# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Marius Andruh' _publ_contact_author_email MARIUS.ANDRUH@DNT.RO _publ_section_title ; New photomagnetic cyanido-bridged Cu(II)-Mo(IV) oligonuclear complexes: slight modification of the blocking ligands inducing different structures ; loop_ _publ_author_name 'Marius Andruh' 'Corine Mathoniere' 'Catalin Maxim' # Attachment '1_CCD_723821revised.cif' data_max26c _database_code_depnum_ccdc_archive 'CCDC 723821' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H60 Cu4 Mo N16 O12' _chemical_formula_weight 1547.34 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' 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' 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' _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 11.5805(8) _cell_length_b 16.5755(15) _cell_length_c 17.1402(14) _cell_angle_alpha 101.645(7) _cell_angle_beta 91.739(6) _cell_angle_gamma 94.410(7) _cell_volume 3209.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17154 _cell_measurement_theta_min 3.84 _cell_measurement_theta_max 57.67 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1540 _exptl_absorpt_coefficient_mu 1.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.896 _exptl_absorpt_process_details wingx _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17439 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.1782 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 29.25 _reflns_number_total 12044 _reflns_number_gt 5147 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr. _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12044 _refine_ls_number_parameters 796 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1682 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 0.852 _refine_ls_restrained_S_all 0.852 _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 N1D N 0.1655(9) 0.5164(6) 0.4573(6) 0.121(4) Uiso 1 1 d G . . C6D C 0.1923(10) 0.6007(7) 0.4855(7) 0.154(6) Uiso 1 1 d G . . C7D C 0.1265(15) 0.6573(5) 0.4589(9) 0.296(13) Uiso 1 1 d G . . H7D H 0.1445 0.7137 0.4778 0.355 Uiso 1 1 calc R . . C16D C 0.0340(14) 0.6297(10) 0.4040(9) 0.285(12) Uiso 1 1 d G . . H16D H -0.0101 0.6676 0.3862 0.342 Uiso 1 1 calc R . . C17D C 0.0072(10) 0.5455(11) 0.3758(7) 0.253(11) Uiso 1 1 d G . . H17D H -0.0548 0.5270 0.3391 0.303 Uiso 1 1 calc R . . C5D C 0.0730(11) 0.4888(6) 0.4024(7) 0.179(7) Uiso 1 1 d G . . H5D H 0.0550 0.4325 0.3835 0.215 Uiso 1 1 calc R . . C1A C 0.5940(8) 0.3177(5) 0.1679(5) 0.045(2) Uani 1 1 d . . . H1A H 0.5304 0.3195 0.1999 0.054 Uiso 1 1 calc R . . C1B C 0.5062(9) -0.1266(5) -0.0241(6) 0.055(3) Uani 1 1 d . . . H1B H 0.5553 -0.1407 -0.0657 0.066 Uiso 1 1 calc R . . C2B C 0.5398(8) -0.1463(5) 0.0500(6) 0.049(2) Uani 1 1 d . . . C1C C -0.0375(8) -0.1296(5) 0.3794(5) 0.049(2) Uani 1 1 d . . . C1D C 0.4698(9) 0.4193(6) 0.5890(5) 0.059(3) Uani 1 1 d . . . C1M C 0.2792(7) 0.2853(4) 0.1614(4) 0.0291(17) Uani 1 1 d . . . C2A C 0.6967(9) 0.2992(5) 0.1976(5) 0.054(2) Uani 1 1 d . . . H2A H 0.7041 0.2889 0.2488 0.064 Uiso 1 1 calc R . . C2C C -0.0278(8) -0.1440(5) 0.4579(5) 0.042(2) Uani 1 1 d . . . C2D C 0.4954(10) 0.5040(7) 0.6224(5) 0.068(3) Uani 1 1 d . . . C2M C 0.2300(7) 0.1136(5) 0.1568(4) 0.0319(18) Uani 1 1 d . . . C3A C 0.7907(9) 0.2962(6) 0.1480(7) 0.066(3) Uani 1 1 d . . . H3A H 0.8620 0.2827 0.1658 0.079 Uiso 1 1 calc R . . C3B C 0.4746(9) -0.1259(5) 0.1188(5) 0.051(2) Uani 1 1 d . . . C3C C 0.0632(8) -0.1060(5) 0.5148(5) 0.041(2) Uani 1 1 d . . . H3C H 0.0625 -0.1202 0.5646 0.049 Uiso 1 1 calc R . . C3D C 0.5379(11) 0.3646(8) 0.6153(7) 0.103(4) Uani 1 1 d . . . H3D H 0.5226 0.3083 0.5948 0.123 Uiso 1 1 calc R . . C3M C 0.1601(6) 0.1236(5) 0.3004(4) 0.0287(17) Uani 1 1 d . . . C4A C 0.7784(9) 0.3128(5) 0.0747(6) 0.058(3) Uani 1 1 d . . . H4A H 0.8413 0.3124 0.0422 0.070 Uiso 1 1 calc R . . C4B C 0.5114(9) -0.1564(6) 0.1844(6) 0.068(3) Uani 1 1 d . . . H4B H 0.4675 -0.1489 0.2294 0.082 Uiso 1 1 calc R . . C4C C 0.3774(8) 0.1076(5) 0.4465(5) 0.053(2) Uani 1 1 d . . . H4C H 0.3627 0.1214 0.3974 0.063 Uiso 1 1 calc R . . C4D C 0.4287(16) 0.5646(7) 0.6044(7) 0.098(5) Uani 1 1 d . . . H4D H 0.4534 0.6192 0.6275 0.118 Uiso 1 1 calc R . . C4M C 0.3556(7) 0.2138(4) 0.2725(4) 0.0323(18) Uani 1 1 d . . . C5A C 0.6709(8) 0.3306(5) 0.0480(5) 0.041(2) Uani 1 1 d . . . C5B C 0.6107(12) -0.1974(7) 0.1852(7) 0.087(4) Uani 1 1 d . . . H5B H 0.6322 -0.2163 0.2306 0.105 Uiso 1 1 calc R . . C5C C 0.4771(9) 0.1418(5) 0.4898(6) 0.061(3) Uani 1 1 d . . . H5C H 0.5283 0.1787 0.4711 0.073 Uiso 1 1 calc R . . C5M C 0.0051(7) 0.2176(4) 0.2849(4) 0.0348(18) Uani 1 1 d . . . C6A C 0.6492(8) 0.3502(5) -0.0327(5) 0.053(2) Uani 1 1 d . . . H6A1 H 0.7058 0.3938 -0.0404 0.064 Uiso 1 1 calc R . . H6A2 H 0.6578 0.3016 -0.0737 0.064 Uiso 1 1 calc R . . C6B C 0.6448(9) -0.1862(5) 0.0540(6) 0.062(3) Uani 1 1 d . . . H6B H 0.6903 -0.1951 0.0098 0.075 Uiso 1 1 calc R . . C6C C 0.4988(9) 0.1198(6) 0.5616(6) 0.066(3) Uani 1 1 d . . . H6C H 0.5658 0.1417 0.5923 0.079 Uiso 1 1 calc R . . C6M C 0.2109(6) 0.3055(4) 0.3506(4) 0.0337(18) Uani 1 1 d . . . C7A C 0.3026(9) 0.4334(5) -0.0662(5) 0.049(2) Uani 1 1 d . . . C7B C 0.6783(10) -0.2108(6) 0.1200(8) 0.079(4) Uani 1 1 d . . . H7B H 0.7465 -0.2367 0.1219 0.095 Uiso 1 1 calc R . . C7C C 0.4220(9) 0.0659(6) 0.5876(5) 0.058(3) Uani 1 1 d . . . H7C H 0.4362 0.0499 0.6357 0.069 Uiso 1 1 calc R . . C7M C 0.1016(6) 0.3362(5) 0.2244(4) 0.0313(18) Uani 1 1 d . . . C8A C 0.1964(9) 0.4594(5) -0.0893(6) 0.065(3) Uani 1 1 d . . . H8A H 0.1354 0.4624 -0.0551 0.078 Uiso 1 1 calc R . . C8B C 0.3926(9) -0.0782(5) -0.1198(5) 0.057(3) Uani 1 1 d . . . H8B1 H 0.3899 -0.1305 -0.1577 0.069 Uiso 1 1 calc R . . H8B2 H 0.4545 -0.0416 -0.1336 0.069 Uiso 1 1 calc R . . C8C C 0.3229(8) 0.0353(5) 0.5413(5) 0.043(2) Uani 1 1 d . . . C8D C 0.6296(14) 0.3916(12) 0.6723(9) 0.147(7) Uani 1 1 d . . . H8D H 0.6738 0.3537 0.6899 0.176 Uiso 1 1 calc R . . C8M C 0.0609(7) 0.1899(4) 0.1319(5) 0.0349(19) Uani 1 1 d . . . C9A C 0.3929(9) 0.4303(5) -0.1187(5) 0.053(2) Uani 1 1 d . . . C9B C 0.2802(9) -0.0413(4) -0.1240(5) 0.044(2) Uani 1 1 d . . . C9C C 0.2344(8) -0.0234(5) 0.5675(5) 0.052(2) Uani 1 1 d . . . H9C1 H 0.2718 -0.0694 0.5811 0.062 Uiso 1 1 calc R . . H9C2 H 0.1983 0.0047 0.6146 0.062 Uiso 1 1 calc R . . C9D C 0.5900(14) 0.5282(10) 0.6789(8) 0.117(6) Uani 1 1 d . . . H9D H 0.6075 0.5841 0.7006 0.141 Uiso 1 1 calc R . . C10A C 0.5040(9) 0.4031(5) -0.1021(5) 0.051(2) Uani 1 1 d . . . H10A H 0.5598 0.4048 -0.1398 0.062 Uiso 1 1 calc R . . C10B C 0.2319(10) -0.0339(5) -0.1955(6) 0.066(3) Uani 1 1 d . . . H10B H 0.2679 -0.0526 -0.2428 0.079 Uiso 1 1 calc R . . C11A C 0.1826(10) 0.4805(6) -0.1628(7) 0.074(3) Uani 1 1 d . . . H11A H 0.1123 0.4984 -0.1772 0.088 Uiso 1 1 calc R . . C11B C 0.1295(11) 0.0016(5) -0.1958(5) 0.064(3) Uani 1 1 d . . . H11B H 0.0955 0.0075 -0.2439 0.077 Uiso 1 1 calc R . . C11C C -0.1076(9) -0.2013(5) 0.4818(5) 0.056(2) Uani 1 1 d . . . H11C H -0.1023 -0.2097 0.5338 0.067 Uiso 1 1 calc R . . C12A C 0.2707(13) 0.4758(6) -0.2151(6) 0.080(4) Uani 1 1 d . . . H12A H 0.2597 0.4898 -0.2645 0.096 Uiso 1 1 calc R . . C12B C 0.0758(9) 0.0287(6) -0.1262(6) 0.064(3) Uani 1 1 d . . . H12B H 0.0058 0.0526 -0.1258 0.077 Uiso 1 1 calc R . . C12C C -0.1923(9) -0.2445(6) 0.4304(7) 0.069(3) Uani 1 1 d . . . H12C H -0.2446 -0.2826 0.4467 0.082 Uiso 1 1 calc R . . C13A C 0.3736(10) 0.4504(6) -0.1943(6) 0.069(3) Uani 1 1 d . . . H13A H 0.4326 0.4462 -0.2302 0.083 Uiso 1 1 calc R . . C13B C 0.1316(8) 0.0186(5) -0.0564(5) 0.047(2) Uani 1 1 d . . . H13B H 0.0974 0.0365 -0.0083 0.056 Uiso 1 1 calc R . . C13C C -0.2002(9) -0.2316(6) 0.3538(7) 0.079(3) Uani 1 1 d . . . H13C H -0.2581 -0.2615 0.3186 0.095 Uiso 1 1 calc R . . C14C C -0.1236(9) -0.1748(6) 0.3275(6) 0.073(3) Uani 1 1 d . . . H14C H -0.1304 -0.1673 0.2753 0.088 Uiso 1 1 calc R . . C15D C 0.2741(19) 0.6242(8) 0.5514(8) 0.210(11) Uani 1 1 d . . . H15A H 0.2345 0.6432 0.5999 0.252 Uiso 1 1 calc R . . H15B H 0.3283 0.6689 0.5430 0.252 Uiso 1 1 calc R . . C18D C 0.6531(14) 0.4747(14) 0.7014(10) 0.149(9) Uani 1 1 d . . . H18D H 0.7153 0.4931 0.7380 0.179 Uiso 1 1 calc R . . Cu1 Cu 0.28025(12) 0.44881(7) 0.49050(6) 0.0620(4) Uani 1 1 d . . . Cu2 Cu 0.43396(9) 0.36209(6) 0.04546(5) 0.0378(3) Uani 1 1 d . . . Cu3 Cu 0.16012(9) -0.00634(6) 0.40879(5) 0.0395(3) Uani 1 1 d . . . Cu4 Cu 0.30810(9) -0.04412(6) 0.03959(5) 0.0432(3) Uani 1 1 d . . . Mo Mo 0.17585(6) 0.22267(4) 0.23609(3) 0.02276(15) Uani 1 1 d . . . N1A N 0.5800(6) 0.3335(3) 0.0947(4) 0.0355(15) Uani 1 1 d . . . N1B N 0.4159(7) -0.0916(4) -0.0396(4) 0.0443(18) Uani 1 1 d . . . N1C N 0.1459(6) -0.0540(4) 0.5034(4) 0.0392(16) Uani 1 1 d . . . N1M N 0.2595(6) 0.0561(4) 0.1163(3) 0.0414(17) Uani 1 1 d . . . N2A N 0.5325(6) 0.3765(4) -0.0395(4) 0.0426(17) Uani 1 1 d . . . N2B N 0.2326(6) -0.0159(4) -0.0553(4) 0.0388(16) Uani 1 1 d . . . N2C N 0.2999(6) 0.0549(4) 0.4718(4) 0.0392(16) Uani 1 1 d . . . N2D N 0.3364(11) 0.5525(5) 0.5588(5) 0.093(4) Uani 1 1 d . . . N2M N 0.4513(6) 0.2105(4) 0.2911(4) 0.0467(18) Uani 1 1 d . . . N3M N 0.1531(5) 0.0725(4) 0.3369(3) 0.0363(16) Uani 1 1 d . . . N4M N -0.0842(6) 0.2180(4) 0.3121(4) 0.0498(19) Uani 1 1 d . . . N5M N 0.2304(6) 0.3512(4) 0.4096(4) 0.050(2) Uani 1 1 d . . . N6M N 0.0639(6) 0.3967(4) 0.2166(4) 0.0503(19) Uani 1 1 d . . . N7M N 0.3355(6) 0.3207(4) 0.1222(4) 0.0373(16) Uani 1 1 d . . . N8M N 0.0038(6) 0.1762(4) 0.0738(4) 0.0497(19) Uani 1 1 d . . . O1A O 0.3098(5) 0.4131(3) 0.0052(3) 0.0517(16) Uani 1 1 d . . . O1B O 0.3876(5) -0.0813(4) 0.1232(3) 0.0557(17) Uani 1 1 d . . . O1C O 0.0295(5) -0.0738(4) 0.3535(3) 0.0572(17) Uani 1 1 d . . . O1D O 0.3871(5) 0.3900(3) 0.5347(3) 0.0568(17) Uani 1 1 d . . . O1W O 0.2868(6) -0.0878(4) 0.3227(4) 0.098(2) Uani 1 1 d . . . O2W O 0.1644(5) -0.1342(4) 0.0510(3) 0.0652(18) Uani 1 1 d . . . O4W O 0.6834(6) 0.1830(4) 0.3622(4) 0.0732(19) Uani 1 1 d . . . O3W O 0.4409(8) 0.0195(5) 0.2682(5) 0.119(3) Uani 1 1 d . . . O5W O 0.1607(7) 0.5077(4) 0.1205(4) 0.100(3) Uani 1 1 d . . . O6W O 0.0846(8) 0.3065(5) -0.0149(5) 0.126(3) Uani 1 1 d . . . O7W O 0.1233(8) -0.1694(6) 0.2049(4) 0.125(3) Uani 1 1 d . . . O8W O 0.0822(9) -0.3317(5) 0.1277(6) 0.142(4) 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 C1A 0.035(6) 0.057(6) 0.048(6) 0.025(4) 0.004(4) 0.003(4) C1B 0.055(8) 0.031(5) 0.072(7) -0.004(4) 0.016(5) 0.001(5) C2B 0.042(7) 0.034(5) 0.064(7) -0.005(4) -0.009(5) -0.003(4) C1C 0.046(7) 0.050(6) 0.062(6) 0.034(4) 0.000(4) 0.002(4) C1D 0.059(8) 0.049(6) 0.065(6) 0.009(5) -0.006(5) -0.015(5) C1M 0.026(5) 0.029(4) 0.033(4) 0.011(3) -0.007(3) -0.002(3) C2A 0.047(7) 0.065(6) 0.055(6) 0.027(5) -0.013(5) 0.006(5) C2C 0.039(6) 0.039(5) 0.054(6) 0.022(4) 0.009(4) 0.005(4) C2D 0.081(9) 0.056(7) 0.052(6) -0.005(5) 0.004(5) -0.039(6) C2M 0.031(5) 0.034(5) 0.031(4) 0.006(3) 0.000(3) 0.006(3) C3A 0.044(8) 0.064(7) 0.094(8) 0.025(6) -0.008(6) 0.011(5) C3B 0.056(7) 0.043(6) 0.048(6) -0.004(4) -0.021(5) 0.012(5) C3C 0.053(7) 0.037(5) 0.040(5) 0.019(4) 0.016(4) 0.018(4) C3D 0.097(11) 0.111(10) 0.090(9) -0.003(7) -0.039(8) 0.022(8) C3M 0.024(5) 0.040(5) 0.020(4) 0.001(3) -0.003(3) 0.007(3) C4A 0.040(7) 0.063(6) 0.077(7) 0.022(5) 0.016(5) 0.015(5) C4B 0.062(8) 0.078(7) 0.059(7) 0.001(5) -0.024(5) 0.026(6) C4C 0.051(7) 0.057(6) 0.050(6) 0.017(4) -0.004(5) -0.005(5) C4D 0.193(16) 0.047(8) 0.042(7) -0.004(5) 0.032(8) -0.042(9) C4M 0.027(5) 0.041(5) 0.030(4) 0.011(3) 0.003(3) -0.001(4) C5A 0.035(6) 0.040(5) 0.050(6) 0.011(4) 0.012(4) -0.001(4) C5B 0.095(11) 0.077(8) 0.083(9) 0.001(6) -0.035(7) 0.023(7) C5C 0.060(8) 0.055(6) 0.066(7) 0.013(5) -0.002(5) -0.008(5) C5M 0.029(6) 0.039(5) 0.041(5) 0.017(3) 0.000(4) 0.005(4) C6A 0.032(7) 0.068(6) 0.062(6) 0.020(5) 0.010(4) -0.002(5) C6B 0.042(7) 0.053(6) 0.082(8) -0.008(5) -0.009(5) 0.001(5) C6C 0.055(8) 0.059(7) 0.073(7) -0.003(5) -0.026(6) 0.000(5) C6M 0.025(5) 0.039(5) 0.040(5) 0.016(3) 0.000(3) 0.000(3) C7A 0.054(8) 0.042(5) 0.055(6) 0.024(4) -0.017(5) -0.005(4) C7B 0.061(9) 0.054(7) 0.107(10) -0.022(6) -0.023(7) 0.019(6) C7C 0.062(8) 0.054(6) 0.057(6) 0.015(5) -0.019(5) 0.002(5) C7M 0.027(5) 0.042(5) 0.027(4) 0.012(3) -0.002(3) 0.003(4) C8A 0.048(8) 0.075(7) 0.083(7) 0.046(6) -0.006(5) 0.006(5) C8B 0.084(9) 0.042(5) 0.045(6) 0.000(4) 0.026(5) 0.014(5) C8C 0.050(7) 0.037(5) 0.043(5) 0.006(4) -0.004(4) 0.010(4) C8D 0.113(14) 0.193(17) 0.120(12) -0.001(11) -0.064(11) 0.038(12) C8M 0.028(5) 0.032(5) 0.046(5) 0.011(3) -0.005(4) 0.008(3) C9A 0.052(8) 0.050(6) 0.059(6) 0.022(4) -0.006(5) -0.005(5) C9B 0.079(8) 0.027(5) 0.024(5) 0.003(3) 0.005(4) -0.003(4) C9C 0.062(7) 0.053(6) 0.045(5) 0.019(4) -0.007(5) 0.011(5) C9D 0.091(14) 0.134(14) 0.093(11) -0.026(9) 0.015(9) -0.068(10) C10A 0.063(8) 0.044(5) 0.051(6) 0.021(4) 0.011(5) -0.005(5) C10B 0.099(10) 0.052(6) 0.055(7) 0.017(5) 0.021(6) 0.029(6) C11A 0.069(9) 0.071(7) 0.091(8) 0.048(6) -0.025(7) -0.008(6) C11B 0.104(10) 0.051(6) 0.034(6) 0.006(4) -0.010(5) -0.009(6) C11C 0.063(8) 0.053(6) 0.058(6) 0.020(5) 0.019(5) 0.010(5) C12A 0.112(12) 0.079(8) 0.056(7) 0.038(6) -0.019(7) -0.007(7) C12B 0.055(8) 0.072(7) 0.072(7) 0.031(5) -0.010(6) 0.003(5) C12C 0.046(8) 0.048(6) 0.116(9) 0.030(6) 0.004(6) -0.006(5) C13A 0.085(10) 0.078(7) 0.053(7) 0.038(5) -0.005(6) 0.000(6) C13B 0.048(7) 0.053(6) 0.039(5) 0.010(4) -0.002(4) -0.001(5) C13C 0.060(9) 0.082(8) 0.098(9) 0.039(7) -0.038(6) -0.011(6) C14C 0.056(8) 0.089(8) 0.084(8) 0.056(6) -0.026(6) -0.026(6) C15D 0.44(3) 0.068(9) 0.115(11) -0.022(8) -0.057(15) 0.130(15) C18D 0.071(13) 0.22(2) 0.115(13) -0.052(14) -0.029(10) -0.032(13) Cu1 0.0933(11) 0.0514(7) 0.0368(6) -0.0051(5) -0.0031(6) 0.0186(7) Cu2 0.0327(7) 0.0437(6) 0.0420(6) 0.0212(4) 0.0035(4) 0.0012(5) Cu3 0.0365(7) 0.0452(6) 0.0423(6) 0.0245(5) -0.0027(4) -0.0004(5) Cu4 0.0389(7) 0.0514(7) 0.0353(6) -0.0008(4) -0.0008(5) 0.0069(5) Mo 0.0214(4) 0.0260(4) 0.0219(3) 0.0076(2) -0.0010(2) 0.0017(3) N1A 0.034(5) 0.029(4) 0.044(4) 0.012(3) 0.002(3) -0.002(3) N1B 0.054(6) 0.033(4) 0.040(4) -0.005(3) 0.004(3) -0.001(4) N1C 0.038(5) 0.038(4) 0.047(4) 0.019(3) 0.003(3) 0.009(3) N1M 0.049(5) 0.041(4) 0.033(4) 0.004(3) -0.004(3) 0.011(3) N2A 0.046(5) 0.048(4) 0.036(4) 0.018(3) 0.004(3) -0.004(3) N2B 0.039(5) 0.038(4) 0.035(4) 0.002(3) 0.001(3) -0.006(3) N2C 0.046(5) 0.036(4) 0.038(4) 0.009(3) 0.000(3) 0.007(3) N2D 0.178(12) 0.049(6) 0.045(6) -0.007(4) 0.002(6) 0.020(6) N2M 0.032(5) 0.050(4) 0.058(5) 0.016(3) -0.005(4) -0.005(3) N3M 0.033(5) 0.046(4) 0.033(4) 0.017(3) 0.001(3) -0.001(3) N4M 0.030(5) 0.064(5) 0.062(5) 0.026(4) 0.015(4) 0.008(4) N5M 0.058(6) 0.057(5) 0.029(4) -0.004(3) -0.008(3) 0.002(4) N6M 0.049(5) 0.046(5) 0.062(5) 0.023(4) -0.002(4) 0.013(4) N7M 0.027(4) 0.043(4) 0.046(4) 0.019(3) -0.002(3) 0.003(3) N8M 0.040(5) 0.051(4) 0.054(5) 0.007(3) -0.019(4) 0.000(3) O1A 0.048(4) 0.061(4) 0.057(4) 0.034(3) 0.008(3) 0.015(3) O1B 0.055(5) 0.071(4) 0.043(3) 0.010(3) -0.001(3) 0.029(3) O1C 0.047(5) 0.074(4) 0.060(4) 0.046(3) -0.012(3) -0.016(3) O1D 0.068(5) 0.039(3) 0.053(4) -0.003(3) -0.021(3) -0.019(3) O1W 0.063(6) 0.095(5) 0.122(6) -0.014(4) -0.001(4) 0.025(4) O2W 0.053(5) 0.081(4) 0.059(4) 0.023(3) -0.016(3) -0.026(3) O4W 0.056(5) 0.085(5) 0.090(5) 0.043(4) 0.010(4) 0.008(4) O3W 0.132(9) 0.123(7) 0.102(6) 0.015(5) 0.015(5) 0.025(6) O5W 0.128(8) 0.080(5) 0.107(6) 0.047(4) 0.028(5) 0.032(5) O6W 0.105(8) 0.143(8) 0.144(7) 0.071(6) -0.003(6) -0.013(6) O7W 0.123(9) 0.165(8) 0.084(5) 0.026(5) 0.006(5) -0.015(6) O8W 0.121(9) 0.103(6) 0.193(9) 0.021(6) -0.030(7) -0.002(6) _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 N1D C6D 1.3900 . ? N1D C5D 1.3900 . ? N1D Cu1 1.946(8) . ? C6D C7D 1.3900 . ? C6D C15D 1.423(17) . ? C7D C16D 1.3900 . ? C7D H7D 0.9300 . ? C16D C17D 1.3900 . ? C16D H16D 0.9300 . ? C17D C5D 1.3900 . ? C17D H17D 0.9300 . ? C5D H5D 0.9300 . ? C1A N1A 1.339(9) . ? C1A C2A 1.361(11) . ? C1A H1A 0.9300 . ? C1B N1B 1.281(10) . ? C1B C2B 1.423(12) . ? C1B H1B 0.9300 . ? C2B C3B 1.418(12) . ? C2B C6B 1.434(12) . ? C1C O1C 1.315(9) . ? C1C C14C 1.382(12) . ? C1C C2C 1.416(11) . ? C1D O1D 1.309(10) . ? C1D C3D 1.378(13) . ? C1D C2D 1.410(12) . ? C1M N7M 1.160(8) . ? C1M Mo 2.143(8) . ? C2A C3A 1.400(13) . ? C2A H2A 0.9300 . ? C2C C11C 1.403(11) . ? C2C C3C 1.431(11) . ? C2D C4D 1.391(16) . ? C2D C9D 1.418(17) . ? C2M N1M 1.142(8) . ? C2M Mo 2.178(8) . ? C3A C4A 1.346(12) . ? C3A H3A 0.9300 . ? C3B O1B 1.290(9) . ? C3B C4B 1.391(11) . ? C3C N1C 1.285(10) . ? C3C H3C 0.9300 . ? C3D C8D 1.403(16) . ? C3D H3D 0.9300 . ? C3M N3M 1.148(8) . ? C3M Mo 2.155(8) . ? C4A C5A 1.386(11) . ? C4A H4A 0.9300 . ? C4B C5B 1.380(13) . ? C4B H4B 0.9300 . ? C4C N2C 1.346(10) . ? C4C C5C 1.372(12) . ? C4C H4C 0.9300 . ? C4D N2D 1.283(16) . ? C4D H4D 0.9300 . ? C4M N2M 1.152(9) . ? C4M Mo 2.179(8) . ? C5A N1A 1.340(9) . ? C5A C6A 1.502(11) . ? C5B C7B 1.374(15) . ? C5B H5B 0.9300 . ? C5C C6C 1.374(12) . ? C5C H5C 0.9300 . ? C5M N4M 1.146(9) . ? C5M Mo 2.173(9) . ? C6A N2A 1.460(10) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C6B C7B 1.335(13) . ? C6B H6B 0.9300 . ? C6C C7C 1.361(12) . ? C6C H6C 0.9300 . ? C6M N5M 1.138(8) . ? C6M Mo 2.164(8) . ? C7A O1A 1.335(9) . ? C7A C9A 1.397(12) . ? C7A C8A 1.405(12) . ? C7B H7B 0.9300 . ? C7C C8C 1.377(11) . ? C7C H7C 0.9300 . ? C7M N6M 1.155(8) . ? C7M Mo 2.170(8) . ? C8A C11A 1.381(12) . ? C8A H8A 0.9300 . ? C8B N1B 1.456(10) . ? C8B C9B 1.487(12) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C8C N2C 1.322(9) . ? C8C C9C 1.500(12) . ? C8D C18D 1.37(2) . ? C8D H8D 0.9300 . ? C8M N8M 1.152(8) . ? C8M Mo 2.147(8) . ? C9A C13A 1.416(12) . ? C9A C10A 1.434(12) . ? C9B N2B 1.320(9) . ? C9B C10B 1.363(11) . ? C9C N1C 1.464(10) . ? C9C H9C1 0.9700 . ? C9C H9C2 0.9700 . ? C9D C18D 1.30(2) . ? C9D H9D 0.9300 . ? C10A N2A 1.283(9) . ? C10A H10A 0.9300 . ? C10B C11B 1.364(13) . ? C10B H10B 0.9300 . ? C11A C12A 1.374(14) . ? C11A H11A 0.9300 . ? C11B C12B 1.371(13) . ? C11B H11B 0.9300 . ? C11C C12C 1.356(12) . ? C11C H11C 0.9300 . ? C12A C13A 1.356(14) . ? C12A H12A 0.9300 . ? C12B C13B 1.389(11) . ? C12B H12B 0.9300 . ? C12C C13C 1.373(13) . ? C12C H12C 0.9300 . ? C13A H13A 0.9300 . ? C13B N2B 1.342(10) . ? C13B H13B 0.9300 . ? C13C C14C 1.394(13) . ? C13C H13C 0.9300 . ? C14C H14C 0.9300 . ? C15D N2D 1.462(14) . ? C15D H15A 0.9700 . ? C15D H15B 0.9700 . ? C18D H18D 0.9300 . ? Cu1 O1D 1.866(6) . ? Cu1 N2D 1.927(9) . ? Cu1 N5M 1.944(6) . ? Cu2 O1A 1.903(5) . ? Cu2 N2A 1.918(6) . ? Cu2 N7M 1.958(7) . ? Cu2 N1A 1.999(6) . ? Cu3 O1C 1.914(6) . ? Cu3 N1C 1.947(6) . ? Cu3 N3M 1.974(6) . ? Cu3 N2C 2.004(7) . ? Cu3 O1W 2.405(7) . ? Cu4 O1B 1.909(5) . ? Cu4 N1B 1.960(7) . ? Cu4 N2B 1.978(6) . ? Cu4 N1M 2.028(6) . ? Cu4 O2W 2.189(6) . ? 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 C6D N1D C5D 120.0 . . ? C6D N1D Cu1 113.3(8) . . ? C5D N1D Cu1 126.2(8) . . ? C7D C6D N1D 120.0 . . ? C7D C6D C15D 122.2(11) . . ? N1D C6D C15D 116.8(11) . . ? C6D C7D C16D 120.0 . . ? C6D C7D H7D 120.0 . . ? C16D C7D H7D 120.0 . . ? C7D C16D C17D 120.0 . . ? C7D C16D H16D 120.0 . . ? C17D C16D H16D 120.0 . . ? C5D C17D C16D 120.0 . . ? C5D C17D H17D 120.0 . . ? C16D C17D H17D 120.0 . . ? C17D C5D N1D 120.0 . . ? C17D C5D H5D 120.0 . . ? N1D C5D H5D 120.0 . . ? N1A C1A C2A 123.2(8) . . ? N1A C1A H1A 118.4 . . ? C2A C1A H1A 118.4 . . ? N1B C1B C2B 127.1(9) . . ? N1B C1B H1B 116.4 . . ? C2B C1B H1B 116.4 . . ? C3B C2B C1B 122.0(8) . . ? C3B C2B C6B 120.1(9) . . ? C1B C2B C6B 117.8(9) . . ? O1C C1C C14C 117.9(8) . . ? O1C C1C C2C 123.5(8) . . ? C14C C1C C2C 118.6(8) . . ? O1D C1D C3D 118.6(9) . . ? O1D C1D C2D 124.2(10) . . ? C3D C1D C2D 117.1(10) . . ? N7M C1M Mo 178.6(6) . . ? C1A C2A C3A 117.3(8) . . ? C1A C2A H2A 121.3 . . ? C3A C2A H2A 121.3 . . ? C11C C2C C1C 119.5(8) . . ? C11C C2C C3C 116.7(8) . . ? C1C C2C C3C 123.7(8) . . ? C4D C2D C1D 122.5(10) . . ? C4D C2D C9D 118.5(12) . . ? C1D C2D C9D 118.9(13) . . ? N1M C2M Mo 178.8(6) . . ? C4A C3A C2A 120.2(9) . . ? C4A C3A H3A 119.9 . . ? C2A C3A H3A 119.9 . . ? O1B C3B C4B 120.4(9) . . ? O1B C3B C2B 124.1(8) . . ? C4B C3B C2B 115.4(9) . . ? N1C C3C C2C 125.9(7) . . ? N1C C3C H3C 117.1 . . ? C2C C3C H3C 117.1 . . ? C1D C3D C8D 121.8(13) . . ? C1D C3D H3D 119.1 . . ? C8D C3D H3D 119.1 . . ? N3M C3M Mo 177.8(6) . . ? C3A C4A C5A 119.3(9) . . ? C3A C4A H4A 120.3 . . ? C5A C4A H4A 120.3 . . ? C5B C4B C3B 122.5(10) . . ? C5B C4B H4B 118.8 . . ? C3B C4B H4B 118.8 . . ? N2C C4C C5C 123.0(8) . . ? N2C C4C H4C 118.5 . . ? C5C C4C H4C 118.5 . . ? N2D C4D C2D 126.1(10) . . ? N2D C4D H4D 116.9 . . ? C2D C4D H4D 116.9 . . ? N2M C4M Mo 178.5(7) . . ? N1A C5A C4A 121.1(8) . . ? N1A C5A C6A 115.8(7) . . ? C4A C5A C6A 123.0(8) . . ? C7B C5B C4B 121.2(11) . . ? C7B C5B H5B 119.4 . . ? C4B C5B H5B 119.4 . . ? C4C C5C C6C 117.9(9) . . ? C4C C5C H5C 121.0 . . ? C6C C5C H5C 121.0 . . ? N4M C5M Mo 177.4(7) . . ? N2A C6A C5A 110.2(7) . . ? N2A C6A H6A1 109.6 . . ? C5A C6A H6A1 109.6 . . ? N2A C6A H6A2 109.6 . . ? C5A C6A H6A2 109.6 . . ? H6A1 C6A H6A2 108.1 . . ? C7B C6B C2B 121.2(10) . . ? C7B C6B H6B 119.4 . . ? C2B C6B H6B 119.4 . . ? C7C C6C C5C 119.7(9) . . ? C7C C6C H6C 120.1 . . ? C5C C6C H6C 120.1 . . ? N5M C6M Mo 177.7(7) . . ? O1A C7A C9A 124.4(8) . . ? O1A C7A C8A 117.1(9) . . ? C9A C7A C8A 118.5(8) . . ? C6B C7B C5B 119.1(11) . . ? C6B C7B H7B 120.4 . . ? C5B C7B H7B 120.4 . . ? C6C C7C C8C 118.8(9) . . ? C6C C7C H7C 120.6 . . ? C8C C7C H7C 120.6 . . ? N6M C7M Mo 178.2(7) . . ? C11A C8A C7A 120.1(10) . . ? C11A C8A H8A 119.9 . . ? C7A C8A H8A 119.9 . . ? N1B C8B C9B 110.0(7) . . ? N1B C8B H8B1 109.7 . . ? C9B C8B H8B1 109.7 . . ? N1B C8B H8B2 109.7 . . ? C9B C8B H8B2 109.7 . . ? H8B1 C8B H8B2 108.2 . . ? N2C C8C C7C 122.8(9) . . ? N2C C8C C9C 116.0(7) . . ? C7C C8C C9C 121.2(8) . . ? C18D C8D C3D 119.0(15) . . ? C18D C8D H8D 120.5 . . ? C3D C8D H8D 120.5 . . ? N8M C8M Mo 175.3(7) . . ? C7A C9A C13A 119.3(9) . . ? C7A C9A C10A 123.3(8) . . ? C13A C9A C10A 117.3(9) . . ? N2B C9B C10B 123.2(9) . . ? N2B C9B C8B 116.1(7) . . ? C10B C9B C8B 120.6(8) . . ? N1C C9C C8C 109.8(6) . . ? N1C C9C H9C1 109.7 . . ? C8C C9C H9C1 109.7 . . ? N1C C9C H9C2 109.7 . . ? C8C C9C H9C2 109.7 . . ? H9C1 C9C H9C2 108.2 . . ? C18D C9D C2D 122.0(16) . . ? C18D C9D H9D 119.0 . . ? C2D C9D H9D 119.0 . . ? N2A C10A C9A 125.2(8) . . ? N2A C10A H10A 117.4 . . ? C9A C10A H10A 117.4 . . ? C11B C10B C9B 118.2(9) . . ? C11B C10B H10B 120.9 . . ? C9B C10B H10B 120.9 . . ? C12A C11A C8A 121.3(10) . . ? C12A C11A H11A 119.3 . . ? C8A C11A H11A 119.3 . . ? C10B C11B C12B 121.1(9) . . ? C10B C11B H11B 119.4 . . ? C12B C11B H11B 119.4 . . ? C12C C11C C2C 121.1(9) . . ? C12C C11C H11C 119.5 . . ? C2C C11C H11C 119.5 . . ? C13A C12A C11A 119.6(10) . . ? C13A C12A H12A 120.2 . . ? C11A C12A H12A 120.2 . . ? C11B C12B C13B 116.5(9) . . ? C11B C12B H12B 121.7 . . ? C13B C12B H12B 121.7 . . ? C11C C12C C13C 119.3(9) . . ? C11C C12C H12C 120.4 . . ? C13C C12C H12C 120.4 . . ? C12A C13A C9A 121.1(10) . . ? C12A C13A H13A 119.5 . . ? C9A C13A H13A 119.5 . . ? N2B C13B C12B 123.0(8) . . ? N2B C13B H13B 118.5 . . ? C12B C13B H13B 118.5 . . ? C12C C13C C14C 121.8(9) . . ? C12C C13C H13C 119.1 . . ? C14C C13C H13C 119.1 . . ? C1C C14C C13C 119.7(9) . . ? C1C C14C H14C 120.2 . . ? C13C C14C H14C 120.2 . . ? C6D C15D N2D 108.5(11) . . ? C6D C15D H15A 110.0 . . ? N2D C15D H15A 110.0 . . ? C6D C15D H15B 110.0 . . ? N2D C15D H15B 110.0 . . ? H15A C15D H15B 108.4 . . ? C9D C18D C8D 121.1(16) . . ? C9D C18D H18D 119.4 . . ? C8D C18D H18D 119.4 . . ? O1D Cu1 N2D 93.0(4) . . ? O1D Cu1 N5M 90.6(2) . . ? N2D Cu1 N5M 172.2(3) . . ? O1D Cu1 N1D 173.2(3) . . ? N2D Cu1 N1D 82.3(5) . . ? N5M Cu1 N1D 94.7(4) . . ? O1A Cu2 N2A 93.7(3) . . ? O1A Cu2 N7M 92.1(2) . . ? N2A Cu2 N7M 167.0(3) . . ? O1A Cu2 N1A 167.6(2) . . ? N2A Cu2 N1A 83.1(3) . . ? N7M Cu2 N1A 93.5(3) . . ? O1C Cu3 N1C 93.5(3) . . ? O1C Cu3 N3M 91.7(2) . . ? N1C Cu3 N3M 160.9(3) . . ? O1C Cu3 N2C 174.3(2) . . ? N1C Cu3 N2C 81.8(3) . . ? N3M Cu3 N2C 93.8(3) . . ? O1C Cu3 O1W 89.5(3) . . ? N1C Cu3 O1W 107.0(3) . . ? N3M Cu3 O1W 91.4(3) . . ? N2C Cu3 O1W 89.0(3) . . ? O1B Cu4 N1B 92.4(3) . . ? O1B Cu4 N2B 173.6(3) . . ? N1B Cu4 N2B 81.9(3) . . ? O1B Cu4 N1M 91.9(2) . . ? N1B Cu4 N1M 148.7(3) . . ? N2B Cu4 N1M 94.4(2) . . ? O1B Cu4 O2W 87.0(2) . . ? N1B Cu4 O2W 111.6(2) . . ? N2B Cu4 O2W 92.5(2) . . ? N1M Cu4 O2W 99.6(3) . . ? C8M Mo C1M 83.3(3) . . ? C8M Mo C3M 108.2(3) . . ? C1M Mo C3M 147.0(3) . . ? C8M Mo C6M 145.4(3) . . ? C1M Mo C6M 100.8(3) . . ? C3M Mo C6M 87.0(2) . . ? C8M Mo C7M 74.6(2) . . ? C1M Mo C7M 70.2(3) . . ? C3M Mo C7M 142.2(3) . . ? C6M Mo C7M 74.7(2) . . ? C8M Mo C5M 76.6(3) . . ? C1M Mo C5M 141.9(3) . . ? C3M Mo C5M 70.8(3) . . ? C6M Mo C5M 79.7(3) . . ? C7M Mo C5M 73.4(3) . . ? C8M Mo C2M 70.0(3) . . ? C1M Mo C2M 82.3(3) . . ? C3M Mo C2M 73.5(2) . . ? C6M Mo C2M 144.5(3) . . ? C7M Mo C2M 137.2(2) . . ? C5M Mo C2M 119.2(3) . . ? C8M Mo C4M 139.9(3) . . ? C1M Mo C4M 74.2(3) . . ? C3M Mo C4M 77.9(3) . . ? C6M Mo C4M 72.6(3) . . ? C7M Mo C4M 125.1(3) . . ? C5M Mo C4M 138.9(3) . . ? C2M Mo C4M 74.4(3) . . ? C5A N1A C1A 118.8(7) . . ? C5A N1A Cu2 114.7(5) . . ? C1A N1A Cu2 126.5(6) . . ? C1B N1B C8B 120.0(8) . . ? C1B N1B Cu4 124.9(6) . . ? C8B N1B Cu4 114.9(5) . . ? C3C N1C C9C 118.6(7) . . ? C3C N1C Cu3 125.4(6) . . ? C9C N1C Cu3 115.9(5) . . ? C2M N1M Cu4 177.1(6) . . ? C10A N2A C6A 118.0(7) . . ? C10A N2A Cu2 126.5(6) . . ? C6A N2A Cu2 115.4(5) . . ? C9B N2B C13B 118.0(7) . . ? C9B N2B Cu4 116.3(6) . . ? C13B N2B Cu4 125.3(5) . . ? C8C N2C C4C 117.6(7) . . ? C8C N2C Cu3 116.1(6) . . ? C4C N2C Cu3 125.9(6) . . ? C4D N2D C15D 117.9(12) . . ? C4D N2D Cu1 125.4(9) . . ? C15D N2D Cu1 116.4(9) . . ? C3M N3M Cu3 171.8(6) . . ? C6M N5M Cu1 163.9(7) . . ? C1M N7M Cu2 170.5(6) . . ? C7A O1A Cu2 126.0(6) . . ? C3B O1B Cu4 128.6(5) . . ? C1C O1C Cu3 127.6(5) . . ? C1D O1D Cu1 127.8(6) . . ? _diffrn_measured_fraction_theta_max 0.690 _diffrn_reflns_theta_full 29.25 _diffrn_measured_fraction_theta_full 0.690 _refine_diff_density_max 0.701 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.086 # Attachment '2_CCD_723822revised.cif' data_max52at1 _database_code_depnum_ccdc_archive 'CCDC 723822' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H132 Cu8 Mo2 N32 O20' _chemical_formula_weight 3138.86 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' 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' 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' _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 13.239(3) _cell_length_b 14.652(3) _cell_length_c 19.457(4) _cell_angle_alpha 101.50(3) _cell_angle_beta 102.02(3) _cell_angle_gamma 110.42(3) _cell_volume 3303.6(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26229 _cell_measurement_theta_min 3.32 _cell_measurement_theta_max 53.89 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.522 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.831 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details wingx _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18105 _diffrn_reflns_av_R_equivalents 0.0942 _diffrn_reflns_av_sigmaI/netI 0.2839 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.97 _reflns_number_total 10987 _reflns_number_gt 3114 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr. _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10987 _refine_ls_number_parameters 798 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.2699 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2117 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 0.857 _refine_ls_restrained_S_all 0.860 _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 O1AW O -0.184(2) -0.589(2) 0.1078(14) 0.102(9) Uiso 0.40 1 d P . . O2W O -0.1664(11) -0.2219(11) -0.2095(6) 0.159(6) Uani 1 1 d . . . O1BW O 0.743(2) 0.458(2) 0.1854(15) 0.206(11) Uiso 0.60 1 d P . . O4W O 1.068(3) 0.081(2) 0.2926(17) 0.405(16) Uiso 1 1 d . . . O5W O 0.393(2) 0.350(2) 0.1034(16) 0.372(14) Uiso 1 1 d . . . O6W O -0.157(2) -0.0038(11) 0.3615(13) 0.38(2) Uani 1 1 d . . . O7W O 1.322(3) 0.451(4) 0.2032(19) 0.56(3) Uani 1 1 d . . . C1 C 0.3121(11) -0.0749(12) 0.4029(12) 0.215(12) Uiso 1 1 d G . . H1 H 0.3809 -0.0789 0.4035 0.258 Uiso 1 1 calc R . . C2 C 0.2953(16) -0.0334(13) 0.4681(8) 0.201(11) Uiso 1 1 d G . . H2 H 0.3528 -0.0096 0.5123 0.241 Uiso 1 1 calc R . . C3 C 0.193(2) -0.0274(13) 0.4671(9) 0.319(19) Uiso 1 1 d G . . H3 H 0.1813 0.0003 0.5107 0.383 Uiso 1 1 calc R . . C4 C 0.1066(13) -0.0629(13) 0.4009(13) 0.223(12) Uiso 1 1 d G . . H4 H 0.0378 -0.0589 0.4002 0.267 Uiso 1 1 calc R . . C5 C 0.1234(13) -0.1044(11) 0.3357(9) 0.160(9) Uiso 1 1 d G . . C6 C 0.0224(16) -0.1648(15) 0.2606(11) 0.139(8) Uiso 1 1 d DU . . H06C H -0.0445 -0.1585 0.2698 0.167 Uiso 1 1 calc R . . H06D H 0.0405 -0.1284 0.2253 0.167 Uiso 1 1 calc R . . C7 C -0.0120(18) -0.2793(17) 0.2219(14) 0.206(11) Uani 1 1 d DU . . H07A H -0.0312 -0.3182 0.2557 0.247 Uiso 1 1 calc R . . H07B H -0.0787 -0.3033 0.1798 0.247 Uiso 1 1 calc R . . C8 C 0.0681(17) -0.3801(19) 0.1489(13) 0.111(8) Uani 1 1 d U . . H077 H -0.0048 -0.4309 0.1337 0.133 Uiso 1 1 calc R . . C8C C 0.6358(14) 0.0967(12) 0.2901(8) 0.097(7) Uani 1 1 d . . . C9 C 0.1450(16) -0.4066(15) 0.1158(10) 0.078(5) Uani 1 1 d U . . C10 C 0.2601(15) -0.3374(14) 0.1393(9) 0.068(4) Uani 1 1 d U . . C11 C 0.3310(14) -0.3736(12) 0.1072(9) 0.082(5) Uani 1 1 d . . . H047 H 0.4074 -0.3311 0.1200 0.098 Uiso 1 1 calc R . . C12 C 0.291(2) -0.4689(16) 0.0578(11) 0.114(7) Uani 1 1 d . . . H060 H 0.3400 -0.4905 0.0376 0.137 Uiso 1 1 calc R . . C13 C 0.176(2) -0.5331(18) 0.0383(12) 0.122(8) Uani 1 1 d . . . H072 H 0.1487 -0.5978 0.0053 0.146 Uiso 1 1 calc R . . C14 C 0.107(2) -0.5049(18) 0.0648(14) 0.119(8) Uani 1 1 d . . . H045 H 0.0313 -0.5493 0.0504 0.143 Uiso 1 1 calc R . . C15 C 0.0696(12) 0.1559(10) 0.0179(9) 0.059(4) Uani 1 1 d . . . C16 C 0.0212(14) 0.2219(11) 0.0442(9) 0.077(5) Uani 1 1 d . . . H070 H 0.0599 0.2710 0.0898 0.092 Uiso 1 1 calc R . . C17 C -0.0796(16) 0.2168(16) 0.0058(15) 0.116(8) Uani 1 1 d . . . H041 H -0.1095 0.2605 0.0261 0.140 Uiso 1 1 calc R . . C18 C -0.1375(18) 0.149(2) -0.0619(14) 0.119(8) Uani 1 1 d . . . H061 H -0.2063 0.1459 -0.0884 0.142 Uiso 1 1 calc R . . C19 C -0.0928(14) 0.0852(13) -0.0899(9) 0.080(5) Uani 1 1 d . . . H059 H -0.1337 0.0375 -0.1358 0.096 Uiso 1 1 calc R . . C20 C 0.0122(11) 0.0869(12) -0.0536(8) 0.058(4) Uani 1 1 d . . . C21 C 0.0560(12) 0.0222(11) -0.0863(7) 0.063(4) Uani 1 1 d . . . H016 H 0.0060 -0.0269 -0.1299 0.076 Uiso 1 1 calc R . . C22 C 0.1721(14) -0.0550(12) -0.1198(8) 0.085(5) Uani 1 1 d . . . H02A H 0.1832 -0.0299 -0.1614 0.102 Uiso 1 1 calc R . . H02B H 0.1061 -0.1194 -0.1382 0.102 Uiso 1 1 calc R . . C23 C 0.2721(17) -0.0720(13) -0.0860(9) 0.091(5) Uani 1 1 d . . . H06A H 0.2779 -0.1258 -0.1210 0.109 Uiso 1 1 calc R . . H06B H 0.2618 -0.0948 -0.0434 0.109 Uiso 1 1 calc R . . C24 C 0.3821(16) 0.0236(16) -0.0621(9) 0.087(6) Uani 1 1 d . . . C25 C 0.4637(17) 0.0363(17) -0.0974(9) 0.099(7) Uani 1 1 d . . . H1A H 0.4555 -0.0133 -0.1388 0.119 Uiso 1 1 calc R . . C26 C 0.5591(15) 0.1278(19) -0.0675(12) 0.118(8) Uani 1 1 d . . . H075 H 0.6178 0.1396 -0.0884 0.142 Uiso 1 1 calc R . . C27 C 0.5678(14) 0.2011(15) -0.0072(10) 0.094(6) Uani 1 1 d . . . H073 H 0.6325 0.2615 0.0138 0.113 Uiso 1 1 calc R . . C28 C 0.4796(14) 0.1827(15) 0.0205(8) 0.079(5) Uani 1 1 d . . . H026 H 0.4839 0.2329 0.0601 0.094 Uiso 1 1 calc R . . C29 C 1.0183(11) 0.2660(10) 0.4108(9) 0.062(5) Uani 1 1 d . . . H11 H 1.0193 0.2074 0.3825 0.074 Uiso 1 1 calc R . . C30 C 0.9485(11) 0.2771(12) 0.2936(7) 0.075(5) Uani 1 1 d . . . H02C H 0.8735 0.2222 0.2736 0.090 Uiso 1 1 calc R . . H02D H 1.0017 0.2506 0.2802 0.090 Uiso 1 1 calc R . . C31 C 0.9514(13) 0.3628(12) 0.2607(8) 0.080(5) Uani 1 1 d . . . H03C H 0.8853 0.3764 0.2628 0.096 Uiso 1 1 calc R . . H03D H 0.9464 0.3404 0.2092 0.096 Uiso 1 1 calc R . . C32 C 1.0571(15) 0.4621(13) 0.2986(9) 0.067(4) Uani 1 1 d . . . C33 C 1.1432(17) 0.5063(17) 0.2702(9) 0.081(5) Uani 1 1 d . . . H049 H 1.1409 0.4735 0.2234 0.097 Uiso 1 1 calc R . . C34 C 1.2314(17) 0.5974(16) 0.3097(11) 0.092(6) Uani 1 1 d . . . H068 H 1.2890 0.6250 0.2898 0.110 Uiso 1 1 calc R . . C35 C 1.2362(17) 0.6480(14) 0.3773(10) 0.087(6) Uani 1 1 d . . . H063 H 1.2954 0.7106 0.4040 0.104 Uiso 1 1 calc R . . C36 C 1.1504(16) 0.6034(13) 0.4050(8) 0.070(5) Uani 1 1 d . . . H032 H 1.1522 0.6375 0.4513 0.084 Uiso 1 1 calc R . . C37 C 0.9206(11) 0.6236(13) 0.4576(9) 0.065(5) Uani 1 1 d . . . C38 C 0.8638(11) 0.6084(12) 0.3824(8) 0.070(5) Uani 1 1 d . . . H031 H 0.8478 0.5487 0.3464 0.084 Uiso 1 1 calc R . . C39 C 0.8325(12) 0.6840(16) 0.3636(9) 0.079(5) Uani 1 1 d . . . H057 H 0.7971 0.6734 0.3143 0.095 Uiso 1 1 calc R . . C40 C 0.8515(15) 0.7740(15) 0.4143(12) 0.102(6) Uani 1 1 d . . . H058 H 0.8329 0.8249 0.4009 0.122 Uiso 1 1 calc R . . C41 C 0.9002(14) 0.7819(13) 0.4865(10) 0.085(5) Uani 1 1 d . . . H056 H 0.9103 0.8395 0.5223 0.102 Uiso 1 1 calc R . . C42 C 0.9350(11) 0.7131(13) 0.5103(9) 0.060(4) Uani 1 1 d . . . C43 C 0.3633(13) 0.4478(12) 0.3711(8) 0.055(4) Uani 1 1 d . . . H021 H 0.3424 0.3979 0.3267 0.066 Uiso 1 1 calc R . . C44 C 0.3030(12) 0.4285(11) 0.4213(9) 0.062(4) Uani 1 1 d . . . H051 H 0.2412 0.3669 0.4105 0.075 Uiso 1 1 calc R . . C45 C 0.3376(13) 0.5034(14) 0.4878(8) 0.065(4) Uani 1 1 d . . . H022 H 0.2999 0.4930 0.5227 0.078 Uiso 1 1 calc R . . C46 C 0.4280(15) 0.5923(12) 0.5007(8) 0.067(5) Uani 1 1 d . . . H030 H 0.4528 0.6429 0.5453 0.081 Uiso 1 1 calc R . . C47 C 0.4829(12) 0.6086(12) 0.4492(8) 0.059(4) Uani 1 1 d . . . C48 C 0.5781(14) 0.7051(12) 0.4594(8) 0.094(6) Uani 1 1 d . . . H03E H 0.6456 0.6924 0.4607 0.113 Uiso 1 1 calc R . . H03F H 0.5919 0.7526 0.5063 0.113 Uiso 1 1 calc R . . C49 C 0.5565(15) 0.7532(11) 0.3986(9) 0.102(7) Uani 1 1 d . . . H03A H 0.4817 0.7532 0.3897 0.122 Uiso 1 1 calc R . . H03B H 0.6115 0.8233 0.4133 0.122 Uiso 1 1 calc R . . C050 C 0.6640(15) 0.7881(14) 0.1856(10) 0.092(6) Uani 1 1 d . . . H050 H 0.6784 0.8559 0.2066 0.110 Uiso 1 1 calc R . . C50 C 0.5982(12) 0.7474(11) 0.2900(8) 0.060(4) Uani 1 1 d . . . H011 H 0.6104 0.8156 0.3059 0.071 Uiso 1 1 calc R . . C51 C 0.6198(12) 0.7171(12) 0.2214(8) 0.055(4) Uani 1 1 d . . . C52 C 0.5945(12) 0.6120(14) 0.1877(8) 0.057(4) Uani 1 1 d . . . C53 C 0.6169(16) 0.5891(14) 0.1202(10) 0.099(6) Uani 1 1 d . . . H048 H 0.6008 0.5217 0.0964 0.118 Uiso 1 1 calc R . . C54 C 0.6613(19) 0.662(2) 0.0886(11) 0.132(8) Uani 1 1 d . . . H069 H 0.6748 0.6442 0.0439 0.159 Uiso 1 1 calc R . . C55 C 0.6866(19) 0.7632(18) 0.1228(13) 0.129(8) Uani 1 1 d . . . H8 H 0.7192 0.8135 0.1019 0.155 Uiso 1 1 calc R . . C56 C 0.4111(11) 0.1516(10) 0.1878(9) 0.056(4) Uani 1 1 d . . . C57 C 0.4173(14) 0.0301(12) 0.2655(8) 0.069(5) Uani 1 1 d . . . C58 C 0.3817(13) 0.1922(10) 0.3257(8) 0.056(4) Uani 1 1 d . . . C59 C 0.5540(15) 0.1649(11) 0.4030(9) 0.085(6) Uani 1 1 d . . . C60 C 0.6998(13) 0.2977(11) 0.3632(7) 0.064(5) Uani 1 1 d . . . C61 C 0.5334(10) 0.3394(11) 0.3002(7) 0.052(4) Uani 1 1 d . . . C62 C 0.6253(14) 0.2362(14) 0.2184(10) 0.084(7) Uani 1 1 d . . . Cu1 Cu 0.25902(13) 0.09869(13) 0.03002(9) 0.0562(5) Uani 1 1 d . . . Cu2 Cu 0.2324(2) -0.18232(16) 0.23695(13) 0.1062(9) Uani 1 1 d . . . Cu3 Cu 0.52565(15) 0.54874(12) 0.30646(9) 0.0600(6) Uani 1 1 d . . . Cu4 Cu 0.95470(15) 0.43384(14) 0.41828(9) 0.0704(6) Uani 1 1 d . . . Mo Mo 0.53152(11) 0.18757(9) 0.29411(7) 0.0575(4) Uani 1 1 d . . . N1 N 0.0828(14) -0.2982(14) 0.1960(11) 0.116(7) Uani 1 1 d DU . . N1C N 0.3565(13) -0.0519(10) 0.2518(8) 0.104(5) Uani 1 1 d . . . N2 N 0.2262(17) -0.1104(10) 0.3367(8) 0.152(7) Uiso 1 1 d G . . N2C N 0.3486(9) 0.1336(10) 0.1325(7) 0.071(4) Uani 1 1 d . . . N3 N 0.3880(11) 0.0971(12) -0.0061(7) 0.075(4) Uani 1 1 d . . . N3C N 0.3022(11) 0.1877(9) 0.3366(7) 0.082(5) Uani 1 1 d . . . N4 N 0.1515(9) 0.0178(8) -0.0678(5) 0.051(3) Uani 1 1 d . . . N4C N 0.5595(16) 0.1483(12) 0.4586(9) 0.142(7) Uani 1 1 d . . . N5 N 0.5654(9) 0.6956(8) 0.3318(7) 0.059(3) Uani 1 1 d . . . N5C N 0.6920(13) 0.0564(12) 0.2881(9) 0.138(7) Uani 1 1 d . . . N6 N 0.4492(10) 0.5356(9) 0.3859(6) 0.058(3) Uani 1 1 d . . . N6C N 0.6761(13) 0.2642(14) 0.1814(8) 0.112(7) Uani 1 1 d . . . N7 N 1.0631(10) 0.5117(11) 0.3679(7) 0.073(4) Uani 1 1 d . . . N7C N 0.5342(9) 0.4176(9) 0.3027(6) 0.056(3) Uani 1 1 d . . . N8 N 0.9777(10) 0.3120(9) 0.3749(6) 0.069(4) Uani 1 1 d . . . N8C N 0.7882(9) 0.3552(9) 0.3954(6) 0.065(4) Uani 1 1 d . . . O1 O 0.3031(8) -0.2467(8) 0.1849(6) 0.089(4) Uani 1 1 d . . . O2 O 0.1678(8) 0.1660(7) 0.0585(5) 0.071(3) Uani 1 1 d . . . O3 O 0.5571(9) 0.5405(7) 0.2161(5) 0.077(3) Uani 1 1 d . . . O4 O 0.9566(8) 0.5588(7) 0.4786(5) 0.070(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 O2W 0.146(12) 0.216(16) 0.088(10) -0.012(10) -0.007(8) 0.099(11) O6W 0.38(3) 0.093(13) 0.38(3) 0.059(15) -0.25(2) -0.022(15) O7W 0.39(4) 1.00(10) 0.38(4) 0.25(5) 0.13(3) 0.36(6) C7 0.164(19) 0.24(3) 0.24(2) 0.070(19) 0.179(17) 0.054(18) C8 0.068(14) 0.13(2) 0.15(2) 0.095(18) 0.034(15) 0.023(16) C8C 0.095(13) 0.072(12) 0.083(12) -0.050(9) -0.037(9) 0.062(11) C9 0.068(14) 0.067(14) 0.068(12) 0.033(11) 0.010(10) -0.009(11) C10 0.057(12) 0.050(12) 0.083(12) 0.024(10) 0.011(9) 0.010(10) C11 0.080(13) 0.047(12) 0.089(13) -0.004(10) 0.010(10) 0.016(10) C12 0.131(19) 0.071(16) 0.131(18) -0.012(13) 0.065(15) 0.039(14) C13 0.14(3) 0.069(17) 0.097(18) 0.001(13) 0.024(17) -0.002(18) C14 0.11(2) 0.065(18) 0.13(2) 0.014(16) 0.013(16) -0.001(14) C15 0.036(10) 0.043(10) 0.082(12) 0.007(9) 0.009(8) 0.008(8) C16 0.058(12) 0.043(10) 0.101(14) -0.005(9) 0.022(10) 0.002(9) C17 0.043(14) 0.106(19) 0.20(3) 0.049(17) 0.035(14) 0.023(13) C18 0.066(16) 0.16(3) 0.14(2) 0.08(2) 0.026(14) 0.048(17) C19 0.047(12) 0.089(15) 0.071(12) 0.018(11) 0.010(9) -0.004(10) C20 0.032(9) 0.086(13) 0.039(9) 0.022(9) -0.009(7) 0.013(9) C21 0.032(9) 0.066(11) 0.053(10) -0.011(8) 0.014(7) -0.009(8) C22 0.087(13) 0.077(13) 0.060(12) -0.009(10) 0.013(10) 0.021(11) C23 0.118(17) 0.091(15) 0.065(12) 0.001(11) 0.048(11) 0.045(14) C24 0.077(15) 0.119(18) 0.051(11) 0.001(12) 0.024(10) 0.035(13) C25 0.078(15) 0.18(2) 0.073(13) 0.032(14) 0.045(12) 0.077(16) C26 0.022(11) 0.20(3) 0.111(18) 0.029(17) 0.026(11) 0.017(14) C27 0.062(14) 0.115(17) 0.067(13) 0.011(12) 0.009(10) 0.007(12) C28 0.035(11) 0.125(17) 0.076(12) 0.034(12) 0.033(10) 0.021(11) C29 0.038(10) 0.032(9) 0.068(12) -0.019(8) -0.005(8) -0.009(7) C30 0.050(10) 0.089(13) 0.044(10) -0.005(10) -0.011(7) 0.007(9) C31 0.092(13) 0.083(14) 0.043(10) -0.002(10) -0.006(9) 0.037(11) C32 0.079(13) 0.072(13) 0.045(10) 0.016(10) 0.010(10) 0.031(11) C33 0.084(14) 0.131(18) 0.051(11) 0.041(13) 0.034(11) 0.054(13) C34 0.096(16) 0.081(16) 0.089(16) 0.041(13) 0.013(12) 0.025(13) C35 0.119(17) 0.092(15) 0.054(12) 0.012(11) 0.023(12) 0.055(13) C36 0.098(14) 0.069(13) 0.043(10) -0.007(9) 0.008(10) 0.053(11) C37 0.033(9) 0.079(13) 0.069(12) 0.004(11) 0.009(8) 0.020(9) C38 0.063(11) 0.086(13) 0.035(9) 0.000(9) 0.000(7) 0.020(10) C39 0.044(10) 0.109(16) 0.066(12) 0.033(12) -0.005(8) 0.018(11) C40 0.123(17) 0.070(15) 0.092(16) 0.037(13) 0.011(13) 0.021(12) C41 0.089(14) 0.072(13) 0.065(13) 0.017(11) 0.018(10) 0.005(11) C42 0.046(10) 0.056(12) 0.069(12) 0.032(11) 0.018(8) 0.005(9) C43 0.056(10) 0.052(11) 0.050(9) 0.007(8) 0.014(8) 0.020(9) C44 0.047(10) 0.054(11) 0.065(11) 0.008(9) 0.013(8) 0.004(8) C45 0.057(11) 0.091(14) 0.043(10) 0.016(10) 0.019(8) 0.025(10) C46 0.104(14) 0.051(12) 0.057(11) 0.018(9) 0.042(11) 0.032(11) C47 0.062(11) 0.053(12) 0.037(9) -0.005(8) 0.014(8) 0.006(9) C48 0.108(14) 0.054(12) 0.046(11) -0.019(9) 0.031(10) -0.036(11) C49 0.182(19) 0.043(11) 0.088(14) 0.000(10) 0.099(14) 0.031(12) C050 0.121(16) 0.071(14) 0.061(13) 0.017(12) 0.016(12) 0.022(12) C50 0.079(12) 0.027(9) 0.056(11) -0.010(8) 0.003(9) 0.025(9) C51 0.068(11) 0.041(10) 0.045(10) 0.021(9) 0.004(8) 0.012(8) C52 0.060(11) 0.079(14) 0.044(10) 0.025(10) 0.020(8) 0.035(10) C53 0.148(18) 0.067(13) 0.083(15) 0.020(12) 0.060(14) 0.034(13) C54 0.17(2) 0.17(3) 0.078(16) 0.041(18) 0.080(15) 0.05(2) C55 0.18(2) 0.089(19) 0.11(2) 0.043(17) 0.069(18) 0.022(17) C56 0.035(10) 0.052(10) 0.070(11) 0.013(9) 0.016(8) 0.007(8) C57 0.125(15) 0.042(10) 0.051(10) 0.004(9) 0.023(10) 0.056(11) C58 0.051(11) 0.035(9) 0.061(10) 0.014(7) 0.023(8) -0.010(8) C59 0.143(16) 0.054(11) 0.045(11) 0.020(9) -0.013(10) 0.046(11) C60 0.077(12) 0.062(12) 0.038(9) 0.008(8) -0.010(8) 0.030(10) C61 0.033(8) 0.061(11) 0.032(8) -0.009(8) 0.000(6) 0.005(8) C62 0.039(12) 0.098(15) 0.070(14) -0.036(11) -0.029(9) 0.035(11) Cu1 0.0426(11) 0.0583(12) 0.0419(11) -0.0031(9) 0.0037(8) 0.0060(9) Cu2 0.152(2) 0.0632(16) 0.134(2) 0.0396(15) 0.0839(18) 0.0493(17) Cu3 0.0753(14) 0.0411(12) 0.0501(12) 0.0054(9) 0.0216(10) 0.0110(10) Cu4 0.0648(13) 0.0776(15) 0.0445(12) -0.0091(10) -0.0057(9) 0.0288(11) Mo 0.0637(9) 0.0505(9) 0.0422(8) -0.0064(7) -0.0009(6) 0.0256(7) N1 0.099(13) 0.131(17) 0.168(19) 0.093(14) 0.060(13) 0.068(14) N1C 0.146(14) 0.033(9) 0.126(14) 0.020(10) 0.049(11) 0.027(10) N2C 0.039(8) 0.100(11) 0.051(9) 0.002(8) 0.006(6) 0.016(7) N3 0.041(9) 0.093(12) 0.065(10) 0.023(9) 0.014(7) 0.001(8) N3C 0.060(10) 0.068(10) 0.071(9) -0.011(7) 0.026(8) -0.014(8) N4 0.047(8) 0.050(8) 0.034(7) -0.011(6) 0.021(6) 0.003(6) N4C 0.23(2) 0.104(13) 0.101(15) 0.065(12) 0.024(14) 0.076(13) N5 0.068(9) 0.032(8) 0.066(9) 0.012(7) 0.020(7) 0.009(7) N5C 0.116(13) 0.126(14) 0.150(15) -0.015(11) -0.017(11) 0.088(12) N6 0.060(9) 0.034(8) 0.054(8) 0.005(7) 0.007(6) 0.001(7) N6C 0.063(12) 0.165(16) 0.063(12) -0.026(11) 0.001(8) 0.038(11) N7 0.068(9) 0.084(11) 0.052(9) 0.008(8) -0.005(7) 0.031(8) N7C 0.055(8) 0.039(8) 0.061(9) 0.005(7) 0.013(6) 0.014(7) N8 0.067(9) 0.076(10) 0.030(7) -0.021(7) -0.010(6) 0.025(7) N8C 0.051(8) 0.069(10) 0.052(8) -0.013(7) -0.002(6) 0.025(7) O1 0.078(8) 0.046(7) 0.101(9) -0.012(6) 0.004(6) 0.007(6) O2 0.045(7) 0.069(7) 0.065(7) -0.011(5) 0.000(5) 0.011(5) O3 0.133(10) 0.052(7) 0.050(7) 0.017(6) 0.039(6) 0.035(7) O4 0.072(7) 0.077(8) 0.036(6) -0.016(5) -0.018(5) 0.038(6) _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 C1 C2 1.3900 . ? C1 N2 1.3900 . ? C1 H1 0.9300 . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 N2 1.3900 . ? C5 C6 1.60(2) . ? C6 C7 1.552(16) . ? C6 H06C 0.9700 . ? C6 H06D 0.9700 . ? C7 N1 1.536(15) . ? C7 H07A 0.9700 . ? C7 H07B 0.9700 . ? C8 N1 1.28(2) . ? C8 C9 1.43(2) . ? C8 H077 0.9300 . ? C8C N5C 1.102(15) . ? C8C Mo 2.230(14) . ? C9 C10 1.42(2) . ? C9 C14 1.43(2) . ? C10 O1 1.292(16) . ? C10 C11 1.419(19) . ? C11 C12 1.376(19) . ? C11 H047 0.9300 . ? C12 C13 1.41(3) . ? C12 H060 0.9300 . ? C13 C14 1.28(2) . ? C13 H072 0.9300 . ? C14 H045 0.9300 . ? C15 O2 1.314(14) . ? C15 C16 1.408(17) . ? C15 C20 1.414(17) . ? C16 C17 1.36(2) . ? C16 H070 0.9300 . ? C17 C18 1.35(2) . ? C17 H041 0.9300 . ? C18 C19 1.36(2) . ? C18 H061 0.9300 . ? C19 C20 1.411(18) . ? C19 H059 0.9300 . ? C20 C21 1.391(18) . ? C21 N4 1.269(15) . ? C21 H016 0.9300 . ? C22 N4 1.459(15) . ? C22 C23 1.477(18) . ? C22 H02A 0.9700 . ? C22 H02B 0.9700 . ? C23 C24 1.53(2) . ? C23 H06A 0.9700 . ? C23 H06B 0.9700 . ? C24 N3 1.339(17) . ? C24 C25 1.38(2) . ? C25 C26 1.39(2) . ? C25 H1A 0.9300 . ? C26 C27 1.38(2) . ? C26 H075 0.9300 . ? C27 C28 1.352(19) . ? C27 H073 0.9300 . ? C28 N3 1.315(17) . ? C28 H026 0.9300 . ? C29 N8 1.233(16) . ? C29 C42 1.455(18) 2_766 ? C29 H11 0.9300 . ? C30 N8 1.481(15) . ? C30 C31 1.512(18) . ? C30 H02C 0.9700 . ? C30 H02D 0.9700 . ? C31 C32 1.530(19) . ? C31 H03C 0.9700 . ? C31 H03D 0.9700 . ? C32 N7 1.369(17) . ? C32 C33 1.384(19) . ? C33 C34 1.37(2) . ? C33 H049 0.9300 . ? C34 C35 1.35(2) . ? C34 H068 0.9300 . ? C35 C36 1.37(2) . ? C35 H063 0.9300 . ? C36 N7 1.359(17) . ? C36 H032 0.9300 . ? C37 O4 1.297(16) . ? C37 C42 1.420(19) . ? C37 C38 1.432(17) . ? C38 C39 1.397(19) . ? C38 H031 0.9300 . ? C39 C40 1.39(2) . ? C39 H057 0.9300 . ? C40 C41 1.38(2) . ? C40 H058 0.9300 . ? C41 C42 1.364(19) . ? C41 H056 0.9300 . ? C42 C29 1.455(18) 2_766 ? C43 N6 1.315(15) . ? C43 C44 1.395(17) . ? C43 H021 0.9300 . ? C44 C45 1.387(17) . ? C44 H051 0.9300 . ? C45 C46 1.360(17) . ? C45 H022 0.9300 . ? C46 C47 1.365(17) . ? C46 H030 0.9300 . ? C47 N6 1.332(14) . ? C47 C48 1.473(18) . ? C48 C49 1.520(19) . ? C48 H03E 0.9700 . ? C48 H03F 0.9700 . ? C49 N5 1.452(15) . ? C49 H03A 0.9700 . ? C49 H03B 0.9700 . ? C050 C55 1.33(2) . ? C050 C51 1.394(19) . ? C050 H050 0.9300 . ? C50 N5 1.261(15) . ? C50 C51 1.439(18) . ? C50 H011 0.9300 . ? C51 C52 1.434(18) . ? C52 O3 1.278(16) . ? C52 C53 1.408(19) . ? C53 C54 1.36(2) . ? C53 H048 0.9300 . ? C54 C55 1.39(2) . ? C54 H069 0.9300 . ? C55 H8 0.9300 . ? C56 N2C 1.129(14) . ? C56 Mo 2.168(15) . ? C57 N1C 1.127(16) . ? C57 Mo 2.150(17) . ? C58 N3C 1.100(14) . ? C58 Mo 2.213(16) . ? C59 N4C 1.149(16) . ? C59 Mo 2.185(17) . ? C60 N8C 1.126(14) . ? C60 Mo 2.180(15) . ? C61 N7C 1.133(14) . ? C61 Mo 2.196(16) . ? C62 N6C 1.13(2) . ? C62 Mo 2.19(2) . ? Cu1 O2 1.905(9) . ? Cu1 N2C 1.957(12) . ? Cu1 N4 1.961(10) . ? Cu1 N3 1.982(13) . ? Cu2 O1 1.849(11) . ? Cu2 N1C 1.956(15) . ? Cu2 N1 1.974(18) . ? Cu2 N2 2.049(12) . ? Cu3 O3 1.879(10) . ? Cu3 N7C 1.952(11) . ? Cu3 N5 1.957(11) . ? Cu3 N6 2.021(12) . ? Cu4 O4 1.958(9) . ? Cu4 N8 1.968(12) . ? Cu4 N8C 2.000(12) . ? Cu4 N7 2.052(14) . ? Cu4 O4 2.064(9) 2_766 ? O4 Cu4 2.064(9) 2_766 ? 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 C2 C1 N2 120.0 . . ? C2 C1 H1 120.0 . . ? N2 C1 H1 120.0 . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N2 C5 C4 120.0 . . ? N2 C5 C6 116.6(17) . . ? C4 C5 C6 122.5(17) . . ? C7 C6 C5 121.6(18) . . ? C7 C6 H06C 106.9 . . ? C5 C6 H06C 106.9 . . ? C7 C6 H06D 106.9 . . ? C5 C6 H06D 106.9 . . ? H06C C6 H06D 106.7 . . ? N1 C7 C6 112.3(17) . . ? N1 C7 H07A 109.1 . . ? C6 C7 H07A 109.1 . . ? N1 C7 H07B 109.1 . . ? C6 C7 H07B 109.1 . . ? H07A C7 H07B 107.9 . . ? N1 C8 C9 131(2) . . ? N1 C8 H077 114.6 . . ? C9 C8 H077 114.6 . . ? N5C C8C Mo 176.1(19) . . ? C10 C9 C14 121(2) . . ? C10 C9 C8 119.0(19) . . ? C14 C9 C8 120(2) . . ? O1 C10 C11 119.2(16) . . ? O1 C10 C9 126.0(17) . . ? C11 C10 C9 114.8(18) . . ? C12 C11 C10 122.6(17) . . ? C12 C11 H047 118.7 . . ? C10 C11 H047 118.7 . . ? C11 C12 C13 118.7(18) . . ? C11 C12 H060 120.7 . . ? C13 C12 H060 120.7 . . ? C14 C13 C12 122(3) . . ? C14 C13 H072 119.1 . . ? C12 C13 H072 119.1 . . ? C13 C14 C9 121(3) . . ? C13 C14 H045 119.5 . . ? C9 C14 H045 119.5 . . ? O2 C15 C16 118.9(14) . . ? O2 C15 C20 123.9(13) . . ? C16 C15 C20 117.1(14) . . ? C17 C16 C15 122.6(17) . . ? C17 C16 H070 118.7 . . ? C15 C16 H070 118.7 . . ? C16 C17 C18 121(2) . . ? C16 C17 H041 119.5 . . ? C18 C17 H041 119.5 . . ? C17 C18 C19 118(2) . . ? C17 C18 H061 120.8 . . ? C19 C18 H061 120.8 . . ? C18 C19 C20 123.9(18) . . ? C18 C19 H059 118.0 . . ? C20 C19 H059 118.0 . . ? C21 C20 C19 121.4(14) . . ? C21 C20 C15 121.7(13) . . ? C19 C20 C15 116.9(15) . . ? N4 C21 C20 131.9(13) . . ? N4 C21 H016 114.1 . . ? C20 C21 H016 114.1 . . ? N4 C22 C23 112.0(12) . . ? N4 C22 H02A 109.2 . . ? C23 C22 H02A 109.2 . . ? N4 C22 H02B 109.2 . . ? C23 C22 H02B 109.2 . . ? H02A C22 H02B 107.9 . . ? C22 C23 C24 112.9(15) . . ? C22 C23 H06A 109.0 . . ? C24 C23 H06A 109.0 . . ? C22 C23 H06B 109.0 . . ? C24 C23 H06B 109.0 . . ? H06A C23 H06B 107.8 . . ? N3 C24 C25 123.0(19) . . ? N3 C24 C23 113.0(15) . . ? C25 C24 C23 123.9(18) . . ? C24 C25 C26 116.0(19) . . ? C24 C25 H1A 122.0 . . ? C26 C25 H1A 122.0 . . ? C27 C26 C25 120.8(18) . . ? C27 C26 H075 119.6 . . ? C25 C26 H075 119.6 . . ? C28 C27 C26 118.1(18) . . ? C28 C27 H073 121.0 . . ? C26 C27 H073 121.0 . . ? N3 C28 C27 123.0(17) . . ? N3 C28 H026 118.5 . . ? C27 C28 H026 118.5 . . ? N8 C29 C42 131.6(14) . 2_766 ? N8 C29 H11 114.2 . . ? C42 C29 H11 114.2 2_766 . ? N8 C30 C31 111.6(13) . . ? N8 C30 H02C 109.3 . . ? C31 C30 H02C 109.3 . . ? N8 C30 H02D 109.3 . . ? C31 C30 H02D 109.3 . . ? H02C C30 H02D 108.0 . . ? C30 C31 C32 114.4(12) . . ? C30 C31 H03C 108.7 . . ? C32 C31 H03C 108.7 . . ? C30 C31 H03D 108.7 . . ? C32 C31 H03D 108.7 . . ? H03C C31 H03D 107.6 . . ? N7 C32 C33 118.2(16) . . ? N7 C32 C31 114.4(16) . . ? C33 C32 C31 127.4(17) . . ? C34 C33 C32 121.1(17) . . ? C34 C33 H049 119.5 . . ? C32 C33 H049 119.5 . . ? C35 C34 C33 121(2) . . ? C35 C34 H068 119.5 . . ? C33 C34 H068 119.5 . . ? C34 C35 C36 117.5(19) . . ? C34 C35 H063 121.2 . . ? C36 C35 H063 121.2 . . ? N7 C36 C35 122.9(15) . . ? N7 C36 H032 118.5 . . ? C35 C36 H032 118.5 . . ? O4 C37 C42 120.0(15) . . ? O4 C37 C38 122.9(15) . . ? C42 C37 C38 117.1(15) . . ? C39 C38 C37 119.5(15) . . ? C39 C38 H031 120.3 . . ? C37 C38 H031 120.3 . . ? C40 C39 C38 123.6(16) . . ? C40 C39 H057 118.2 . . ? C38 C39 H057 118.2 . . ? C41 C40 C39 114.6(17) . . ? C41 C40 H058 122.7 . . ? C39 C40 H058 122.7 . . ? C42 C41 C40 126.2(18) . . ? C42 C41 H056 116.9 . . ? C40 C41 H056 116.9 . . ? C41 C42 C37 118.9(16) . . ? C41 C42 C29 117.9(17) . 2_766 ? C37 C42 C29 123.2(15) . 2_766 ? N6 C43 C44 120.8(14) . . ? N6 C43 H021 119.6 . . ? C44 C43 H021 119.6 . . ? C43 C44 C45 118.3(14) . . ? C43 C44 H051 120.8 . . ? C45 C44 H051 120.8 . . ? C46 C45 C44 118.5(15) . . ? C46 C45 H022 120.7 . . ? C44 C45 H022 120.7 . . ? C45 C46 C47 121.0(15) . . ? C45 C46 H030 119.5 . . ? C47 C46 H030 119.5 . . ? N6 C47 C46 119.8(15) . . ? N6 C47 C48 117.1(13) . . ? C46 C47 C48 123.1(14) . . ? C47 C48 C49 112.7(13) . . ? C47 C48 H03E 109.1 . . ? C49 C48 H03E 109.1 . . ? C47 C48 H03F 109.1 . . ? C49 C48 H03F 109.1 . . ? H03E C48 H03F 107.8 . . ? N5 C49 C48 109.3(13) . . ? N5 C49 H03A 109.8 . . ? C48 C49 H03A 109.8 . . ? N5 C49 H03B 109.8 . . ? C48 C49 H03B 109.8 . . ? H03A C49 H03B 108.3 . . ? C55 C050 C51 123.0(19) . . ? C55 C050 H050 118.5 . . ? C51 C050 H050 118.5 . . ? N5 C50 C51 129.9(14) . . ? N5 C50 H011 115.0 . . ? C51 C50 H011 115.0 . . ? C050 C51 C52 118.4(15) . . ? C050 C51 C50 121.3(16) . . ? C52 C51 C50 120.4(14) . . ? O3 C52 C53 119.2(16) . . ? O3 C52 C51 124.2(13) . . ? C53 C52 C51 116.5(16) . . ? C54 C53 C52 122.2(18) . . ? C54 C53 H048 118.9 . . ? C52 C53 H048 118.9 . . ? C53 C54 C55 120.3(19) . . ? C53 C54 H069 119.9 . . ? C55 C54 H069 119.9 . . ? C050 C55 C54 120(2) . . ? C050 C55 H8 120.2 . . ? C54 C55 H8 120.2 . . ? N2C C56 Mo 179.4(13) . . ? N1C C57 Mo 178.5(15) . . ? N3C C58 Mo 174.3(13) . . ? N4C C59 Mo 175.9(18) . . ? N8C C60 Mo 176.2(14) . . ? N7C C61 Mo 179.5(12) . . ? N6C C62 Mo 177.6(18) . . ? O2 Cu1 N2C 91.5(5) . . ? O2 Cu1 N4 94.9(4) . . ? N2C Cu1 N4 160.5(5) . . ? O2 Cu1 N3 151.0(5) . . ? N2C Cu1 N3 92.0(5) . . ? N4 Cu1 N3 91.2(5) . . ? O1 Cu2 N1C 88.6(5) . . ? O1 Cu2 N1 94.7(6) . . ? N1C Cu2 N1 160.6(7) . . ? O1 Cu2 N2 148.3(7) . . ? N1C Cu2 N2 83.9(6) . . ? N1 Cu2 N2 102.6(8) . . ? O3 Cu3 N7C 89.0(4) . . ? O3 Cu3 N5 94.4(5) . . ? N7C Cu3 N5 161.7(5) . . ? O3 Cu3 N6 164.7(5) . . ? N7C Cu3 N6 89.9(5) . . ? N5 Cu3 N6 91.4(5) . . ? O4 Cu4 N8 168.4(5) . . ? O4 Cu4 N8C 94.3(4) . . ? N8 Cu4 N8C 92.9(5) . . ? O4 Cu4 N7 93.0(5) . . ? N8 Cu4 N7 87.8(5) . . ? N8C Cu4 N7 137.5(5) . . ? O4 Cu4 O4 78.9(4) . 2_766 ? N8 Cu4 O4 90.0(4) . 2_766 ? N8C Cu4 O4 112.1(4) . 2_766 ? N7 Cu4 O4 110.4(4) . 2_766 ? C57 Mo C56 72.9(5) . . ? C57 Mo C60 142.4(5) . . ? C56 Mo C60 140.8(5) . . ? C57 Mo C62 118.5(6) . . ? C56 Mo C62 71.6(5) . . ? C60 Mo C62 74.1(6) . . ? C57 Mo C61 141.6(5) . . ? C56 Mo C61 80.8(5) . . ? C60 Mo C61 73.5(5) . . ? C62 Mo C61 77.0(6) . . ? C57 Mo C59 79.7(6) . . ? C56 Mo C59 145.3(6) . . ? C60 Mo C59 72.8(6) . . ? C62 Mo C59 142.1(6) . . ? C61 Mo C59 110.2(5) . . ? C57 Mo C58 75.5(5) . . ? C56 Mo C58 78.3(5) . . ? C60 Mo C58 119.4(5) . . ? C62 Mo C58 139.7(6) . . ? C61 Mo C58 72.2(5) . . ? C59 Mo C58 74.4(6) . . ? C57 Mo C8C 73.2(6) . . ? C56 Mo C8C 112.0(5) . . ? C60 Mo C8C 76.8(5) . . ? C62 Mo C8C 76.0(7) . . ? C61 Mo C8C 144.1(6) . . ? C59 Mo C8C 78.9(6) . . ? C58 Mo C8C 141.8(6) . . ? C8 N1 C7 124(2) . . ? C8 N1 Cu2 120.9(15) . . ? C7 N1 Cu2 114.9(14) . . ? C57 N1C Cu2 168.3(15) . . ? C5 N2 C1 120.0 . . ? C5 N2 Cu2 114.7(13) . . ? C1 N2 Cu2 125.2(13) . . ? C56 N2C Cu1 170.7(13) . . ? C28 N3 C24 118.9(16) . . ? C28 N3 Cu1 115.3(12) . . ? C24 N3 Cu1 124.9(12) . . ? C21 N4 C22 116.8(12) . . ? C21 N4 Cu1 120.2(9) . . ? C22 N4 Cu1 122.8(10) . . ? C50 N5 C49 114.6(12) . . ? C50 N5 Cu3 122.2(10) . . ? C49 N5 Cu3 123.3(10) . . ? C43 N6 C47 121.6(14) . . ? C43 N6 Cu3 114.8(10) . . ? C47 N6 Cu3 123.6(10) . . ? C36 N7 C32 119.3(15) . . ? C36 N7 Cu4 121.8(12) . . ? C32 N7 Cu4 118.1(12) . . ? C61 N7C Cu3 176.5(11) . . ? C29 N8 C30 118.5(13) . . ? C29 N8 Cu4 124.3(10) . . ? C30 N8 Cu4 117.1(10) . . ? C60 N8C Cu4 158.5(13) . . ? C10 O1 Cu2 128.4(10) . . ? C15 O2 Cu1 126.7(9) . . ? C52 O3 Cu3 128.8(10) . . ? C37 O4 Cu4 128.7(9) . . ? C37 O4 Cu4 130.0(9) . 2_766 ? Cu4 O4 Cu4 101.1(4) . 2_766 ? _diffrn_measured_fraction_theta_max 0.691 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.691 _refine_diff_density_max 0.670 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.090 data_max40c _database_code_depnum_ccdc_archive 'CCDC 731835' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H104 Cu8 N32 O22 W2' _chemical_formula_weight 3318.45 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' Cu Cu 0.3201 1.2651 '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' W W -0.8490 6.8722 '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 13.2979(13) _cell_length_b 15.4193(12) _cell_length_c 19.3265(12) _cell_angle_alpha 102.557(6) _cell_angle_beta 99.755(7) _cell_angle_gamma 113.155(16) _cell_volume 3409.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18991 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 2.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7085 _exptl_absorpt_correction_T_max 0.7273 _exptl_absorpt_process_details wingx _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24294 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.2001 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 29.35 _reflns_number_total 14622 _reflns_number_gt 6334 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr. _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14622 _refine_ls_number_parameters 855 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1782 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 2.558 _refine_ls_shift/su_mean 0.072 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1W O 0.6731(13) 0.1036(12) 0.4088(10) 0.197(7) Uani 1 1 d . . . O2W O 0.751(2) 0.0365(16) 0.3104(14) 0.277(11) Uani 1 1 d . . . O3W O 0.3358(13) 0.2767(11) 0.2906(7) 0.171(6) Uani 1 1 d . . . O5W O 0.015(2) 0.6361(13) 0.1906(11) 0.311(16) Uani 1 1 d . . . O7W O 0.0936(19) 0.1454(11) 0.3947(9) 0.222(9) Uani 1 1 d . . . O6W O 0.6852(17) 0.4991(10) 0.1316(14) 0.321(17) Uani 1 1 d . . . O8W O 0.1591(19) 0.038(2) 0.2958(14) 0.328(15) Uani 1 1 d . . . C3C5 C 0.5891(10) 0.4112(11) 0.5890(8) 0.071(4) Uani 1 1 d . . . H3C5 H 0.6340 0.4606 0.6338 0.085 Uiso 1 1 calc R . . C3C3 C 0.5627(12) 0.2738(12) 0.4940(10) 0.085(5) Uani 1 1 d . . . H3C3 H 0.5868 0.2269 0.4754 0.102 Uiso 1 1 calc R . . C3C4 C 0.6266(12) 0.3458(14) 0.5609(10) 0.092(5) Uani 1 1 d . . . H3C4 H 0.6947 0.3492 0.5864 0.111 Uiso 1 1 calc R . . C3C1 C 0.4217(10) 0.3364(8) 0.4824(7) 0.060(3) Uani 1 1 d . . . C3C2 C 0.4623(11) 0.2695(9) 0.4532(8) 0.074(4) Uani 1 1 d . . . H3C2 H 0.4227 0.2224 0.4068 0.089 Uiso 1 1 calc R . . C8D C 0.512(2) 0.8039(16) 0.2865(13) 0.157(8) Uiso 1 1 d . . . H8D1 H 0.5033 0.8124 0.2379 0.189 Uiso 1 1 calc R . . H8D2 H 0.5771 0.8630 0.3203 0.189 Uiso 1 1 calc R . . C7D C 0.4245(15) 0.8792(14) 0.3541(10) 0.096(6) Uani 1 1 d . . . H7D H 0.4961 0.9335 0.3697 0.115 Uiso 1 1 calc R . . C2D C 0.1513(16) 0.8451(11) 0.3886(8) 0.094(5) Uani 1 1 d G . . H2D H 0.0757 0.7972 0.3743 0.112 Uiso 1 1 calc R . . N2D N 0.4136(10) 0.8000(12) 0.3084(9) 0.093(4) Uani 1 1 d . . . C3D C 0.180(2) 0.9351(18) 0.4355(12) 0.136(8) Uiso 1 1 d G . . H3D H 0.1285 0.9533 0.4535 0.163 Uiso 1 1 calc R . . C4D C 0.296(2) 0.9980(15) 0.4542(13) 0.156(14) Uani 1 1 d G . . H4D H 0.3196 1.0578 0.4907 0.187 Uiso 1 1 calc R . . N8 N 0.2030(10) 0.3019(8) 0.1660(7) 0.083(4) Uani 1 1 d . . . C13B C -0.1676(14) -0.2757(11) 0.3182(9) 0.099(5) Uani 1 1 d . . . H13B H -0.1819 -0.3408 0.2958 0.118 Uiso 1 1 calc R . . C11C C 0.0437(13) 0.4872(11) 0.5970(7) 0.080(4) Uani 1 1 d . . . H11C H 0.0561 0.5419 0.6354 0.096 Uiso 1 1 calc R . . C14B C 0.1673(11) -0.0004(10) 0.0141(8) 0.067(4) Uani 1 1 d . . . H14B H 0.2088 0.0086 -0.0202 0.080 Uiso 1 1 calc R . . C5D C 0.375(2) 0.9893(12) 0.4312(11) 0.120(8) Uani 1 1 d G . . H5D H 0.4483 1.0408 0.4443 0.144 Uiso 1 1 calc R . . C11B C -0.1555(18) -0.1500(16) 0.4218(9) 0.137(8) Uani 1 1 d . . . H11B H -0.1625 -0.1309 0.4691 0.165 Uiso 1 1 calc R . . C12B C -0.181(2) -0.2502(15) 0.3884(10) 0.149(9) Uani 1 1 d . . . H12B H -0.2048 -0.2973 0.4127 0.179 Uiso 1 1 calc R . . W1 W -0.02628(4) 0.30533(3) 0.20955(2) 0.03996(14) Uani 1 1 d . . . Cu2 Cu 0.24251(11) 0.40149(9) 0.47435(7) 0.0493(4) Uani 1 1 d . . . Cu3 Cu -0.03767(11) -0.04431(9) 0.19372(7) 0.0467(4) Uani 1 1 d . . . Cu4 Cu -0.45607(12) 0.06224(10) 0.08315(7) 0.0575(4) Uani 1 1 d . . . Cu5 Cu 0.27576(16) 0.67572(11) 0.26649(11) 0.0799(5) Uani 1 1 d . . . C4 C 0.0898(9) 0.3417(7) 0.3161(5) 0.044(3) Uani 1 1 d . . . O1A O -0.4638(7) -0.0587(6) 0.0200(4) 0.064(2) Uani 1 1 d . . . N1B N 0.0443(7) -0.0296(6) 0.1160(4) 0.042(2) Uani 1 1 d . . . N3 N 0.1541(7) 0.3639(6) 0.3718(5) 0.053(2) Uani 1 1 d . . . N2 N -0.0385(8) 0.0851(7) 0.2011(4) 0.048(2) Uani 1 1 d . . . C6 C -0.1246(10) 0.2602(9) 0.2851(6) 0.053(3) Uani 1 1 d . . . N2A N -0.4713(8) 0.1798(7) 0.1299(5) 0.063(3) Uani 1 1 d . . . N2C N 0.3551(7) 0.4841(6) 0.5701(4) 0.050(2) Uani 1 1 d . . . N1C N 0.1148(7) 0.4103(6) 0.5116(5) 0.050(2) Uani 1 1 d . . . O1D O 0.1951(7) 0.7308(6) 0.3166(5) 0.069(2) Uani 1 1 d . . . C7C C 0.1282(10) 0.4884(8) 0.5643(6) 0.052(3) Uani 1 1 d . . . O2B O -0.0778(8) -0.0379(6) 0.2836(4) 0.071(3) Uani 1 1 d . . . N2B N -0.0857(7) -0.1873(6) 0.1678(5) 0.050(2) Uani 1 1 d . . . O1C O 0.3270(6) 0.3338(5) 0.4440(4) 0.063(2) Uani 1 1 d . . . C3B C 0.0093(10) -0.1000(7) 0.0499(6) 0.046(3) Uani 1 1 d . . . C7B C -0.1236(9) -0.2405(8) 0.2087(6) 0.051(3) Uani 1 1 d . . . H7B H -0.1466 -0.3082 0.1893 0.061 Uiso 1 1 calc R . . C1 C -0.0339(8) 0.1611(8) 0.2035(5) 0.040(3) Uani 1 1 d . . . C9A C -0.4325(9) -0.1245(8) 0.0387(6) 0.053(3) Uani 1 1 d . . . C4B C 0.0685(11) -0.0872(9) -0.0011(6) 0.056(3) Uani 1 1 d . . . H4B H 0.0425 -0.1368 -0.0463 0.068 Uiso 1 1 calc R . . C2C C 0.4835(10) 0.4089(9) 0.5538(7) 0.059(3) Uani 1 1 d . . . C8C C 0.0135(10) 0.3291(9) 0.4875(7) 0.062(3) Uani 1 1 d . . . H8C H 0.0034 0.2736 0.4509 0.074 Uiso 1 1 calc R . . C8 C -0.0367(14) 0.3310(9) 0.1032(7) 0.079(4) Uani 1 1 d . . . N1 N -0.2867(8) 0.1386(7) 0.1071(5) 0.062(3) Uani 1 1 d . . . C2B C 0.1373(10) 0.0538(9) 0.1302(6) 0.053(3) Uani 1 1 d . . . H2B H 0.1606 0.1031 0.1752 0.063 Uiso 1 1 calc R . . C7 C 0.1224(12) 0.3030(8) 0.1790(7) 0.057(3) Uani 1 1 d . . . C10A C -0.3778(9) -0.1088(9) 0.1118(6) 0.056(3) Uani 1 1 d . . . H10A H -0.3609 -0.0503 0.1479 0.067 Uiso 1 1 calc R . . C3 C 0.0929(11) 0.4576(10) 0.2424(6) 0.056(3) Uani 1 1 d . . . C8A C -0.6601(11) -0.1005(9) 0.0951(7) 0.063(3) Uani 1 1 d . . . H8A H -0.6641 -0.1323 0.0472 0.075 Uiso 1 1 calc R . . C2A C -0.5044(9) 0.2305(8) 0.0968(7) 0.059(3) Uani 1 1 d . . . H2A H -0.5033 0.2870 0.1270 0.070 Uiso 1 1 calc R . . C6C C 0.2434(11) 0.5778(8) 0.5891(7) 0.067(4) Uani 1 1 d . . . H6C1 H 0.2592 0.5990 0.5468 0.081 Uiso 1 1 calc R . . H6C2 H 0.2410 0.6317 0.6245 0.081 Uiso 1 1 calc R . . C14A C -0.4553(9) -0.2111(8) -0.0157(6) 0.053(3) Uani 1 1 d . . . N6 N -0.1787(9) 0.2344(8) 0.3237(6) 0.071(3) Uani 1 1 d . . . C6B C -0.0861(12) -0.2433(8) 0.0951(7) 0.077(4) Uani 1 1 d . . . H6B1 H -0.1499 -0.3091 0.0782 0.092 Uiso 1 1 calc R . . H6B2 H -0.0164 -0.2508 0.1002 0.092 Uiso 1 1 calc R . . N1A N -0.5705(8) -0.0139(7) 0.1336(5) 0.061(3) Uani 1 1 d . . . C12A C -0.3728(12) -0.2647(11) 0.0785(9) 0.082(4) Uani 1 1 d . . . H12A H -0.3563 -0.3129 0.0923 0.098 Uiso 1 1 calc R . . C6D C 0.3414(14) 0.8925(9) 0.3828(7) 0.071(4) Uani 1 1 d G . . C4A C -0.5615(12) 0.0345(10) 0.2021(7) 0.064(4) Uani 1 1 d . . . C5C C 0.3381(10) 0.5577(9) 0.6238(6) 0.067(4) Uani 1 1 d . . . H5C1 H 0.4081 0.6192 0.6434 0.080 Uiso 1 1 calc R . . H5C2 H 0.3207 0.5333 0.6646 0.080 Uiso 1 1 calc R . . C2 C -0.1943(10) 0.1937(8) 0.1387(6) 0.050(3) Uani 1 1 d . . . C11A C -0.3490(11) -0.1765(11) 0.1313(7) 0.073(4) Uani 1 1 d . . . H11A H -0.3128 -0.1642 0.1805 0.087 Uiso 1 1 calc R . . C3A C -0.4533(11) 0.1310(10) 0.2413(6) 0.080(4) Uani 1 1 d . . . H3A1 H -0.4495 0.1521 0.2932 0.096 Uiso 1 1 calc R . . H3A2 H -0.3880 0.1185 0.2383 0.096 Uiso 1 1 calc R . . C10C C -0.0591(12) 0.4040(11) 0.5719(8) 0.083(4) Uani 1 1 d . . . H10C H -0.1175 0.4011 0.5933 0.099 Uiso 1 1 calc R . . C7A C -0.7453(14) -0.1429(11) 0.1242(9) 0.085(5) Uani 1 1 d . . . H7A H -0.8072 -0.2038 0.0972 0.102 Uiso 1 1 calc R . . C5B C -0.0956(11) -0.1903(9) 0.0377(6) 0.071(4) Uani 1 1 d . . . H5B1 H -0.1137 -0.2356 -0.0112 0.085 Uiso 1 1 calc R . . H5B2 H -0.1580 -0.1728 0.0389 0.085 Uiso 1 1 calc R . . C1C C 0.4515(10) 0.4762(9) 0.5902(6) 0.064(4) Uani 1 1 d . . . H1C H 0.5036 0.5222 0.6345 0.077 Uiso 1 1 calc R . . C9B C -0.1340(11) -0.2072(9) 0.2800(6) 0.062(4) Uani 1 1 d . . . C1B C 0.2026(10) 0.0715(9) 0.0801(7) 0.062(3) Uani 1 1 d . . . H1B H 0.2682 0.1308 0.0919 0.074 Uiso 1 1 calc R . . N5 N -0.1864(11) 0.4255(9) 0.2122(7) 0.097(4) Uani 1 1 d . . . N4 N 0.1601(10) 0.5420(8) 0.2575(6) 0.070(3) Uani 1 1 d . . . C5A C -0.6469(15) -0.0042(12) 0.2338(7) 0.084(5) Uani 1 1 d . . . H5A H -0.6428 0.0301 0.2810 0.101 Uiso 1 1 calc R . . C5 C -0.1288(12) 0.3867(9) 0.2140(7) 0.073(4) Uani 1 1 d . . . C8B C -0.1113(11) -0.1079(10) 0.3151(6) 0.068(4) Uani 1 1 d . . . C6A C -0.7382(14) -0.0938(13) 0.1950(10) 0.088(5) Uani 1 1 d . . . H6A H -0.7957 -0.1217 0.2163 0.106 Uiso 1 1 calc R . . C1A C -0.4449(13) 0.2134(10) 0.2108(6) 0.082(4) Uani 1 1 d . . . H1A1 H -0.4977 0.2381 0.2248 0.098 Uiso 1 1 calc R . . H1A2 H -0.3684 0.2674 0.2317 0.098 Uiso 1 1 calc R . . C9C C -0.0748(12) 0.3263(10) 0.5157(7) 0.072(4) Uani 1 1 d . . . H9C H -0.1456 0.2709 0.4961 0.087 Uiso 1 1 calc R . . N7 N -0.0390(14) 0.3476(9) 0.0486(6) 0.113(5) Uani 1 1 d . . . C1D C 0.2311(11) 0.8207(9) 0.3603(7) 0.056(3) Uani 1 1 d G . . C10B C -0.1220(15) -0.0820(11) 0.3870(8) 0.101(6) Uani 1 1 d . . . H10B H -0.1056 -0.0166 0.4106 0.121 Uiso 1 1 calc R . . C13A C -0.4210(12) -0.2791(9) 0.0057(8) 0.074(4) Uani 1 1 d . . . H13A H -0.4313 -0.3353 -0.0303 0.089 Uiso 1 1 calc R . . C9D C 0.537(3) 0.720(3) 0.283(3) 0.34(3) Uani 1 1 d . . . H9D1 H 0.5396 0.7033 0.3290 0.411 Uiso 1 1 calc R . . H9D2 H 0.6079 0.7307 0.2708 0.411 Uiso 1 1 calc R . . N1D N 0.309(3) 0.6140(18) 0.1880(19) 0.74(6) Uani 1 1 d GU . . C14D C 0.245(2) 0.545(2) 0.119(2) 0.70(6) Uani 1 1 d GU . . H14D H 0.1684 0.5304 0.1008 0.839 Uiso 1 1 calc R . . C13D C 0.294(3) 0.4985(19) 0.0761(17) 1.55(13) Uani 1 1 d GU . . H13D H 0.2512 0.4525 0.0297 1.861 Uiso 1 1 calc R . . C12D C 0.408(3) 0.5206(19) 0.1028(19) 1.53(13) Uani 1 1 d GU . . H12D H 0.4414 0.4893 0.0742 1.841 Uiso 1 1 calc R . . C11D C 0.473(3) 0.5894(15) 0.1721(19) 0.74(8) Uani 1 1 d G . . H11D H 0.5489 0.6041 0.1899 0.890 Uiso 1 1 calc R . . C10D C 0.423(3) 0.6361(11) 0.2147(13) 0.32(3) Uani 1 1 d G . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1W 0.136(12) 0.177(14) 0.220(17) 0.073(13) 0.012(12) 0.024(11) O2W 0.34(3) 0.23(2) 0.32(3) 0.13(2) 0.11(2) 0.16(2) O3W 0.173(13) 0.227(15) 0.093(9) -0.027(9) -0.013(9) 0.130(12) O5W 0.43(3) 0.200(17) 0.23(2) -0.043(14) -0.14(2) 0.22(2) O7W 0.34(3) 0.128(12) 0.155(14) 0.020(10) 0.081(16) 0.075(14) O6W 0.26(2) 0.092(10) 0.43(3) 0.037(14) -0.19(2) 0.041(12) O8W 0.22(2) 0.52(4) 0.26(3) 0.20(3) 0.035(19) 0.15(3) C3C5 0.041(7) 0.101(11) 0.070(9) 0.037(8) 0.019(7) 0.023(8) C3C3 0.053(9) 0.101(11) 0.131(14) 0.068(11) 0.040(10) 0.041(9) C3C4 0.042(8) 0.141(15) 0.109(13) 0.071(12) 0.018(9) 0.040(10) C3C1 0.042(7) 0.043(7) 0.082(9) 0.020(7) 0.014(7) 0.005(6) C3C2 0.068(9) 0.047(8) 0.097(10) 0.014(7) 0.017(8) 0.023(7) C7D 0.059(11) 0.083(12) 0.103(14) 0.043(10) 0.004(10) -0.011(10) C2D 0.126(14) 0.067(10) 0.088(11) 0.010(8) 0.032(11) 0.050(10) N2D 0.060(8) 0.128(12) 0.133(13) 0.087(10) 0.056(9) 0.048(9) C4D 0.28(4) 0.106(17) 0.078(14) 0.009(11) 0.04(2) 0.10(3) N8 0.062(8) 0.074(8) 0.088(9) 0.007(6) 0.038(7) 0.010(7) C13B 0.114(13) 0.079(10) 0.090(11) 0.042(9) 0.043(10) 0.017(9) C11C 0.074(10) 0.121(12) 0.038(7) -0.003(7) 0.010(7) 0.054(10) C14B 0.062(9) 0.085(10) 0.071(9) 0.033(8) 0.033(8) 0.040(8) C5D 0.15(2) 0.052(12) 0.093(15) 0.008(10) 0.003(14) 0.001(11) C11B 0.19(2) 0.133(16) 0.058(10) 0.041(11) 0.052(12) 0.023(15) C12B 0.22(2) 0.107(15) 0.083(13) 0.056(12) 0.054(15) 0.024(15) W1 0.0449(3) 0.0371(2) 0.0292(2) 0.00365(17) 0.00480(19) 0.0156(2) Cu2 0.0431(8) 0.0501(8) 0.0356(7) 0.0023(6) 0.0008(6) 0.0121(7) Cu3 0.0580(9) 0.0414(7) 0.0378(7) 0.0130(6) 0.0183(7) 0.0172(7) Cu4 0.0557(9) 0.0625(9) 0.0373(7) -0.0024(7) -0.0003(7) 0.0247(8) Cu5 0.0997(14) 0.0486(9) 0.1043(14) 0.0315(9) 0.0611(12) 0.0289(9) C4 0.042(6) 0.044(6) 0.035(5) 0.011(5) 0.014(5) 0.008(5) O1A 0.076(6) 0.064(5) 0.039(4) 0.000(4) -0.001(4) 0.032(5) N1B 0.036(5) 0.039(5) 0.037(5) 0.006(4) 0.011(4) 0.007(4) N3 0.040(5) 0.062(6) 0.036(5) 0.008(4) 0.005(4) 0.010(5) N2 0.057(6) 0.038(5) 0.042(5) 0.008(4) 0.013(5) 0.016(5) C6 0.043(7) 0.066(8) 0.034(6) -0.004(6) 0.001(6) 0.021(6) N2A 0.055(6) 0.068(7) 0.042(5) 0.002(5) -0.005(5) 0.021(5) N2C 0.033(5) 0.060(6) 0.036(5) 0.006(4) 0.003(4) 0.007(5) N1C 0.043(6) 0.047(6) 0.038(5) 0.004(4) 0.004(4) 0.007(5) O1D 0.052(5) 0.045(5) 0.095(6) 0.007(5) 0.022(5) 0.012(4) C7C 0.051(7) 0.053(7) 0.037(6) 0.007(5) 0.007(6) 0.013(6) O2B 0.116(7) 0.059(5) 0.043(4) 0.023(4) 0.035(5) 0.035(5) N2B 0.055(6) 0.045(5) 0.042(5) 0.012(4) 0.023(5) 0.014(5) O1C 0.048(5) 0.063(5) 0.063(5) -0.001(4) 0.000(4) 0.026(4) C3B 0.057(7) 0.043(7) 0.038(6) 0.011(5) 0.014(6) 0.023(6) C7B 0.061(7) 0.047(7) 0.051(7) 0.020(6) 0.016(6) 0.029(6) C1 0.033(6) 0.040(6) 0.029(5) 0.002(5) 0.007(5) 0.003(5) C9A 0.037(6) 0.049(7) 0.062(7) 0.016(6) 0.008(6) 0.012(6) C4B 0.063(8) 0.061(8) 0.045(7) 0.019(6) 0.022(6) 0.024(7) C2C 0.044(7) 0.044(7) 0.077(9) 0.024(7) 0.008(7) 0.011(6) C8C 0.051(8) 0.066(8) 0.055(7) 0.021(6) 0.009(7) 0.014(7) C8 0.129(13) 0.055(8) 0.046(7) 0.015(6) 0.017(8) 0.037(8) N1 0.047(6) 0.087(7) 0.031(5) -0.005(5) 0.001(5) 0.024(6) C2B 0.053(7) 0.062(8) 0.044(6) 0.014(5) 0.014(6) 0.028(7) C7 0.064(9) 0.035(7) 0.065(8) 0.013(6) 0.025(8) 0.014(6) C10A 0.043(7) 0.076(8) 0.049(7) 0.022(6) 0.016(6) 0.024(6) C3 0.070(8) 0.066(8) 0.044(6) 0.010(6) 0.017(6) 0.043(7) C8A 0.056(8) 0.064(8) 0.053(7) 0.012(7) 0.006(7) 0.020(7) C2A 0.043(7) 0.050(7) 0.056(7) -0.008(6) 0.019(6) 0.006(6) C6C 0.076(9) 0.053(8) 0.056(7) -0.004(6) 0.020(7) 0.024(7) C14A 0.041(6) 0.045(7) 0.057(7) 0.006(6) 0.012(6) 0.011(6) N6 0.051(7) 0.094(8) 0.045(6) 0.003(6) 0.007(6) 0.023(6) C6B 0.087(10) 0.038(7) 0.083(10) -0.004(7) 0.048(9) 0.008(7) N1A 0.059(6) 0.078(7) 0.043(5) 0.012(5) 0.007(5) 0.035(6) C12A 0.077(10) 0.078(10) 0.102(12) 0.050(10) 0.023(9) 0.036(9) C6D 0.072(10) 0.047(9) 0.066(9) 0.024(7) -0.002(8) 0.005(8) C4A 0.080(10) 0.084(10) 0.039(7) 0.016(7) 0.014(7) 0.050(8) C5C 0.055(8) 0.068(8) 0.045(7) -0.006(6) 0.011(6) 0.010(7) C2 0.045(7) 0.059(7) 0.036(6) 0.002(5) 0.010(5) 0.021(6) C11A 0.068(9) 0.084(10) 0.051(7) 0.023(7) 0.012(7) 0.020(8) C3A 0.071(9) 0.103(11) 0.040(7) -0.002(7) -0.007(7) 0.036(8) C10C 0.054(9) 0.106(11) 0.060(9) 0.011(9) 0.024(8) 0.014(9) C7A 0.073(11) 0.087(11) 0.090(12) 0.031(9) 0.008(10) 0.035(9) C5B 0.079(9) 0.057(8) 0.040(6) 0.002(6) 0.019(7) 0.000(7) C1C 0.040(7) 0.066(9) 0.048(7) 0.015(6) 0.000(6) -0.008(6) C9B 0.071(9) 0.054(8) 0.046(7) 0.024(6) 0.014(6) 0.012(7) C1B 0.041(7) 0.063(8) 0.072(9) 0.021(7) 0.018(7) 0.013(6) N5 0.089(9) 0.108(10) 0.094(9) 0.016(7) 0.002(8) 0.063(8) N4 0.091(8) 0.046(6) 0.075(7) 0.018(5) 0.039(7) 0.026(6) C5A 0.121(14) 0.094(12) 0.047(8) 0.027(8) 0.020(9) 0.055(11) C5 0.070(9) 0.064(8) 0.055(8) 0.006(6) -0.014(7) 0.021(7) C8B 0.071(9) 0.082(10) 0.047(7) 0.033(7) 0.015(7) 0.024(8) C6A 0.095(12) 0.098(12) 0.088(12) 0.047(10) 0.043(11) 0.044(11) C1A 0.097(11) 0.096(11) 0.037(6) -0.005(7) 0.005(7) 0.048(9) C9C 0.056(9) 0.076(10) 0.056(8) 0.015(7) 0.009(7) 0.007(8) N7 0.202(15) 0.108(10) 0.049(7) 0.038(7) 0.037(9) 0.080(10) C1D 0.071(9) 0.054(8) 0.054(7) 0.018(6) 0.019(7) 0.037(7) C10B 0.152(15) 0.085(10) 0.059(9) 0.031(8) 0.052(10) 0.032(10) C13A 0.083(10) 0.058(8) 0.075(9) 0.009(7) 0.024(8) 0.030(8) C9D 0.24(3) 0.49(6) 0.72(9) 0.51(7) 0.39(5) 0.30(4) N1D 0.92(9) 0.14(3) 0.87(12) -0.01(4) 0.80(10) -0.16(4) C14D 0.85(9) 0.11(2) 0.93(12) -0.04(4) 0.84(10) -0.11(4) C13D 1.50(16) 0.31(4) 1.95(18) -0.59(7) 1.67(16) -0.45(6) C12D 1.45(16) 0.33(4) 1.97(18) -0.58(7) 1.66(16) -0.42(6) C11D 1.01(16) 0.18(4) 1.05(15) 0.26(7) 0.81(15) 0.03(7) C10D 0.67(9) 0.047(12) 0.42(5) 0.12(2) 0.46(6) 0.18(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C3C5 C3C4 1.34(2) . ? C3C5 C2C 1.437(16) . ? C3C3 C3C4 1.37(2) . ? C3C3 C3C2 1.400(17) . ? C3C1 O1C 1.330(13) . ? C3C1 C3C2 1.401(17) . ? C3C1 C2C 1.432(17) . ? C8D C9D 1.45(3) . ? C8D N2D 1.42(3) . ? C7D N2D 1.28(2) . ? C7D C6D 1.38(2) . ? C2D C3D 1.34(2) . ? C2D C1D 1.410(19) . ? N2D Cu5 1.936(15) . ? C3D C4D 1.3900 . ? C4D C5D 1.25(3) . ? N8 C7 1.148(15) . ? C13B C12B 1.39(2) . ? C13B C9B 1.392(16) . ? C11C C10C 1.370(18) . ? C11C C7C 1.375(17) . ? C14B C1B 1.360(17) . ? C14B C4B 1.386(16) . ? C5D C6D 1.42(2) . ? C11B C10B 1.34(2) . ? C11B C12B 1.42(2) . ? W1 C3 2.124(14) . ? W1 C1 2.162(12) . ? W1 C4 2.163(10) . ? W1 C6 2.168(14) . ? W1 C7 2.168(15) . ? W1 C2 2.178(11) . ? W1 C8 2.168(13) . ? W1 C5 2.186(16) . ? Cu2 O1C 1.891(8) . ? Cu2 N3 1.955(8) . ? Cu2 N2C 1.956(8) . ? Cu2 N1C 1.993(10) . ? Cu3 O2B 1.895(8) . ? Cu3 N2B 1.955(9) . ? Cu3 N2 1.973(9) . ? Cu3 N1B 2.000(9) . ? Cu4 O1A 1.948(8) . ? Cu4 N2A 1.944(11) . ? Cu4 N1 2.000(10) . ? Cu4 N1A 2.059(11) . ? Cu4 O1A 2.073(7) 2_455 ? Cu5 O1D 1.877(9) . ? Cu5 N4 1.976(11) . ? Cu5 N1D 1.83(2) . ? C4 N3 1.142(11) . ? O1A C9A 1.332(12) . ? O1A Cu4 2.073(7) 2_455 ? N1B C2B 1.319(13) . ? N1B C3B 1.351(12) . ? N2 C1 1.140(11) . ? C6 N6 1.146(14) . ? N2A C2A 1.269(14) . ? N2A C1A 1.468(14) . ? N2C C1C 1.335(15) . ? N2C C5C 1.478(14) . ? N1C C8C 1.345(13) . ? N1C C7C 1.325(14) . ? O1D C1D 1.303(13) . ? C7C C6C 1.510(15) . ? O2B C8B 1.316(13) . ? N2B C7B 1.282(12) . ? N2B C6B 1.478(14) . ? C3B C4B 1.363(15) . ? C3B C5B 1.470(15) . ? C7B C9B 1.414(16) . ? C9A C10A 1.396(14) . ? C9A C14A 1.394(15) . ? C2C C1C 1.373(17) . ? C8C C9C 1.365(18) . ? C8 N7 1.138(14) . ? N1 C2 1.141(12) . ? C2B C1B 1.407(16) . ? C10A C11A 1.347(16) . ? C3 N4 1.187(13) . ? C8A N1A 1.331(14) . ? C8A C7A 1.348(19) . ? C2A C14A 1.489(16) 2_455 ? C6C C5C 1.497(16) . ? C14A C13A 1.408(16) . ? C14A C2A 1.489(16) 2_455 ? C6B C5B 1.531(17) . ? N1A C4A 1.331(14) . ? C12A C13A 1.373(18) . ? C12A C11A 1.393(19) . ? C6D C1D 1.365(18) . ? C4A C5A 1.371(19) . ? C4A C3A 1.522(17) . ? C3A C1A 1.486(17) . ? C10C C9C 1.349(18) . ? C7A C6A 1.38(2) . ? C9B C8B 1.418(17) . ? N5 C5 1.142(16) . ? C5A C6A 1.366(19) . ? C8B C10B 1.407(18) . ? C9D C10D 1.66(5) . ? N1D C14D 1.3900 . ? N1D C10D 1.3900 . ? C14D C13D 1.3900 . ? C13D C12D 1.3900 . ? C12D C11D 1.3900 . ? C11D C10D 1.3900 . ? 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 C3C4 C3C5 C2C 123.6(14) . . ? C3C4 C3C3 C3C2 121.6(15) . . ? C3C5 C3C4 C3C3 119.0(13) . . ? O1C C3C1 C3C2 120.5(11) . . ? O1C C3C1 C2C 119.8(12) . . ? C3C2 C3C1 C2C 119.7(12) . . ? C3C1 C3C2 C3C3 119.8(14) . . ? C9D C8D N2D 118(2) . . ? N2D C7D C6D 127.0(15) . . ? C3D C2D C1D 122.4(18) . . ? C7D N2D C8D 116.9(18) . . ? C7D N2D Cu5 125.9(13) . . ? C8D N2D Cu5 117.2(15) . . ? C4D C3D C2D 113(2) . . ? C3D C4D C5D 132(2) . . ? C12B C13B C9B 122.4(16) . . ? C10C C11C C7C 118.6(13) . . ? C1B C14B C4B 118.7(13) . . ? C6D C5D C4D 113(2) . . ? C10B C11B C12B 121.7(17) . . ? C13B C12B C11B 117.5(15) . . ? C3 W1 C1 141.0(4) . . ? C3 W1 C4 71.6(4) . . ? C1 W1 C4 80.1(3) . . ? C3 W1 C6 116.3(4) . . ? C1 W1 C6 77.3(4) . . ? C4 W1 C6 71.1(4) . . ? C3 W1 C7 75.9(4) . . ? C1 W1 C7 72.4(4) . . ? C4 W1 C7 78.2(4) . . ? C6 W1 C7 139.9(4) . . ? C3 W1 C2 144.6(4) . . ? C1 W1 C2 72.5(4) . . ? C4 W1 C2 140.2(4) . . ? C6 W1 C2 75.1(4) . . ? C7 W1 C2 118.3(4) . . ? C3 W1 C8 79.4(4) . . ? C1 W1 C8 112.0(4) . . ? C4 W1 C8 143.6(5) . . ? C6 W1 C8 143.7(5) . . ? C7 W1 C8 73.6(5) . . ? C2 W1 C8 74.9(5) . . ? C3 W1 C5 74.7(5) . . ? C1 W1 C5 142.6(5) . . ? C4 W1 C5 112.5(4) . . ? C6 W1 C5 74.4(5) . . ? C7 W1 C5 143.1(5) . . ? C2 W1 C5 77.0(4) . . ? C8 W1 C5 79.4(5) . . ? O1C Cu2 N3 90.7(4) . . ? O1C Cu2 N2C 94.7(4) . . ? N3 Cu2 N2C 159.6(4) . . ? O1C Cu2 N1C 152.9(4) . . ? N3 Cu2 N1C 91.6(4) . . ? N2C Cu2 N1C 92.5(4) . . ? O2B Cu3 N2B 93.1(4) . . ? O2B Cu3 N2 88.0(4) . . ? N2B Cu3 N2 162.0(4) . . ? O2B Cu3 N1B 165.6(4) . . ? N2B Cu3 N1B 93.0(4) . . ? N2 Cu3 N1B 90.2(4) . . ? O1A Cu4 N2A 168.8(3) . . ? O1A Cu4 N1 94.7(4) . . ? N2A Cu4 N1 92.3(4) . . ? O1A Cu4 N1A 93.1(4) . . ? N2A Cu4 N1A 87.6(4) . . ? N1 Cu4 N1A 136.7(4) . . ? O1A Cu4 O1A 78.8(4) . 2_455 ? N2A Cu4 O1A 90.6(3) . 2_455 ? N1 Cu4 O1A 111.0(4) . 2_455 ? N1A Cu4 O1A 112.3(3) . 2_455 ? O1D Cu5 N2D 91.0(5) . . ? O1D Cu5 N4 89.0(4) . . ? N2D Cu5 N4 158.7(5) . . ? O1D Cu5 N1D 157.7(14) . . ? N2D Cu5 N1D 101.1(11) . . ? N4 Cu5 N1D 86.3(8) . . ? N3 C4 W1 177.3(9) . . ? C9A O1A Cu4 129.3(7) . . ? C9A O1A Cu4 129.4(7) . 2_455 ? Cu4 O1A Cu4 101.2(4) . 2_455 ? C2B N1B C3B 118.3(10) . . ? C2B N1B Cu3 118.0(7) . . ? C3B N1B Cu3 123.7(7) . . ? C4 N3 Cu2 170.1(9) . . ? C1 N2 Cu3 176.1(9) . . ? N6 C6 W1 178.3(10) . . ? C2A N2A C1A 115.7(11) . . ? C2A N2A Cu4 126.0(8) . . ? C1A N2A Cu4 118.3(8) . . ? C1C N2C C5C 116.7(9) . . ? C1C N2C Cu2 121.2(8) . . ? C5C N2C Cu2 122.1(7) . . ? C8C N1C C7C 118.5(11) . . ? C8C N1C Cu2 118.0(8) . . ? C7C N1C Cu2 123.1(8) . . ? C1D O1D Cu5 128.9(8) . . ? N1C C7C C11C 122.2(11) . . ? N1C C7C C6C 116.3(12) . . ? C11C C7C C6C 121.4(12) . . ? C8B O2B Cu3 128.7(8) . . ? C7B N2B C6B 114.7(9) . . ? C7B N2B Cu3 124.6(8) . . ? C6B N2B Cu3 120.6(7) . . ? C3C1 O1C Cu2 129.4(8) . . ? N1B C3B C4B 121.7(10) . . ? N1B C3B C5B 115.3(10) . . ? C4B C3B C5B 123.0(10) . . ? N2B C7B C9B 127.0(10) . . ? N2 C1 W1 179.2(9) . . ? O1A C9A C10A 121.3(11) . . ? O1A C9A C14A 119.4(10) . . ? C10A C9A C14A 119.3(11) . . ? C3B C4B C14B 120.1(11) . . ? C1C C2C C3C1 125.9(11) . . ? C1C C2C C3C5 118.0(12) . . ? C3C1 C2C C3C5 116.1(13) . . ? N1C C8C C9C 121.4(12) . . ? N7 C8 W1 177.7(14) . . ? C2 N1 Cu4 160.9(9) . . ? N1B C2B C1B 122.8(11) . . ? N8 C7 W1 176.9(12) . . ? C11A C10A C9A 121.5(12) . . ? N4 C3 W1 176.9(10) . . ? N1A C8A C7A 121.3(13) . . ? N2A C2A C14A 128.2(11) . 2_455 ? C5C C6C C7C 113.0(10) . . ? C9A C14A C13A 118.1(11) . . ? C9A C14A C2A 125.1(11) . 2_455 ? C13A C14A C2A 116.0(11) . 2_455 ? N2B C6B C5B 111.3(10) . . ? C4A N1A C8A 121.4(12) . . ? C4A N1A Cu4 116.8(9) . . ? C8A N1A Cu4 120.8(9) . . ? C13A C12A C11A 118.7(12) . . ? C7D C6D C5D 115.8(18) . . ? C7D C6D C1D 122.0(14) . . ? C5D C6D C1D 121.9(19) . . ? N1A C4A C5A 119.8(13) . . ? N1A C4A C3A 116.5(13) . . ? C5A C4A C3A 123.8(12) . . ? N2C C5C C6C 111.8(9) . . ? N1 C2 W1 173.1(10) . . ? C10A C11A C12A 120.6(12) . . ? C1A C3A C4A 114.3(10) . . ? C9C C10C C11C 119.3(14) . . ? C8A C7A C6A 118.3(15) . . ? C3B C5B C6B 113.1(10) . . ? N2C C1C C2C 128.3(10) . . ? C13B C9B C7B 118.0(13) . . ? C13B C9B C8B 118.3(13) . . ? C7B C9B C8B 123.7(10) . . ? C14B C1B C2B 118.4(12) . . ? C3 N4 Cu5 170.5(10) . . ? C6A C5A C4A 119.1(14) . . ? N5 C5 W1 176.0(11) . . ? O2B C8B C10B 118.4(13) . . ? O2B C8B C9B 122.5(12) . . ? C10B C8B C9B 119.1(12) . . ? C5A C6A C7A 120.1(15) . . ? N2A C1A C3A 111.0(10) . . ? C10C C9C C8C 119.9(13) . . ? O1D C1D C6D 124.9(13) . . ? O1D C1D C2D 117.8(12) . . ? C6D C1D C2D 117.3(14) . . ? C11B C10B C8B 121.0(16) . . ? C12A C13A C14A 121.7(12) . . ? C8D C9D C10D 97(2) . . ? C14D N1D C10D 120.0 . . ? C14D N1D Cu5 135(2) . . ? C10D N1D Cu5 105(2) . . ? N1D C14D C13D 120.0 . . ? C12D C13D C14D 120.0 . . ? C13D C12D C11D 120.0 . . ? C10D C11D C12D 120.0 . . ? C11D C10D N1D 120.0 . . ? C11D C10D C9D 101(3) . . ? N1D C10D C9D 139(2) . . ? _diffrn_measured_fraction_theta_max 0.780 _diffrn_reflns_theta_full 29.35 _diffrn_measured_fraction_theta_full 0.780 _refine_diff_density_max 1.371 _refine_diff_density_min -1.016 _refine_diff_density_rms 0.121