# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_i4122 _database_code_depnum_ccdc_archive 'CCDC 900272' #TrackingRef 'I4122-900272.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H76 Cl Cu5 N20 O38.5 V16' _chemical_formula_weight 3077.8 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' Cl Cl 0.1484 0.1585 '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 tetragonal _symmetry_space_group_name_H-M I4122 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-y, x+1/2, z+1/4' 'y+1/2, -x, z+3/4' '-x+1/2, y, -z+3/4' 'x, -y+1/2, -z+1/4' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1, z+1' '-y+1/2, x+1, z+3/4' 'y+1, -x+1/2, z+5/4' '-x+1, y+1/2, -z+5/4' 'x+1/2, -y+1, -z+3/4' 'y+1, x+1, -z+1' '-y+1/2, -x+1/2, -z+1/2' _cell_length_a 27.600(4) _cell_length_b 27.600(4) _cell_length_c 26.700(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20339(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8955 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12160 _exptl_absorpt_coefficient_mu 2.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.497 _exptl_absorpt_correction_T_max 0.603 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; The high value of the final R indices and Rint might be caused by the weak diffraction of the Vanadium atoms as well as the bigger volume of the single cell. ; _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 73861 _diffrn_reflns_av_R_equivalents 0.1410 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8955 _reflns_number_gt 6078 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1242P)^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 0.07(3) _refine_ls_number_reflns 8955 _refine_ls_number_parameters 638 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2084 _refine_ls_wR_factor_gt 0.1861 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.042 _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 V1 V 0.51805(7) 0.88466(7) 0.53715(8) 0.0402(5) Uani 1 1 d . . . V2 V 0.57647(6) 1.06730(7) 0.55932(7) 0.0349(4) Uani 1 1 d . . . V3 V 0.61635(6) 1.01728(7) 0.44204(7) 0.0339(4) Uani 1 1 d . . . V4 V 0.46894(7) 0.88672(7) 0.44211(7) 0.0367(5) Uani 1 1 d . . . V5 V 0.56822(6) 0.92227(6) 0.41804(6) 0.0317(4) Uani 1 1 d . . . V6 V 0.61192(6) 0.96746(7) 0.53728(7) 0.0357(5) Uani 1 1 d . . . V7 V 0.46093(12) 1.04518(14) 0.61570(12) 0.1022(12) Uani 1 1 d . . . V8 V 0.45499(7) 0.96064(7) 0.36411(7) 0.0394(5) Uani 1 1 d . . . Cu1 Cu 0.99195(8) 0.7500 0.6250 0.0491(5) Uani 1 2 d S . . Cu2 Cu 0.75420(13) 0.30167(9) 0.43287(9) 0.1237(12) Uani 1 1 d . . . Cu3 Cu 0.72120(9) 0.66759(8) 0.55932(10) 0.0966(8) Uani 1 1 d . . . Cl1 Cl 0.5000 1.0000 0.48380(15) 0.0441(9) Uani 1 2 d S . . O1 O 0.5754(3) 0.9138(3) 0.5537(3) 0.0450(19) Uani 1 1 d . . . O2 O 0.5998(3) 0.8850(3) 0.3872(3) 0.050(2) Uani 1 1 d . . . O3 O 0.6117(3) 1.0983(3) 0.5926(3) 0.048(2) Uani 1 1 d . . . O4 O 0.6700(3) 1.0242(3) 0.4217(3) 0.046(2) Uani 1 1 d . . . O5 O 0.4548(3) 0.8333(3) 0.4229(3) 0.057(2) Uani 1 1 d . . . O6 O 0.5333(3) 0.8837(3) 0.4684(3) 0.0383(17) Uani 1 1 d . . . O7 O 0.5028(3) 0.9189(2) 0.3891(2) 0.0358(17) Uani 1 1 d . . . O8 O 0.4188(3) 0.9282(3) 0.4230(3) 0.0418(19) Uani 1 1 d . . . O9 O 0.4279(3) 0.9376(3) 0.3176(3) 0.051(2) Uani 1 1 d . . . O10 O 0.6638(3) 0.9573(3) 0.5583(3) 0.052(2) Uani 1 1 d . . . O11 O 0.5754(3) 1.0023(3) 0.5866(2) 0.0413(18) Uani 1 1 d . . . O12 O 0.6162(2) 1.0337(2) 0.5097(2) 0.0329(16) Uani 1 1 d . . . O13 O 0.5213(3) 0.8317(3) 0.5591(3) 0.054(2) Uani 1 1 d . . . O14 O 0.5116(3) 1.0761(3) 0.5859(3) 0.046(2) Uani 1 1 d . . . O15 O 0.5804(2) 0.9857(2) 0.3890(2) 0.0323(16) Uani 1 1 d . . . O16 O 0.5000 1.0000 0.3372(3) 0.038(2) Uani 1 2 d S . . O17 O 0.5000 1.0000 0.6033(3) 0.0190(18) Uani 1 2 d S . . O17' O 0.5000 1.0000 0.6515(5) 0.064(4) Uani 1 2 d S . . O18 O 0.4511(2) 0.8899(3) 0.5089(3) 0.0379(18) Uani 1 1 d . . . O19 O 0.6114(2) 0.9521(3) 0.4688(3) 0.0356(17) Uani 1 1 d . . . O20 O 0.4375(5) 1.0737(5) 0.6619(5) 0.038(3) Uiso 0.50 1 d P . . N1 N 0.9884(3) 0.7801(3) 0.5626(3) 0.040(2) Uani 1 1 d . . . N2 N 0.9805(4) 0.8368(3) 0.5048(3) 0.045(2) Uani 1 1 d D . . N3 N 0.8140(5) 0.2621(4) 0.4300(4) 0.059(3) Uani 1 1 d . . . N4 N 0.7232(4) 0.2355(4) 0.4414(4) 0.061(3) Uani 1 1 d . . . N5 N 0.7389(5) 0.3680(4) 0.4354(5) 0.067(3) Uani 1 1 d . . . N6 N 0.6963(5) 0.4343(4) 0.4317(4) 0.069(3) Uani 1 1 d . . . N9 N 0.6944(5) 0.7322(5) 0.5608(5) 0.076(4) Uiso 1 1 d . . . N10 N 0.7862(4) 0.7044(4) 0.5581(5) 0.069(3) Uani 1 1 d . . . N8 N 0.7170(5) 0.5989(5) 0.5632(6) 0.090(4) Uani 1 1 d . . . N7 N 0.6887(5) 0.5256(4) 0.5730(5) 0.073(4) Uani 1 1 d . . . C1 C 0.9853(4) 0.8260(4) 0.5540(3) 0.037(3) Uani 1 1 d . . . H1A H 0.9863 0.8493 0.5792 0.044 Uiso 1 1 calc R . . C2 C 0.9790(5) 0.7934(5) 0.4796(5) 0.055(3) Uani 1 1 d . . . H2A H 0.9752 0.7890 0.4453 0.066 Uiso 1 1 calc R . . C3 C 0.9843(5) 0.7573(5) 0.5160(5) 0.059(3) Uani 1 1 d . . . H3A H 0.9849 0.7240 0.5102 0.071 Uiso 1 1 calc R . . C4 C 0.9815(6) 0.8823(4) 0.4831(6) 0.083(5) Uiso 1 1 d D . . C6 C 0.8643(9) 0.2726(7) 0.4241(6) 0.107(7) Uani 1 1 d . . . H6A H 0.8741 0.3048 0.4222 0.128 Uiso 1 1 calc R . . C7 C 0.8994(7) 0.2358(10) 0.4211(7) 0.113(8) Uani 1 1 d . . . H7A H 0.9313 0.2450 0.4153 0.135 Uiso 1 1 calc R . . C8 C 0.8903(11) 0.1906(11) 0.4258(10) 0.142(10) Uiso 1 1 d . . . H8A H 0.9151 0.1678 0.4268 0.171 Uiso 1 1 calc R . . C9 C 0.8419(6) 0.1769(6) 0.4294(5) 0.078(5) Uani 1 1 d . . . C10 C 0.8204(8) 0.1285(8) 0.4356(7) 0.100(6) Uiso 1 1 d . . . H10A H 0.8428 0.1033 0.4354 0.120 Uiso 1 1 calc R . . C11 C 0.7790(8) 0.1156(9) 0.4408(8) 0.112(7) Uiso 1 1 d . . . H11A H 0.7713 0.0829 0.4431 0.134 Uiso 1 1 calc R . . C12 C 0.7429(7) 0.1510(7) 0.4433(5) 0.084(5) Uani 1 1 d . . . C13 C 0.6919(7) 0.1429(8) 0.4498(7) 0.095(6) Uiso 1 1 d . . . H13A H 0.6790 0.1119 0.4528 0.114 Uiso 1 1 calc R . . C14 C 0.6648(10) 0.1813(10) 0.4511(9) 0.134(8) Uiso 1 1 d . . . H14A H 0.6317 0.1753 0.4536 0.160 Uiso 1 1 calc R . . C15 C 0.6762(8) 0.2250(8) 0.4496(7) 0.103(6) Uiso 1 1 d . . . H15A H 0.6532 0.2493 0.4539 0.123 Uiso 1 1 calc R . . C16 C 0.7562(6) 0.2007(5) 0.4395(5) 0.062(4) Uani 1 1 d . . . C17 C 0.8044(5) 0.2152(5) 0.4324(5) 0.055(3) Uani 1 1 d . . . C18 C 0.6952(6) 0.3851(5) 0.4292(5) 0.065(4) Uani 1 1 d . . . H18A H 0.6676 0.3664 0.4239 0.077 Uiso 1 1 calc R . . C19 C 0.7433(5) 0.4464(6) 0.4390(6) 0.075(4) Uani 1 1 d . . . H19A H 0.7557 0.4774 0.4434 0.090 Uiso 1 1 calc R . . C20 C 0.7677(5) 0.4068(6) 0.4385(6) 0.069(4) Uani 1 1 d . . . H20A H 0.8013 0.4052 0.4401 0.083 Uiso 1 1 calc R . . C21 C 0.6527(6) 0.4658(6) 0.4325(5) 0.074(4) Uani 1 1 d . . . H21A H 0.6540 0.4885 0.4048 0.089 Uiso 1 1 calc R . . H21B H 0.6238 0.4461 0.4286 0.089 Uiso 1 1 calc R . . C22 C 0.6499(6) 0.4925(6) 0.4795(6) 0.080(5) Uiso 1 1 d . . . H22A H 0.6197 0.5105 0.4803 0.096 Uiso 1 1 calc R . . H22B H 0.6762 0.5158 0.4806 0.096 Uiso 1 1 calc R . . C23 C 0.6526(6) 0.4609(6) 0.5250(6) 0.084(5) Uani 1 1 d . . . H23A H 0.6819 0.4416 0.5234 0.101 Uiso 1 1 calc R . . H23B H 0.6252 0.4390 0.5251 0.101 Uiso 1 1 calc R . . C24 C 0.6527(6) 0.4896(7) 0.5729(7) 0.089(5) Uiso 1 1 d . . . H24A H 0.6212 0.5047 0.5774 0.107 Uiso 1 1 calc R . . H24B H 0.6580 0.4678 0.6009 0.107 Uiso 1 1 calc R . . C25 C 0.6781(5) 0.5726(5) 0.5675(6) 0.060(4) Uani 1 1 d . . . H25A H 0.6468 0.5849 0.5668 0.072 Uiso 1 1 calc R . . C26 C 0.7572(7) 0.5664(7) 0.5659(9) 0.112(7) Uani 1 1 d . . . H26A H 0.7897 0.5750 0.5637 0.135 Uiso 1 1 calc R . . C27 C 0.7399(6) 0.5211(7) 0.5723(7) 0.084(5) Uani 1 1 d . . . H27A H 0.7578 0.4927 0.5755 0.101 Uiso 1 1 calc R . . C28 C 0.6484(7) 0.7444(8) 0.5598(7) 0.105(6) Uani 1 1 d . . . H28A H 0.6248 0.7205 0.5569 0.125 Uiso 1 1 calc R . . C29 C 0.6346(9) 0.7936(9) 0.5630(8) 0.116(7) Uiso 1 1 d . . . H29A H 0.6016 0.8005 0.5632 0.139 Uiso 1 1 calc R . . C30 C 0.6661(6) 0.8319(7) 0.5659(7) 0.093(5) Uani 1 1 d . . . H30A H 0.6563 0.8641 0.5661 0.112 Uiso 1 1 calc R . . C31 C 0.7183(7) 0.8163(7) 0.5687(7) 0.091(5) Uiso 1 1 d . . . C32 C 0.7561(8) 0.8494(7) 0.5710(7) 0.097(6) Uiso 1 1 d . . . H32A H 0.7483 0.8820 0.5738 0.116 Uiso 1 1 calc R . . C33 C 0.8018(7) 0.8377(7) 0.5693(6) 0.087(6) Uani 1 1 d . . . H33A H 0.8261 0.8610 0.5695 0.104 Uiso 1 1 calc R . . C34 C 0.8122(5) 0.7890(7) 0.5673(6) 0.077(5) Uani 1 1 d . . . C35 C 0.8629(8) 0.7693(9) 0.5633(8) 0.112(7) Uiso 1 1 d . . . H35A H 0.8888 0.7909 0.5638 0.135 Uiso 1 1 calc R . . C36 C 0.8717(6) 0.7233(8) 0.5590(7) 0.096(6) Uani 1 1 d . . . H36A H 0.9032 0.7116 0.5576 0.115 Uiso 1 1 calc R . . C37 C 0.8324(7) 0.6926(6) 0.5567(6) 0.082(5) Uiso 1 1 d . . . H37A H 0.8393 0.6597 0.5538 0.098 Uiso 1 1 calc R . . C38 C 0.7789(4) 0.7546(4) 0.5621(5) 0.048(3) Uiso 1 1 d . . . C39 C 0.7293(6) 0.7691(5) 0.5633(5) 0.069(4) Uani 1 1 d . . . O1W O 0.5274(11) 0.4726(11) 0.5000 0.16(2) Uani 0.50 2 d SP . . C5 C 0.9375(11) 0.9017(17) 0.497(2) 0.134(16) Uiso 0.50 1 d PD . . C5' C 0.9626(11) 0.9267(8) 0.5074(10) 0.067(8) Uiso 0.50 1 d PD . . 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 0.0364(11) 0.0357(11) 0.0486(12) 0.0080(9) 0.0003(9) 0.0060(9) V2 0.0273(10) 0.0382(11) 0.0391(10) -0.0059(8) 0.0009(8) -0.0055(8) V3 0.0246(9) 0.0397(11) 0.0373(10) 0.0018(8) 0.0047(8) 0.0010(8) V4 0.0340(10) 0.0296(10) 0.0465(12) -0.0023(9) -0.0068(9) -0.0019(8) V5 0.0286(10) 0.0305(10) 0.0359(9) -0.0032(8) -0.0025(8) 0.0056(8) V6 0.0273(10) 0.0432(11) 0.0365(10) 0.0021(8) -0.0048(8) 0.0039(8) V7 0.086(2) 0.135(3) 0.0856(19) -0.038(2) 0.0233(17) -0.048(2) V8 0.0369(11) 0.0454(12) 0.0357(9) -0.0081(8) -0.0093(8) 0.0152(9) Cu1 0.0445(12) 0.0459(12) 0.0569(12) 0.0191(10) 0.000 0.000 Cu2 0.206(3) 0.0730(15) 0.0916(16) -0.0169(13) -0.0375(19) 0.0697(18) Cu3 0.1104(18) 0.0617(12) 0.1176(18) -0.0035(13) 0.0120(15) -0.0299(12) Cl1 0.037(2) 0.039(2) 0.057(2) 0.000 0.000 -0.0041(18) O1 0.025(4) 0.057(5) 0.053(5) 0.009(4) -0.009(4) -0.002(4) O2 0.034(4) 0.056(5) 0.061(5) -0.027(4) -0.008(4) 0.027(4) O3 0.038(4) 0.049(5) 0.056(5) -0.024(4) 0.008(4) -0.006(4) O4 0.025(4) 0.053(5) 0.059(5) 0.000(4) 0.008(4) -0.005(4) O5 0.051(5) 0.037(5) 0.085(6) -0.024(5) -0.017(5) 0.001(4) O6 0.045(5) 0.028(4) 0.042(4) -0.003(3) 0.002(3) -0.003(3) O7 0.035(4) 0.036(4) 0.037(4) -0.004(3) -0.008(3) 0.012(3) O8 0.028(4) 0.054(5) 0.044(4) -0.015(4) -0.005(3) -0.003(4) O9 0.061(6) 0.053(5) 0.040(4) -0.021(4) -0.013(4) 0.011(4) O10 0.021(4) 0.083(6) 0.053(5) 0.022(5) -0.016(4) -0.004(4) O11 0.042(5) 0.051(5) 0.031(4) -0.002(4) 0.005(3) -0.005(4) O12 0.027(4) 0.032(4) 0.040(4) -0.002(3) 0.000(3) -0.008(3) O13 0.039(5) 0.039(4) 0.083(6) 0.029(4) -0.009(4) -0.001(4) O14 0.043(5) 0.057(5) 0.038(4) 0.007(4) 0.006(4) 0.006(4) O15 0.033(4) 0.032(4) 0.032(4) 0.000(3) -0.001(3) -0.003(3) O16 0.029(6) 0.048(7) 0.036(5) 0.000 0.000 0.016(4) O17 0.019(4) 0.032(5) 0.007(4) 0.000 0.000 0.011(4) O17' 0.032(7) 0.072(9) 0.088(10) 0.000 0.000 -0.004(6) O18 0.028(4) 0.037(4) 0.049(5) -0.001(4) 0.002(3) 0.003(3) O19 0.027(4) 0.041(4) 0.038(4) 0.001(3) -0.001(3) 0.008(3) N1 0.042(5) 0.036(5) 0.043(5) -0.003(4) -0.010(4) -0.005(4) N2 0.053(6) 0.036(5) 0.045(5) 0.007(5) -0.006(5) 0.008(4) N3 0.086(9) 0.031(6) 0.061(7) 0.005(5) 0.009(6) -0.012(5) N4 0.051(7) 0.075(8) 0.057(7) -0.004(6) -0.005(6) 0.009(6) N5 0.071(8) 0.052(7) 0.077(8) -0.004(6) -0.014(7) 0.019(7) N6 0.082(9) 0.065(8) 0.060(7) 0.005(6) -0.009(7) 0.010(7) N10 0.066(8) 0.059(7) 0.080(8) 0.018(7) 0.007(7) 0.020(6) N8 0.079(10) 0.079(10) 0.113(12) -0.012(9) 0.006(9) -0.002(8) N7 0.091(10) 0.056(8) 0.072(8) -0.004(6) 0.023(7) -0.020(7) C1 0.065(8) 0.028(6) 0.018(5) 0.004(4) 0.004(5) 0.005(5) C2 0.055(8) 0.057(8) 0.054(8) -0.018(7) 0.002(6) -0.001(7) C3 0.063(9) 0.048(8) 0.066(8) -0.014(7) 0.014(7) -0.004(7) C6 0.17(2) 0.082(13) 0.072(11) -0.002(10) 0.017(13) -0.058(14) C7 0.054(10) 0.18(3) 0.101(14) 0.029(15) 0.026(10) 0.025(14) C9 0.090(12) 0.082(12) 0.061(9) 0.022(8) -0.002(9) 0.014(10) C12 0.107(14) 0.090(13) 0.055(9) -0.012(8) -0.001(9) 0.008(11) C16 0.091(12) 0.048(8) 0.047(8) -0.015(6) 0.002(8) -0.022(8) C17 0.047(8) 0.070(10) 0.046(7) -0.016(7) -0.002(6) 0.011(7) C18 0.095(12) 0.031(7) 0.068(9) -0.008(7) -0.004(8) -0.003(7) C19 0.060(9) 0.060(10) 0.104(12) -0.001(9) -0.035(9) -0.011(8) C20 0.043(8) 0.086(12) 0.079(10) -0.005(9) -0.008(8) 0.009(8) C21 0.080(11) 0.081(11) 0.061(9) 0.000(8) -0.019(8) 0.028(9) C23 0.087(12) 0.078(11) 0.086(11) -0.032(10) 0.029(9) -0.017(9) C25 0.053(8) 0.041(8) 0.087(10) -0.014(7) -0.012(7) 0.000(6) C26 0.069(12) 0.079(13) 0.19(2) -0.020(14) -0.035(14) 0.005(11) C27 0.057(10) 0.086(12) 0.109(13) 0.005(10) -0.011(9) 0.021(9) C28 0.088(13) 0.115(16) 0.110(15) -0.010(13) -0.011(11) 0.034(12) C30 0.069(11) 0.097(13) 0.113(13) 0.028(12) 0.006(11) 0.033(10) C33 0.097(14) 0.097(14) 0.065(10) 0.028(10) -0.018(9) -0.038(11) C34 0.049(9) 0.100(13) 0.082(11) 0.039(10) -0.003(8) -0.008(8) C36 0.055(10) 0.141(18) 0.092(12) 0.042(12) -0.011(9) 0.010(10) C39 0.093(11) 0.036(7) 0.078(10) 0.016(7) -0.008(9) 0.018(7) O1W 0.21(3) 0.21(3) 0.043(16) -0.003(19) -0.003(19) 0.10(4) _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 O13 1.579(8) . ? V1 O1 1.829(8) . ? V1 O14 1.881(8) 10_564 ? V1 O6 1.882(7) . ? V1 O18 2.001(7) . ? V1 V4 2.878(3) . ? V1 V7 2.913(4) 10_564 ? V1 V2 2.985(3) 10_564 ? V2 O3 1.571(7) . ? V2 O11 1.935(8) . ? V2 O14 1.940(8) . ? V2 O18 1.946(7) 10_564 ? V2 O12 1.956(7) . ? V2 V6 2.983(3) . ? V2 V1 2.985(3) 10_564 ? V3 O4 1.588(7) . ? V3 O12 1.861(7) . ? V3 O8 1.863(8) 10_564 ? V3 O15 1.936(7) . ? V3 O19 1.940(7) . ? V3 V6 2.893(3) . ? V3 V8 2.929(3) 10_564 ? V3 V5 3.009(3) . ? V4 O5 1.610(8) . ? V4 O18 1.852(7) . ? V4 O8 1.866(8) . ? V4 O6 1.913(8) . ? V4 O7 1.914(7) . ? V4 V8 2.941(3) . ? V4 V5 2.981(3) . ? V5 O2 1.580(7) . ? V5 O15 1.942(7) . ? V5 O7 1.965(7) . ? V5 O6 1.968(7) . ? V5 O19 1.983(7) . ? V6 O10 1.564(7) . ? V6 O1 1.845(8) . ? V6 O19 1.877(7) . ? V6 O11 1.917(7) . ? V6 O12 1.975(7) . ? V6 V7 2.924(4) 10_564 ? V7 O20 1.600(14) . ? V7 O17 1.682(4) . ? V7 O14 1.822(8) . ? V7 O11 1.825(8) 10_564 ? V7 O17' 1.906(8) . ? V7 O1 2.241(9) 10_564 ? V7 V1 2.913(4) 10_564 ? V7 V6 2.924(4) 10_564 ? V8 O9 1.583(7) . ? V8 O16 1.800(4) . ? V8 O7 1.875(7) . ? V8 O15 1.896(7) 10_564 ? V8 O8 2.066(8) . ? V8 V3 2.929(3) 10_564 ? Cu1 N1 1.864(9) 6_566 ? Cu1 N1 1.864(9) . ? Cu2 N5 1.880(11) . ? Cu2 N3 1.980(12) . ? Cu2 N4 2.029(12) . ? Cu3 N8 1.903(15) . ? Cu3 N9 1.930(14) . ? Cu3 N10 2.062(13) . ? O1 V7 2.241(9) 10_564 ? O8 V3 1.863(8) 10_564 ? O11 V7 1.825(8) 10_564 ? O14 V1 1.881(8) 10_564 ? O15 V8 1.896(7) 10_564 ? O16 V8 1.800(4) 10_564 ? O17 O17' 1.288(15) . ? O17 V7 1.682(4) 10_564 ? O17' V7 1.906(8) 10_564 ? O18 V2 1.946(7) 10_564 ? N1 C1 1.290(13) . ? N1 C3 1.399(15) . ? N2 C1 1.355(13) . ? N2 C2 1.375(14) . ? N2 C4 1.382(9) . ? N3 C17 1.322(17) . ? N3 C6 1.43(2) . ? N4 C16 1.327(18) . ? N4 C15 1.35(2) . ? N5 C18 1.306(18) . ? N5 C20 1.334(19) . ? N6 C19 1.356(19) . ? N6 C18 1.360(16) . ? N6 C21 1.485(18) . ? N9 C28 1.31(2) . ? N9 C39 1.40(2) . ? N10 C37 1.317(19) . ? N10 C38 1.404(16) . ? N8 C25 1.301(18) . ? N8 C26 1.43(2) . ? N7 C25 1.337(17) . ? N7 C24 1.41(2) . ? N7 C27 1.417(19) . ? C1 H1A 0.9300 . ? C2 C3 1.401(18) . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4 C5 1.378(10) . ? C4 C5' 1.482(10) . ? C6 C7 1.41(3) . ? C6 H6A 0.9300 . ? C7 C8 1.28(3) . ? C7 H7A 0.9300 . ? C8 C9 1.39(3) . ? C8 H8A 0.9300 . ? C9 C10 1.47(2) . ? C9 C17 1.48(2) . ? C10 C11 1.20(2) . ? C10 H10A 0.9300 . ? C11 C12 1.40(3) . ? C11 H11A 0.9300 . ? C12 C16 1.42(2) . ? C12 C13 1.44(3) . ? C13 C14 1.30(3) . ? C13 H13A 0.9300 . ? C14 C15 1.25(3) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.403(19) . ? C18 H18A 0.9300 . ? C19 C20 1.28(2) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.46(2) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.50(2) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.50(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9300 . ? C26 C27 1.35(2) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C29 1.41(3) . ? C28 H28A 0.9300 . ? C29 C30 1.37(3) . ? C29 H29A 0.9300 . ? C30 C31 1.50(2) . ? C30 H30A 0.9300 . ? C31 C39 1.35(2) . ? C31 C32 1.39(2) . ? C32 C33 1.30(2) . ? C32 H32A 0.9300 . ? C33 C34 1.38(2) . ? C33 H33A 0.9300 . ? C34 C38 1.33(2) . ? C34 C35 1.50(3) . ? C35 C36 1.30(3) . ? C35 H35A 0.9300 . ? C36 C37 1.38(2) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 C39 1.427(18) . ? C5 C5' 1.01(5) . ? C5 C5 1.41(5) 15_445 ? C5 C5' 1.71(4) 15_445 ? C5' C5' 1.45(5) 15_445 ? C5' C5 1.71(4) 15_445 ? 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 O13 V1 O1 105.5(4) . . ? O13 V1 O14 107.5(4) . 10_564 ? O1 V1 O14 87.5(4) . 10_564 ? O13 V1 O6 109.6(4) . . ? O1 V1 O6 92.8(3) . . ? O14 V1 O6 141.3(4) 10_564 . ? O13 V1 O18 105.1(4) . . ? O1 V1 O18 149.1(3) . . ? O14 V1 O18 79.4(3) 10_564 . ? O6 V1 O18 80.8(3) . . ? O13 V1 V4 111.9(3) . . ? O1 V1 V4 127.7(2) . . ? O14 V1 V4 113.2(2) 10_564 . ? O6 V1 V4 41.1(2) . . ? O18 V1 V4 39.8(2) . . ? O13 V1 V7 109.7(4) . 10_564 ? O1 V1 V7 50.3(3) . 10_564 ? O14 V1 V7 37.4(3) 10_564 10_564 ? O6 V1 V7 131.8(2) . 10_564 ? O18 V1 V7 114.0(2) . 10_564 ? V4 V1 V7 135.70(10) . 10_564 ? O13 V1 V2 112.8(3) . 10_564 ? O1 V1 V2 120.8(3) . 10_564 ? O14 V1 V2 39.3(2) 10_564 10_564 ? O6 V1 V2 113.3(2) . 10_564 ? O18 V1 V2 40.2(2) . 10_564 ? V4 V1 V2 75.78(7) . 10_564 ? V7 V1 V2 74.70(9) 10_564 10_564 ? O3 V2 O11 107.5(4) . . ? O3 V2 O14 107.2(4) . . ? O11 V2 O14 88.0(3) . . ? O3 V2 O18 107.7(4) . 10_564 ? O11 V2 O18 144.7(3) . 10_564 ? O14 V2 O18 79.4(3) . 10_564 ? O3 V2 O12 107.1(3) . . ? O11 V2 O12 79.8(3) . . ? O14 V2 O12 145.6(3) . . ? O18 V2 O12 92.2(3) 10_564 . ? O3 V2 V6 114.3(3) . . ? O11 V2 V6 39.0(2) . . ? O14 V2 V6 119.4(3) . . ? O18 V2 V6 123.5(2) 10_564 . ? O12 V2 V6 40.9(2) . . ? O3 V2 V1 114.3(3) . 10_564 ? O11 V2 V1 118.2(2) . 10_564 ? O14 V2 V1 37.9(2) . 10_564 ? O18 V2 V1 41.6(2) 10_564 10_564 ? O12 V2 V1 124.5(2) . 10_564 ? V6 V2 V1 131.13(8) . 10_564 ? O4 V3 O12 107.7(4) . . ? O4 V3 O8 107.2(4) . 10_564 ? O12 V3 O8 93.9(3) . 10_564 ? O4 V3 O15 106.4(4) . . ? O12 V3 O15 144.9(3) . . ? O8 V3 O15 84.1(3) 10_564 . ? O4 V3 O19 107.6(4) . . ? O12 V3 O19 82.4(3) . . ? O8 V3 O19 144.4(3) 10_564 . ? O15 V3 O19 79.3(3) . . ? O4 V3 V6 113.4(3) . . ? O12 V3 V6 42.5(2) . . ? O8 V3 V6 127.0(2) 10_564 . ? O15 V3 V6 114.0(2) . . ? O19 V3 V6 39.9(2) . . ? O4 V3 V8 111.0(3) . 10_564 ? O12 V3 V8 129.6(2) . 10_564 ? O8 V3 V8 44.5(2) 10_564 10_564 ? O15 V3 V8 39.6(2) . 10_564 ? O19 V3 V8 114.0(2) . 10_564 ? V6 V3 V8 134.02(8) . 10_564 ? O4 V3 V5 116.3(3) . . ? O12 V3 V5 114.7(2) . . ? O8 V3 V5 114.6(2) 10_564 . ? O15 V3 V5 39.2(2) . . ? O19 V3 V5 40.5(2) . . ? V6 V3 V5 75.78(6) . . ? V8 V3 V5 74.53(7) 10_564 . ? O5 V4 O18 106.6(4) . . ? O5 V4 O8 107.1(4) . . ? O18 V4 O8 92.2(3) . . ? O5 V4 O6 107.6(4) . . ? O18 V4 O6 84.0(3) . . ? O8 V4 O6 144.7(3) . . ? O5 V4 O7 107.9(4) . . ? O18 V4 O7 145.0(3) . . ? O8 V4 O7 82.8(3) . . ? O6 V4 O7 80.7(3) . . ? O5 V4 V1 112.2(3) . . ? O18 V4 V1 43.7(2) . . ? O8 V4 V1 127.1(2) . . ? O6 V4 V1 40.3(2) . . ? O7 V4 V1 115.5(2) . . ? O5 V4 V8 112.2(3) . . ? O18 V4 V8 127.9(2) . . ? O8 V4 V8 44.2(2) . . ? O6 V4 V8 114.3(2) . . ? O7 V4 V8 38.6(2) . . ? V1 V4 V8 134.42(8) . . ? O5 V4 V5 117.1(3) . . ? O18 V4 V5 115.9(2) . . ? O8 V4 V5 114.9(2) . . ? O6 V4 V5 40.5(2) . . ? O7 V4 V5 40.4(2) . . ? V1 V4 V5 76.32(7) . . ? V8 V4 V5 74.89(7) . . ? O2 V5 O15 106.5(4) . . ? O2 V5 O7 105.8(3) . . ? O15 V5 O7 92.6(3) . . ? O2 V5 O6 105.9(4) . . ? O15 V5 O6 147.6(3) . . ? O7 V5 O6 78.1(3) . . ? O2 V5 O19 107.1(4) . . ? O15 V5 O19 78.2(3) . . ? O7 V5 O19 147.1(3) . . ? O6 V5 O19 92.9(3) . . ? O2 V5 V4 113.9(3) . . ? O15 V5 V4 122.8(2) . . ? O7 V5 V4 39.2(2) . . ? O6 V5 V4 39.1(2) . . ? O19 V5 V4 122.8(2) . . ? O2 V5 V3 115.8(3) . . ? O15 V5 V3 39.07(19) . . ? O7 V5 V3 122.0(2) . . ? O6 V5 V3 122.8(2) . . ? O19 V5 V3 39.4(2) . . ? V4 V5 V3 130.30(7) . . ? O10 V6 O1 105.8(4) . . ? O10 V6 O19 108.4(4) . . ? O1 V6 O19 92.7(3) . . ? O10 V6 O11 109.0(4) . . ? O1 V6 O11 87.3(3) . . ? O19 V6 O11 141.1(3) . . ? O10 V6 O12 104.1(4) . . ? O1 V6 O12 149.9(3) . . ? O19 V6 O12 81.1(3) . . ? O11 V6 O12 79.8(3) . . ? O10 V6 V3 111.2(3) . . ? O1 V6 V3 127.9(2) . . ? O19 V6 V3 41.5(2) . . ? O11 V6 V3 112.7(2) . . ? O12 V6 V3 39.6(2) . . ? O10 V6 V7 110.6(3) . 10_564 ? O1 V6 V7 50.0(3) . 10_564 ? O19 V6 V7 131.7(2) . 10_564 ? O11 V6 V7 37.5(2) . 10_564 ? O12 V6 V7 114.8(2) . 10_564 ? V3 V6 V7 135.65(10) . 10_564 ? O10 V6 V2 113.3(4) . . ? O1 V6 V2 121.0(2) . . ? O19 V6 V2 113.5(2) . . ? O11 V6 V2 39.5(2) . . ? O12 V6 V2 40.4(2) . . ? V3 V6 V2 75.41(7) . . ? V7 V6 V2 75.13(10) 10_564 . ? O20 V7 O17 140.9(6) . . ? O20 V7 O14 114.6(6) . . ? O17 V7 O14 76.6(3) . . ? O20 V7 O11 117.4(6) . 10_564 ? O17 V7 O11 74.6(3) . 10_564 ? O14 V7 O11 124.9(4) . 10_564 ? O20 V7 O17' 99.4(6) . . ? O17 V7 O17' 41.5(4) . . ? O14 V7 O17' 95.2(3) . . ? O11 V7 O17' 93.1(3) 10_564 . ? O20 V7 O1 98.1(6) . 10_564 ? O17 V7 O1 121.0(3) . 10_564 ? O14 V7 O1 77.6(3) . 10_564 ? O11 V7 O1 78.6(3) 10_564 10_564 ? O17' V7 O1 162.5(4) . 10_564 ? O20 V7 V1 108.0(5) . 10_564 ? O17 V7 V1 102.9(2) . 10_564 ? O14 V7 V1 38.9(3) . 10_564 ? O11 V7 V1 106.3(3) 10_564 10_564 ? O17' V7 V1 133.1(3) . 10_564 ? O1 V7 V1 38.9(2) 10_564 10_564 ? O20 V7 V6 109.5(5) . 10_564 ? O17 V7 V6 102.2(2) . 10_564 ? O14 V7 V6 105.8(3) . 10_564 ? O11 V7 V6 39.8(2) 10_564 10_564 ? O17' V7 V6 132.1(3) . 10_564 ? O1 V7 V6 39.1(2) 10_564 10_564 ? V1 V7 V6 72.58(10) 10_564 10_564 ? O9 V8 O16 104.8(4) . . ? O9 V8 O7 111.4(4) . . ? O16 V8 O7 91.6(3) . . ? O9 V8 O15 110.3(4) . 10_564 ? O16 V8 O15 91.4(2) . 10_564 ? O7 V8 O15 135.9(3) . 10_564 ? O9 V8 O8 101.2(4) . . ? O16 V8 O8 154.0(3) . . ? O7 V8 O8 78.6(3) . . ? O15 V8 O8 79.8(3) 10_564 . ? O9 V8 V3 108.9(3) . 10_564 ? O16 V8 V3 128.5(2) . 10_564 ? O7 V8 V3 110.4(2) . 10_564 ? O15 V8 V3 40.7(2) 10_564 10_564 ? O8 V8 V3 39.2(2) . 10_564 ? O9 V8 V4 109.8(3) . . ? O16 V8 V4 127.7(2) . . ? O7 V8 V4 39.6(2) . . ? O15 V8 V4 111.2(2) 10_564 . ? O8 V8 V4 39.1(2) . . ? V3 V8 V4 74.30(7) 10_564 . ? N1 Cu1 N1 174.0(6) 6_566 . ? N5 Cu2 N3 136.5(6) . . ? N5 Cu2 N4 141.0(6) . . ? N3 Cu2 N4 82.0(4) . . ? N8 Cu3 N9 153.7(6) . . ? N8 Cu3 N10 123.0(6) . . ? N9 Cu3 N10 83.0(5) . . ? V1 O1 V6 140.2(4) . . ? V1 O1 V7 90.8(3) . 10_564 ? V6 O1 V7 90.9(3) . 10_564 ? V1 O6 V4 98.6(4) . . ? V1 O6 V5 140.2(4) . . ? V4 O6 V5 100.3(3) . . ? V8 O7 V4 101.8(3) . . ? V8 O7 V5 139.2(4) . . ? V4 O7 V5 100.4(3) . . ? V3 O8 V4 143.8(4) 10_564 . ? V3 O8 V8 96.3(4) 10_564 . ? V4 O8 V8 96.7(3) . . ? V7 O11 V6 102.7(4) 10_564 . ? V7 O11 V2 146.6(5) 10_564 . ? V6 O11 V2 101.5(3) . . ? V3 O12 V2 140.7(4) . . ? V3 O12 V6 97.9(3) . . ? V2 O12 V6 98.7(3) . . ? V7 O14 V1 103.7(4) . 10_564 ? V7 O14 V2 144.0(5) . . ? V1 O14 V2 102.7(3) 10_564 . ? V8 O15 V3 99.7(3) 10_564 . ? V8 O15 V5 139.0(4) 10_564 . ? V3 O15 V5 101.7(3) . . ? V8 O16 V8 132.9(6) . 10_564 ? O17' O17 V7 78.6(3) . . ? O17' O17 V7 78.6(3) . 10_564 ? V7 O17 V7 157.2(5) . 10_564 ? O17 O17' V7 59.9(4) . . ? O17 O17' V7 59.9(4) . 10_564 ? V7 O17' V7 119.8(7) . 10_564 ? V4 O18 V2 143.0(4) . 10_564 ? V4 O18 V1 96.5(3) . . ? V2 O18 V1 98.3(3) 10_564 . ? V6 O19 V3 98.5(3) . . ? V6 O19 V5 139.8(4) . . ? V3 O19 V5 100.1(3) . . ? C1 N1 C3 106.2(9) . . ? C1 N1 Cu1 126.8(7) . . ? C3 N1 Cu1 126.8(8) . . ? C1 N2 C2 106.6(9) . . ? C1 N2 C4 127.2(11) . . ? C2 N2 C4 125.9(11) . . ? C17 N3 C6 113.5(13) . . ? C17 N3 Cu2 111.8(9) . . ? C6 N3 Cu2 134.7(11) . . ? C16 N4 C15 120.7(15) . . ? C16 N4 Cu2 111.0(9) . . ? C15 N4 Cu2 128.3(12) . . ? C18 N5 C20 105.6(12) . . ? C18 N5 Cu2 123.6(11) . . ? C20 N5 Cu2 130.5(11) . . ? C19 N6 C18 105.9(13) . . ? C19 N6 C21 129.1(13) . . ? C18 N6 C21 124.6(14) . . ? C28 N9 C39 118.5(15) . . ? C28 N9 Cu3 127.4(14) . . ? C39 N9 Cu3 114.2(10) . . ? C37 N10 C38 112.7(13) . . ? C37 N10 Cu3 136.1(11) . . ? C38 N10 Cu3 111.1(8) . . ? C25 N8 C26 106.6(14) . . ? C25 N8 Cu3 127.6(11) . . ? C26 N8 Cu3 125.6(12) . . ? C25 N7 C24 122.0(14) . . ? C25 N7 C27 107.6(12) . . ? C24 N7 C27 130.0(15) . . ? N1 C1 N2 113.3(9) . . ? N1 C1 H1A 123.4 . . ? N2 C1 H1A 123.4 . . ? N2 C2 C3 106.1(11) . . ? N2 C2 H2A 126.9 . . ? C3 C2 H2A 126.9 . . ? N1 C3 C2 107.8(11) . . ? N1 C3 H3A 126.1 . . ? C2 C3 H3A 126.1 . . ? C5 C4 N2 103(2) . . ? C5 C4 C5' 41(2) . . ? N2 C4 C5' 124.1(16) . . ? C7 C6 N3 122.0(17) . . ? C7 C6 H6A 119.0 . . ? N3 C6 H6A 119.0 . . ? C8 C7 C6 124(2) . . ? C8 C7 H7A 117.8 . . ? C6 C7 H7A 117.8 . . ? C7 C8 C9 117(3) . . ? C7 C8 H8A 121.3 . . ? C9 C8 H8A 121.3 . . ? C8 C9 C10 130(2) . . ? C8 C9 C17 118.6(19) . . ? C10 C9 C17 111.1(16) . . ? C11 C10 C9 132(2) . . ? C11 C10 H10A 114.2 . . ? C9 C10 H10A 114.2 . . ? C10 C11 C12 118(2) . . ? C10 C11 H11A 120.8 . . ? C12 C11 H11A 120.8 . . ? C11 C12 C16 119.0(19) . . ? C11 C12 C13 127(2) . . ? C16 C12 C13 114.3(17) . . ? C14 C13 C12 116(2) . . ? C14 C13 H13A 121.9 . . ? C12 C13 H13A 121.9 . . ? C15 C14 C13 130(3) . . ? C15 C14 H14A 115.0 . . ? C13 C14 H14A 115.0 . . ? C14 C15 N4 117(2) . . ? C14 C15 H15A 121.4 . . ? N4 C15 H15A 121.4 . . ? N4 C16 C17 116.7(12) . . ? N4 C16 C12 121.2(15) . . ? C17 C16 C12 122.1(16) . . ? N3 C17 C16 118.4(13) . . ? N3 C17 C9 123.9(14) . . ? C16 C17 C9 117.7(14) . . ? N5 C18 N6 109.5(14) . . ? N5 C18 H18A 125.3 . . ? N6 C18 H18A 125.3 . . ? C20 C19 N6 106.9(14) . . ? C20 C19 H19A 126.5 . . ? N6 C19 H19A 126.5 . . ? C19 C20 N5 111.8(14) . . ? C19 C20 H20A 124.1 . . ? N5 C20 H20A 124.1 . . ? C22 C21 N6 110.6(13) . . ? C22 C21 H21A 109.5 . . ? N6 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? N6 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C23 113.7(14) . . ? C21 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? C21 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C22 C23 C24 112.6(14) . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? N7 C24 C23 112.0(15) . . ? N7 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? N7 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N8 C25 N7 111.7(13) . . ? N8 C25 H25A 124.2 . . ? N7 C25 H25A 124.2 . . ? C27 C26 N8 108.3(16) . . ? C27 C26 H26A 125.9 . . ? N8 C26 H26A 125.9 . . ? C26 C27 N7 105.8(15) . . ? C26 C27 H27A 127.1 . . ? N7 C27 H27A 127.1 . . ? N9 C28 C29 120(2) . . ? N9 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C30 C29 C28 125(2) . . ? C30 C29 H29A 117.5 . . ? C28 C29 H29A 117.5 . . ? C29 C30 C31 113.0(18) . . ? C29 C30 H30A 123.5 . . ? C31 C30 H30A 123.5 . . ? C39 C31 C32 118.2(19) . . ? C39 C31 C30 119.0(18) . . ? C32 C31 C30 122.3(19) . . ? C33 C32 C31 124(2) . . ? C33 C32 H32A 117.9 . . ? C31 C32 H32A 117.9 . . ? C32 C33 C34 116.5(17) . . ? C32 C33 H33A 121.8 . . ? C34 C33 H33A 121.8 . . ? C38 C34 C33 123.8(15) . . ? C38 C34 C35 112.3(18) . . ? C33 C34 C35 123.3(17) . . ? C36 C35 C34 122(2) . . ? C36 C35 H35A 118.9 . . ? C34 C35 H35A 118.9 . . ? C35 C36 C37 117.3(19) . . ? C35 C36 H36A 121.3 . . ? C37 C36 H36A 121.3 . . ? N10 C37 C36 127.4(17) . . ? N10 C37 H37A 116.3 . . ? C36 C37 H37A 116.3 . . ? C34 C38 N10 127.7(13) . . ? C34 C38 C39 117.5(13) . . ? N10 C38 C39 114.7(12) . . ? C31 C39 N9 123.7(16) . . ? C31 C39 C38 119.4(16) . . ? N9 C39 C38 116.9(11) . . ? C5' C5 C4 74.8(16) . . ? C5' C5 C5 88.3(19) . 15_445 ? C4 C5 C5 157(3) . 15_445 ? C5' C5 C5' 58(3) . 15_445 ? C4 C5 C5' 121(3) . 15_445 ? C5 C5 C5' 36.4(16) 15_445 15_445 ? C5 C5' C5' 86(3) . 15_445 ? C5 C5' C4 63.8(10) . . ? C5' C5' C4 133(3) 15_445 . ? C5 C5' C5 55(2) . 15_445 ? C5' C5' C5 36.3(15) 15_445 15_445 ? C4 C5' C5 117(2) . 15_445 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.702 _refine_diff_density_min -1.257 _refine_diff_density_rms 0.137 data_ds _database_code_depnum_ccdc_archive 'CCDC 900273' #TrackingRef 'I4122-900273.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H76 Cl Cu5 N20 O38.5 V16' _chemical_formula_weight 3077.8 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' Cl Cl 0.1484 0.1585 '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 tetragonal _symmetry_space_group_name_H-M I4122 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-y, x+1/2, z+1/4' 'y+1/2, -x, z+3/4' '-x+1/2, y, -z+3/4' 'x, -y+1/2, -z+1/4' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1, z+1' '-y+1/2, x+1, z+3/4' 'y+1, -x+1/2, z+5/4' '-x+1, y+1/2, -z+5/4' 'x+1/2, -y+1, -z+3/4' 'y+1, x+1, -z+1' '-y+1/2, -x+1/2, -z+1/2' _cell_length_a 27.672(4) _cell_length_b 27.672(4) _cell_length_c 26.693(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20440(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8514 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 24.50 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12160 _exptl_absorpt_coefficient_mu 2.519 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.499 _exptl_absorpt_correction_T_max 0.604 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; The high value of the final R indices and Rint might be caused by the weak diffraction of the Vanadium atoms as well as the bigger volume of the single cell. ; _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64690 _diffrn_reflns_av_R_equivalents 0.1209 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 24.50 _reflns_number_total 8514 _reflns_number_gt 4807 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1005P)^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 0.04(3) _refine_ls_number_reflns 8514 _refine_ls_number_parameters 643 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1721 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.927 _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 Cu1 Cu 0.2500 0.50846(7) 0.8750 0.0599(5) Uani 1 2 d S . . Cu2 Cu 0.30091(8) 0.25373(12) 0.68315(8) 0.1406(11) Uani 1 1 d . . . Cu3 Cu 0.66797(8) 0.22094(10) 0.80929(9) 0.1221(8) Uani 1 1 d . . . V1 V 0.45517(7) 0.46061(7) 0.88560(6) 0.0513(5) Uani 1 1 d . . . V2 V 0.53131(7) 0.61316(7) 0.80768(7) 0.0512(5) Uani 1 1 d . . . V3 V 0.42359(6) 0.43289(7) 0.69078(6) 0.0469(4) Uani 1 1 d . . . V4 V 0.38386(6) 0.48272(7) 0.80791(6) 0.0460(5) Uani 1 1 d . . . V5 V 0.51806(7) 0.38455(7) 0.71309(8) 0.0568(5) Uani 1 1 d . . . V6 V 0.43192(6) 0.57771(6) 0.83201(6) 0.0432(4) Uani 1 1 d . . . V7 V 0.38819(7) 0.53280(7) 0.71308(7) 0.0497(5) Uani 1 1 d . . . V8 V 0.46139(11) 0.54513(13) 0.63473(10) 0.1153(11) Uani 1 1 d . . . N1 N 0.2807(3) 0.5114(3) 0.9377(3) 0.052(2) Uani 1 1 d . . . N2 N 0.3372(3) 0.5200(3) 0.9944(3) 0.054(2) Uani 1 1 d D . . N5 N 0.3668(4) 0.2380(6) 0.6850(4) 0.097(4) Uani 1 1 d . . . N6 N 0.4334(4) 0.1967(5) 0.6821(4) 0.078(3) Uani 1 1 d . . . N7 N 0.5253(5) 0.1896(5) 0.8237(4) 0.091(4) Uani 1 1 d . . . N8 N 0.5987(5) 0.2171(6) 0.8142(6) 0.121(5) Uani 1 1 d . . . N9 N 0.7325(5) 0.1941(5) 0.8110(5) 0.095(4) Uiso 1 1 d . . . N10 N 0.7063(4) 0.2846(4) 0.8089(4) 0.084(3) Uani 1 1 d . . . O1 O 0.4663(3) 0.6165(2) 0.7813(3) 0.0489(17) Uani 1 1 d . . . O2 O 0.4186(2) 0.4283(3) 0.8280(3) 0.0533(18) Uani 1 1 d . . . O3 O 0.4249(2) 0.5866(3) 0.6962(3) 0.0561(19) Uani 1 1 d . . . O4 O 0.3889(3) 0.4016(3) 0.6578(3) 0.066(2) Uani 1 1 d . . . O5 O 0.5453(3) 0.6673(3) 0.8266(3) 0.072(2) Uani 1 1 d . . . O6 O 0.4002(3) 0.6159(3) 0.8634(3) 0.060(2) Uani 1 1 d . . . O7 O 0.3305(2) 0.4759(3) 0.8288(3) 0.0553(19) Uani 1 1 d . . . O8 O 0.4880(2) 0.4238(3) 0.6639(2) 0.057(2) Uani 1 1 d . . . O9 O 0.5213(3) 0.3308(3) 0.6915(3) 0.072(2) Uani 1 1 d . . . O10 O 0.4195(2) 0.5136(2) 0.8609(2) 0.0450(17) Uani 1 1 d . . . O11 O 0.3849(2) 0.4657(2) 0.7408(2) 0.0475(17) Uani 1 1 d . . . O12 O 0.5000 0.5000 0.9128(3) 0.049(2) Uani 1 2 d S . . O13 O 0.3362(3) 0.5425(3) 0.6914(3) 0.067(2) Uani 1 1 d . . . O14 O 0.4969(2) 0.5808(2) 0.8609(2) 0.0471(17) Uani 1 1 d . . . O15 O 0.4509(2) 0.3897(2) 0.7408(2) 0.0482(17) Uani 1 1 d . . . O16 O 0.3895(2) 0.5478(2) 0.7815(2) 0.0438(17) Uani 1 1 d . . . O17 O 0.4242(2) 0.4984(3) 0.6632(2) 0.0502(18) Uani 1 1 d . . . O18 O 0.4365(5) 0.5727(5) 0.5884(4) 0.047(3) Uani 0.50 1 d P . . O19 O 0.5000 0.5000 0.5998(5) 0.078(3) Uani 1 2 d S . . O19' O 0.5000 0.5000 0.6467(3) 0.043(2) Uani 1 2 d S . . O20 O 0.4282(3) 0.4389(3) 0.9325(3) 0.067(2) Uani 1 1 d . . . Cl1 Cl 0.5000 0.5000 0.76592(13) 0.0541(9) Uani 1 2 d S . . C1 C 0.2593(5) 0.5157(4) 0.9847(4) 0.068(3) Uani 1 1 d . . . H1A H 0.2263 0.5150 0.9915 0.081 Uiso 1 1 calc R . . C2 C 0.2950(5) 0.5209(4) 1.0186(4) 0.065(3) Uani 1 1 d . . . H2A H 0.2909 0.5246 1.0530 0.078 Uiso 1 1 calc R . . C3 C 0.3271(4) 0.5150(4) 0.9454(4) 0.052(3) Uani 1 1 d . . . H3A H 0.3503 0.5141 0.9202 0.062 Uiso 1 1 calc R . . C4 C 0.3827(4) 0.5188(6) 1.0153(5) 0.100(5) Uiso 1 1 d D . . H4A H 0.3803 0.5347 1.0476 0.120 Uiso 1 1 calc R . . H4B H 0.3899 0.4851 1.0220 0.120 Uiso 1 1 calc R . . C6 C 0.2748(7) 0.3644(8) 0.6733(6) 0.122(7) Uani 1 1 d . . . H6A H 0.3069 0.3737 0.6700 0.146 Uiso 1 1 calc R . . C7 C 0.2387(8) 0.3985(8) 0.6718(7) 0.119(6) Uiso 1 1 d . . . H7A H 0.2473 0.4309 0.6694 0.142 Uiso 1 1 calc R . . C8 C 0.1970(10) 0.3884(9) 0.6734(8) 0.147(8) Uiso 1 1 d . . . H8A H 0.1754 0.4140 0.6703 0.176 Uiso 1 1 calc R . . C9 C 0.1765(6) 0.3428(7) 0.6796(5) 0.102(5) Uani 1 1 d . . . C17 C 0.2148(5) 0.3059(5) 0.6828(4) 0.069(4) Uani 1 1 d . . . N4 N 0.2623(4) 0.3144(5) 0.6799(4) 0.078(3) Uani 1 1 d . . . C10 C 0.1283(8) 0.3247(8) 0.6828(7) 0.134(7) Uiso 1 1 d . . . H10A H 0.1034 0.3472 0.6803 0.160 Uiso 1 1 calc R . . C11 C 0.1156(9) 0.2784(9) 0.6893(8) 0.145(7) Uiso 1 1 d . . . H11A H 0.0832 0.2697 0.6917 0.174 Uiso 1 1 calc R . . C12 C 0.1495(7) 0.2458(6) 0.6921(6) 0.103(5) Uani 1 1 d . . . C13 C 0.1421(8) 0.1953(8) 0.6986(7) 0.132(7) Uiso 1 1 d . . . H13A H 0.1106 0.1837 0.6999 0.159 Uiso 1 1 calc R . . C14 C 0.1768(10) 0.1657(10) 0.7025(8) 0.154(8) Uiso 1 1 d . . . H14A H 0.1688 0.1337 0.7093 0.185 Uiso 1 1 calc R . . C15 C 0.2228(9) 0.1758(7) 0.6981(6) 0.127(7) Uani 1 1 d . . . H15A H 0.2464 0.1519 0.7001 0.152 Uiso 1 1 calc R . . C16 C 0.1997(5) 0.2567(6) 0.6893(4) 0.074(4) Uani 1 1 d . . . C18 C 0.3855(5) 0.1955(6) 0.6814(5) 0.080(4) Uani 1 1 d . . . H18A H 0.3674 0.1673 0.6786 0.096 Uiso 1 1 calc R . . C19 C 0.4056(7) 0.2675(6) 0.6899(5) 0.094(5) Uani 1 1 d . . . H19A H 0.4041 0.3009 0.6941 0.112 Uiso 1 1 calc R . . C20 C 0.4456(6) 0.2423(7) 0.6880(5) 0.086(4) Uani 1 1 d . . . H20A H 0.4769 0.2544 0.6903 0.103 Uiso 1 1 calc R . . C21 C 0.4655(6) 0.1530(6) 0.6825(5) 0.099(5) Uani 1 1 d . . . H21A H 0.4460 0.1240 0.6789 0.119 Uiso 1 1 calc R . . H21B H 0.4877 0.1544 0.6544 0.119 Uiso 1 1 calc R . . C22 C 0.4929(5) 0.1506(6) 0.7296(5) 0.097(5) Uani 1 1 d . . . H22A H 0.5159 0.1771 0.7307 0.116 Uiso 1 1 calc R . . H22B H 0.5111 0.1206 0.7306 0.116 Uiso 1 1 calc R . . C23 C 0.4609(6) 0.1533(7) 0.7743(6) 0.105(5) Uani 1 1 d . . . H23A H 0.4385 0.1264 0.7735 0.126 Uiso 1 1 calc R . . H23B H 0.4422 0.1829 0.7728 0.126 Uiso 1 1 calc R . . C24 C 0.4885(5) 0.1521(6) 0.8231(6) 0.101(5) Uani 1 1 d . . . H24A H 0.4663 0.1569 0.8508 0.121 Uiso 1 1 calc R . . H24B H 0.5036 0.1207 0.8272 0.121 Uiso 1 1 calc R . . C25 C 0.5213(6) 0.2402(6) 0.8227(7) 0.111(5) Uani 1 1 d . . . H25A H 0.4928 0.2577 0.8258 0.133 Uiso 1 1 calc R . . C26 C 0.5651(8) 0.2587(8) 0.8164(7) 0.130(6) Uiso 1 1 d . . . H26A H 0.5731 0.2913 0.8139 0.156 Uiso 1 1 calc R . . C27 C 0.5728(5) 0.1778(5) 0.8185(6) 0.079(4) Uani 1 1 d . . . H27A H 0.5849 0.1465 0.8182 0.094 Uiso 1 1 calc R . . C28 C 0.6925(6) 0.3327(6) 0.8071(6) 0.104(5) Uiso 1 1 d . . . H28A H 0.6599 0.3404 0.8038 0.125 Uiso 1 1 calc R . . C29 C 0.7260(7) 0.3691(7) 0.8103(6) 0.110(5) Uiso 1 1 d . . . H29A H 0.7158 0.4011 0.8091 0.132 Uiso 1 1 calc R . . C30 C 0.7715(8) 0.3595(8) 0.8148(7) 0.138(7) Uiso 1 1 d . . . H30A H 0.7933 0.3850 0.8172 0.165 Uiso 1 1 calc R . . C31 C 0.7892(7) 0.3124(5) 0.8163(6) 0.091(5) Uani 1 1 d . . . C32 C 0.8379(6) 0.3008(6) 0.8187(6) 0.097(5) Uani 1 1 d . . . H32A H 0.8616 0.3246 0.8188 0.116 Uiso 1 1 calc R . . C33 C 0.8486(7) 0.2571(7) 0.8208(6) 0.111(5) Uiso 1 1 d . . . H33A H 0.8812 0.2499 0.8248 0.133 Uiso 1 1 calc R . . C34 C 0.8162(7) 0.2164(8) 0.8179(7) 0.122(6) Uiso 1 1 d . . . C35 C 0.8322(8) 0.1672(7) 0.8166(6) 0.123(6) Uani 1 1 d . . . H35A H 0.8645 0.1581 0.8170 0.147 Uiso 1 1 calc R . . C36 C 0.7918(9) 0.1326(7) 0.8147(8) 0.140(8) Uani 1 1 d . . . H36A H 0.7982 0.0997 0.8169 0.168 Uiso 1 1 calc R . . C37 C 0.7455(9) 0.1479(7) 0.8098(7) 0.130(7) Uani 1 1 d . . . H37A H 0.7215 0.1247 0.8055 0.156 Uiso 1 1 calc R . . C38 C 0.7686(5) 0.2297(6) 0.8130(5) 0.086(4) Uani 1 1 d . . . C39 C 0.7542(5) 0.2784(5) 0.8115(5) 0.070(3) Uani 1 1 d . . . O1W O 0.4689(10) 0.4689(10) 0.5000 0.140(12) Uiso 0.50 2 d SP . . N3 N 0.2344(4) 0.2238(4) 0.6904(4) 0.079(3) Uiso 1 1 d . . . C5' C 0.4158(6) 0.5842(6) 1.0000 0.098(6) Uiso 1 2 d S . . C5 C 0.4216(7) 0.5371(9) 0.9927(9) 0.075(7) Uiso 0.50 1 d PD . . 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 Cu1 0.0569(13) 0.0547(13) 0.0683(11) 0.000 -0.0226(10) 0.000 Cu2 0.0887(15) 0.223(3) 0.1103(15) -0.0382(18) -0.0205(13) 0.0748(18) Cu3 0.0853(15) 0.141(2) 0.1397(19) 0.0117(16) -0.0011(14) -0.0436(14) V1 0.0461(12) 0.0609(13) 0.0471(9) 0.0114(9) 0.0087(8) 0.0164(9) V2 0.0491(12) 0.0419(11) 0.0626(12) -0.0044(9) -0.0085(9) -0.0026(9) V3 0.0387(11) 0.0501(12) 0.0520(10) -0.0090(9) 0.0010(8) -0.0052(9) V4 0.0317(10) 0.0551(12) 0.0513(10) 0.0032(8) 0.0032(8) 0.0007(9) V5 0.0519(13) 0.0523(12) 0.0662(12) -0.0115(10) 0.0007(10) 0.0037(11) V6 0.0377(11) 0.0420(11) 0.0500(9) -0.0035(8) -0.0028(8) 0.0065(8) V7 0.0379(11) 0.0594(13) 0.0516(10) 0.0041(9) -0.0041(8) 0.0037(9) V8 0.095(2) 0.154(3) 0.0971(19) 0.0409(19) -0.0255(16) -0.0468(19) N1 0.054(6) 0.042(5) 0.059(5) -0.003(4) 0.007(5) 0.009(4) N2 0.046(5) 0.059(6) 0.057(5) 0.000(5) -0.008(5) 0.000(4) N5 0.066(8) 0.134(13) 0.092(8) -0.025(9) -0.013(7) 0.044(9) N6 0.069(8) 0.087(9) 0.078(7) -0.010(6) 0.006(6) 0.015(7) N7 0.077(9) 0.102(10) 0.093(8) 0.020(7) -0.014(7) -0.003(8) N8 0.090(10) 0.113(12) 0.159(13) -0.004(10) -0.016(9) 0.010(9) N10 0.094(9) 0.060(8) 0.097(8) -0.010(6) 0.026(7) 0.020(6) O1 0.052(5) 0.038(4) 0.057(4) 0.000(3) 0.002(3) -0.006(4) O2 0.040(4) 0.050(5) 0.070(4) 0.020(4) 0.006(3) -0.004(3) O3 0.030(4) 0.067(5) 0.071(4) 0.015(4) -0.010(3) -0.006(3) O4 0.054(5) 0.074(6) 0.069(4) -0.025(4) 0.004(4) -0.019(4) O5 0.069(6) 0.041(5) 0.107(6) -0.021(4) -0.025(5) 0.000(4) O6 0.043(4) 0.062(5) 0.076(5) -0.019(4) -0.007(4) 0.020(4) O7 0.027(4) 0.069(5) 0.070(5) 0.002(4) 0.011(3) 0.001(4) O8 0.042(5) 0.077(6) 0.050(4) -0.003(4) 0.005(3) 0.007(4) O9 0.067(6) 0.041(5) 0.108(6) -0.029(4) 0.013(5) 0.004(4) O10 0.030(4) 0.056(5) 0.049(4) 0.005(3) -0.003(3) 0.009(3) O11 0.025(4) 0.054(4) 0.063(4) 0.011(4) 0.001(3) -0.005(3) O12 0.025(5) 0.063(7) 0.058(5) 0.000 0.000 0.017(4) O13 0.036(4) 0.095(6) 0.070(5) 0.024(4) -0.029(4) 0.003(4) O14 0.046(4) 0.044(4) 0.051(4) -0.014(3) -0.007(3) 0.009(3) O15 0.046(4) 0.041(4) 0.057(4) -0.002(3) 0.006(3) -0.003(3) O16 0.030(4) 0.051(5) 0.050(4) 0.005(3) -0.003(3) 0.003(3) O17 0.047(5) 0.060(5) 0.044(3) 0.001(3) 0.005(3) -0.002(4) O18 0.055(9) 0.064(10) 0.022(6) 0.018(6) -0.012(6) -0.002(7) O19 0.046(7) 0.094(10) 0.093(9) 0.000 0.000 0.004(6) O19' 0.030(5) 0.061(7) 0.038(5) 0.000 0.000 0.017(4) O20 0.062(5) 0.081(6) 0.058(4) 0.024(4) 0.015(4) 0.010(4) Cl1 0.043(2) 0.053(3) 0.066(2) 0.000 0.000 -0.0032(19) C1 0.066(8) 0.072(9) 0.065(7) -0.005(6) 0.016(7) 0.006(7) C2 0.075(9) 0.066(8) 0.054(7) 0.000(6) 0.005(7) 0.006(7) C3 0.037(6) 0.076(8) 0.043(6) -0.011(5) -0.013(5) -0.006(6) C6 0.088(13) 0.18(2) 0.100(12) -0.002(12) 0.011(10) -0.060(14) C9 0.092(12) 0.152(17) 0.063(8) 0.000(9) 0.000(8) 0.002(12) C17 0.070(10) 0.079(10) 0.059(7) 0.003(7) -0.013(6) 0.029(8) N4 0.051(7) 0.100(9) 0.082(7) 0.007(6) 0.003(6) -0.010(6) C12 0.104(13) 0.089(12) 0.114(12) 0.005(10) -0.012(10) 0.008(10) C15 0.16(2) 0.135(17) 0.085(11) 0.028(11) 0.001(12) 0.021(14) C16 0.058(9) 0.099(12) 0.066(7) 0.001(8) -0.016(6) -0.009(8) C18 0.054(9) 0.089(11) 0.097(10) -0.010(8) 0.004(8) -0.009(8) C19 0.117(14) 0.069(10) 0.094(10) -0.015(8) -0.023(10) -0.011(11) C20 0.070(10) 0.100(13) 0.088(10) -0.008(9) -0.003(8) -0.006(10) C21 0.112(13) 0.097(12) 0.089(10) -0.020(9) -0.019(10) 0.030(10) C22 0.070(10) 0.137(15) 0.084(9) 0.004(9) -0.014(9) 0.042(10) C23 0.075(10) 0.138(15) 0.102(11) 0.010(11) -0.032(10) -0.031(10) C24 0.073(10) 0.119(14) 0.111(12) 0.041(10) 0.009(9) -0.021(10) C25 0.091(12) 0.081(12) 0.160(15) -0.020(11) 0.000(11) 0.029(10) C27 0.063(9) 0.046(8) 0.127(11) 0.015(8) -0.035(8) -0.012(7) C31 0.116(14) 0.067(10) 0.091(10) -0.011(8) 0.033(10) -0.018(10) C32 0.094(13) 0.096(13) 0.101(11) -0.021(9) 0.038(10) -0.036(10) C35 0.144(18) 0.105(15) 0.119(13) 0.016(12) 0.031(13) 0.058(13) C36 0.17(2) 0.069(13) 0.18(2) 0.002(13) 0.049(17) 0.037(14) C37 0.16(2) 0.104(15) 0.129(15) -0.022(11) -0.006(14) 0.049(14) C38 0.037(8) 0.141(15) 0.081(8) -0.006(9) 0.009(7) 0.014(8) C39 0.056(8) 0.067(9) 0.087(9) 0.001(7) 0.016(7) 0.001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.879(9) 5_556 ? Cu1 N1 1.879(9) . ? Cu2 N5 1.875(11) . ? Cu2 N4 1.991(12) . ? Cu2 N3 2.028(11) . ? Cu3 N8 1.923(15) . ? Cu3 N9 1.934(13) . ? Cu3 N10 2.055(12) . ? V1 O20 1.577(7) . ? V1 O12 1.804(4) . ? V1 O14 1.872(7) 10_554 ? V1 O10 1.884(6) . ? V1 O2 2.046(7) . ? V1 V4 2.927(3) . ? V1 V2 2.938(3) 10_554 ? V2 O5 1.628(7) . ? V2 O15 1.852(7) 10_554 ? V2 O2 1.880(8) 10_554 ? V2 O14 1.931(7) . ? V2 O1 1.934(7) . ? V2 V5 2.871(3) 10_554 ? V2 V1 2.938(3) 10_554 ? V2 V6 2.992(3) . ? V3 O4 1.565(7) . ? V3 O8 1.938(7) . ? V3 O11 1.938(7) . ? V3 O15 1.946(7) . ? V3 O17 1.957(7) . ? V3 V7 2.993(3) . ? V3 V5 2.996(3) . ? V4 O7 1.589(7) . ? V4 O11 1.852(7) . ? V4 O2 1.866(7) . ? V4 O10 1.925(7) . ? V4 O16 1.941(7) . ? V4 V7 2.888(3) . ? V4 V6 3.015(3) . ? V5 O9 1.598(7) . ? V5 O3 1.825(7) 10_554 ? V5 O1 1.871(7) 10_554 ? V5 O8 1.895(7) . ? V5 O15 2.005(7) . ? V5 V2 2.871(3) 10_554 ? V5 V8 2.913(4) 10_554 ? V6 O6 1.609(7) . ? V6 O14 1.959(7) . ? V6 O10 1.966(7) . ? V6 O16 1.970(7) . ? V6 O1 1.973(7) . ? V7 O13 1.575(7) . ? V7 O3 1.859(7) . ? V7 O16 1.873(6) . ? V7 O17 1.916(7) . ? V7 O11 2.000(7) . ? V7 V8 2.932(4) . ? V8 O18 1.607(11) . ? V8 O19' 1.674(4) . ? V8 O17 1.819(7) . ? V8 O8 1.819(8) 10_554 ? V8 O19 1.890(7) . ? V8 O3 2.242(8) . ? V8 V5 2.913(4) 10_554 ? N1 C3 1.303(12) . ? N1 C1 1.394(12) . ? N2 C2 1.334(14) . ? N2 C3 1.345(12) . ? N2 C4 1.377(9) . ? N5 C18 1.288(18) . ? N5 C19 1.356(19) . ? N6 C20 1.317(18) . ? N6 C18 1.326(16) . ? N6 C21 1.501(17) . ? N7 C27 1.361(17) . ? N7 C25 1.405(18) . ? N7 C24 1.454(18) . ? N8 C27 1.309(17) . ? N8 C26 1.48(2) . ? N9 C37 1.330(19) . ? N9 C38 1.40(2) . ? N10 C39 1.340(16) . ? N10 C28 1.386(18) . ? O1 V5 1.871(7) 10_554 ? O2 V2 1.880(8) 10_554 ? O3 V5 1.825(7) 10_554 ? O8 V8 1.819(8) 10_554 ? O12 V1 1.804(4) 10_554 ? O14 V1 1.872(7) 10_554 ? O15 V2 1.852(7) 10_554 ? O19 O19' 1.253(13) . ? O19 V8 1.890(7) 10_554 ? O19' V8 1.674(4) 10_554 ? C1 C2 1.347(15) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4 C5 1.333(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 C7 1.37(3) . ? C6 N4 1.44(2) . ? C6 H6A 0.9300 . ? C7 C8 1.19(3) . ? C7 H7A 0.9300 . ? C8 C9 1.39(3) . ? C8 H8A 0.9300 . ? C9 C10 1.43(2) . ? C9 C17 1.47(2) . ? C17 N4 1.339(17) . ? C17 C16 1.435(19) . ? C10 C11 1.34(3) . ? C10 H10A 0.9300 . ? C11 C12 1.30(2) . ? C11 H11A 0.9300 . ? C12 C13 1.42(3) . ? C12 C16 1.42(2) . ? C13 C14 1.27(3) . ? C13 H13A 0.9300 . ? C14 C15 1.31(3) . ? C14 H14A 0.9300 . ? C15 N3 1.38(2) . ? C15 H15A 0.9300 . ? C16 N3 1.322(17) . ? C18 H18A 0.9300 . ? C19 C20 1.309(19) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.471(18) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.488(19) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.510(19) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.33(2) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C29 1.37(2) . ? C28 H28A 0.9300 . ? C29 C30 1.29(2) . ? C29 H29A 0.9300 . ? C30 C31 1.39(2) . ? C30 H30A 0.9300 . ? C31 C39 1.356(19) . ? C31 C32 1.39(2) . ? C32 C33 1.24(2) . ? C32 H32A 0.9300 . ? C33 C34 1.44(2) . ? C33 H33A 0.9300 . ? C34 C38 1.37(2) . ? C34 C35 1.43(2) . ? C35 C36 1.47(3) . ? C35 H35A 0.9300 . ? C36 C37 1.36(3) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? C38 C39 1.407(17) . ? C5' C5 1.33(3) . ? C5' C5 1.33(3) 8_667 ? C5 C5 1.66(4) 8_667 ? 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 N1 Cu1 N1 175.0(5) 5_556 . ? N5 Cu2 N4 135.9(6) . . ? N5 Cu2 N3 141.8(7) . . ? N4 Cu2 N3 82.0(5) . . ? N8 Cu3 N9 153.7(6) . . ? N8 Cu3 N10 124.2(6) . . ? N9 Cu3 N10 81.5(5) . . ? O20 V1 O12 103.6(4) . . ? O20 V1 O14 112.4(4) . 10_554 ? O12 V1 O14 91.4(2) . 10_554 ? O20 V1 O10 109.1(3) . . ? O12 V1 O10 91.8(2) . . ? O14 V1 O10 136.3(3) 10_554 . ? O20 V1 O2 101.3(4) . . ? O12 V1 O2 155.1(3) . . ? O14 V1 O2 79.6(3) 10_554 . ? O10 V1 O2 79.6(3) . . ? O20 V1 V4 108.9(3) . . ? O12 V1 V4 128.50(18) . . ? O14 V1 V4 110.9(2) 10_554 . ? O10 V1 V4 40.3(2) . . ? O2 V1 V4 39.3(2) . . ? O20 V1 V2 110.9(3) . 10_554 ? O12 V1 V2 128.11(18) . 10_554 ? O14 V1 V2 40.1(2) 10_554 10_554 ? O10 V1 V2 111.1(2) . 10_554 ? O2 V1 V2 39.4(2) . 10_554 ? V4 V1 V2 74.31(7) . 10_554 ? O5 V2 O15 105.9(4) . 10_554 ? O5 V2 O2 107.2(4) . 10_554 ? O15 V2 O2 93.2(3) 10_554 10_554 ? O5 V2 O14 108.4(4) . . ? O15 V2 O14 145.1(3) 10_554 . ? O2 V2 O14 82.4(3) 10_554 . ? O5 V2 O1 106.8(4) . . ? O15 V2 O1 84.2(3) 10_554 . ? O2 V2 O1 145.2(3) 10_554 . ? O14 V2 O1 80.3(3) . . ? O5 V2 V5 111.4(3) . 10_554 ? O15 V2 V5 44.0(2) 10_554 10_554 ? O2 V2 V5 128.2(2) 10_554 10_554 ? O14 V2 V5 115.0(2) . 10_554 ? O1 V2 V5 40.2(2) . 10_554 ? O5 V2 V1 113.0(3) . 10_554 ? O15 V2 V1 128.2(2) 10_554 10_554 ? O2 V2 V1 43.8(2) 10_554 10_554 ? O14 V2 V1 38.7(2) . 10_554 ? O1 V2 V1 114.2(2) . 10_554 ? V5 V2 V1 134.29(8) 10_554 10_554 ? O5 V2 V6 117.0(3) . . ? O15 V2 V6 116.1(2) 10_554 . ? O2 V2 V6 114.6(2) 10_554 . ? O14 V2 V6 40.1(2) . . ? O1 V2 V6 40.5(2) . . ? V5 V2 V6 76.15(7) 10_554 . ? V1 V2 V6 74.67(6) 10_554 . ? O4 V3 O8 106.5(4) . . ? O4 V3 O11 108.0(4) . . ? O8 V3 O11 145.4(3) . . ? O4 V3 O15 106.6(4) . . ? O8 V3 O15 79.4(3) . . ? O11 V3 O15 91.7(3) . . ? O4 V3 O17 107.8(4) . . ? O8 V3 O17 88.5(3) . . ? O11 V3 O17 80.2(3) . . ? O15 V3 O17 145.5(3) . . ? O4 V3 V7 115.0(3) . . ? O8 V3 V7 119.6(2) . . ? O11 V3 V7 41.3(2) . . ? O15 V3 V7 123.9(2) . . ? O17 V3 V7 38.91(19) . . ? O4 V3 V5 113.6(3) . . ? O8 V3 V5 38.1(2) . . ? O11 V3 V5 123.6(2) . . ? O15 V3 V5 41.4(2) . . ? O17 V3 V5 118.7(2) . . ? V7 V3 V5 131.17(8) . . ? O7 V4 O11 108.9(3) . . ? O7 V4 O2 106.3(3) . . ? O11 V4 O2 93.8(3) . . ? O7 V4 O10 105.7(3) . . ? O11 V4 O10 144.6(3) . . ? O2 V4 O10 83.2(3) . . ? O7 V4 O16 108.2(3) . . ? O11 V4 O16 83.3(3) . . ? O2 V4 O16 144.4(3) . . ? O10 V4 O16 79.3(3) . . ? O7 V4 V7 113.7(3) . . ? O11 V4 V7 43.4(2) . . ? O2 V4 V7 128.2(2) . . ? O10 V4 V7 114.2(2) . . ? O16 V4 V7 39.90(19) . . ? O7 V4 V1 110.7(3) . . ? O11 V4 V1 128.4(2) . . ? O2 V4 V1 44.0(2) . . ? O10 V4 V1 39.29(19) . . ? O16 V4 V1 113.4(2) . . ? V7 V4 V1 133.89(8) . . ? O7 V4 V6 116.0(3) . . ? O11 V4 V6 114.9(2) . . ? O2 V4 V6 114.6(2) . . ? O10 V4 V6 39.7(2) . . ? O16 V4 V6 39.93(19) . . ? V7 V4 V6 75.55(6) . . ? V1 V4 V6 74.56(6) . . ? O9 V5 O3 105.6(4) . 10_554 ? O9 V5 O1 108.8(4) . 10_554 ? O3 V5 O1 92.7(3) 10_554 10_554 ? O9 V5 O8 108.0(4) . . ? O3 V5 O8 87.6(3) 10_554 . ? O1 V5 O8 141.6(3) 10_554 . ? O9 V5 O15 104.6(4) . . ? O3 V5 O15 149.5(3) 10_554 . ? O1 V5 O15 81.7(3) 10_554 . ? O8 V5 O15 79.0(3) . . ? O9 V5 V2 111.4(3) . 10_554 ? O3 V5 V2 128.3(2) 10_554 10_554 ? O1 V5 V2 41.8(2) 10_554 10_554 ? O8 V5 V2 112.8(2) . 10_554 ? O15 V5 V2 39.90(19) . 10_554 ? O9 V5 V8 110.6(3) . 10_554 ? O3 V5 V8 50.3(2) 10_554 10_554 ? O1 V5 V8 131.6(2) 10_554 10_554 ? O8 V5 V8 37.4(2) . 10_554 ? O15 V5 V8 113.5(2) . 10_554 ? V2 V5 V8 135.20(10) 10_554 10_554 ? O9 V5 V3 113.2(3) . . ? O3 V5 V3 120.7(2) 10_554 . ? O1 V5 V3 113.7(2) 10_554 . ? O8 V5 V3 39.1(2) . . ? O15 V5 V3 39.95(19) . . ? V2 V5 V3 75.51(7) 10_554 . ? V8 V5 V3 74.30(9) 10_554 . ? O6 V6 O14 105.5(3) . . ? O6 V6 O10 107.0(3) . . ? O14 V6 O10 92.5(3) . . ? O6 V6 O16 107.9(3) . . ? O14 V6 O16 146.6(3) . . ? O10 V6 O16 77.7(3) . . ? O6 V6 O1 105.3(4) . . ? O14 V6 O1 78.7(3) . . ? O10 V6 O1 147.7(3) . . ? O16 V6 O1 92.7(3) . . ? O6 V6 V2 113.5(3) . . ? O14 V6 V2 39.38(19) . . ? O10 V6 V2 122.79(19) . . ? O16 V6 V2 122.5(2) . . ? O1 V6 V2 39.5(2) . . ? O6 V6 V4 116.3(3) . . ? O14 V6 V4 121.8(2) . . ? O10 V6 V4 38.72(19) . . ? O16 V6 V4 39.22(19) . . ? O1 V6 V4 122.8(2) . . ? V2 V6 V4 130.17(7) . . ? O13 V7 O3 105.9(4) . . ? O13 V7 O16 109.7(4) . . ? O3 V7 O16 92.8(3) . . ? O13 V7 O17 107.8(4) . . ? O3 V7 O17 86.9(3) . . ? O16 V7 O17 141.1(3) . . ? O13 V7 O11 104.7(4) . . ? O3 V7 O11 149.1(3) . . ? O16 V7 O11 81.2(3) . . ? O17 V7 O11 79.6(3) . . ? O13 V7 V4 111.4(3) . . ? O3 V7 V4 128.3(2) . . ? O16 V7 V4 41.7(2) . . ? O17 V7 V4 113.1(2) . . ? O11 V7 V4 39.5(2) . . ? O13 V7 V8 110.5(3) . . ? O3 V7 V8 49.9(2) . . ? O16 V7 V8 131.0(2) . . ? O17 V7 V8 37.1(2) . . ? O11 V7 V8 113.8(2) . . ? V4 V7 V8 135.22(10) . . ? O13 V7 V3 112.6(3) . . ? O3 V7 V3 120.9(2) . . ? O16 V7 V3 113.1(2) . . ? O17 V7 V3 39.9(2) . . ? O11 V7 V3 39.76(19) . . ? V4 V7 V3 75.21(7) . . ? V8 V7 V3 74.90(9) . . ? O18 V8 O19' 140.7(6) . . ? O18 V8 O17 114.6(6) . . ? O19' V8 O17 75.6(3) . . ? O18 V8 O8 115.8(6) . 10_554 ? O19' V8 O8 77.3(3) . 10_554 ? O17 V8 O8 126.3(3) . 10_554 ? O18 V8 O19 100.1(6) . . ? O19' V8 O19 40.6(4) . . ? O17 V8 O19 93.2(3) . . ? O8 V8 O19 95.1(3) 10_554 . ? O18 V8 O3 97.3(5) . . ? O19' V8 O3 122.0(4) . . ? O17 V8 O3 78.7(3) . . ? O8 V8 O3 77.9(3) 10_554 . ? O19 V8 O3 162.6(4) . . ? O18 V8 V5 108.6(5) . 10_554 ? O19' V8 V5 103.7(3) . 10_554 ? O17 V8 V5 106.6(2) . 10_554 ? O8 V8 V5 39.3(2) 10_554 10_554 ? O19 V8 V5 133.3(2) . 10_554 ? O3 V8 V5 38.78(19) . 10_554 ? O18 V8 V7 107.9(5) . . ? O19' V8 V7 102.6(3) . . ? O17 V8 V7 39.5(2) . . ? O8 V8 V7 106.3(2) 10_554 . ? O19 V8 V7 131.7(2) . . ? O3 V8 V7 39.35(19) . . ? V5 V8 V7 72.56(10) 10_554 . ? C3 N1 C1 105.7(9) . . ? C3 N1 Cu1 126.1(7) . . ? C1 N1 Cu1 127.8(8) . . ? C2 N2 C3 106.8(9) . . ? C2 N2 C4 127.3(11) . . ? C3 N2 C4 125.5(10) . . ? C18 N5 C19 103.8(12) . . ? C18 N5 Cu2 126.9(13) . . ? C19 N5 Cu2 129.3(14) . . ? C20 N6 C18 106.4(12) . . ? C20 N6 C21 128.3(14) . . ? C18 N6 C21 124.9(14) . . ? C27 N7 C25 108.1(12) . . ? C27 N7 C24 120.2(13) . . ? C25 N7 C24 131.1(14) . . ? C27 N8 C26 107.3(15) . . ? C27 N8 Cu3 126.8(12) . . ? C26 N8 Cu3 125.8(14) . . ? C37 N9 C38 118.8(16) . . ? C37 N9 Cu3 128.2(14) . . ? C38 N9 Cu3 112.9(10) . . ? C39 N10 C28 113.4(13) . . ? C39 N10 Cu3 113.7(9) . . ? C28 N10 Cu3 132.9(11) . . ? V5 O1 V2 98.0(3) 10_554 . ? V5 O1 V6 140.4(4) 10_554 . ? V2 O1 V6 99.9(3) . . ? V4 O2 V2 142.1(4) . 10_554 ? V4 O2 V1 96.8(3) . . ? V2 O2 V1 96.8(3) 10_554 . ? V5 O3 V7 139.7(4) 10_554 . ? V5 O3 V8 90.9(3) 10_554 . ? V7 O3 V8 90.8(3) . . ? V8 O8 V5 103.3(4) 10_554 . ? V8 O8 V3 143.6(5) 10_554 . ? V5 O8 V3 102.8(3) . . ? V1 O10 V4 100.4(3) . . ? V1 O10 V6 138.4(4) . . ? V4 O10 V6 101.6(3) . . ? V4 O11 V3 142.6(4) . . ? V4 O11 V7 97.1(3) . . ? V3 O11 V7 98.9(3) . . ? V1 O12 V1 132.5(5) 10_554 . ? V1 O14 V2 101.2(3) 10_554 . ? V1 O14 V6 139.7(4) 10_554 . ? V2 O14 V6 100.5(3) . . ? V2 O15 V3 142.3(4) 10_554 . ? V2 O15 V5 96.1(3) 10_554 . ? V3 O15 V5 98.6(3) . . ? V7 O16 V4 98.4(3) . . ? V7 O16 V6 140.5(4) . . ? V4 O16 V6 100.8(3) . . ? V8 O17 V7 103.4(4) . . ? V8 O17 V3 145.2(4) . . ? V7 O17 V3 101.2(3) . . ? O19' O19 V8 60.4(3) . . ? O19' O19 V8 60.4(3) . 10_554 ? V8 O19 V8 120.8(7) . 10_554 ? O19 O19' V8 79.0(3) . . ? O19 O19' V8 79.0(3) . 10_554 ? V8 O19' V8 158.0(6) . 10_554 ? C2 C1 N1 107.5(11) . . ? C2 C1 H1A 126.3 . . ? N1 C1 H1A 126.3 . . ? N2 C2 C1 108.4(10) . . ? N2 C2 H2A 125.8 . . ? C1 C2 H2A 125.8 . . ? N1 C3 N2 111.5(9) . . ? N1 C3 H3A 124.2 . . ? N2 C3 H3A 124.2 . . ? C5 C4 N2 123.1(16) . . ? C5 C4 H4A 106.5 . . ? N2 C4 H4A 106.5 . . ? C5 C4 H4B 106.5 . . ? N2 C4 H4B 106.5 . . ? H4A C4 H4B 106.5 . . ? C7 C6 N4 119.3(16) . . ? C7 C6 H6A 120.3 . . ? N4 C6 H6A 120.3 . . ? C8 C7 C6 123(2) . . ? C8 C7 H7A 118.5 . . ? C6 C7 H7A 118.5 . . ? C7 C8 C9 128(3) . . ? C7 C8 H8A 116.1 . . ? C9 C8 H8A 116.1 . . ? C8 C9 C10 135(2) . . ? C8 C9 C17 110.0(18) . . ? C10 C9 C17 115.2(18) . . ? N4 C17 C16 117.3(12) . . ? N4 C17 C9 125.6(15) . . ? C16 C17 C9 117.1(14) . . ? C17 N4 C6 114.3(13) . . ? C17 N4 Cu2 112.2(10) . . ? C6 N4 Cu2 133.5(11) . . ? C11 C10 C9 126(2) . . ? C11 C10 H10A 117.0 . . ? C9 C10 H10A 117.0 . . ? C12 C11 C10 119(2) . . ? C12 C11 H11A 120.6 . . ? C10 C11 H11A 120.6 . . ? C11 C12 C13 126(2) . . ? C11 C12 C16 123.6(19) . . ? C13 C12 C16 110.8(17) . . ? C14 C13 C12 122(3) . . ? C14 C13 H13A 118.8 . . ? C12 C13 H13A 118.8 . . ? C13 C14 C15 126(3) . . ? C13 C14 H14A 116.9 . . ? C15 C14 H14A 116.9 . . ? C14 C15 N3 116(2) . . ? C14 C15 H15A 121.8 . . ? N3 C15 H15A 121.8 . . ? N3 C16 C12 124.1(14) . . ? N3 C16 C17 116.4(12) . . ? C12 C16 C17 119.4(14) . . ? N5 C18 N6 112.2(14) . . ? N5 C18 H18A 123.9 . . ? N6 C18 H18A 123.9 . . ? C20 C19 N5 110.2(15) . . ? C20 C19 H19A 124.9 . . ? N5 C19 H19A 124.9 . . ? C19 C20 N6 107.3(14) . . ? C19 C20 H20A 126.3 . . ? N6 C20 H20A 126.3 . . ? C22 C21 N6 110.4(12) . . ? C22 C21 H21A 109.6 . . ? N6 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? N6 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C23 112.0(13) . . ? C21 C22 H22A 109.2 . . ? C23 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? C23 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? C22 C23 C24 112.9(13) . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N7 C24 C23 110.3(12) . . ? N7 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? N7 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C26 C25 N7 108.6(16) . . ? C26 C25 H25A 125.7 . . ? N7 C25 H25A 125.7 . . ? C25 C26 N8 106.1(18) . . ? C25 C26 H26A 127.0 . . ? N8 C26 H26A 127.0 . . ? N8 C27 N7 109.9(13) . . ? N8 C27 H27A 125.1 . . ? N7 C27 H27A 125.1 . . ? C29 C28 N10 121.1(17) . . ? C29 C28 H28A 119.4 . . ? N10 C28 H28A 119.4 . . ? C30 C29 C28 121(2) . . ? C30 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? C29 C30 C31 122(2) . . ? C29 C30 H30A 118.8 . . ? C31 C30 H30A 118.8 . . ? C39 C31 C32 122.3(15) . . ? C39 C31 C30 113.4(18) . . ? C32 C31 C30 124.1(17) . . ? C33 C32 C31 117.3(16) . . ? C33 C32 H32A 121.3 . . ? C31 C32 H32A 121.3 . . ? C32 C33 C34 127(2) . . ? C32 C33 H33A 116.3 . . ? C34 C33 H33A 116.3 . . ? C38 C34 C35 123(2) . . ? C38 C34 C33 113.1(19) . . ? C35 C34 C33 124(2) . . ? C34 C35 C36 112.6(18) . . ? C34 C35 H35A 123.7 . . ? C36 C35 H35A 123.7 . . ? C37 C36 C35 121.3(19) . . ? C37 C36 H36A 119.4 . . ? C35 C36 H36A 119.4 . . ? N9 C37 C36 124(2) . . ? N9 C37 H37A 118.2 . . ? C36 C37 H37A 118.2 . . ? C34 C38 N9 120.0(17) . . ? C34 C38 C39 122.0(16) . . ? N9 C38 C39 117.9(12) . . ? N10 C39 C31 128.5(14) . . ? N10 C39 C38 113.9(12) . . ? C31 C39 C38 117.5(14) . . ? C16 N3 C15 119.8(15) . . ? C16 N3 Cu2 112.1(9) . . ? C15 N3 Cu2 128.1(13) . . ? C5 C5' C5 78(2) . 8_667 ? C5' C5 C4 102.1(17) . . ? C5' C5 C5 51.2(11) . 8_667 ? C4 C5 C5 135(2) . 8_667 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.899 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.102