# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Spontaneous resolution of 3D chiral polyoxometalate-based polythreaded framework consisting of achiral ligand ; _publ_contact_author_name 'Prof. Zhong-Min Su' _publ_contact_author_email ZMSU@NENU.EDU.CN loop_ _publ_author_name 'Zhong-Min Su' 'Ya-Qian Lan' 'Shun-Li Li' 'Jian-Fang Ma' 'Kuizhan Shao' ; Xin-Long Wang ; 'Enbo Wang' # Attachment 'D-1-right658056.cif' data_mm_right _database_code_depnum_ccdc_archive 'CCDC 658056' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H58 Cu3 N16 O27 V10' _chemical_formula_weight 1895.04 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' V V 0.3005 0.5294 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M I222 _symmetry_space_group_name_Hall I22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 23.0670(14) _cell_length_b 23.1760(14) _cell_length_c 24.9480(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13337.2(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 25.02 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7544 _exptl_absorpt_coefficient_mu 2.353 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.499 _exptl_absorpt_correction_T_max 0.582 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33818 _diffrn_reflns_av_R_equivalents 0.0841 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.02 _reflns_number_total 11790 _reflns_number_gt 8234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 11790 _refine_ls_number_parameters 801 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1269 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 V1 V 0.75295(5) 0.74557(5) 0.03474(4) 0.0231(3) Uani 1 1 d . . . V2 V 0.72014(6) 0.60116(6) 0.07794(5) 0.0357(3) Uani 1 1 d . . . V3 V 0.89381(6) 0.70875(7) 0.08259(5) 0.0348(3) Uani 1 1 d . . . V4 V 0.78357(7) 0.88293(6) 0.09021(5) 0.0361(3) Uani 1 1 d . . . V5 V 0.67049(6) 0.85404(6) 0.16792(6) 0.0409(4) Uani 1 1 d . . . V6 V 0.61018(6) 0.77339(7) 0.08487(6) 0.0372(4) Uani 1 1 d . . . V7 V 0.62520(6) 0.65439(7) 0.15916(6) 0.0390(4) Uani 1 1 d . . . V8 V 0.74703(5) 0.72757(5) 0.21120(5) 0.0280(3) Uani 1 1 d . . . V9 V 0.82829(6) 0.61027(6) 0.15877(6) 0.0371(4) Uani 1 1 d . . . V10 V 0.86790(6) 0.80938(7) 0.16517(6) 0.0389(4) Uani 1 1 d . . . Cu1 Cu 0.74863(4) 0.75520(4) -0.12188(3) 0.0264(2) Uani 1 1 d . . . Cu2 Cu 0.48410(6) 0.56872(6) 0.22735(5) 0.0650(4) Uani 1 1 d . . . Cu3 Cu 0.93194(6) 0.48057(6) 0.22851(5) 0.0686(4) Uani 1 1 d . . . C1 C 0.6286(3) 0.7459(4) -0.1649(3) 0.045(2) Uani 1 1 d . . . H1 H 0.6421 0.7316 -0.1974 0.055 Uiso 1 1 calc R . . C2 C 0.6260(3) 0.7775(4) -0.0837(3) 0.037(2) Uani 1 1 d . . . H2 H 0.6373 0.7896 -0.0497 0.045 Uiso 1 1 calc R . . C3 C 0.5698(4) 0.7754(4) -0.1021(4) 0.052(3) Uani 1 1 d . . . H3 H 0.5365 0.7853 -0.0832 0.063 Uiso 1 1 calc R . . C4 C 0.5257(4) 0.7484(6) -0.1912(3) 0.061(3) Uani 1 1 d . . . H4A H 0.4908 0.7396 -0.1710 0.073 Uiso 1 1 calc R . . H4B H 0.5338 0.7156 -0.2141 0.073 Uiso 1 1 calc R . . C5 C 0.5144(5) 0.7999(6) -0.2255(4) 0.083(4) Uani 1 1 d . . . H5A H 0.5489 0.8077 -0.2467 0.100 Uiso 1 1 calc R . . H5B H 0.5078 0.8330 -0.2026 0.100 Uiso 1 1 calc R . . C6 C 0.4625(5) 0.7934(6) -0.2637(5) 0.089(4) Uiso 1 1 d . . . H6A H 0.4277 0.7875 -0.2426 0.106 Uiso 1 1 calc R . . H6B H 0.4576 0.8291 -0.2835 0.106 Uiso 1 1 calc R . . C7 C 0.4681(5) 0.7472(5) -0.3008(4) 0.072(3) Uiso 1 1 d . . . H7A H 0.4652 0.7108 -0.2817 0.086 Uiso 1 1 calc R . . H7B H 0.5060 0.7489 -0.3175 0.086 Uiso 1 1 calc R . . C8 C 0.3648(4) 0.7408(5) -0.3327(4) 0.059(3) Uiso 1 1 d . . . H8 H 0.3495 0.7310 -0.2995 0.071 Uiso 1 1 calc R . . C9 C 0.3730(4) 0.7598(4) -0.4162(3) 0.042(2) Uiso 1 1 d . . . H9 H 0.3633 0.7646 -0.4521 0.051 Uiso 1 1 calc R . . C10 C 0.4274(4) 0.7635(4) -0.3959(3) 0.047(2) Uiso 1 1 d . . . H10 H 0.4610 0.7734 -0.4143 0.057 Uiso 1 1 calc R . . C11 C 0.7533(5) 0.6387(4) -0.1734(3) 0.059(3) Uani 1 1 d . . . H11 H 0.7643 0.6540 -0.2063 0.071 Uiso 1 1 calc R . . C12 C 0.7316(4) 0.6303(4) -0.0912(3) 0.040(2) Uani 1 1 d . . . H12 H 0.7251 0.6390 -0.0553 0.048 Uiso 1 1 calc R . . C13 C 0.7294(4) 0.5767(4) -0.1123(3) 0.046(2) Uani 1 1 d . . . H13 H 0.7197 0.5428 -0.0945 0.055 Uiso 1 1 calc R . . C14 C 0.7463(6) 0.5365(4) -0.2046(4) 0.078(4) Uani 1 1 d . . . H14A H 0.7386 0.4998 -0.1873 0.094 Uiso 1 1 calc R . . H14B H 0.7851 0.5348 -0.2197 0.094 Uiso 1 1 calc R . . C15 C 0.7040(5) 0.5451(5) -0.2487(4) 0.070(3) Uani 1 1 d . . . H15A H 0.7147 0.5789 -0.2694 0.084 Uiso 1 1 calc R . . H15B H 0.6657 0.5516 -0.2337 0.084 Uiso 1 1 calc R . . C16 C 0.7023(5) 0.4926(5) -0.2854(4) 0.076(3) Uiso 1 1 d . . . H16A H 0.6903 0.4595 -0.2643 0.091 Uiso 1 1 calc R . . H16B H 0.6728 0.4990 -0.3124 0.091 Uiso 1 1 calc R . . C17 C 0.7564(6) 0.4782(4) -0.3124(3) 0.066(3) Uani 1 1 d . . . H17A H 0.7850 0.4680 -0.2856 0.079 Uiso 1 1 calc R . . H17B H 0.7704 0.5124 -0.3309 0.079 Uiso 1 1 calc R . . C18 C 0.7600(4) 0.3749(4) -0.3390(4) 0.050(2) Uiso 1 1 d . . . H18 H 0.7722 0.3619 -0.3056 0.060 Uiso 1 1 calc R . . C19 C 0.7332(4) 0.4324(5) -0.4038(4) 0.059(3) Uiso 1 1 d . . . H19 H 0.7237 0.4651 -0.4236 0.070 Uiso 1 1 calc R . . C20 C 0.7313(3) 0.3771(4) -0.4204(3) 0.040(2) Uiso 1 1 d . . . H20 H 0.7201 0.3652 -0.4545 0.048 Uiso 1 1 calc R . . C21 C 0.4522(4) 0.6050(5) 0.1248(4) 0.059(3) Uani 1 1 d . . . H21 H 0.4681 0.6412 0.1315 0.071 Uiso 1 1 calc R . . C22 C 0.4240(4) 0.5187(5) 0.1331(5) 0.069(3) Uani 1 1 d . . . H22 H 0.4176 0.4826 0.1481 0.083 Uiso 1 1 calc R . . C23 C 0.4078(5) 0.5340(5) 0.0837(5) 0.070(3) Uani 1 1 d . . . H23 H 0.3878 0.5121 0.0587 0.084 Uiso 1 1 calc R . . C24 C 0.4238(6) 0.6271(6) 0.0294(4) 0.098(5) Uani 1 1 d . . . H24A H 0.3866 0.6203 0.0125 0.118 Uiso 1 1 calc R . . H24B H 0.4247 0.6671 0.0408 0.118 Uiso 1 1 calc R . . C25 C 0.4703(5) 0.6184(6) -0.0115(5) 0.090(4) Uani 1 1 d . . . H25A H 0.4675 0.6488 -0.0381 0.108 Uiso 1 1 calc R . . H25B H 0.4637 0.5819 -0.0296 0.108 Uiso 1 1 calc R . . C26 C 0.4815(5) 0.5754(4) 0.3423(4) 0.058(3) Uani 1 1 d . . . H26 H 0.4419 0.5680 0.3436 0.070 Uiso 1 1 calc R . . C27 C 0.5659(5) 0.5900(7) 0.3131(5) 0.095(5) Uani 1 1 d . . . H27 H 0.5969 0.5949 0.2898 0.114 Uiso 1 1 calc R . . C28 C 0.5691(6) 0.5949(9) 0.3670(5) 0.139(8) Uani 1 1 d . . . H28 H 0.6018 0.6028 0.3875 0.167 Uiso 1 1 calc R . . C29 C 0.4941(7) 0.5835(7) 0.4414(4) 0.115(6) Uani 1 1 d . . . H29A H 0.4523 0.5790 0.4426 0.138 Uiso 1 1 calc R . . H29B H 0.5111 0.5498 0.4582 0.138 Uiso 1 1 calc R . . C30 C 0.5098(9) 0.6334(6) 0.4713(5) 0.134(7) Uani 1 1 d . . . H30A H 0.4936 0.6671 0.4537 0.161 Uiso 1 1 calc R . . H30B H 0.5517 0.6372 0.4706 0.161 Uiso 1 1 calc R . . C31 C 0.9276(5) 0.4791(5) 0.3426(4) 0.067(3) Uani 1 1 d . . . H31 H 0.9356 0.4398 0.3443 0.080 Uiso 1 1 calc R . . C32 C 0.9116(6) 0.5624(6) 0.3125(5) 0.089(4) Uani 1 1 d . . . H32 H 0.9060 0.5935 0.2894 0.107 Uiso 1 1 calc R . . C33 C 0.9069(8) 0.5647(6) 0.3664(6) 0.128(6) Uani 1 1 d . . . H33 H 0.8984 0.5972 0.3868 0.154 Uiso 1 1 calc R . . C34 C 0.9150(10) 0.4933(7) 0.4422(5) 0.153(9) Uani 1 1 d . . . H34A H 0.9158 0.4514 0.4432 0.183 Uiso 1 1 calc R . . H34B H 0.9500 0.5069 0.4597 0.183 Uiso 1 1 calc R . . C35 C 0.8692(7) 0.5113(15) 0.4712(6) 0.265(19) Uani 1 1 d . . . H35A H 0.8338 0.4987 0.4535 0.318 Uiso 1 1 calc R . . H35B H 0.8690 0.5531 0.4719 0.318 Uiso 1 1 calc R . . C36 C 0.8935(5) 0.4515(4) 0.1248(4) 0.059(3) Uani 1 1 d . . . H36 H 0.8570 0.4666 0.1321 0.071 Uiso 1 1 calc R . . C37 C 0.9831(5) 0.4229(5) 0.1325(5) 0.077(4) Uani 1 1 d . . . H37 H 1.0197 0.4158 0.1467 0.092 Uiso 1 1 calc R . . C38 C 0.9651(6) 0.4084(5) 0.0829(6) 0.077(4) Uani 1 1 d . . . H38 H 0.9866 0.3891 0.0569 0.092 Uiso 1 1 calc R . . C39 C 0.8719(6) 0.4247(6) 0.0307(5) 0.097(5) Uani 1 1 d . . . H39A H 0.8319 0.4278 0.0422 0.116 Uiso 1 1 calc R . . H39B H 0.8767 0.3872 0.0139 0.116 Uiso 1 1 calc R . . C40 C 0.8832(6) 0.4703(5) -0.0105(5) 0.086(4) Uani 1 1 d . . . H40A H 0.9206 0.4628 -0.0270 0.104 Uiso 1 1 calc R . . H40B H 0.8540 0.4674 -0.0383 0.104 Uiso 1 1 calc R . . N1 N 0.6629(3) 0.7589(3) -0.1237(2) 0.0340(16) Uani 1 1 d . . . N2 N 0.5729(3) 0.7557(4) -0.1544(3) 0.049(2) Uani 1 1 d . . . N3 N 0.4225(3) 0.7495(4) -0.3430(3) 0.057(2) Uiso 1 1 d . . . N4 N 0.3347(3) 0.7482(3) -0.3763(3) 0.0347(16) Uiso 1 1 d . . . N5 N 0.7447(3) 0.6697(3) -0.1297(2) 0.0344(16) Uani 1 1 d . . . N6 N 0.7442(4) 0.5823(3) -0.1645(3) 0.052(2) Uani 1 1 d . . . N7 N 0.7521(3) 0.4304(3) -0.3517(3) 0.0497(19) Uiso 1 1 d . . . N8 N 0.7482(3) 0.3411(3) -0.3800(2) 0.0350(15) Uiso 1 1 d . . . N9 N 0.4510(3) 0.5635(4) 0.1587(3) 0.057(2) Uani 1 1 d . . . N10 N 0.4276(4) 0.5895(4) 0.0785(3) 0.064(2) Uani 1 1 d . . . N11 N 0.5106(4) 0.5767(4) 0.2976(3) 0.060(2) Uani 1 1 d . . . N12 N 0.5125(4) 0.5854(4) 0.3852(3) 0.076(3) Uani 1 1 d . . . N13 N 0.9169(5) 0.5119(5) 0.3847(4) 0.085(3) Uani 1 1 d . . . N14 N 0.9254(4) 0.5094(4) 0.2974(3) 0.065(2) Uani 1 1 d . . . N15 N 0.9373(4) 0.4507(4) 0.1590(3) 0.058(2) Uani 1 1 d . . . N16 N 0.9091(4) 0.4272(4) 0.0780(3) 0.063(2) Uani 1 1 d . . . O1 O 0.7480(2) 0.7448(2) -0.02890(16) 0.0347(12) Uani 1 1 d . . . O2 O 0.5641(3) 0.7841(3) 0.0370(2) 0.0641(19) Uani 1 1 d . . . O3 O 0.7966(3) 0.9368(2) 0.0509(2) 0.0543(17) Uani 1 1 d . . . O4 O 0.6509(3) 0.8906(3) 0.2183(3) 0.073(2) Uani 1 1 d . . . O5 O 0.9433(2) 0.6964(3) 0.0390(2) 0.0536(18) Uani 1 1 d . . . O6 O 0.9001(3) 0.8253(3) 0.2203(2) 0.065(2) Uani 1 1 d . . . O7 O 0.8570(3) 0.5638(3) 0.1984(2) 0.0557(17) Uani 1 1 d . . . O8 O 0.7532(2) 0.7353(2) 0.27436(18) 0.0389(13) Uani 1 1 d . . . O9 O 0.5758(3) 0.6257(3) 0.1964(2) 0.0589(19) Uani 1 1 d . . . O10 O 0.7087(3) 0.5628(3) 0.0257(2) 0.067(2) Uani 1 1 d . . . O11 O 0.5910(2) 0.7089(3) 0.1190(2) 0.0424(15) Uani 1 1 d . . . O12 O 0.6081(2) 0.8350(3) 0.1295(2) 0.0446(15) Uani 1 1 d . . . O13 O 0.7200(3) 0.8968(3) 0.1286(2) 0.0464(15) Uani 1 1 d . . . O14 O 0.6769(3) 0.7673(3) 0.0594(2) 0.0522(17) Uani 1 1 d . . . O15 O 0.8451(2) 0.8749(3) 0.1336(2) 0.0454(15) Uani 1 1 d . . . O16 O 0.7760(3) 0.8234(3) 0.0529(2) 0.0435(15) Uani 1 1 d . . . O17 O 0.8321(2) 0.7240(2) 0.0493(2) 0.0424(14) Uani 1 1 d . . . O18 O 0.8099(3) 0.7679(3) 0.1786(3) 0.067(2) Uani 1 1 d . . . O19 O 0.7332(3) 0.6701(3) 0.0600(2) 0.0565(18) Uani 1 1 d . . . O20 O 0.7032(3) 0.7939(3) 0.1895(3) 0.066(2) Uani 1 1 d . . . O21 O 0.6768(2) 0.6833(3) 0.1985(2) 0.0469(15) Uani 1 1 d . . . O22 O 0.6560(2) 0.5989(2) 0.1175(2) 0.0462(16) Uani 1 1 d . . . O23 O 0.7814(2) 0.5721(2) 0.1140(2) 0.0418(14) Uani 1 1 d . . . O24 O 0.7892(3) 0.6573(3) 0.1953(2) 0.0492(16) Uani 1 1 d . . . O25 O 0.8851(2) 0.6455(3) 0.1229(2) 0.0483(16) Uani 1 1 d . . . O26 O 0.9162(2) 0.7694(3) 0.1225(2) 0.0460(15) Uani 1 1 d . . . O1W O 0.8869(6) 0.0000 0.0000 0.140(6) Uani 1 2 d S . . O2W O 0.5000 0.8830(6) 0.0000 0.140(6) Uani 1 2 d S . . 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 V1 0.0233(6) 0.0251(7) 0.0207(6) 0.0008(5) -0.0001(5) -0.0002(6) V2 0.0466(9) 0.0275(8) 0.0330(8) 0.0023(6) 0.0008(7) -0.0045(7) V3 0.0226(7) 0.0471(9) 0.0346(8) 0.0018(7) -0.0003(6) 0.0045(7) V4 0.0489(9) 0.0232(8) 0.0362(8) 0.0012(6) -0.0043(7) -0.0043(7) V5 0.0444(9) 0.0391(9) 0.0393(9) 0.0002(7) -0.0018(7) 0.0131(7) V6 0.0244(7) 0.0527(10) 0.0344(8) -0.0019(7) 0.0025(6) 0.0057(7) V7 0.0314(8) 0.0503(10) 0.0352(9) 0.0009(7) 0.0034(7) -0.0127(7) V8 0.0284(7) 0.0318(7) 0.0239(7) 0.0028(5) 0.0007(6) -0.0005(7) V9 0.0430(9) 0.0332(9) 0.0351(8) 0.0026(6) 0.0039(7) 0.0095(7) V10 0.0356(8) 0.0441(9) 0.0369(9) 0.0045(7) 0.0010(7) -0.0056(7) Cu1 0.0241(4) 0.0264(5) 0.0287(5) 0.0006(4) -0.0005(4) 0.0004(5) Cu2 0.0700(9) 0.0755(10) 0.0494(8) 0.0012(7) -0.0061(7) 0.0056(8) Cu3 0.0743(9) 0.0766(10) 0.0548(8) -0.0074(7) -0.0004(7) -0.0055(8) C1 0.025(4) 0.084(7) 0.027(4) -0.008(5) 0.016(4) 0.001(5) C2 0.029(4) 0.059(6) 0.025(4) -0.004(4) -0.004(4) 0.015(4) C3 0.026(5) 0.087(8) 0.043(6) -0.013(5) 0.013(4) 0.008(5) C4 0.027(5) 0.114(10) 0.042(6) -0.001(6) 0.000(4) 0.002(6) C5 0.063(7) 0.110(11) 0.076(8) 0.001(7) -0.047(6) 0.002(7) C11 0.106(9) 0.038(6) 0.035(5) -0.001(4) 0.006(6) 0.009(6) C12 0.049(6) 0.033(5) 0.038(5) -0.008(4) 0.007(4) -0.002(4) C13 0.068(6) 0.024(5) 0.045(5) 0.005(4) 0.002(5) -0.008(4) C14 0.150(11) 0.025(5) 0.060(7) -0.004(4) -0.012(8) 0.017(7) C15 0.097(9) 0.065(8) 0.048(7) -0.031(5) 0.015(6) -0.006(7) C17 0.119(10) 0.028(5) 0.051(6) -0.009(4) -0.013(6) -0.029(6) C21 0.069(7) 0.052(7) 0.056(7) -0.014(5) -0.025(6) 0.007(6) C22 0.056(7) 0.052(8) 0.100(10) -0.013(6) -0.010(7) -0.001(6) C23 0.056(7) 0.067(8) 0.086(9) -0.037(7) -0.010(7) 0.002(6) C24 0.117(12) 0.122(13) 0.056(8) 0.004(7) -0.020(8) 0.033(10) C25 0.096(10) 0.117(12) 0.056(8) -0.009(7) -0.019(7) 0.009(9) C26 0.055(6) 0.063(7) 0.057(7) 0.002(5) 0.002(6) -0.001(6) C27 0.063(8) 0.173(16) 0.050(8) -0.008(8) 0.006(6) 0.007(9) C28 0.060(9) 0.30(3) 0.055(9) -0.011(11) 0.000(7) 0.010(12) C29 0.134(13) 0.163(17) 0.046(8) 0.014(9) 0.040(8) 0.008(12) C30 0.25(2) 0.072(11) 0.078(11) -0.006(7) 0.058(12) 0.025(12) C31 0.071(8) 0.073(8) 0.056(7) -0.006(6) -0.002(6) -0.018(6) C32 0.158(13) 0.062(9) 0.047(8) -0.006(6) -0.011(7) -0.023(9) C33 0.25(2) 0.066(10) 0.069(10) -0.012(8) -0.017(11) 0.006(12) C34 0.31(3) 0.108(13) 0.040(8) 0.003(8) -0.009(12) -0.014(16) C35 0.069(11) 0.64(6) 0.086(14) 0.15(2) 0.007(9) 0.01(2) C36 0.061(7) 0.056(7) 0.059(7) -0.010(5) 0.018(6) 0.001(6) C37 0.075(8) 0.050(8) 0.107(11) 0.001(7) 0.038(8) 0.010(6) C38 0.079(9) 0.049(7) 0.102(11) -0.009(7) 0.047(8) -0.004(6) C39 0.123(11) 0.108(12) 0.059(8) -0.021(7) -0.002(8) -0.053(10) C40 0.104(10) 0.092(11) 0.063(8) -0.030(7) -0.001(7) -0.032(8) N1 0.028(3) 0.042(4) 0.032(4) -0.002(3) -0.017(3) 0.003(3) N2 0.020(4) 0.092(6) 0.034(4) -0.001(4) -0.002(3) -0.006(4) N5 0.052(4) 0.029(4) 0.022(3) 0.001(3) -0.001(3) -0.002(4) N6 0.095(6) 0.031(4) 0.031(4) -0.002(3) -0.007(4) 0.000(5) N9 0.062(5) 0.060(6) 0.050(5) -0.003(5) -0.009(4) -0.004(5) N10 0.066(6) 0.075(7) 0.052(6) -0.010(5) -0.014(5) 0.014(5) N11 0.058(6) 0.071(6) 0.051(5) 0.005(4) 0.009(5) 0.016(5) N12 0.073(7) 0.118(9) 0.039(5) -0.002(5) 0.001(5) 0.004(6) N13 0.131(9) 0.075(8) 0.050(6) 0.001(5) -0.020(6) -0.009(7) N14 0.080(6) 0.056(6) 0.058(6) 0.004(5) -0.017(5) -0.016(5) N15 0.053(5) 0.072(6) 0.048(5) -0.002(4) 0.005(4) 0.010(5) N16 0.077(6) 0.057(6) 0.055(6) -0.021(4) 0.019(5) -0.018(5) O1 0.040(3) 0.043(3) 0.021(3) 0.000(2) -0.005(2) -0.004(3) O2 0.056(4) 0.094(6) 0.042(4) 0.008(4) -0.005(3) 0.008(4) O3 0.095(5) 0.023(3) 0.045(4) 0.007(3) 0.001(3) -0.006(3) O4 0.080(5) 0.081(6) 0.059(5) -0.013(4) -0.004(4) 0.017(4) O5 0.032(3) 0.083(5) 0.047(4) -0.001(3) 0.013(3) 0.003(3) O6 0.077(5) 0.076(5) 0.042(4) -0.006(3) -0.019(3) 0.013(4) O7 0.071(4) 0.052(4) 0.044(4) 0.010(3) -0.005(3) 0.018(4) O8 0.047(3) 0.046(4) 0.024(3) 0.000(2) -0.006(3) -0.006(3) O9 0.050(4) 0.087(5) 0.040(4) 0.007(3) 0.012(3) -0.028(4) O10 0.092(5) 0.072(5) 0.038(4) -0.018(3) -0.004(3) -0.007(5) O11 0.032(3) 0.053(4) 0.042(4) 0.003(3) 0.001(3) -0.006(3) O12 0.038(3) 0.055(4) 0.041(4) -0.008(3) 0.000(3) 0.018(3) O13 0.061(4) 0.037(4) 0.041(3) 0.000(3) -0.002(3) 0.007(3) O14 0.043(4) 0.044(4) 0.070(4) -0.006(3) 0.027(3) 0.000(3) O15 0.045(4) 0.042(4) 0.050(4) 0.003(3) -0.012(3) -0.008(3) O16 0.046(4) 0.041(4) 0.043(3) -0.011(3) -0.008(3) -0.005(3) O17 0.029(3) 0.037(4) 0.061(4) 0.001(3) -0.013(3) 0.008(3) O18 0.049(4) 0.058(5) 0.093(6) 0.022(4) 0.027(4) -0.009(3) O19 0.044(4) 0.043(4) 0.082(5) 0.032(3) 0.007(3) -0.001(3) O20 0.051(4) 0.050(5) 0.097(5) 0.029(4) -0.022(4) 0.002(4) O21 0.040(3) 0.051(4) 0.050(4) -0.004(3) -0.011(3) -0.012(3) O22 0.049(4) 0.043(4) 0.046(4) 0.001(3) 0.009(3) -0.019(3) O23 0.052(4) 0.036(3) 0.038(3) 0.002(3) 0.000(3) 0.010(3) O24 0.048(4) 0.042(4) 0.058(4) -0.008(3) 0.017(3) -0.001(3) O25 0.044(4) 0.046(4) 0.055(4) 0.013(3) 0.008(3) 0.016(3) O26 0.032(3) 0.064(4) 0.042(3) -0.006(3) 0.003(3) -0.004(3) O1W 0.077(9) 0.167(16) 0.175(14) 0.081(12) 0.000 0.000 O2W 0.121(12) 0.071(10) 0.228(17) 0.000 -0.041(12) 0.000 _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 V1 O1 1.592(4) . ? V1 O19 1.914(6) . ? V1 O14 1.925(6) . ? V1 O17 1.928(5) . ? V1 O16 1.933(6) . ? V2 O10 1.600(6) . ? V2 O19 1.687(6) . ? V2 O22 1.779(6) . ? V2 O23 1.805(5) . ? V3 O5 1.602(5) . ? V3 O17 1.685(5) . ? V3 O25 1.790(6) . ? V3 O26 1.800(6) . ? V4 O3 1.617(6) . ? V4 O16 1.674(6) . ? V4 O13 1.781(6) . ? V4 O15 1.794(6) . ? V5 O4 1.582(7) . ? V5 O20 1.673(6) . ? V5 O12 1.784(6) . ? V5 O13 1.802(6) . ? V5 V6 3.118(2) . ? V6 O2 1.618(6) . ? V6 O14 1.672(6) . ? V6 O11 1.776(6) . ? V6 O12 1.811(6) . ? V7 O9 1.614(6) . ? V7 O21 1.682(5) . ? V7 O11 1.795(6) . ? V7 O22 1.800(6) . ? V8 O8 1.592(5) . ? V8 O18 1.908(6) . ? V8 O20 1.919(6) . ? V8 O24 1.939(6) . ? V8 O21 1.944(6) . ? V9 O7 1.604(6) . ? V9 O24 1.682(6) . ? V9 O25 1.785(6) . ? V9 O23 1.789(6) . ? V10 O6 1.605(6) . ? V10 O18 1.681(6) . ? V10 O15 1.790(6) . ? V10 O26 1.798(6) . ? Cu1 N1 1.981(6) . ? Cu1 N4 1.987(6) 7_564 ? Cu1 N5 1.992(6) . ? Cu1 N8 1.992(6) 8_654 ? Cu1 O1 2.332(4) . ? Cu2 N11 1.866(8) . ? Cu2 N9 1.879(8) . ? Cu3 N14 1.850(9) . ? Cu3 N15 1.872(8) . ? C1 N1 1.332(9) . ? C1 N2 1.331(9) . ? C1 H1 0.9300 . ? C2 C3 1.375(11) . ? C2 N1 1.380(9) . ? C2 H2 0.9300 . ? C3 N2 1.385(10) . ? C3 H3 0.9300 . ? C4 N2 1.434(10) . ? C4 C5 1.492(15) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.538(14) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.422(15) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.489(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.301(11) . ? C8 N3 1.370(11) . ? C8 H8 0.9300 . ? C9 C10 1.355(11) . ? C9 N4 1.357(10) . ? C9 H9 0.9300 . ? C10 N3 1.365(11) . ? C10 H10 0.9300 . ? C11 N5 1.322(9) . ? C11 N6 1.341(11) . ? C11 H11 0.9300 . ? C12 C13 1.350(11) . ? C12 N5 1.360(10) . ? C12 H12 0.9300 . ? C13 N6 1.353(10) . ? C13 H13 0.9300 . ? C14 N6 1.461(10) . ? C14 C15 1.485(14) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.521(14) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.457(14) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N7 1.484(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N8 1.317(10) . ? C18 N7 1.336(11) . ? C18 H18 0.9300 . ? C19 C20 1.348(12) . ? C19 N7 1.372(10) . ? C19 H19 0.9300 . ? C20 N8 1.367(10) . ? C20 H20 0.9300 . ? C21 N9 1.283(12) . ? C21 N10 1.336(11) . ? C21 H21 0.9300 . ? C22 C23 1.335(15) . ? C22 N9 1.367(13) . ? C22 H22 0.9300 . ? C23 N10 1.371(14) . ? C23 H23 0.9300 . ? C24 C25 1.494(16) . ? C24 N10 1.504(14) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C25 1.49(2) 4_655 ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N11 1.300(11) . ? C26 N12 1.309(12) . ? C26 H26 0.9300 . ? C27 C28 1.352(15) . ? C27 N11 1.368(14) . ? C27 H27 0.9300 . ? C28 N12 1.401(14) . ? C28 H28 0.9300 . ? C29 C30 1.425(19) . ? C29 N12 1.464(12) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C30 1.50(2) 4_656 ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 N13 1.320(13) . ? C31 N14 1.331(13) . ? C31 H31 0.9300 . ? C32 N14 1.323(14) . ? C32 C33 1.351(15) . ? C32 H32 0.9300 . ? C33 N13 1.326(16) . ? C33 H33 0.9300 . ? C34 C35 1.35(2) . ? C34 N13 1.499(14) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C35 1.53(3) 3_566 ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N15 1.322(12) . ? C36 N16 1.345(11) . ? C36 H36 0.9300 . ? C37 C38 1.349(16) . ? C37 N15 1.402(12) . ? C37 H37 0.9300 . ? C38 N16 1.367(14) . ? C38 H38 0.9300 . ? C39 N16 1.462(13) . ? C39 C40 1.497(16) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C40 1.47(2) 3_565 ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? N4 Cu1 1.987(6) 7_464 ? N8 Cu1 1.992(6) 8_644 ? 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 O1 V1 O19 107.6(3) . . ? O1 V1 O14 104.8(3) . . ? O19 V1 O14 85.2(3) . . ? O1 V1 O17 104.7(3) . . ? O19 V1 O17 85.8(3) . . ? O14 V1 O17 150.5(3) . . ? O1 V1 O16 105.3(3) . . ? O19 V1 O16 147.2(3) . . ? O14 V1 O16 86.1(3) . . ? O17 V1 O16 86.4(3) . . ? O10 V2 O19 109.9(4) . . ? O10 V2 O22 107.4(3) . . ? O19 V2 O22 108.9(3) . . ? O10 V2 O23 109.1(3) . . ? O19 V2 O23 110.3(3) . . ? O22 V2 O23 111.3(3) . . ? O5 V3 O17 107.8(3) . . ? O5 V3 O25 108.3(3) . . ? O17 V3 O25 110.8(3) . . ? O5 V3 O26 108.1(3) . . ? O17 V3 O26 110.6(3) . . ? O25 V3 O26 111.2(3) . . ? O3 V4 O16 108.6(3) . . ? O3 V4 O13 109.9(3) . . ? O16 V4 O13 111.2(3) . . ? O3 V4 O15 107.4(3) . . ? O16 V4 O15 109.5(3) . . ? O13 V4 O15 110.2(3) . . ? O4 V5 O20 108.6(4) . . ? O4 V5 O12 109.2(3) . . ? O20 V5 O12 109.2(3) . . ? O4 V5 O13 108.6(4) . . ? O20 V5 O13 110.3(3) . . ? O12 V5 O13 110.8(3) . . ? O4 V5 V6 136.2(3) . . ? O20 V5 V6 85.1(2) . . ? O12 V5 V6 30.10(18) . . ? O13 V5 V6 104.52(19) . . ? O2 V6 O14 109.7(3) . . ? O2 V6 O11 108.6(3) . . ? O14 V6 O11 109.9(3) . . ? O2 V6 O12 108.4(3) . . ? O14 V6 O12 109.0(3) . . ? O11 V6 O12 111.2(3) . . ? O2 V6 V5 133.8(3) . . ? O14 V6 V5 83.8(2) . . ? O11 V6 V5 107.25(19) . . ? O12 V6 V5 29.62(17) . . ? O9 V7 O21 109.1(3) . . ? O9 V7 O11 107.6(3) . . ? O21 V7 O11 110.9(3) . . ? O9 V7 O22 108.5(3) . . ? O21 V7 O22 110.0(3) . . ? O11 V7 O22 110.8(3) . . ? O8 V8 O18 107.4(3) . . ? O8 V8 O20 103.7(3) . . ? O18 V8 O20 83.6(3) . . ? O8 V8 O24 104.6(3) . . ? O18 V8 O24 86.7(3) . . ? O20 V8 O24 151.7(3) . . ? O8 V8 O21 107.1(3) . . ? O18 V8 O21 145.4(3) . . ? O20 V8 O21 86.4(3) . . ? O24 V8 O21 86.6(3) . . ? O7 V9 O24 108.8(3) . . ? O7 V9 O25 108.2(3) . . ? O24 V9 O25 111.7(3) . . ? O7 V9 O23 107.6(3) . . ? O24 V9 O23 109.6(3) . . ? O25 V9 O23 111.0(3) . . ? O6 V10 O18 109.2(4) . . ? O6 V10 O15 108.6(3) . . ? O18 V10 O15 109.9(3) . . ? O6 V10 O26 109.7(3) . . ? O18 V10 O26 108.4(3) . . ? O15 V10 O26 111.0(3) . . ? N1 Cu1 N4 177.4(2) . 7_564 ? N1 Cu1 N5 89.8(3) . . ? N4 Cu1 N5 90.2(3) 7_564 . ? N1 Cu1 N8 89.6(3) . 8_654 ? N4 Cu1 N8 90.1(3) 7_564 8_654 ? N5 Cu1 N8 175.7(2) . 8_654 ? N1 Cu1 O1 91.2(2) . . ? N4 Cu1 O1 91.5(2) 7_564 . ? N5 Cu1 O1 89.7(2) . . ? N8 Cu1 O1 94.6(2) 8_654 . ? N11 Cu2 N9 174.8(4) . . ? N14 Cu3 N15 178.9(4) . . ? N1 C1 N2 112.5(7) . . ? N1 C1 H1 123.7 . . ? N2 C1 H1 123.7 . . ? C3 C2 N1 109.1(7) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C2 C3 N2 106.2(7) . . ? C2 C3 H3 126.9 . . ? N2 C3 H3 126.9 . . ? N2 C4 C5 113.9(9) . . ? N2 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? N2 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 114.4(10) . . ? C4 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? C4 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C7 C6 C5 113.9(11) . . ? C7 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? C7 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C6 C7 N3 111.5(10) . . ? C6 C7 H7A 109.3 . . ? N3 C7 H7A 109.3 . . ? C6 C7 H7B 109.3 . . ? N3 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N4 C8 N3 110.1(9) . . ? N4 C8 H8 124.9 . . ? N3 C8 H8 124.9 . . ? C10 C9 N4 110.0(8) . . ? C10 C9 H9 125.0 . . ? N4 C9 H9 125.0 . . ? C9 C10 N3 105.6(8) . . ? C9 C10 H10 127.2 . . ? N3 C10 H10 127.2 . . ? N5 C11 N6 111.7(8) . . ? N5 C11 H11 124.1 . . ? N6 C11 H11 124.1 . . ? C13 C12 N5 110.6(7) . . ? C13 C12 H12 124.7 . . ? N5 C12 H12 124.7 . . ? C12 C13 N6 106.1(7) . . ? C12 C13 H13 126.9 . . ? N6 C13 H13 126.9 . . ? N6 C14 C15 112.9(8) . . ? N6 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? N6 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C16 110.8(9) . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 116.0(9) . . ? C17 C16 H16A 108.3 . . ? C15 C16 H16A 108.3 . . ? C17 C16 H16B 108.3 . . ? C15 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C16 C17 N7 114.8(9) . . ? C16 C17 H17A 108.6 . . ? N7 C17 H17A 108.6 . . ? C16 C17 H17B 108.6 . . ? N7 C17 H17B 108.6 . . ? H17A C17 H17B 107.5 . . ? N8 C18 N7 111.1(8) . . ? N8 C18 H18 124.4 . . ? N7 C18 H18 124.4 . . ? C20 C19 N7 105.6(9) . . ? C20 C19 H19 127.2 . . ? N7 C19 H19 127.2 . . ? C19 C20 N8 110.2(8) . . ? C19 C20 H20 124.9 . . ? N8 C20 H20 124.9 . . ? N9 C21 N10 111.0(10) . . ? N9 C21 H21 124.5 . . ? N10 C21 H21 124.5 . . ? C23 C22 N9 110.9(11) . . ? C23 C22 H22 124.6 . . ? N9 C22 H22 124.6 . . ? C22 C23 N10 104.2(9) . . ? C22 C23 H23 127.9 . . ? N10 C23 H23 127.9 . . ? C25 C24 N10 115.9(11) . . ? C25 C24 H24A 108.3 . . ? N10 C24 H24A 108.3 . . ? C25 C24 H24B 108.3 . . ? N10 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? C24 C25 C25 113.4(12) . 4_655 ? C24 C25 H25A 108.9 . . ? C25 C25 H25A 108.9 4_655 . ? C24 C25 H25B 108.9 . . ? C25 C25 H25B 108.9 4_655 . ? H25A C25 H25B 107.7 . . ? N11 C26 N12 114.6(10) . . ? N11 C26 H26 122.7 . . ? N12 C26 H26 122.7 . . ? C28 C27 N11 110.6(11) . . ? C28 C27 H27 124.7 . . ? N11 C27 H27 124.7 . . ? C27 C28 N12 104.9(12) . . ? C27 C28 H28 127.5 . . ? N12 C28 H28 127.5 . . ? C30 C29 N12 113.8(12) . . ? C30 C29 H29A 108.8 . . ? N12 C29 H29A 108.8 . . ? C30 C29 H29B 108.8 . . ? N12 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C29 C30 C30 115.1(12) . 4_656 ? C29 C30 H30A 108.5 . . ? C30 C30 H30A 108.5 4_656 . ? C29 C30 H30B 108.5 . . ? C30 C30 H30B 108.5 4_656 . ? H30A C30 H30B 107.5 . . ? N13 C31 N14 111.3(11) . . ? N13 C31 H31 124.4 . . ? N14 C31 H31 124.4 . . ? N14 C32 C33 109.8(12) . . ? N14 C32 H32 125.1 . . ? C33 C32 H32 125.1 . . ? N13 C33 C32 107.1(12) . . ? N13 C33 H33 126.5 . . ? C32 C33 H33 126.5 . . ? C35 C34 N13 116.6(17) . . ? C35 C34 H34A 108.2 . . ? N13 C34 H34A 108.2 . . ? C35 C34 H34B 108.2 . . ? N13 C34 H34B 108.2 . . ? H34A C34 H34B 107.3 . . ? C34 C35 C35 113(2) . 3_566 ? C34 C35 H35A 108.9 . . ? C35 C35 H35A 108.9 3_566 . ? C34 C35 H35B 108.9 . . ? C35 C35 H35B 108.9 3_566 . ? H35A C35 H35B 107.7 . . ? N15 C36 N16 110.4(9) . . ? N15 C36 H36 124.8 . . ? N16 C36 H36 124.8 . . ? C38 C37 N15 108.4(11) . . ? C38 C37 H37 125.8 . . ? N15 C37 H37 125.8 . . ? C37 C38 N16 107.0(10) . . ? C37 C38 H38 126.5 . . ? N16 C38 H38 126.5 . . ? N16 C39 C40 115.0(10) . . ? N16 C39 H39A 108.5 . . ? C40 C39 H39A 108.5 . . ? N16 C39 H39B 108.5 . . ? C40 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? C40 C40 C39 114.6(13) 3_565 . ? C40 C40 H40A 108.6 3_565 . ? C39 C40 H40A 108.6 . . ? C40 C40 H40B 108.6 3_565 . ? C39 C40 H40B 108.6 . . ? H40A C40 H40B 107.6 . . ? C1 N1 C2 105.3(6) . . ? C1 N1 Cu1 126.9(5) . . ? C2 N1 Cu1 127.8(5) . . ? C1 N2 C3 106.9(7) . . ? C1 N2 C4 126.0(7) . . ? C3 N2 C4 127.1(7) . . ? C10 N3 C8 107.1(8) . . ? C10 N3 C7 129.5(8) . . ? C8 N3 C7 123.3(8) . . ? C8 N4 C9 106.9(7) . . ? C8 N4 Cu1 123.2(6) . 7_464 ? C9 N4 Cu1 129.8(6) . 7_464 ? C11 N5 C12 104.5(7) . . ? C11 N5 Cu1 128.0(6) . . ? C12 N5 Cu1 127.5(5) . . ? C11 N6 C13 107.0(7) . . ? C11 N6 C14 126.1(7) . . ? C13 N6 C14 126.8(7) . . ? C18 N7 C19 107.5(8) . . ? C18 N7 C17 123.6(7) . . ? C19 N7 C17 128.4(8) . . ? C18 N8 C20 105.6(7) . . ? C18 N8 Cu1 124.7(6) . 8_644 ? C20 N8 Cu1 129.6(5) . 8_644 ? C21 N9 C22 105.8(9) . . ? C21 N9 Cu2 122.9(8) . . ? C22 N9 Cu2 131.3(9) . . ? C21 N10 C23 108.1(9) . . ? C21 N10 C24 124.9(11) . . ? C23 N10 C24 126.9(10) . . ? C26 N11 C27 104.1(9) . . ? C26 N11 Cu2 129.4(8) . . ? C27 N11 Cu2 126.3(7) . . ? C26 N12 C28 105.7(9) . . ? C26 N12 C29 128.3(11) . . ? C28 N12 C29 125.8(11) . . ? C31 N13 C33 106.8(11) . . ? C31 N13 C34 127.0(12) . . ? C33 N13 C34 126.2(12) . . ? C32 N14 C31 105.0(10) . . ? C32 N14 Cu3 128.3(8) . . ? C31 N14 Cu3 126.4(8) . . ? C36 N15 C37 106.1(9) . . ? C36 N15 Cu3 122.8(7) . . ? C37 N15 Cu3 131.0(9) . . ? C36 N16 C38 108.0(10) . . ? C36 N16 C39 124.1(11) . . ? C38 N16 C39 127.8(10) . . ? V1 O1 Cu1 172.1(3) . . ? V6 O11 V7 138.6(3) . . ? V5 O12 V6 120.3(3) . . ? V4 O13 V5 135.7(3) . . ? V6 O14 V1 169.3(4) . . ? V10 O15 V4 125.9(3) . . ? V4 O16 V1 158.1(4) . . ? V3 O17 V1 161.3(4) . . ? V10 O18 V8 165.9(5) . . ? V2 O19 V1 174.6(4) . . ? V5 O20 V8 174.7(4) . . ? V7 O21 V8 153.5(4) . . ? V2 O22 V7 128.9(3) . . ? V9 O23 V2 126.8(3) . . ? V9 O24 V8 157.5(4) . . ? V9 O25 V3 137.6(3) . . ? V10 O26 V3 123.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 V5 V6 O2 68.6(5) . . . . ? O20 V5 V6 O2 -179.4(4) . . . . ? O12 V5 V6 O2 36.9(5) . . . . ? O13 V5 V6 O2 -69.7(4) . . . . ? O4 V5 V6 O14 -179.9(5) . . . . ? O20 V5 V6 O14 -67.9(3) . . . . ? O12 V5 V6 O14 148.4(5) . . . . ? O13 V5 V6 O14 41.9(3) . . . . ? O4 V5 V6 O11 -70.9(5) . . . . ? O20 V5 V6 O11 41.1(3) . . . . ? O12 V5 V6 O11 -102.6(4) . . . . ? O13 V5 V6 O11 150.8(3) . . . . ? O4 V5 V6 O12 31.7(6) . . . . ? O20 V5 V6 O12 143.7(5) . . . . ? O13 V5 V6 O12 -106.6(4) . . . . ? N1 C2 C3 N2 -0.5(11) . . . . ? N2 C4 C5 C6 -177.8(9) . . . . ? C4 C5 C6 C7 -60.3(14) . . . . ? C5 C6 C7 N3 -169.3(9) . . . . ? N4 C9 C10 N3 4.4(11) . . . . ? N5 C12 C13 N6 3.0(11) . . . . ? N6 C14 C15 C16 -172.5(9) . . . . ? C14 C15 C16 C17 -61.0(14) . . . . ? C15 C16 C17 N7 -174.5(9) . . . . ? N7 C19 C20 N8 0.3(10) . . . . ? N9 C22 C23 N10 2.1(12) . . . . ? N10 C24 C25 C25 -49.0(13) . . . 4_655 ? N11 C27 C28 N12 -1(2) . . . . ? N12 C29 C30 C30 178.5(18) . . . 4_656 ? N14 C32 C33 N13 -1.3(19) . . . . ? N13 C34 C35 C35 178(2) . . . 3_566 ? N15 C37 C38 N16 0.7(13) . . . . ? N16 C39 C40 C40 -52.5(13) . . . 3_565 ? N2 C1 N1 C2 1.0(11) . . . . ? N2 C1 N1 Cu1 -176.8(6) . . . . ? C3 C2 N1 C1 -0.3(10) . . . . ? C3 C2 N1 Cu1 177.5(7) . . . . ? N5 Cu1 N1 C1 -66.0(8) . . . . ? N8 Cu1 N1 C1 109.8(8) 8_654 . . . ? O1 Cu1 N1 C1 -155.6(8) . . . . ? N5 Cu1 N1 C2 116.7(7) . . . . ? N8 Cu1 N1 C2 -67.5(7) 8_654 . . . ? O1 Cu1 N1 C2 27.0(7) . . . . ? N1 C1 N2 C3 -1.3(12) . . . . ? N1 C1 N2 C4 177.1(9) . . . . ? C2 C3 N2 C1 1.1(11) . . . . ? C2 C3 N2 C4 -177.3(10) . . . . ? C5 C4 N2 C1 -86.3(13) . . . . ? C5 C4 N2 C3 91.8(12) . . . . ? C9 C10 N3 C8 -2.9(11) . . . . ? C9 C10 N3 C7 -179.1(10) . . . . ? N4 C8 N3 C10 0.5(12) . . . . ? N4 C8 N3 C7 176.9(9) . . . . ? C6 C7 N3 C10 108.3(12) . . . . ? C6 C7 N3 C8 -67.3(14) . . . . ? N3 C8 N4 C9 2.2(11) . . . . ? N3 C8 N4 Cu1 -175.7(6) . . . 7_464 ? C10 C9 N4 C8 -4.1(10) . . . . ? C10 C9 N4 Cu1 173.6(6) . . . 7_464 ? N6 C11 N5 C12 2.2(12) . . . . ? N6 C11 N5 Cu1 -176.8(7) . . . . ? C13 C12 N5 C11 -3.2(11) . . . . ? C13 C12 N5 Cu1 175.8(6) . . . . ? N1 Cu1 N5 C11 101.4(9) . . . . ? N4 Cu1 N5 C11 -75.9(9) 7_564 . . . ? O1 Cu1 N5 C11 -167.4(9) . . . . ? N1 Cu1 N5 C12 -77.3(7) . . . . ? N4 Cu1 N5 C12 105.3(7) 7_564 . . . ? O1 Cu1 N5 C12 13.9(7) . . . . ? N5 C11 N6 C13 -0.4(13) . . . . ? N5 C11 N6 C14 176.0(10) . . . . ? C12 C13 N6 C11 -1.5(11) . . . . ? C12 C13 N6 C14 -177.9(10) . . . . ? C15 C14 N6 C11 -59.4(16) . . . . ? C15 C14 N6 C13 116.4(10) . . . . ? N8 C18 N7 C19 1.0(11) . . . . ? N8 C18 N7 C17 173.8(9) . . . . ? C20 C19 N7 C18 -0.8(10) . . . . ? C20 C19 N7 C17 -173.2(9) . . . . ? C16 C17 N7 C18 -89.5(12) . . . . ? C16 C17 N7 C19 81.7(12) . . . . ? N7 C18 N8 C20 -0.8(10) . . . . ? N7 C18 N8 Cu1 -177.8(6) . . . 8_644 ? C19 C20 N8 C18 0.3(10) . . . . ? C19 C20 N8 Cu1 177.1(6) . . . 8_644 ? N10 C21 N9 C22 -0.3(12) . . . . ? N10 C21 N9 Cu2 177.7(6) . . . . ? C23 C22 N9 C21 -1.2(13) . . . . ? C23 C22 N9 Cu2 -178.9(7) . . . . ? N9 C21 N10 C23 1.6(12) . . . . ? N9 C21 N10 C24 -177.5(10) . . . . ? C22 C23 N10 C21 -2.2(12) . . . . ? C22 C23 N10 C24 176.9(10) . . . . ? C25 C24 N10 C21 95.7(14) . . . . ? C25 C24 N10 C23 -83.3(15) . . . . ? N12 C26 N11 C27 -1.2(13) . . . . ? N12 C26 N11 Cu2 -176.7(8) . . . . ? C28 C27 N11 C26 1.6(17) . . . . ? C28 C27 N11 Cu2 177.2(11) . . . . ? N11 C26 N12 C28 0.4(15) . . . . ? N11 C26 N12 C29 -175.8(12) . . . . ? C27 C28 N12 C26 0.6(18) . . . . ? C27 C28 N12 C29 176.9(13) . . . . ? C30 C29 N12 C26 -130.0(15) . . . . ? C30 C29 N12 C28 54(2) . . . . ? N14 C31 N13 C33 0.6(16) . . . . ? N14 C31 N13 C34 179.4(13) . . . . ? C32 C33 N13 C31 0.4(18) . . . . ? C32 C33 N13 C34 -178.5(14) . . . . ? C35 C34 N13 C31 -133(2) . . . . ? C35 C34 N13 C33 46(3) . . . . ? C33 C32 N14 C31 1.6(16) . . . . ? C33 C32 N14 Cu3 175.1(10) . . . . ? N13 C31 N14 C32 -1.3(13) . . . . ? N13 C31 N14 Cu3 -175.0(8) . . . . ? N16 C36 N15 C37 -1.4(12) . . . . ? N16 C36 N15 Cu3 -179.9(7) . . . . ? C38 C37 N15 C36 0.4(12) . . . . ? C38 C37 N15 Cu3 178.7(8) . . . . ? N15 C36 N16 C38 1.9(12) . . . . ? N15 C36 N16 C39 -175.9(10) . . . . ? C37 C38 N16 C36 -1.6(12) . . . . ? C37 C38 N16 C39 176.1(11) . . . . ? C40 C39 N16 C36 98.4(13) . . . . ? C40 C39 N16 C38 -78.9(16) . . . . ? O2 V6 O11 V7 155.2(5) . . . . ? O14 V6 O11 V7 35.2(6) . . . . ? O12 V6 O11 V7 -85.6(5) . . . . ? V5 V6 O11 V7 -54.4(5) . . . . ? O9 V7 O11 V6 155.4(5) . . . . ? O21 V7 O11 V6 36.2(6) . . . . ? O22 V7 O11 V6 -86.3(5) . . . . ? O4 V5 O12 V6 -157.3(4) . . . . ? O20 V5 O12 V6 -38.7(5) . . . . ? O13 V5 O12 V6 83.1(4) . . . . ? O2 V6 O12 V5 -152.8(4) . . . . ? O14 V6 O12 V5 -33.4(5) . . . . ? O11 V6 O12 V5 87.9(4) . . . . ? O3 V4 O13 V5 163.4(4) . . . . ? O16 V4 O13 V5 43.1(5) . . . . ? O15 V4 O13 V5 -78.5(5) . . . . ? O4 V5 O13 V4 143.3(5) . . . . ? O20 V5 O13 V4 24.4(6) . . . . ? O12 V5 O13 V4 -96.7(5) . . . . ? V6 V5 O13 V4 -65.8(5) . . . . ? O2 V6 O14 V1 -114(2) . . . . ? O11 V6 O14 V1 5(2) . . . . ? O12 V6 O14 V1 127(2) . . . . ? V5 V6 O14 V1 112(2) . . . . ? O1 V1 O14 V6 110(2) . . . . ? O19 V1 O14 V6 3(2) . . . . ? O17 V1 O14 V6 -69(2) . . . . ? O16 V1 O14 V6 -145(2) . . . . ? O6 V10 O15 V4 -151.0(4) . . . . ? O18 V10 O15 V4 -31.6(5) . . . . ? O26 V10 O15 V4 88.3(4) . . . . ? O3 V4 O15 V10 -153.6(4) . . . . ? O16 V4 O15 V10 -35.9(5) . . . . ? O13 V4 O15 V10 86.7(5) . . . . ? O3 V4 O16 V1 -160.8(9) . . . . ? O13 V4 O16 V1 -39.7(11) . . . . ? O15 V4 O16 V1 82.3(10) . . . . ? O1 V1 O16 V4 155.3(9) . . . . ? O19 V1 O16 V4 -23.9(13) . . . . ? O14 V1 O16 V4 51.0(10) . . . . ? O17 V1 O16 V4 -100.4(10) . . . . ? O5 V3 O17 V1 -176.1(11) . . . . ? O25 V3 O17 V1 65.6(12) . . . . ? O26 V3 O17 V1 -58.2(12) . . . . ? O1 V1 O17 V3 178.2(11) . . . . ? O19 V1 O17 V3 -74.7(11) . . . . ? O14 V1 O17 V3 -2.2(15) . . . . ? O16 V1 O17 V3 73.4(11) . . . . ? O6 V10 O18 V8 16.3(19) . . . . ? O15 V10 O18 V8 -102.7(18) . . . . ? O26 V10 O18 V8 135.9(18) . . . . ? O8 V8 O18 V10 -9.3(19) . . . . ? O20 V8 O18 V10 93.0(18) . . . . ? O24 V8 O18 V10 -113.6(18) . . . . ? O21 V8 O18 V10 167.2(16) . . . . ? O9 V7 O21 V8 -174.2(8) . . . . ? O11 V7 O21 V8 -55.9(9) . . . . ? O22 V7 O21 V8 67.0(9) . . . . ? O8 V8 O21 V7 171.7(8) . . . . ? O18 V8 O21 V7 -4.8(12) . . . . ? O20 V8 O21 V7 68.5(9) . . . . ? O24 V8 O21 V7 -84.1(9) . . . . ? O10 V2 O22 V7 -145.9(4) . . . . ? O19 V2 O22 V7 -27.0(5) . . . . ? O23 V2 O22 V7 94.7(5) . . . . ? O9 V7 O22 V2 -167.1(4) . . . . ? O21 V7 O22 V2 -47.8(5) . . . . ? O11 V7 O22 V2 75.1(5) . . . . ? O7 V9 O23 V2 156.5(4) . . . . ? O24 V9 O23 V2 38.4(5) . . . . ? O25 V9 O23 V2 -85.4(4) . . . . ? O10 V2 O23 V9 155.2(4) . . . . ? O19 V2 O23 V9 34.5(5) . . . . ? O22 V2 O23 V9 -86.5(4) . . . . ? O7 V9 O24 V8 163.8(9) . . . . ? O25 V9 O24 V8 44.5(10) . . . . ? O23 V9 O24 V8 -78.9(10) . . . . ? O8 V8 O24 V9 -152.6(9) . . . . ? O18 V8 O24 V9 -45.4(10) . . . . ? O20 V8 O24 V9 24.5(13) . . . . ? O21 V8 O24 V9 100.6(10) . . . . ? O7 V9 O25 V3 -165.2(5) . . . . ? O24 V9 O25 V3 -45.6(6) . . . . ? O23 V9 O25 V3 77.0(6) . . . . ? O5 V3 O25 V9 -149.2(5) . . . . ? O17 V3 O25 V9 -31.2(6) . . . . ? O26 V3 O25 V9 92.2(6) . . . . ? O6 V10 O26 V3 139.8(4) . . . . ? O18 V10 O26 V3 20.6(5) . . . . ? O15 V10 O26 V3 -100.1(4) . . . . ? O5 V3 O26 V10 164.6(4) . . . . ? O17 V3 O26 V10 46.8(5) . . . . ? O25 V3 O26 V10 -76.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.577 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.096 # Attachment 'L-1-left658057.cif' data_mm_left _database_code_depnum_ccdc_archive 'CCDC 658057' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H58 Cu3 N16 O27 V10' _chemical_formula_weight 1895.04 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' V V 0.3005 0.5294 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M I222 _symmetry_space_group_name_Hall I22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 23.0670(10) _cell_length_b 23.1760(10) _cell_length_c 24.9480(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13337.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 26.1 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7544 _exptl_absorpt_coefficient_mu 2.353 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.485 _exptl_absorpt_correction_T_max 0.569 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37072 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.10 _reflns_number_total 13213 _reflns_number_gt 9790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.0532P)^2^+0.6307P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.017(17) _refine_ls_number_reflns 13213 _refine_ls_number_parameters 801 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1232 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.24710(5) 0.25441(4) 0.96527(4) 0.0206(2) Uani 1 1 d . . . V2 V 0.27979(5) 0.39878(5) 0.92212(5) 0.0327(3) Uani 1 1 d . . . V3 V 0.10624(5) 0.29127(6) 0.91763(5) 0.0318(3) Uani 1 1 d . . . V4 V 0.21627(6) 0.11736(5) 0.90991(5) 0.0332(3) Uani 1 1 d . . . V5 V 0.32952(5) 0.14615(5) 0.83224(5) 0.0373(3) Uani 1 1 d . . . V6 V 0.38962(5) 0.22653(6) 0.91502(5) 0.0347(3) Uani 1 1 d . . . V7 V 0.37486(5) 0.34560(6) 0.84089(5) 0.0360(3) Uani 1 1 d . . . V8 V 0.25302(5) 0.27254(5) 0.78889(4) 0.0256(2) Uani 1 1 d . . . V9 V 0.17184(5) 0.38986(5) 0.84134(5) 0.0334(3) Uani 1 1 d . . . V10 V 0.13227(5) 0.19079(6) 0.83491(5) 0.0354(3) Uani 1 1 d . . . Cu1 Cu 0.25138(3) 0.24478(3) 1.12192(3) 0.02275(17) Uani 1 1 d . . . Cu2 Cu 0.51606(5) 0.43129(5) 0.77261(4) 0.0599(3) Uani 1 1 d . . . Cu3 Cu 0.06800(5) 0.51963(5) 0.77153(4) 0.0634(3) Uani 1 1 d . . . C1 C 0.3714(3) 0.2553(4) 1.1649(3) 0.0382(18) Uani 1 1 d . . . H1 H 0.3580 0.2713 1.1967 0.046 Uiso 1 1 calc R . . C2 C 0.3745(3) 0.2222(3) 1.0839(3) 0.0336(17) Uani 1 1 d . . . H2 H 0.3634 0.2103 1.0498 0.040 Uiso 1 1 calc R . . C3 C 0.4297(3) 0.2243(4) 1.1024(3) 0.045(2) Uani 1 1 d . . . H3 H 0.4630 0.2142 1.0836 0.054 Uiso 1 1 calc R . . C4 C 0.4753(3) 0.2537(4) 1.1908(3) 0.053(2) Uani 1 1 d . . . H4A H 0.4670 0.2865 1.2136 0.064 Uiso 1 1 calc R . . H4B H 0.5100 0.2624 1.1703 0.064 Uiso 1 1 calc R . . C5 C 0.4857(4) 0.2011(5) 1.2248(4) 0.081(3) Uani 1 1 d . . . H5A H 0.4917 0.1682 1.2014 0.098 Uiso 1 1 calc R . . H5B H 0.4511 0.1936 1.2458 0.098 Uiso 1 1 calc R . . C6 C 0.5383(4) 0.2059(5) 1.2635(4) 0.073(3) Uiso 1 1 d . . . H6A H 0.5424 0.1700 1.2832 0.088 Uiso 1 1 calc R . . H6B H 0.5733 0.2117 1.2427 0.088 Uiso 1 1 calc R . . C7 C 0.5320(4) 0.2528(4) 1.3012(3) 0.060(2) Uiso 1 1 d . . . H7A H 0.4942 0.2505 1.3181 0.073 Uiso 1 1 calc R . . H7B H 0.5342 0.2893 1.2821 0.073 Uiso 1 1 calc R . . C8 C 0.6349(3) 0.2604(4) 1.3323(4) 0.053(2) Uiso 1 1 d . . . H8 H 0.6500 0.2709 1.2991 0.064 Uiso 1 1 calc R . . C9 C 0.6269(3) 0.2396(3) 1.4161(3) 0.0390(18) Uiso 1 1 d . . . H9 H 0.6367 0.2336 1.4519 0.047 Uiso 1 1 calc R . . C10 C 0.5731(3) 0.2370(3) 1.3961(3) 0.0426(19) Uiso 1 1 d . . . H10 H 0.5394 0.2276 1.4146 0.051 Uiso 1 1 calc R . . C11 C 0.2462(4) 0.3612(3) 1.1735(3) 0.048(2) Uani 1 1 d . . . H11 H 0.2347 0.3457 1.2062 0.057 Uiso 1 1 calc R . . C12 C 0.2687(3) 0.3698(3) 1.0912(3) 0.0361(18) Uani 1 1 d . . . H12 H 0.2754 0.3611 1.0553 0.043 Uiso 1 1 calc R . . C13 C 0.2708(3) 0.4236(3) 1.1123(3) 0.0418(19) Uani 1 1 d . . . H13 H 0.2807 0.4575 1.0945 0.050 Uiso 1 1 calc R . . C14 C 0.2530(5) 0.4633(3) 1.2046(3) 0.069(3) Uani 1 1 d . . . H14A H 0.2143 0.4647 1.2197 0.083 Uiso 1 1 calc R . . H14B H 0.2606 0.5002 1.1876 0.083 Uiso 1 1 calc R . . C15 C 0.2957(4) 0.4544(4) 1.2487(3) 0.061(3) Uani 1 1 d . . . H15A H 0.3337 0.4472 1.2334 0.073 Uiso 1 1 calc R . . H15B H 0.2846 0.4207 1.2694 0.073 Uiso 1 1 calc R . . C16 C 0.2987(4) 0.5075(4) 1.2860(4) 0.071(3) Uiso 1 1 d . . . H16A H 0.3278 0.5007 1.3133 0.085 Uiso 1 1 calc R . . H16B H 0.3109 0.5408 1.2652 0.085 Uiso 1 1 calc R . . C17 C 0.2418(4) 0.5212(3) 1.3129(3) 0.055(2) Uani 1 1 d . . . H17A H 0.2133 0.5314 1.2859 0.067 Uiso 1 1 calc R . . H17B H 0.2279 0.4871 1.3316 0.067 Uiso 1 1 calc R . . C18 C 0.2391(3) 0.6244(3) 1.3391(3) 0.0420(18) Uiso 1 1 d . . . H18 H 0.2264 0.6372 1.3058 0.050 Uiso 1 1 calc R . . C19 C 0.2668(3) 0.5676(4) 1.4037(3) 0.049(2) Uiso 1 1 d . . . H19 H 0.2764 0.5347 1.4232 0.058 Uiso 1 1 calc R . . C20 C 0.2691(3) 0.6226(3) 1.4207(3) 0.0412(19) Uiso 1 1 d . . . H20 H 0.2809 0.6343 1.4547 0.049 Uiso 1 1 calc R . . C21 C 0.5473(3) 0.3950(4) 0.8753(3) 0.050(2) Uani 1 1 d . . . H21 H 0.5310 0.3591 0.8683 0.059 Uiso 1 1 calc R . . C22 C 0.5764(3) 0.4814(4) 0.8663(4) 0.062(3) Uani 1 1 d . . . H22 H 0.5838 0.5172 0.8509 0.074 Uiso 1 1 calc R . . C23 C 0.5910(4) 0.4659(5) 0.9155(4) 0.069(3) Uani 1 1 d . . . H23 H 0.6101 0.4883 0.9408 0.083 Uiso 1 1 calc R . . C24 C 0.5768(5) 0.3733(5) 0.9709(4) 0.083(3) Uani 1 1 d . . . H24A H 0.5767 0.3332 0.9600 0.099 Uiso 1 1 calc R . . H24B H 0.6138 0.3810 0.9880 0.099 Uiso 1 1 calc R . . C25 C 0.5304(4) 0.3819(5) 1.0110(4) 0.083(3) Uani 1 1 d . . . H25A H 0.5371 0.4184 1.0290 0.100 Uiso 1 1 calc R . . H25B H 0.5334 0.3516 1.0377 0.100 Uiso 1 1 calc R . . C26 C 0.5186(4) 0.4250(4) 0.6577(4) 0.058(2) Uani 1 1 d . . . H26 H 0.5581 0.4330 0.6564 0.070 Uiso 1 1 calc R . . C27 C 0.4332(4) 0.4104(6) 0.6877(3) 0.088(4) Uani 1 1 d . . . H27 H 0.4021 0.4066 0.7112 0.105 Uiso 1 1 calc R . . C28 C 0.4303(4) 0.4045(7) 0.6327(4) 0.114(5) Uani 1 1 d . . . H28 H 0.3981 0.3956 0.6119 0.137 Uiso 1 1 calc R . . C29 C 0.5073(6) 0.4161(6) 0.5588(4) 0.105(4) Uani 1 1 d . . . H29A H 0.4911 0.4499 0.5414 0.126 Uiso 1 1 calc R . . H29B H 0.5492 0.4195 0.5577 0.126 Uiso 1 1 calc R . . C30 C 0.4906(8) 0.3665(5) 0.5297(4) 0.125(6) Uani 1 1 d . . . H30A H 0.4488 0.3630 0.5313 0.150 Uiso 1 1 calc R . . H30B H 0.5070 0.3328 0.5470 0.150 Uiso 1 1 calc R . . C31 C 0.0719(4) 0.5202(5) 0.6565(3) 0.061(3) Uani 1 1 d . . . H31 H 0.0634 0.5594 0.6545 0.074 Uiso 1 1 calc R . . C32 C 0.0878(5) 0.4370(4) 0.6876(4) 0.080(3) Uani 1 1 d . . . H32 H 0.0926 0.4064 0.7114 0.096 Uiso 1 1 calc R . . C33 C 0.0934(6) 0.4338(5) 0.6339(4) 0.112(5) Uani 1 1 d . . . H33 H 0.1027 0.4013 0.6138 0.134 Uiso 1 1 calc R . . C34 C 0.0834(6) 0.5080(6) 0.5582(4) 0.142(7) Uani 1 1 d D . . H34A H 0.0479 0.4957 0.5409 0.171 Uiso 1 1 calc R . . H34B H 0.0842 0.5498 0.5577 0.171 Uiso 1 1 calc R . . C35 C 0.1328(5) 0.4863(10) 0.5274(5) 0.228(13) Uani 1 1 d D . . H35A H 0.1302 0.4447 0.5239 0.274 Uiso 1 1 calc R . . H35B H 0.1687 0.4955 0.5458 0.274 Uiso 1 1 calc R . . C36 C 0.1061(4) 0.5475(4) 0.8749(4) 0.055(2) Uani 1 1 d . . . H36 H 0.1421 0.5309 0.8680 0.066 Uiso 1 1 calc R . . C37 C 0.0172(4) 0.5776(4) 0.8668(4) 0.067(3) Uani 1 1 d . . . H37 H -0.0192 0.5846 0.8521 0.081 Uiso 1 1 calc R . . C38 C 0.0336(5) 0.5928(4) 0.9159(5) 0.075(3) Uani 1 1 d . . . H38 H 0.0118 0.6125 0.9414 0.090 Uiso 1 1 calc R . . C39 C 0.1285(5) 0.5754(5) 0.9692(4) 0.088(4) Uani 1 1 d . . . H39A H 0.1245 0.6131 0.9857 0.106 Uiso 1 1 calc R . . H39B H 0.1685 0.5715 0.9576 0.106 Uiso 1 1 calc R . . C40 C 0.1160(5) 0.5297(4) 1.0108(4) 0.085(4) Uani 1 1 d . . . H40A H 0.1449 0.5323 1.0390 0.102 Uiso 1 1 calc R . . H40B H 0.0785 0.5374 1.0268 0.102 Uiso 1 1 calc R . . N1 N 0.3374(2) 0.2408(3) 1.1241(2) 0.0296(13) Uani 1 1 d . . . N2 N 0.4272(2) 0.2442(3) 1.1545(2) 0.0440(17) Uani 1 1 d . . . N3 N 0.5777(3) 0.2510(3) 1.3429(3) 0.0534(18) Uiso 1 1 d . . . N4 N 0.6652(2) 0.2524(2) 1.3763(2) 0.0317(13) Uiso 1 1 d . . . N5 N 0.2554(2) 0.3303(2) 1.12932(19) 0.0316(13) Uani 1 1 d . . . N6 N 0.2556(3) 0.4179(2) 1.1645(2) 0.0455(16) Uani 1 1 d . . . N7 N 0.2476(3) 0.5696(3) 1.3518(2) 0.0483(16) Uiso 1 1 d . . . N8 N 0.2513(2) 0.6590(2) 1.3804(2) 0.0332(13) Uiso 1 1 d . . . N9 N 0.5490(3) 0.4368(3) 0.8417(3) 0.0545(19) Uani 1 1 d . . . N10 N 0.5723(3) 0.4101(4) 0.9219(3) 0.060(2) Uani 1 1 d . . . N11 N 0.4899(3) 0.4229(3) 0.7025(3) 0.0538(19) Uani 1 1 d . . . N12 N 0.4884(3) 0.4152(4) 0.6150(3) 0.070(2) Uani 1 1 d . . . N13 N 0.0826(4) 0.4880(4) 0.6152(3) 0.077(3) Uani 1 1 d . . . N14 N 0.0744(3) 0.4911(3) 0.7014(3) 0.0575(19) Uani 1 1 d . . . N15 N 0.0624(3) 0.5497(3) 0.8407(3) 0.0566(19) Uani 1 1 d . . . N16 N 0.0904(3) 0.5730(3) 0.9213(3) 0.057(2) Uani 1 1 d . . . O1 O 0.25194(19) 0.25499(19) 1.02897(14) 0.0307(10) Uani 1 1 d . . . O2 O 0.4354(2) 0.2162(3) 0.9629(2) 0.0596(16) Uani 1 1 d . . . O3 O 0.2042(3) 0.0632(2) 0.9494(2) 0.0559(16) Uani 1 1 d . . . O4 O 0.3491(3) 0.1091(3) 0.7815(2) 0.0727(19) Uani 1 1 d . . . O5 O 0.0567(2) 0.3046(3) 0.9613(2) 0.0529(16) Uani 1 1 d . . . O6 O 0.0999(3) 0.1741(3) 0.7798(2) 0.0623(17) Uani 1 1 d . . . O7 O 0.1430(2) 0.4365(2) 0.8014(2) 0.0509(14) Uani 1 1 d . . . O8 O 0.24698(19) 0.2641(2) 0.72565(16) 0.0382(12) Uani 1 1 d . . . O9 O 0.4249(2) 0.3744(3) 0.8043(2) 0.0554(16) Uani 1 1 d . . . O10 O 0.2918(3) 0.4380(3) 0.9736(2) 0.0617(17) Uani 1 1 d . . . O11 O 0.40872(19) 0.2912(2) 0.88060(19) 0.0426(13) Uani 1 1 d . . . O12 O 0.3920(2) 0.1655(2) 0.8705(2) 0.0427(13) Uani 1 1 d . . . O13 O 0.2798(2) 0.1034(2) 0.87133(19) 0.0437(13) Uani 1 1 d . . . O14 O 0.3233(2) 0.2327(2) 0.9402(2) 0.0517(15) Uani 1 1 d . . . O15 O 0.1551(2) 0.1253(2) 0.86635(19) 0.0398(13) Uani 1 1 d . . . O16 O 0.2247(2) 0.1765(2) 0.94741(18) 0.0375(12) Uani 1 1 d . . . O17 O 0.16802(19) 0.2763(2) 0.9507(2) 0.0397(12) Uani 1 1 d . . . O18 O 0.1900(2) 0.2329(2) 0.8222(2) 0.0613(17) Uani 1 1 d . . . O19 O 0.2668(2) 0.3296(2) 0.9400(2) 0.0562(16) Uani 1 1 d . . . O20 O 0.2970(2) 0.2060(2) 0.8108(3) 0.0631(18) Uani 1 1 d . . . O21 O 0.3231(2) 0.3166(2) 0.8015(2) 0.0453(13) Uani 1 1 d . . . O22 O 0.3441(2) 0.4014(2) 0.8823(2) 0.0472(14) Uani 1 1 d . . . O23 O 0.2189(2) 0.4283(2) 0.88628(18) 0.0407(12) Uani 1 1 d . . . O24 O 0.2105(2) 0.3427(2) 0.8048(2) 0.0477(14) Uani 1 1 d . . . O25 O 0.1149(2) 0.3550(2) 0.8776(2) 0.0468(13) Uani 1 1 d . . . O26 O 0.08401(18) 0.2309(2) 0.87784(18) 0.0406(13) Uani 1 1 d . . . O1W O 0.1134(4) 1.0000 1.0000 0.125(5) Uani 1 2 d S . . O2W O 0.5000 0.1185(5) 1.0000 0.123(4) Uani 1 2 d S . . 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 V1 0.0222(5) 0.0210(5) 0.0185(5) 0.0008(4) -0.0004(4) 0.0006(5) V2 0.0438(7) 0.0240(6) 0.0302(6) 0.0023(5) 0.0018(6) -0.0032(6) V3 0.0203(6) 0.0436(8) 0.0317(7) 0.0041(6) -0.0008(5) 0.0044(6) V4 0.0458(7) 0.0214(6) 0.0324(7) 0.0007(5) -0.0040(6) -0.0023(6) V5 0.0414(7) 0.0359(7) 0.0346(7) 0.0016(6) -0.0030(6) 0.0117(6) V6 0.0233(6) 0.0498(8) 0.0309(7) -0.0016(6) 0.0028(5) 0.0042(6) V7 0.0292(6) 0.0450(8) 0.0339(7) 0.0014(6) 0.0037(5) -0.0134(6) V8 0.0265(6) 0.0274(6) 0.0227(5) 0.0019(4) 0.0014(5) 0.0001(5) V9 0.0410(7) 0.0275(7) 0.0318(7) 0.0024(5) 0.0020(6) 0.0088(6) V10 0.0319(6) 0.0410(8) 0.0333(7) 0.0044(6) 0.0015(6) -0.0052(6) Cu1 0.0220(4) 0.0219(4) 0.0243(4) 0.0005(3) -0.0014(3) 0.0003(4) Cu2 0.0671(7) 0.0704(8) 0.0423(6) 0.0006(6) -0.0057(6) 0.0051(7) Cu3 0.0708(8) 0.0732(9) 0.0462(7) -0.0063(6) -0.0012(6) -0.0050(7) C1 0.028(4) 0.063(5) 0.023(4) -0.013(4) 0.009(3) -0.003(4) C2 0.025(3) 0.055(5) 0.021(4) -0.003(3) -0.001(3) 0.000(3) C3 0.024(4) 0.072(6) 0.039(4) -0.011(4) 0.007(3) 0.002(4) C4 0.023(4) 0.101(8) 0.036(4) -0.010(5) 0.004(3) -0.006(4) C5 0.061(6) 0.093(9) 0.090(8) -0.002(6) -0.053(6) -0.005(6) C11 0.078(6) 0.033(4) 0.033(4) -0.003(3) 0.007(4) 0.009(5) C12 0.048(4) 0.028(4) 0.032(4) -0.005(3) 0.012(3) -0.005(3) C13 0.060(5) 0.015(4) 0.050(5) 0.004(3) 0.006(4) 0.000(3) C14 0.121(8) 0.029(4) 0.059(5) -0.010(4) -0.018(7) 0.020(6) C15 0.074(6) 0.057(6) 0.051(6) -0.018(4) 0.017(5) 0.003(5) C17 0.095(7) 0.027(4) 0.044(5) -0.011(3) -0.004(5) -0.010(5) C21 0.052(5) 0.048(6) 0.049(5) -0.015(4) -0.009(4) -0.003(4) C22 0.038(5) 0.057(6) 0.091(8) -0.011(5) -0.012(5) -0.002(5) C23 0.048(5) 0.083(8) 0.075(7) -0.040(6) -0.003(5) -0.008(5) C24 0.091(8) 0.103(9) 0.054(6) 0.004(6) -0.016(6) 0.023(7) C25 0.078(7) 0.120(10) 0.051(6) -0.002(6) -0.019(5) 0.020(7) C26 0.049(5) 0.068(6) 0.058(6) 0.002(5) -0.004(5) 0.001(5) C27 0.043(5) 0.191(14) 0.029(5) 0.008(6) 0.009(4) 0.021(7) C28 0.050(6) 0.246(18) 0.047(7) 0.002(8) 0.000(5) 0.012(9) C29 0.119(10) 0.155(14) 0.040(6) 0.009(7) 0.012(6) -0.003(10) C30 0.242(18) 0.066(8) 0.066(8) -0.008(6) 0.061(10) -0.007(10) C31 0.069(6) 0.073(7) 0.041(5) 0.002(5) -0.011(5) -0.018(5) C32 0.137(10) 0.054(7) 0.048(6) -0.012(5) -0.012(6) -0.022(7) C33 0.225(16) 0.060(8) 0.051(7) -0.018(6) -0.019(8) 0.007(10) C34 0.27(2) 0.117(11) 0.036(7) 0.012(7) -0.014(9) -0.027(14) C35 0.067(8) 0.53(4) 0.087(11) 0.130(18) -0.005(7) 0.012(16) C36 0.052(5) 0.056(6) 0.056(6) -0.010(5) 0.008(5) 0.009(5) C37 0.072(6) 0.042(6) 0.088(8) 0.011(5) 0.043(6) 0.014(5) C38 0.077(7) 0.052(6) 0.095(9) -0.007(6) 0.043(7) 0.004(6) C39 0.098(8) 0.116(10) 0.051(6) -0.030(6) -0.001(6) -0.050(8) C40 0.117(9) 0.081(8) 0.058(7) -0.027(6) 0.005(6) -0.043(7) N1 0.024(3) 0.043(4) 0.022(3) -0.005(3) -0.006(2) 0.004(3) N2 0.013(3) 0.089(5) 0.029(3) -0.006(3) -0.009(2) 0.000(3) N5 0.039(3) 0.031(3) 0.025(3) 0.002(2) 0.001(3) 0.001(3) N6 0.084(5) 0.027(3) 0.025(3) -0.008(2) -0.001(4) -0.001(4) N9 0.062(4) 0.060(5) 0.042(4) -0.008(4) -0.007(4) -0.006(4) N10 0.065(5) 0.074(6) 0.042(4) -0.008(4) -0.005(4) 0.003(4) N11 0.051(4) 0.069(5) 0.042(4) 0.007(4) 0.007(4) 0.021(4) N12 0.064(5) 0.113(7) 0.034(4) -0.002(4) 0.005(4) 0.002(5) N13 0.126(8) 0.063(6) 0.040(5) 0.000(4) -0.017(5) -0.002(6) N14 0.067(5) 0.062(5) 0.044(4) -0.005(4) -0.010(4) -0.019(4) N15 0.058(4) 0.062(5) 0.050(5) -0.005(4) 0.007(4) 0.003(4) N16 0.064(5) 0.061(5) 0.047(4) -0.018(4) 0.018(4) -0.017(4) O1 0.035(2) 0.041(3) 0.016(2) 0.0004(19) -0.0012(19) 0.000(3) O2 0.048(3) 0.089(5) 0.042(3) 0.001(3) -0.008(3) 0.007(3) O3 0.095(4) 0.023(3) 0.050(3) 0.006(2) 0.001(3) 0.000(3) O4 0.081(4) 0.088(5) 0.050(4) -0.017(3) -0.003(3) 0.019(4) O5 0.033(3) 0.082(5) 0.044(3) 0.004(3) 0.011(2) 0.010(3) O6 0.075(4) 0.080(5) 0.032(3) -0.002(3) -0.016(3) 0.004(4) O7 0.069(4) 0.046(3) 0.037(3) 0.007(3) -0.005(3) 0.020(3) O8 0.048(3) 0.043(3) 0.023(2) -0.002(2) -0.005(2) 0.001(3) O9 0.041(3) 0.088(5) 0.038(3) 0.003(3) 0.008(3) -0.028(3) O10 0.087(4) 0.062(4) 0.036(3) -0.012(3) -0.001(3) -0.006(4) O11 0.030(3) 0.057(4) 0.041(3) 0.007(3) -0.001(2) -0.008(3) O12 0.037(3) 0.047(3) 0.044(3) -0.008(3) 0.001(2) 0.016(3) O13 0.054(3) 0.031(3) 0.046(3) -0.007(2) 0.001(3) 0.006(3) O14 0.040(3) 0.048(4) 0.067(4) -0.010(3) 0.020(3) 0.002(3) O15 0.040(3) 0.038(3) 0.041(3) 0.000(2) -0.008(2) -0.009(2) O16 0.045(3) 0.033(3) 0.035(3) -0.005(2) -0.006(2) -0.006(2) O17 0.031(3) 0.039(3) 0.049(3) 0.004(2) -0.012(2) 0.008(2) O18 0.052(3) 0.046(4) 0.086(5) 0.019(3) 0.031(3) -0.003(3) O19 0.045(3) 0.037(3) 0.086(4) 0.029(3) 0.011(3) -0.004(3) O20 0.050(3) 0.045(4) 0.094(5) 0.023(3) -0.019(3) 0.005(3) O21 0.037(3) 0.053(4) 0.045(3) 0.000(3) -0.014(3) -0.013(3) O22 0.055(3) 0.041(3) 0.046(3) 0.002(3) 0.004(3) -0.022(3) O23 0.052(3) 0.034(3) 0.037(3) 0.004(2) -0.010(2) 0.010(3) O24 0.050(3) 0.030(3) 0.063(4) -0.006(3) 0.017(3) 0.003(3) O25 0.046(3) 0.039(3) 0.055(3) 0.011(3) 0.008(3) 0.008(3) O26 0.025(2) 0.057(4) 0.039(3) -0.005(3) 0.002(2) -0.001(2) O1W 0.050(6) 0.151(12) 0.173(12) 0.057(10) 0.000 0.000 O2W 0.113(9) 0.079(9) 0.177(12) 0.000 -0.032(10) 0.000 _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 V1 O1 1.593(4) . ? V1 O19 1.908(5) . ? V1 O17 1.928(4) . ? V1 O16 1.930(5) . ? V1 O14 1.931(5) . ? V2 O10 1.598(5) . ? V2 O19 1.691(5) . ? V2 O22 1.785(5) . ? V2 O23 1.800(5) . ? V3 O5 1.608(5) . ? V3 O17 1.683(5) . ? V3 O26 1.791(5) . ? V3 O25 1.794(5) . ? V4 O3 1.619(5) . ? V4 O16 1.671(5) . ? V4 O13 1.782(5) . ? V4 O15 1.790(5) . ? V5 O4 1.595(6) . ? V5 O20 1.665(5) . ? V5 O12 1.786(5) . ? V5 O13 1.802(5) . ? V5 V6 3.1076(18) . ? V6 O2 1.613(5) . ? V6 O14 1.661(5) . ? V6 O11 1.782(5) . ? V6 O12 1.799(5) . ? V7 O9 1.615(5) . ? V7 O21 1.686(5) . ? V7 O11 1.784(5) . ? V7 O22 1.802(5) . ? V8 O8 1.596(4) . ? V8 O18 1.909(5) . ? V8 O20 1.926(5) . ? V8 O21 1.938(5) . ? V8 O24 1.941(5) . ? V9 O7 1.612(5) . ? V9 O24 1.678(5) . ? V9 O25 1.787(5) . ? V9 O23 1.797(5) . ? V10 O6 1.613(5) . ? V10 O18 1.682(5) . ? V10 O15 1.788(5) . ? V10 O26 1.803(5) . ? Cu1 N1 1.988(5) . ? Cu1 N4 1.989(5) 7_457 ? Cu1 N8 1.990(6) 8_547 ? Cu1 N5 1.992(5) . ? Cu1 O1 2.331(4) . ? Cu2 N11 1.861(7) . ? Cu2 N9 1.889(7) . ? Cu3 N15 1.866(7) . ? Cu3 N14 1.876(7) . ? C1 N1 1.328(8) . ? C1 N2 1.337(8) . ? C1 H1 0.9300 . ? C2 C3 1.355(9) . ? C2 N1 1.386(8) . ? C2 H2 0.9300 . ? C3 N2 1.381(9) . ? C3 H3 0.9300 . ? C4 N2 1.448(8) . ? C4 C5 1.506(13) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.555(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.444(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N3 1.482(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N4 1.316(9) . ? C8 N3 1.363(10) . ? C8 H8 0.9300 . ? C9 C10 1.340(10) . ? C9 N4 1.364(8) . ? C9 H9 0.9300 . ? C10 N3 1.372(10) . ? C10 H10 0.9300 . ? C11 N5 1.332(8) . ? C11 N6 1.352(9) . ? C11 H11 0.9300 . ? C12 C13 1.355(9) . ? C12 N5 1.356(8) . ? C12 H12 0.9300 . ? C13 N6 1.356(9) . ? C13 H13 0.9300 . ? C14 N6 1.454(9) . ? C14 C15 1.489(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.545(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.509(12) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N7 1.490(9) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N7 1.323(9) . ? C18 N8 1.334(9) . ? C18 H18 0.9300 . ? C19 C20 1.346(11) . ? C19 N7 1.370(9) . ? C19 H19 0.9300 . ? C20 N8 1.376(9) . ? C20 H20 0.9300 . ? C21 N9 1.282(10) . ? C21 N10 1.343(10) . ? C21 H21 0.9300 . ? C22 C23 1.323(13) . ? C22 N9 1.357(11) . ? C22 H22 0.9300 . ? C23 N10 1.372(12) . ? C23 H23 0.9300 . ? C24 C25 1.477(13) . ? C24 N10 1.495(12) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C25 1.508(17) 4_657 ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N12 1.293(10) . ? C26 N11 1.301(10) . ? C26 H26 0.9300 . ? C27 C28 1.381(12) . ? C27 N11 1.388(11) . ? C27 H27 0.9300 . ? C28 N12 1.431(12) . ? C28 H28 0.9300 . ? C29 C30 1.413(15) . ? C29 N12 1.469(10) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C30 1.542(18) 4_656 ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 N13 1.295(11) . ? C31 N14 1.309(10) . ? C31 H31 0.9300 . ? C32 N14 1.337(12) . ? C32 C33 1.348(13) . ? C32 H32 0.9300 . ? C33 N13 1.364(13) . ? C33 H33 0.9300 . ? C34 C35 1.464(19) . ? C34 N13 1.495(12) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C35 1.51(2) 3_566 ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N15 1.321(10) . ? C36 N16 1.351(10) . ? C36 H36 0.9300 . ? C37 C38 1.331(14) . ? C37 N15 1.389(10) . ? C37 H37 0.9300 . ? C38 N16 1.395(12) . ? C38 H38 0.9300 . ? C39 N16 1.483(11) . ? C39 C40 1.512(14) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C40 1.478(18) 3_567 ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? N4 Cu1 1.989(5) 7_557 ? N8 Cu1 1.990(5) 8_557 ? 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 O1 V1 O19 107.7(2) . . ? O1 V1 O17 104.6(2) . . ? O19 V1 O17 85.6(2) . . ? O1 V1 O16 104.9(2) . . ? O19 V1 O16 147.4(2) . . ? O17 V1 O16 87.1(2) . . ? O1 V1 O14 105.2(2) . . ? O19 V1 O14 85.1(2) . . ? O17 V1 O14 150.3(2) . . ? O16 V1 O14 85.7(2) . . ? O10 V2 O19 111.0(3) . . ? O10 V2 O22 106.5(3) . . ? O19 V2 O22 109.0(3) . . ? O10 V2 O23 108.5(3) . . ? O19 V2 O23 110.7(3) . . ? O22 V2 O23 111.0(2) . . ? O5 V3 O17 108.0(3) . . ? O5 V3 O26 108.8(3) . . ? O17 V3 O26 110.7(2) . . ? O5 V3 O25 107.4(3) . . ? O17 V3 O25 110.4(2) . . ? O26 V3 O25 111.5(2) . . ? O3 V4 O16 108.4(2) . . ? O3 V4 O13 109.2(3) . . ? O16 V4 O13 110.8(2) . . ? O3 V4 O15 108.3(3) . . ? O16 V4 O15 110.3(2) . . ? O13 V4 O15 109.8(2) . . ? O4 V5 O20 108.7(3) . . ? O4 V5 O12 109.3(3) . . ? O20 V5 O12 109.0(3) . . ? O4 V5 O13 108.3(3) . . ? O20 V5 O13 110.1(3) . . ? O12 V5 O13 111.3(2) . . ? O4 V5 V6 136.4(2) . . ? O20 V5 V6 85.1(2) . . ? O12 V5 V6 30.02(15) . . ? O13 V5 V6 104.70(16) . . ? O2 V6 O14 109.6(3) . . ? O2 V6 O11 108.6(3) . . ? O14 V6 O11 109.7(3) . . ? O2 V6 O12 108.7(3) . . ? O14 V6 O12 109.3(2) . . ? O11 V6 O12 110.8(2) . . ? O2 V6 V5 134.1(2) . . ? O14 V6 V5 83.80(19) . . ? O11 V6 V5 107.09(16) . . ? O12 V6 V5 29.79(15) . . ? O9 V7 O21 109.9(3) . . ? O9 V7 O11 107.1(3) . . ? O21 V7 O11 110.6(2) . . ? O9 V7 O22 108.0(3) . . ? O21 V7 O22 110.0(2) . . ? O11 V7 O22 111.2(2) . . ? O8 V8 O18 107.7(3) . . ? O8 V8 O20 103.2(3) . . ? O18 V8 O20 83.8(3) . . ? O8 V8 O21 107.3(2) . . ? O18 V8 O21 144.9(3) . . ? O20 V8 O21 86.4(2) . . ? O8 V8 O24 105.2(2) . . ? O18 V8 O24 86.0(2) . . ? O20 V8 O24 151.6(3) . . ? O21 V8 O24 86.9(2) . . ? O7 V9 O24 108.7(3) . . ? O7 V9 O25 108.2(3) . . ? O24 V9 O25 111.7(3) . . ? O7 V9 O23 107.6(3) . . ? O24 V9 O23 109.9(2) . . ? O25 V9 O23 110.6(2) . . ? O6 V10 O18 110.2(3) . . ? O6 V10 O15 107.9(3) . . ? O18 V10 O15 110.0(2) . . ? O6 V10 O26 110.1(3) . . ? O18 V10 O26 107.6(3) . . ? O15 V10 O26 111.0(2) . . ? N1 Cu1 N4 177.1(2) . 7_457 ? N1 Cu1 N8 89.1(2) . 8_547 ? N4 Cu1 N8 90.2(2) 7_457 8_547 ? N1 Cu1 N5 89.9(2) . . ? N4 Cu1 N5 90.7(2) 7_457 . ? N8 Cu1 N5 176.2(2) 8_547 . ? N1 Cu1 O1 91.48(18) . . ? N4 Cu1 O1 91.43(19) 7_457 . ? N8 Cu1 O1 94.20(18) 8_547 . ? N5 Cu1 O1 89.48(18) . . ? N11 Cu2 N9 174.9(3) . . ? N15 Cu3 N14 178.6(3) . . ? N1 C1 N2 111.8(6) . . ? N1 C1 H1 124.1 . . ? N2 C1 H1 124.1 . . ? C3 C2 N1 108.9(6) . . ? C3 C2 H2 125.6 . . ? N1 C2 H2 125.6 . . ? C2 C3 N2 107.1(6) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? N2 C4 C5 110.5(7) . . ? N2 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 114.5(8) . . ? C4 C5 H5A 108.6 . . ? C6 C5 H5A 108.6 . . ? C4 C5 H5B 108.6 . . ? C6 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C7 C6 C5 112.3(8) . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6B 109.1 . . ? C5 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? C6 C7 N3 111.3(8) . . ? C6 C7 H7A 109.4 . . ? N3 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? N3 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? N4 C8 N3 109.3(7) . . ? N4 C8 H8 125.3 . . ? N3 C8 H8 125.3 . . ? C10 C9 N4 109.8(7) . . ? C10 C9 H9 125.1 . . ? N4 C9 H9 125.1 . . ? C9 C10 N3 106.2(7) . . ? C9 C10 H10 126.9 . . ? N3 C10 H10 126.9 . . ? N5 C11 N6 111.1(6) . . ? N5 C11 H11 124.5 . . ? N6 C11 H11 124.5 . . ? C13 C12 N5 110.9(6) . . ? C13 C12 H12 124.5 . . ? N5 C12 H12 124.5 . . ? C12 C13 N6 105.9(6) . . ? C12 C13 H13 127.0 . . ? N6 C13 H13 127.0 . . ? N6 C14 C15 112.3(7) . . ? N6 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N6 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 111.3(7) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 113.3(7) . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? C15 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? N7 C17 C16 111.7(7) . . ? N7 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? N7 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? N7 C18 N8 111.2(7) . . ? N7 C18 H18 124.4 . . ? N8 C18 H18 124.4 . . ? C20 C19 N7 106.1(7) . . ? C20 C19 H19 126.9 . . ? N7 C19 H19 126.9 . . ? C19 C20 N8 109.8(7) . . ? C19 C20 H20 125.1 . . ? N8 C20 H20 125.1 . . ? N9 C21 N10 110.8(8) . . ? N9 C21 H21 124.6 . . ? N10 C21 H21 124.6 . . ? C23 C22 N9 109.3(9) . . ? C23 C22 H22 125.3 . . ? N9 C22 H22 125.3 . . ? C22 C23 N10 106.5(8) . . ? C22 C23 H23 126.8 . . ? N10 C23 H23 126.8 . . ? C25 C24 N10 115.3(9) . . ? C25 C24 H24A 108.5 . . ? N10 C24 H24A 108.5 . . ? C25 C24 H24B 108.5 . . ? N10 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C24 C25 C25 115.3(10) . 4_657 ? C24 C25 H25A 108.4 . . ? C25 C25 H25A 108.4 4_657 . ? C24 C25 H25B 108.4 . . ? C25 C25 H25B 108.4 4_657 . ? H25A C25 H25B 107.5 . . ? N12 C26 N11 115.3(8) . . ? N12 C26 H26 122.4 . . ? N11 C26 H26 122.4 . . ? C28 C27 N11 109.2(8) . . ? C28 C27 H27 125.4 . . ? N11 C27 H27 125.4 . . ? C27 C28 N12 104.2(9) . . ? C27 C28 H28 127.9 . . ? N12 C28 H28 127.9 . . ? C30 C29 N12 113.4(10) . . ? C30 C29 H29A 108.9 . . ? N12 C29 H29A 108.9 . . ? C30 C29 H29B 108.9 . . ? N12 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C29 C30 C30 114.6(10) . 4_656 ? C29 C30 H30A 108.6 . . ? C30 C30 H30A 108.6 4_656 . ? C29 C30 H30B 108.6 . . ? C30 C30 H30B 108.6 4_656 . ? H30A C30 H30B 107.6 . . ? N13 C31 N14 112.1(9) . . ? N13 C31 H31 124.0 . . ? N14 C31 H31 124.0 . . ? N14 C32 C33 109.2(10) . . ? N14 C32 H32 125.4 . . ? C33 C32 H32 125.4 . . ? C32 C33 N13 105.8(10) . . ? C32 C33 H33 127.1 . . ? N13 C33 H33 127.1 . . ? C35 C34 N13 113.9(11) . . ? C35 C34 H34A 108.8 . . ? N13 C34 H34A 108.8 . . ? C35 C34 H34B 108.8 . . ? N13 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C34 C35 C35 109.4(15) . 3_566 ? C34 C35 H35A 109.8 . . ? C35 C35 H35A 109.8 3_566 . ? C34 C35 H35B 109.8 . . ? C35 C35 H35B 109.8 3_566 . ? H35A C35 H35B 108.2 . . ? N15 C36 N16 109.4(7) . . ? N15 C36 H36 125.3 . . ? N16 C36 H36 125.3 . . ? C38 C37 N15 109.9(10) . . ? C38 C37 H37 125.0 . . ? N15 C37 H37 125.0 . . ? C37 C38 N16 105.6(9) . . ? C37 C38 H38 127.2 . . ? N16 C38 H38 127.2 . . ? N16 C39 C40 114.5(8) . . ? N16 C39 H39A 108.6 . . ? C40 C39 H39A 108.6 . . ? N16 C39 H39B 108.6 . . ? C40 C39 H39B 108.6 . . ? H39A C39 H39B 107.6 . . ? C40 C40 C39 113.7(11) 3_567 . ? C40 C40 H40A 108.8 3_567 . ? C39 C40 H40A 108.8 . . ? C40 C40 H40B 108.8 3_567 . ? C39 C40 H40B 108.8 . . ? H40A C40 H40B 107.7 . . ? C1 N1 C2 105.5(5) . . ? C1 N1 Cu1 126.7(4) . . ? C2 N1 Cu1 127.7(4) . . ? C1 N2 C3 106.6(5) . . ? C1 N2 C4 126.0(6) . . ? C3 N2 C4 127.3(6) . . ? C8 N3 C10 107.5(7) . . ? C8 N3 C7 123.2(7) . . ? C10 N3 C7 129.2(7) . . ? C8 N4 C9 107.1(6) . . ? C8 N4 Cu1 123.1(5) . 7_557 ? C9 N4 Cu1 129.7(5) . 7_557 ? C11 N5 C12 104.7(6) . . ? C11 N5 Cu1 127.2(5) . . ? C12 N5 Cu1 128.1(4) . . ? C11 N6 C13 107.2(6) . . ? C11 N6 C14 125.7(6) . . ? C13 N6 C14 127.0(6) . . ? C18 N7 C19 107.9(7) . . ? C18 N7 C17 123.7(6) . . ? C19 N7 C17 128.2(7) . . ? C18 N8 C20 105.0(6) . . ? C18 N8 Cu1 124.9(5) . 8_557 ? C20 N8 Cu1 129.9(5) . 8_557 ? C21 N9 C22 107.1(8) . . ? C21 N9 Cu2 122.2(6) . . ? C22 N9 Cu2 130.7(7) . . ? C21 N10 C23 106.3(8) . . ? C21 N10 C24 126.2(9) . . ? C23 N10 C24 127.6(8) . . ? C26 N11 C27 105.0(7) . . ? C26 N11 Cu2 129.7(6) . . ? C27 N11 Cu2 125.2(5) . . ? C26 N12 C28 106.3(8) . . ? C26 N12 C29 128.6(9) . . ? C28 N12 C29 125.1(9) . . ? C31 N13 C33 107.0(8) . . ? C31 N13 C34 125.5(10) . . ? C33 N13 C34 127.4(9) . . ? C31 N14 C32 105.9(8) . . ? C31 N14 Cu3 127.8(7) . . ? C32 N14 Cu3 126.1(6) . . ? C36 N15 C37 106.8(8) . . ? C36 N15 Cu3 121.9(6) . . ? C37 N15 Cu3 131.2(7) . . ? C36 N16 C38 108.2(8) . . ? C36 N16 C39 123.3(8) . . ? C38 N16 C39 128.4(8) . . ? V1 O1 Cu1 172.3(3) . . ? V6 O11 V7 138.9(3) . . ? V5 O12 V6 120.2(3) . . ? V4 O13 V5 135.7(3) . . ? V6 O14 V1 169.5(4) . . ? V10 O15 V4 125.9(3) . . ? V4 O16 V1 158.1(3) . . ? V3 O17 V1 161.4(3) . . ? V10 O18 V8 164.7(4) . . ? V2 O19 V1 174.5(4) . . ? V5 O20 V8 174.9(4) . . ? V7 O21 V8 153.5(3) . . ? V2 O22 V7 128.5(3) . . ? V9 O23 V2 126.4(3) . . ? V9 O24 V8 157.7(3) . . ? V9 O25 V3 137.4(3) . . ? V3 O26 V10 123.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 V5 V6 O2 -68.6(5) . . . . ? O20 V5 V6 O2 179.2(4) . . . . ? O12 V5 V6 O2 -37.6(5) . . . . ? O13 V5 V6 O2 69.6(3) . . . . ? O4 V5 V6 O14 179.9(4) . . . . ? O20 V5 V6 O14 67.7(3) . . . . ? O12 V5 V6 O14 -149.0(4) . . . . ? O13 V5 V6 O14 -41.8(3) . . . . ? O4 V5 V6 O11 71.1(4) . . . . ? O20 V5 V6 O11 -41.1(3) . . . . ? O12 V5 V6 O11 102.2(4) . . . . ? O13 V5 V6 O11 -150.6(2) . . . . ? O4 V5 V6 O12 -31.0(5) . . . . ? O20 V5 V6 O12 -143.2(4) . . . . ? O13 V5 V6 O12 107.2(4) . . . . ? N1 C2 C3 N2 0.0(10) . . . . ? N2 C4 C5 C6 177.5(7) . . . . ? C4 C5 C6 C7 60.3(11) . . . . ? C5 C6 C7 N3 171.0(8) . . . . ? N4 C9 C10 N3 -2.7(9) . . . . ? N5 C12 C13 N6 -3.1(9) . . . . ? N6 C14 C15 C16 171.3(8) . . . . ? C14 C15 C16 C17 60.7(11) . . . . ? C15 C16 C17 N7 175.4(7) . . . . ? N7 C19 C20 N8 0.3(9) . . . . ? N9 C22 C23 N10 0.1(10) . . . . ? N10 C24 C25 C25 48.1(11) . . . 4_657 ? N11 C27 C28 N12 -0.9(16) . . . . ? N12 C29 C30 C30 179.5(15) . . . 4_656 ? N14 C32 C33 N13 -0.3(16) . . . . ? N13 C34 C35 C35 -174.2(16) . . . 3_566 ? N15 C37 C38 N16 -1.1(11) . . . . ? N16 C39 C40 C40 53.6(10) . . . 3_567 ? N2 C1 N1 C2 -3.6(9) . . . . ? N2 C1 N1 Cu1 176.2(5) . . . . ? C3 C2 N1 C1 2.1(9) . . . . ? C3 C2 N1 Cu1 -177.7(6) . . . . ? N8 Cu1 N1 C1 -112.2(6) 8_547 . . . ? N5 Cu1 N1 C1 64.1(6) . . . . ? O1 Cu1 N1 C1 153.6(6) . . . . ? N8 Cu1 N1 C2 67.6(6) 8_547 . . . ? N5 Cu1 N1 C2 -116.1(6) . . . . ? O1 Cu1 N1 C2 -26.6(6) . . . . ? N1 C1 N2 C3 3.7(10) . . . . ? N1 C1 N2 C4 -178.6(8) . . . . ? C2 C3 N2 C1 -2.2(10) . . . . ? C2 C3 N2 C4 -179.9(8) . . . . ? C5 C4 N2 C1 89.5(10) . . . . ? C5 C4 N2 C3 -93.2(10) . . . . ? N4 C8 N3 C10 0.5(10) . . . . ? N4 C8 N3 C7 -176.0(7) . . . . ? C9 C10 N3 C8 1.3(10) . . . . ? C9 C10 N3 C7 177.6(8) . . . . ? C6 C7 N3 C8 67.3(11) . . . . ? C6 C7 N3 C10 -108.5(10) . . . . ? N3 C8 N4 C9 -2.2(9) . . . . ? N3 C8 N4 Cu1 174.8(5) . . . 7_557 ? C10 C9 N4 C8 3.0(9) . . . . ? C10 C9 N4 Cu1 -173.7(5) . . . 7_557 ? N6 C11 N5 C12 -2.6(9) . . . . ? N6 C11 N5 Cu1 176.8(5) . . . . ? C13 C12 N5 C11 3.5(9) . . . . ? C13 C12 N5 Cu1 -175.9(5) . . . . ? N1 Cu1 N5 C11 -101.9(7) . . . . ? N4 Cu1 N5 C11 75.2(7) 7_457 . . . ? O1 Cu1 N5 C11 166.6(7) . . . . ? N1 Cu1 N5 C12 77.3(6) . . . . ? N4 Cu1 N5 C12 -105.6(6) 7_457 . . . ? O1 Cu1 N5 C12 -14.2(6) . . . . ? N5 C11 N6 C13 0.8(10) . . . . ? N5 C11 N6 C14 -176.0(8) . . . . ? C12 C13 N6 C11 1.4(9) . . . . ? C12 C13 N6 C14 178.1(8) . . . . ? C15 C14 N6 C11 60.2(13) . . . . ? C15 C14 N6 C13 -116.0(9) . . . . ? N8 C18 N7 C19 -0.7(9) . . . . ? N8 C18 N7 C17 -175.5(7) . . . . ? C20 C19 N7 C18 0.2(9) . . . . ? C20 C19 N7 C17 174.7(8) . . . . ? C16 C17 N7 C18 91.3(10) . . . . ? C16 C17 N7 C19 -82.4(10) . . . . ? N7 C18 N8 C20 0.9(8) . . . . ? N7 C18 N8 Cu1 176.7(5) . . . 8_557 ? C19 C20 N8 C18 -0.7(8) . . . . ? C19 C20 N8 Cu1 -176.2(5) . . . 8_557 ? N10 C21 N9 C22 0.6(10) . . . . ? N10 C21 N9 Cu2 -178.4(5) . . . . ? C23 C22 N9 C21 -0.4(10) . . . . ? C23 C22 N9 Cu2 178.4(6) . . . . ? N9 C21 N10 C23 -0.5(10) . . . . ? N9 C21 N10 C24 178.0(8) . . . . ? C22 C23 N10 C21 0.2(10) . . . . ? C22 C23 N10 C24 -178.2(8) . . . . ? C25 C24 N10 C21 -94.6(12) . . . . ? C25 C24 N10 C23 83.6(13) . . . . ? N12 C26 N11 C27 -0.3(12) . . . . ? N12 C26 N11 Cu2 177.3(7) . . . . ? C28 C27 N11 C26 0.8(14) . . . . ? C28 C27 N11 Cu2 -176.9(9) . . . . ? N11 C26 N12 C28 -0.3(13) . . . . ? N11 C26 N12 C29 177.9(10) . . . . ? C27 C28 N12 C26 0.7(15) . . . . ? C27 C28 N12 C29 -177.5(11) . . . . ? C30 C29 N12 C26 130.5(13) . . . . ? C30 C29 N12 C28 -51.7(18) . . . . ? N14 C31 N13 C33 -0.4(13) . . . . ? N14 C31 N13 C34 -179.7(10) . . . . ? C32 C33 N13 C31 0.4(15) . . . . ? C32 C33 N13 C34 179.6(11) . . . . ? C35 C34 N13 C31 135.3(14) . . . . ? C35 C34 N13 C33 -44(2) . . . . ? N13 C31 N14 C32 0.3(11) . . . . ? N13 C31 N14 Cu3 174.8(7) . . . . ? C33 C32 N14 C31 0.0(13) . . . . ? C33 C32 N14 Cu3 -174.6(8) . . . . ? N16 C36 N15 C37 -0.2(10) . . . . ? N16 C36 N15 Cu3 179.1(6) . . . . ? C38 C37 N15 C36 0.8(11) . . . . ? C38 C37 N15 Cu3 -178.4(7) . . . . ? N15 C36 N16 C38 -0.4(10) . . . . ? N15 C36 N16 C39 176.9(8) . . . . ? C37 C38 N16 C36 0.9(10) . . . . ? C37 C38 N16 C39 -176.2(9) . . . . ? C40 C39 N16 C36 -98.0(11) . . . . ? C40 C39 N16 C38 78.7(13) . . . . ? O2 V6 O11 V7 -154.5(4) . . . . ? O14 V6 O11 V7 -34.6(5) . . . . ? O12 V6 O11 V7 86.1(5) . . . . ? V5 V6 O11 V7 54.8(5) . . . . ? O9 V7 O11 V6 -156.3(4) . . . . ? O21 V7 O11 V6 -36.5(5) . . . . ? O22 V7 O11 V6 85.9(5) . . . . ? O4 V5 O12 V6 157.9(4) . . . . ? O20 V5 O12 V6 39.1(4) . . . . ? O13 V5 O12 V6 -82.5(4) . . . . ? O2 V6 O12 V5 152.4(3) . . . . ? O14 V6 O12 V5 32.8(4) . . . . ? O11 V6 O12 V5 -88.2(3) . . . . ? O3 V4 O13 V5 -162.5(4) . . . . ? O16 V4 O13 V5 -43.2(5) . . . . ? O15 V4 O13 V5 78.9(4) . . . . ? O4 V5 O13 V4 -143.7(4) . . . . ? O20 V5 O13 V4 -24.9(5) . . . . ? O12 V5 O13 V4 96.1(4) . . . . ? V6 V5 O13 V4 65.3(4) . . . . ? O2 V6 O14 V1 112(2) . . . . ? O11 V6 O14 V1 -7(2) . . . . ? O12 V6 O14 V1 -129.1(19) . . . . ? V5 V6 O14 V1 -113(2) . . . . ? O1 V1 O14 V6 -109(2) . . . . ? O19 V1 O14 V6 -2(2) . . . . ? O17 V1 O14 V6 70(2) . . . . ? O16 V1 O14 V6 147(2) . . . . ? O6 V10 O15 V4 151.6(4) . . . . ? O18 V10 O15 V4 31.4(4) . . . . ? O26 V10 O15 V4 -87.6(4) . . . . ? O3 V4 O15 V10 153.8(3) . . . . ? O16 V4 O15 V10 35.3(4) . . . . ? O13 V4 O15 V10 -87.1(4) . . . . ? O3 V4 O16 V1 162.8(8) . . . . ? O13 V4 O16 V1 43.0(9) . . . . ? O15 V4 O16 V1 -78.8(9) . . . . ? O1 V1 O16 V4 -158.5(8) . . . . ? O19 V1 O16 V4 20.0(11) . . . . ? O17 V1 O16 V4 97.2(8) . . . . ? O14 V1 O16 V4 -54.0(8) . . . . ? O5 V3 O17 V1 175.3(9) . . . . ? O26 V3 O17 V1 56.3(10) . . . . ? O25 V3 O17 V1 -67.6(10) . . . . ? O1 V1 O17 V3 -176.4(10) . . . . ? O19 V1 O17 V3 76.4(10) . . . . ? O16 V1 O17 V3 -71.8(10) . . . . ? O14 V1 O17 V3 4.4(13) . . . . ? O6 V10 O18 V8 -18.3(15) . . . . ? O15 V10 O18 V8 100.5(14) . . . . ? O26 V10 O18 V8 -138.4(13) . . . . ? O8 V8 O18 V10 11.2(14) . . . . ? O20 V8 O18 V10 -90.7(14) . . . . ? O21 V8 O18 V10 -165.3(12) . . . . ? O24 V8 O18 V10 115.9(14) . . . . ? O9 V7 O21 V8 174.1(7) . . . . ? O11 V7 O21 V8 56.0(8) . . . . ? O22 V7 O21 V8 -67.2(8) . . . . ? O8 V8 O21 V7 -171.1(7) . . . . ? O18 V8 O21 V7 5.4(10) . . . . ? O20 V8 O21 V7 -68.4(8) . . . . ? O24 V8 O21 V7 83.9(8) . . . . ? O10 V2 O22 V7 146.4(4) . . . . ? O19 V2 O22 V7 26.6(5) . . . . ? O23 V2 O22 V7 -95.6(4) . . . . ? O9 V7 O22 V2 168.2(4) . . . . ? O21 V7 O22 V2 48.3(4) . . . . ? O11 V7 O22 V2 -74.6(4) . . . . ? O7 V9 O23 V2 -156.5(3) . . . . ? O24 V9 O23 V2 -38.3(4) . . . . ? O25 V9 O23 V2 85.5(4) . . . . ? O10 V2 O23 V9 -156.4(3) . . . . ? O19 V2 O23 V9 -34.4(4) . . . . ? O22 V2 O23 V9 86.8(4) . . . . ? O7 V9 O24 V8 -165.0(8) . . . . ? O25 V9 O24 V8 -45.7(9) . . . . ? O23 V9 O24 V8 77.5(9) . . . . ? O8 V8 O24 V9 153.6(8) . . . . ? O18 V8 O24 V9 46.3(9) . . . . ? O20 V8 O24 V9 -22.6(11) . . . . ? O21 V8 O24 V9 -99.3(9) . . . . ? O7 V9 O25 V3 164.3(5) . . . . ? O24 V9 O25 V3 44.8(6) . . . . ? O23 V9 O25 V3 -78.0(5) . . . . ? O5 V3 O25 V9 149.7(5) . . . . ? O17 V3 O25 V9 32.2(6) . . . . ? O26 V3 O25 V9 -91.3(5) . . . . ? O5 V3 O26 V10 -165.2(3) . . . . ? O17 V3 O26 V10 -46.7(4) . . . . ? O25 V3 O26 V10 76.6(4) . . . . ? O6 V10 O26 V3 -140.4(3) . . . . ? O18 V10 O26 V3 -20.3(4) . . . . ? O15 V10 O26 V3 100.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.646 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.096