? N14 C27 H27B 110.7 . . ? C28 C27 H27B 110.7 . . ? H27A C27 H27B 108.8 . . ? C33 C34 N16 112(3) . . ? C33 C34 C25 144(7) . 2_856 ? N16 C34 C25 32(7) . 2_856 ? C33 C34 N14 98(5) . 2_856 ? N16 C34 N14 24(5) . 2_856 ? C25 C34 N14 48(4) 2_856 2_856 ? C33 C34 C28 24.1(17) . 2_856 ? N16 C34 C28 99(3) . 2_856 ? C25 C34 C28 127(7) 2_856 2_856 ? N14 C34 C28 79(5) 2_856 2_856 ? C33 C34 H34A 109.4 . . ? N16 C34 H34A 109.0 . . ? C25 C34 H34A 93.5 2_856 . ? N14 C34 H34A 132.7 2_856 . ? C28 C34 H34A 133.5 2_856 . ? C33 C34 H34B 109.2 . . ? N16 C34 H34B 108.8 . . ? C25 C34 H34B 87.8 2_856 . ? N14 C34 H34B 97.7 2_856 . ? C28 C34 H34B 96.5 2_856 . ? H34A C34 H34B 108.2 . . ? C26 N13 C25 108.0 . . ? C26 N13 N17 50(6) . 2_856 ? C25 N13 N17 81(6) . 2_856 ? C26 N13 C36 4(5) . 2_856 ? C25 N13 C36 112(5) . 2_856 ? N17 N13 C36 52(7) 2_856 2_856 ? C26 N13 N16 80.0(13) . 2_856 ? C25 N13 N16 30.7(14) . 2_856 ? N17 N13 N16 52(6) 2_856 2_856 ? C36 N13 N16 84(5) 2_856 2_856 ? C26 N13 Cu2 120.1(19) . . ? C25 N13 Cu2 131.7(19) . . ? N17 N13 Cu2 133(6) 2_856 . ? C36 N13 Cu2 117(5) 2_856 . ? N16 N13 Cu2 159(2) 2_856 . ? N16 C25 N14 28(2) 2_856 . ? N16 C25 N13 95(3) 2_856 . ? N14 C25 N13 108.0 . . ? N16 C25 C35 65(6) 2_856 2_856 ? N14 C25 C35 43(6) . 2_856 ? N13 C25 C35 90(6) . 2_856 ? N16 C25 C34 66(3) 2_856 2_856 ? N14 C25 C34 73(2) . 2_856 ? N13 C25 C34 137(2) . 2_856 ? C35 C25 C34 112(5) 2_856 2_856 ? N16 C25 N17 48(4) 2_856 2_856 ? N14 C25 N17 70(5) . 2_856 ? N13 C25 N17 50(4) . 2_856 ? C35 C25 N17 84(9) 2_856 2_856 ? C34 C25 N17 94(4) 2_856 2_856 ? N16 C25 H25A 132.8 2_856 . ? N14 C25 H25A 126.0 . . ? N13 C25 H25A 126.0 . . ? C35 C25 H25A 128.6 2_856 . ? C34 C25 H25A 68.1 2_856 . ? N17 C25 H25A 146.3 2_856 . ? N16 N14 C35 100(10) 2_856 2_856 ? N16 N14 C25 34(3) 2_856 . ? C35 N14 C25 76(9) 2_856 . ? N16 N14 N15 92(3) 2_856 . ? C35 N14 N15 76(10) 2_856 . ? C25 N14 N15 108.0 . . ? N16 N14 C27 137(5) 2_856 . ? C35 N14 C27 115(9) 2_856 . ? C25 N14 C27 134(3) . . ? N15 N14 C27 118(3) . . ? N16 N14 C34 54(3) 2_856 2_856 ? C35 N14 C34 129(10) 2_856 2_856 ? C25 N14 C34 59(2) . 2_856 ? N15 N14 C34 137(2) . 2_856 ? C27 N14 C34 85(2) . 2_856 ? N16 N14 N17 40(6) 2_856 2_856 ? C35 N14 N17 96(9) 2_856 2_856 ? C25 N14 N17 66(6) . 2_856 ? N15 N14 N17 53(5) . 2_856 ? C27 N14 N17 145(5) . 2_856 ? C34 N14 N17 87(5) 2_856 2_856 ? N14 N15 C26 108.0 . . ? N14 N15 N18 98(8) . 2_856 ? C26 N15 N18 58(7) . 2_856 ? N14 N15 C36 121(9) . 2_856 ? C26 N15 C36 13(9) . 2_856 ? N18 N15 C36 59(6) 2_856 2_856 ? N14 N15 C35 43(5) . 2_856 ? C26 N15 C35 90(6) . 2_856 ? N18 N15 C35 57(6) 2_856 2_856 ? C36 N15 C35 100(10) 2_856 2_856 ? N14 N15 N17 80(7) . 2_856 ? C26 N15 N17 48(5) . 2_856 ? N18 N15 N17 100(10) 2_856 2_856 ? C36 N15 N17 56(6) 2_856 2_856 ? C35 N15 N17 95(10) 2_856 2_856 ? N14 N15 N16 27.6(13) . 2_856 ? C26 N15 N16 83.8(13) . 2_856 ? N18 N15 N16 97(9) 2_856 2_856 ? C36 N15 N16 97(9) 2_856 2_856 ? C35 N15 N16 53(6) 2_856 2_856 ? N17 N15 N16 53(7) 2_856 2_856 ? C36 C26 N17 124(10) 2_856 2_856 ? C36 C26 N18 88(10) 2_856 2_856 ? N17 C26 N18 124(10) 2_856 2_856 ? C36 C26 N13 161(10) 2_856 . ? N17 C26 N13 67(9) 2_856 . ? N18 C26 N13 97(9) 2_856 . ? C36 C26 N15 90(10) 2_856 . ? N17 C26 N15 73(7) 2_856 . ? N18 C26 N15 62(7) 2_856 . ? N13 C26 N15 108.0 . . ? C36 C26 N16 142(10) 2_856 2_856 ? N17 C26 N16 44(8) 2_856 2_856 ? N18 C26 N16 82(7) 2_856 2_856 ? N13 C26 N16 56.9(10) . 2_856 ? N15 C26 N16 52.5(9) . 2_856 ? C36 C26 C35 123(10) 2_856 2_856 ? N17 C26 C35 83(9) 2_856 2_856 ? N18 C26 C35 42(5) 2_856 2_856 ? N13 C26 C35 70(5) . 2_856 ? N15 C26 C35 48(5) . 2_856 ? N16 C26 C35 40(3) 2_856 2_856 ? C36 C26 H26A 35.7 2_856 . ? N17 C26 H26A 126.0 2_856 . ? N18 C26 H26A 106.8 2_856 . ? N13 C26 H26A 126.0 . . ? N15 C26 H26A 126.0 . . ? N16 C26 H26A 169.1 2_856 . ? C35 C26 H26A 149.1 2_856 . ? C31 C29 C33 80(4) 2_856 2_856 ? C31 C29 C32 88(5) 2_856 . ? C33 C29 C32 122(2) 2_856 . ? C31 C29 C28 117(5) 2_856 . ? C33 C29 C28 37(2) 2_856 . ? C32 C29 C28 120.0 . . ? C31 C29 C30 58(3) 2_856 2_856 ? C33 C29 C30 111(3) 2_856 2_856 ? C32 C29 C30 31(2) . 2_856 ? C28 C29 C30 131(2) . 2_856 ? C31 C29 H29A 64.3 2_856 . ? C33 C29 H29A 105.6 2_856 . ? C32 C29 H29A 119.7 . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 101.4 2_856 . ? C33 C28 C32 79(3) 2_856 2_856 ? C33 C28 C29 63(4) 2_856 . ? C32 C28 C29 104(2) 2_856 . ? C33 C28 C30 115(4) 2_856 . ? C32 C28 C30 36(2) 2_856 . ? C29 C28 C30 120.0 . . ? C33 C28 C27 119(3) 2_856 . ? C32 C28 C27 113(3) 2_856 . ? C29 C28 C27 142.9(17) . . ? C30 C28 C27 93.5(16) . . ? C33 C28 C31 40(3) 2_856 2_856 ? C32 C28 C31 95(2) 2_856 2_856 ? C29 C28 C31 23(2) . 2_856 ? C30 C28 C31 123.2(19) . 2_856 ? C27 C28 C31 142.1(18) . 2_856 ? C33 C28 C34 45(3) 2_856 2_856 ? C32 C28 C34 107(2) 2_856 2_856 ? C29 C28 C34 89(2) . 2_856 ? C30 C28 C34 134(2) . 2_856 ? C27 C28 C34 76.1(18) . 2_856 ? C31 C28 C34 71.5(17) 2_856 2_856 ? C32 C30 C31 88(3) 2_856 . ? C32 C30 C28 65(3) 2_856 . ? C31 C30 C28 120.0 . . ? C32 C30 C29 58(3) 2_856 2_856 ? C31 C30 C29 30.7(11) . 2_856 ? C28 C30 C29 101.9(14) . 2_856 ? C32 C30 C33 41(2) 2_856 2_856 ? C31 C30 C33 110.6(16) . 2_856 ? C28 C30 C33 23.5(17) . 2_856 ? C29 C30 C33 85.1(17) 2_856 2_856 ? C32 C30 H30A 117.0 2_856 . ? C31 C30 H30A 120.0 . . ? C28 C30 H30A 120.0 . . ? C29 C30 H30A 130.9 2_856 . ? C33 C30 H30A 124.4 2_856 . ? C29 C31 C33 63(3) 2_856 . ? C29 C31 C30 92(3) 2_856 . ? C33 C31 C30 120.0 . . ? C29 C31 C32 60(2) 2_856 2_856 ? C33 C31 C32 101.3(17) . 2_856 ? C30 C31 C32 31.6(17) . 2_856 ? C29 C31 C28 40(2) 2_856 2_856 ? C33 C31 C28 22.9(19) . 2_856 ? C30 C31 C28 112.0(17) . 2_856 ? C32 C31 C28 85.6(19) 2_856 2_856 ? C29 C31 H31A 115.1 2_856 . ? C33 C31 H31A 120.0 . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 131.0 2_856 . ? C28 C31 H31A 123.2 2_856 . ? C28 C33 C29 80(4) 2_856 2_856 ? C28 C33 C31 117(4) 2_856 . ? C29 C33 C31 36.6(13) 2_856 . ? C28 C33 C32 65(4) 2_856 . ? C29 C33 C32 105.6(17) 2_856 . ? C31 C33 C32 120.0 . . ? C28 C33 C34 111(4) 2_856 . ? C29 C33 C34 121(4) 2_856 . ? C31 C33 C34 104(3) . . ? C32 C33 C34 132(3) . . ? C28 C33 C30 41(3) 2_856 2_856 ? C29 C33 C30 97(3) 2_856 2_856 ? C31 C33 C30 124(2) . 2_856 ? C32 C33 C30 24(2) . 2_856 ? C34 C33 C30 131(3) . 2_856 ? C30 C32 C28 79(4) 2_856 2_856 ? C30 C32 C29 92(5) 2_856 . ? C28 C32 C29 124(3) 2_856 . ? C30 C32 C33 115(5) 2_856 . ? C28 C32 C33 36(3) 2_856 . ? C29 C32 C33 120.0 . . ? C30 C32 C31 60(3) 2_856 2_856 ? C28 C32 C31 113(4) 2_856 2_856 ? C29 C32 C31 32(2) . 2_856 ? C33 C32 C31 131(2) . 2_856 ? C30 C32 H32A 63.0 2_856 . ? C28 C32 H32A 104.2 2_856 . ? C29 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 101.3 2_856 . ? N14 N16 C25 118(10) 2_856 2_856 ? N14 N16 C35 49(10) 2_856 . ? C25 N16 C35 81(10) 2_856 . ? N14 N16 N17 121(10) 2_856 . ? C25 N16 N17 105(10) 2_856 . ? C35 N16 N17 108.0 . . ? N14 N16 C34 103(10) 2_856 . ? C25 N16 C34 82(10) 2_856 . ? C35 N16 C34 129(3) . . ? N17 N16 C34 123(3) . . ? N14 N16 N15 60(10) 2_856 2_856 ? C25 N16 N15 128(10) 2_856 2_856 ? C35 N16 N15 61(6) . 2_856 ? N17 N16 N15 61(6) . 2_856 ? C34 N16 N15 149(6) . 2_856 ? N14 N16 N13 129(10) 2_856 2_856 ? C25 N16 N13 54(10) 2_856 2_856 ? C35 N16 N13 83.2(13) . 2_856 ? N17 N16 N13 53.7(15) . 2_856 ? C34 N16 N13 122(3) . 2_856 ? N15 N16 N13 86(6) 2_856 2_856 ? N14 N16 C26 100(10) 2_856 2_856 ? C25 N16 C26 95(9) 2_856 2_856 ? C35 N16 C26 73(6) . 2_856 ? N17 N16 C26 36(6) . 2_856 ? C34 N16 C26 156(6) . 2_856 ? N15 N16 C26 44(4) 2_856 2_856 ? N13 N16 C26 43(6) 2_856 2_856 ? C26 N17 N16 101(10) 2_856 . ? C26 N17 C36 11(10) 2_856 . ? N16 N17 C36 108.0 . . ? C26 N17 N13 63(10) 2_856 2_856 ? N16 N17 N13 74.0(19) . 2_856 ? C36 N17 N13 74.1(19) . 2_856 ? C26 N17 N15 60(8) 2_856 2_856 ? N16 N17 N15 66(7) . 2_856 ? C36 N17 N15 58(5) . 2_856 ? N13 N17 N15 98(7) 2_856 2_856 ? C26 N17 C25 93(10) 2_856 2_856 ? N16 N17 C25 27(4) . 2_856 ? C36 N17 C25 104(5) . 2_856 ? N13 N17 C25 48(4) 2_856 2_856 ? N15 N17 C25 83(8) 2_856 2_856 ? C26 N17 N14 91(10) 2_856 2_856 ? N16 N17 N14 20(5) . 2_856 ? C36 N17 N14 95(4) . 2_856 ? N13 N17 N14 84(5) 2_856 2_856 ? N15 N17 N14 46(5) 2_856 2_856 ? C25 N17 N14 44(4) 2_856 2_856 ? C26 C36 N17 45(10) 2_856 . ? C26 C36 N18 78(10) 2_856 . ? N17 C36 N18 108.0 . . ? C26 C36 N15 76(10) 2_856 2_856 ? N17 C36 N15 66(7) . 2_856 ? N18 C36 N15 60(7) . 2_856 ? C26 C36 N13 15(10) 2_856 2_856 ? N17 C36 N13 53.6(12) . 2_856 ? N18 C36 N13 83.1(13) . 2_856 ? N15 C36 N13 91(7) 2_856 2_856 ? C26 C36 H36A 141.3 2_856 . ? N17 C36 H36A 126.0 . . ? N18 C36 H36A 126.0 . . ? N15 C36 H36A 140.3 2_856 . ? N13 C36 H36A 127.3 2_856 . ? C26 N18 C35 97(7) 2_856 . ? C26 N18 C36 14(9) 2_856 . ? C35 N18 C36 108.0 . . ? C26 N18 N15 60(7) 2_856 2_856 ? C35 N18 N15 66(7) . 2_856 ? C36 N18 N15 61(7) . 2_856 ? C26 N18 Cu2 128(6) 2_856 1_565 ? C35 N18 Cu2 134.4(16) . 1_565 ? C36 N18 Cu2 117.5(16) . 1_565 ? N15 N18 Cu2 142(8) 2_856 1_565 ? N14 C35 N18 118(9) 2_856 . ? N14 C35 N16 31(9) 2_856 . ? N18 C35 N16 108.0 . . ? N14 C35 N15 62(9) 2_856 2_856 ? N18 C35 N15 58(5) . 2_856 ? N16 C35 N15 66(6) . 2_856 ? N14 C35 C25 62(9) 2_856 2_856 ? N18 C35 C25 112(6) . 2_856 ? N16 C35 C25 34(6) . 2_856 ? N15 C35 C25 94(10) 2_856 2_856 ? N14 C35 C26 85(10) 2_856 2_856 ? N18 C35 C26 41(5) . 2_856 ? N16 C35 C26 67(5) . 2_856 ? N15 C35 C26 42(5) 2_856 2_856 ? C25 C35 C26 75(8) 2_856 2_856 ? N14 C35 H35A 108.8 2_856 . ? N18 C35 H35A 126.0 . . ? N16 C35 H35A 126.0 . . ? N15 C35 H35A 143.1 2_856 . ? C25 C35 H35A 112.5 2_856 . ? C26 C35 H35A 166.0 2_856 . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.286 _refine_diff_density_min -1.175 _refine_diff_density_rms 0.201