# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email SBROOKER@ALKALI.OTAGO.AC.NZ _publ_contact_author_name 'Dr Sally Brooker' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; Department of Chemistry Department of Chemistry, University of Otago PO Box 56 Dunedin NEW ZEALAND ; _publ_section_title ; Control of molecular architecture by the degree of deprotonation: self-assembled di- and tetranuclear copper(II) complexes of N,N'-bis(2-pyridylmethyl)pyrazine-2,3-dicarboxamide ; loop_ _publ_author_name 'Sally Brooker' 'Julia Hausmann' 'Geoffrey B. Jameson' data_cuh2l _database_code_depnum_ccdc_archive 'CCDC 212607' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H19 B2 Cu F8 N7 O2' _chemical_formula_weight 626.58 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5129(3) _cell_length_b 10.7093(3) _cell_length_c 11.9977(3) _cell_angle_alpha 87.8400(10) _cell_angle_beta 74.2720(10) _cell_angle_gamma 72.5870(10) _cell_volume 1239.22(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 630 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type Semi-empirical(SADABS) _exptl_absorpt_correction_T_min 0.6961 _exptl_absorpt_correction_T_max 0.9807 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _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 11056 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.40 _reflns_number_total 4480 _reflns_number_gt 4023 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.6846P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4480 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Cu1 Cu 0.70659(2) 0.93345(2) 0.601054(19) 0.02092(8) Uani 1 1 d . . . C1 C 0.8267(2) 1.07682(19) 0.74346(16) 0.0236(4) Uani 1 1 d . . . H1 H 0.7921 1.0326 0.8095 0.028 Uiso 1 1 calc R . . C2 C 0.9058(2) 1.15938(19) 0.75173(17) 0.0253(4) Uani 1 1 d . . . H2 H 0.9244 1.1690 0.8236 0.030 Uiso 1 1 calc R . . C3 C 0.92541(18) 1.20857(18) 0.56181(16) 0.0201(4) Uani 1 1 d . . . C4 C 0.84927(18) 1.12575(17) 0.55078(16) 0.0192(4) Uani 1 1 d . . . N1 N 0.79973(16) 1.06010(15) 0.64368(13) 0.0207(3) Uani 1 1 d . . . N4 N 0.95562(17) 1.22475(16) 0.66207(14) 0.0241(3) Uani 1 1 d . . . C5 C 0.81976(19) 1.09564(18) 0.43969(16) 0.0197(4) Uani 1 1 d . . . C6 C 0.7131(2) 0.96547(19) 0.35777(16) 0.0229(4) Uani 1 1 d . . . H6A H 0.7983 0.9254 0.2952 0.027 Uiso 1 1 calc R . . H6B H 0.6529 1.0397 0.3263 0.027 Uiso 1 1 calc R . . C7 C 0.63798(19) 0.86506(19) 0.40150(17) 0.0232(4) Uani 1 1 d . . . C8 C 0.5877(2) 0.8038(2) 0.32959(19) 0.0305(5) Uani 1 1 d . . . H8 H 0.5978 0.8259 0.2509 0.037 Uiso 1 1 calc R . . C9 C 0.5229(2) 0.7104(2) 0.3743(2) 0.0366(5) Uani 1 1 d . . . H9 H 0.4881 0.6677 0.3267 0.044 Uiso 1 1 calc R . . C10 C 0.5096(2) 0.6800(2) 0.4900(2) 0.0350(5) Uani 1 1 d . . . H10 H 0.4658 0.6161 0.5223 0.042 Uiso 1 1 calc R . . C11 C 0.5608(2) 0.74381(19) 0.55698(19) 0.0294(5) Uani 1 1 d . . . H11 H 0.5517 0.7227 0.6358 0.035 Uiso 1 1 calc R . . N2 N 0.74815(16) 1.01141(15) 0.45483(13) 0.0218(3) Uani 1 1 d . . . O1 O 0.86566(15) 1.14482(14) 0.34669(12) 0.0287(3) Uani 1 1 d . . . N3 N 0.62363(16) 0.83575(15) 0.51407(14) 0.0237(3) Uani 1 1 d . . . C15 C 0.98504(19) 1.28361(18) 0.46141(16) 0.0216(4) Uani 1 1 d . . . C16 C 0.9407(2) 1.4814(2) 0.35047(19) 0.0297(5) Uani 1 1 d . . . H16A H 1.0431 1.4585 0.3271 0.036 Uiso 1 1 calc R . . H16B H 0.9033 1.5740 0.3800 0.036 Uiso 1 1 calc R . . C17 C 0.8922(2) 1.4684(2) 0.24503(18) 0.0274(4) Uani 1 1 d . . . C18 C 0.8729(2) 1.5670(2) 0.16758(19) 0.0346(5) Uani 1 1 d . . . H18 H 0.8887 1.6475 0.1802 0.041 Uiso 1 1 calc R . . C19 C 0.8302(2) 1.5477(2) 0.0712(2) 0.0404(6) Uani 1 1 d . . . H19 H 0.8169 1.6153 0.0181 0.049 Uiso 1 1 calc R . . C20 C 0.8070(2) 1.4307(2) 0.0519(2) 0.0397(5) Uani 1 1 d . . . H20 H 0.7768 1.4175 -0.0133 0.048 Uiso 1 1 calc R . . C21 C 0.8289(2) 1.3337(2) 0.12981(19) 0.0353(5) Uani 1 1 d . . . H21 H 0.8157 1.2518 0.1178 0.042 Uiso 1 1 calc R . . N5 N 0.89845(18) 1.39848(16) 0.44398(15) 0.0243(4) Uani 1 1 d . . . H5 H 0.826(2) 1.425(2) 0.491(2) 0.022(6) Uiso 1 1 d . . . N6 N 0.86900(17) 1.35548(18) 0.22294(16) 0.0282(4) Uani 1 1 d . . . H6 H 0.877(2) 1.294(2) 0.268(2) 0.036(7) Uiso 1 1 d . . . O2 O 1.10640(14) 1.24226(14) 0.40252(13) 0.0291(3) Uani 1 1 d . . . N50 N 0.62031(17) 0.88794(16) 0.75905(15) 0.0258(4) Uani 1 1 d . . . C50 C 0.5735(2) 0.85035(19) 0.84646(17) 0.0239(4) Uani 1 1 d . . . C51 C 0.5130(2) 0.8021(2) 0.95727(18) 0.0309(5) Uani 1 1 d . . . H51A H 0.4131 0.8210 0.9688 0.037 Uiso 1 1 calc R . . H51B H 0.5296 0.8456 1.0200 0.037 Uiso 1 1 calc R . . H51C H 0.5558 0.7073 0.9574 0.037 Uiso 1 1 calc R . . B1 B 0.6313(2) 1.4869(2) 0.7705(2) 0.0287(5) Uani 1 1 d . . . F11 F 0.67746(13) 1.45590(13) 0.64928(11) 0.0392(3) Uani 1 1 d . . . F12 F 0.50424(13) 1.58325(13) 0.79294(12) 0.0414(3) Uani 1 1 d . . . F13 F 0.61858(16) 1.37503(14) 0.82760(13) 0.0494(4) Uani 1 1 d . . . F14 F 0.72737(14) 1.53264(15) 0.80291(13) 0.0492(4) Uani 1 1 d . . . B2 B 1.1819(2) 1.0885(2) -0.0244(2) 0.0286(5) Uani 1 1 d . . . F21 F 1.09424(14) 1.15924(13) -0.08817(12) 0.0404(3) Uani 1 1 d . . . F22 F 1.17097(15) 0.96309(13) -0.00658(13) 0.0439(3) Uani 1 1 d . . . F23 F 1.31848(15) 1.07791(16) -0.08687(14) 0.0550(4) Uani 1 1 d . . . F24 F 1.15469(17) 1.15637(15) 0.08004(12) 0.0534(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02432(13) 0.02272(13) 0.01799(13) 0.00421(9) -0.00569(9) -0.01084(9) C1 0.0274(10) 0.0255(10) 0.0183(9) 0.0055(8) -0.0077(8) -0.0077(8) C2 0.0283(10) 0.0281(10) 0.0207(10) 0.0020(8) -0.0094(8) -0.0077(8) C3 0.0196(9) 0.0190(9) 0.0200(9) 0.0017(7) -0.0056(7) -0.0035(7) C4 0.0201(9) 0.0185(9) 0.0182(9) 0.0026(7) -0.0052(7) -0.0049(7) N1 0.0226(8) 0.0206(8) 0.0191(8) 0.0034(6) -0.0060(6) -0.0068(6) N4 0.0265(8) 0.0243(8) 0.0235(8) 0.0027(7) -0.0095(7) -0.0084(7) C5 0.0214(9) 0.0197(9) 0.0177(9) 0.0017(7) -0.0055(7) -0.0055(7) C6 0.0248(9) 0.0269(10) 0.0188(9) 0.0016(8) -0.0080(8) -0.0087(8) C7 0.0210(9) 0.0221(9) 0.0244(10) -0.0013(8) -0.0065(8) -0.0030(8) C8 0.0311(11) 0.0298(11) 0.0323(11) -0.0040(9) -0.0114(9) -0.0084(9) C9 0.0378(12) 0.0301(11) 0.0479(14) -0.0055(10) -0.0168(11) -0.0135(10) C10 0.0363(12) 0.0236(10) 0.0486(14) 0.0026(10) -0.0120(10) -0.0138(9) C11 0.0308(11) 0.0216(10) 0.0355(12) 0.0041(9) -0.0078(9) -0.0090(8) N2 0.0257(8) 0.0243(8) 0.0181(8) 0.0025(6) -0.0072(7) -0.0107(7) O1 0.0422(8) 0.0308(8) 0.0182(7) 0.0058(6) -0.0075(6) -0.0198(7) N3 0.0241(8) 0.0210(8) 0.0262(9) 0.0009(7) -0.0072(7) -0.0069(7) C15 0.0246(10) 0.0243(10) 0.0207(9) 0.0014(8) -0.0085(8) -0.0124(8) C16 0.0312(11) 0.0242(10) 0.0339(12) 0.0101(9) -0.0075(9) -0.0108(9) C17 0.0207(9) 0.0257(10) 0.0298(11) 0.0066(8) -0.0005(8) -0.0044(8) C18 0.0325(11) 0.0271(11) 0.0337(12) 0.0100(9) -0.0001(9) -0.0028(9) C19 0.0368(12) 0.0395(13) 0.0325(12) 0.0167(10) -0.0038(10) -0.0001(10) C20 0.0360(12) 0.0509(14) 0.0276(12) 0.0112(10) -0.0089(10) -0.0075(11) C21 0.0356(12) 0.0422(13) 0.0293(12) 0.0065(10) -0.0088(9) -0.0138(10) N5 0.0238(9) 0.0227(9) 0.0243(9) 0.0051(7) -0.0036(8) -0.0070(7) N6 0.0281(9) 0.0290(9) 0.0268(9) 0.0111(8) -0.0068(7) -0.0092(7) O2 0.0234(7) 0.0286(7) 0.0311(8) 0.0083(6) -0.0026(6) -0.0069(6) N50 0.0251(8) 0.0283(9) 0.0249(9) 0.0036(7) -0.0057(7) -0.0107(7) C50 0.0242(9) 0.0243(10) 0.0241(11) 0.0001(8) -0.0070(8) -0.0081(8) C51 0.0371(11) 0.0325(11) 0.0224(10) 0.0058(9) -0.0051(9) -0.0129(9) B1 0.0304(12) 0.0291(12) 0.0271(12) 0.0017(10) -0.0059(10) -0.0113(10) F11 0.0404(7) 0.0432(8) 0.0276(7) -0.0006(6) -0.0015(5) -0.0100(6) F12 0.0309(7) 0.0438(8) 0.0384(7) 0.0003(6) -0.0005(6) -0.0030(6) F13 0.0657(10) 0.0389(8) 0.0442(8) 0.0159(6) -0.0124(7) -0.0208(7) F14 0.0413(8) 0.0573(9) 0.0559(9) -0.0065(7) -0.0149(7) -0.0223(7) B2 0.0334(12) 0.0308(12) 0.0254(12) 0.0077(10) -0.0130(10) -0.0117(10) F21 0.0504(8) 0.0404(7) 0.0412(8) 0.0145(6) -0.0292(6) -0.0159(6) F22 0.0533(8) 0.0358(7) 0.0510(9) 0.0151(6) -0.0214(7) -0.0208(6) F23 0.0380(8) 0.0596(10) 0.0671(11) 0.0206(8) -0.0092(7) -0.0208(7) F24 0.0811(11) 0.0474(8) 0.0308(7) 0.0009(6) -0.0247(7) -0.0096(8) _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 N2 1.9126(16) . y Cu1 N50 1.9790(17) . y Cu1 N3 2.0165(16) . y Cu1 N1 2.0442(16) . y Cu1 O2 2.2703(14) 2_776 y C1 N1 1.333(2) . ? C1 C2 1.405(3) . ? C2 N4 1.334(3) . ? C3 N4 1.354(2) . ? C3 C4 1.391(3) . ? C3 C15 1.520(3) . ? C4 N1 1.361(2) . ? C4 C5 1.514(2) . ? C5 O1 1.253(2) . ? C5 N2 1.316(2) . ? C6 N2 1.456(2) . ? C6 C7 1.515(3) . ? C7 N3 1.353(3) . ? C7 C8 1.397(3) . ? C8 C9 1.386(3) . ? C9 C10 1.392(3) . ? C10 C11 1.378(3) . ? C11 N3 1.356(3) . ? C15 O2 1.233(2) . ? C15 N5 1.341(3) . ? C16 N5 1.462(2) . ? C16 C17 1.512(3) . ? C17 N6 1.352(3) . ? C17 C18 1.386(3) . ? C18 C19 1.392(3) . ? C19 C20 1.385(4) . ? C20 C21 1.381(3) . ? C21 N6 1.347(3) . ? O2 Cu1 2.2703(14) 2_776 ? N50 C50 1.145(3) . ? C50 C51 1.458(3) . ? B1 F13 1.381(3) . ? B1 F12 1.387(3) . ? B1 F14 1.391(3) . ? B1 F11 1.420(3) . ? B2 F22 1.386(3) . ? B2 F24 1.389(3) . ? B2 F21 1.389(3) . ? B2 F23 1.401(3) . ? 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 N2 Cu1 N50 165.93(7) . . y N2 Cu1 N3 81.82(7) . . y N50 Cu1 N3 97.39(7) . . y N2 Cu1 N1 81.08(6) . . y N50 Cu1 N1 98.90(7) . . y N3 Cu1 N1 162.85(6) . . y N2 Cu1 O2 106.16(6) . 2_776 y N50 Cu1 O2 87.91(6) . 2_776 y N3 Cu1 O2 93.70(6) . 2_776 y N1 Cu1 O2 92.22(6) . 2_776 y N1 C1 C2 120.49(18) . . ? N4 C2 C1 122.22(18) . . ? N4 C3 C4 122.28(17) . . ? N4 C3 C15 115.09(16) . . ? C4 C3 C15 122.59(16) . . ? N1 C4 C3 119.84(17) . . ? N1 C4 C5 114.83(16) . . ? C3 C4 C5 125.28(16) . . ? C1 N1 C4 118.51(16) . . ? C1 N1 Cu1 129.19(13) . . ? C4 N1 Cu1 112.03(12) . . ? C2 N4 C3 116.63(17) . . ? O1 C5 N2 127.17(17) . . ? O1 C5 C4 121.03(16) . . ? N2 C5 C4 111.74(15) . . ? N2 C6 C7 107.91(15) . . ? N3 C7 C8 121.27(18) . . ? N3 C7 C6 116.55(17) . . ? C8 C7 C6 122.17(18) . . ? C9 C8 C7 119.3(2) . . ? C8 C9 C10 119.1(2) . . ? C11 C10 C9 119.2(2) . . ? N3 C11 C10 122.1(2) . . ? C5 N2 C6 120.61(15) . . ? C5 N2 Cu1 120.08(13) . . ? C6 N2 Cu1 118.96(12) . . ? C7 N3 C11 119.07(18) . . ? C7 N3 Cu1 114.64(13) . . ? C11 N3 Cu1 126.26(14) . . ? O2 C15 N5 122.78(18) . . ? O2 C15 C3 121.57(17) . . ? N5 C15 C3 115.62(16) . . ? N5 C16 C17 113.49(17) . . ? N6 C17 C18 117.9(2) . . ? N6 C17 C16 119.39(17) . . ? C18 C17 C16 122.7(2) . . ? C17 C18 C19 119.7(2) . . ? C20 C19 C18 120.6(2) . . ? C21 C20 C19 118.3(2) . . ? N6 C21 C20 119.8(2) . . ? C15 N5 C16 121.94(17) . . ? C21 N6 C17 123.62(19) . . ? C15 O2 Cu1 137.17(13) . 2_776 y C50 N50 Cu1 173.84(17) . . ? N50 C50 C51 179.5(2) . . ? F13 B1 F12 110.76(18) . . ? F13 B1 F14 110.38(19) . . ? F12 B1 F14 110.30(19) . . ? F13 B1 F11 108.58(18) . . ? F12 B1 F11 107.65(18) . . ? F14 B1 F11 109.08(18) . . ? F22 B2 F24 111.30(18) . . ? F22 B2 F21 111.78(18) . . ? F24 B2 F21 109.65(19) . . ? F22 B2 F23 108.07(19) . . ? F24 B2 F23 107.70(19) . . ? F21 B2 F23 108.18(18) . . ? 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 N1 C1 C2 N4 0.7(3) . . . . ? N4 C3 C4 N1 1.6(3) . . . . ? C15 C3 C4 N1 179.32(16) . . . . ? N4 C3 C4 C5 -175.63(17) . . . . ? C15 C3 C4 C5 2.1(3) . . . . ? C2 C1 N1 C4 -0.7(3) . . . . ? C2 C1 N1 Cu1 172.89(14) . . . . ? C3 C4 N1 C1 -0.4(2) . . . . ? C5 C4 N1 C1 177.10(16) . . . . ? C3 C4 N1 Cu1 -174.99(13) . . . . ? C5 C4 N1 Cu1 2.47(18) . . . . ? N2 Cu1 N1 C1 -177.66(17) . . . . ? N50 Cu1 N1 C1 16.59(17) . . . . ? N3 Cu1 N1 C1 178.18(19) . . . . ? O2 Cu1 N1 C1 -71.65(16) 2_776 . . . ? N2 Cu1 N1 C4 -3.75(12) . . . . ? N50 Cu1 N1 C4 -169.50(12) . . . . ? N3 Cu1 N1 C4 -7.9(3) . . . . ? O2 Cu1 N1 C4 102.27(12) 2_776 . . . ? C1 C2 N4 C3 0.5(3) . . . . ? C4 C3 N4 C2 -1.6(3) . . . . ? C15 C3 N4 C2 -179.49(16) . . . . ? N1 C4 C5 O1 -176.49(16) . . . . ? C3 C4 C5 O1 0.8(3) . . . . ? N1 C4 C5 N2 1.1(2) . . . . ? C3 C4 C5 N2 178.39(17) . . . . ? N2 C6 C7 N3 -2.3(2) . . . . ? N2 C6 C7 C8 178.70(17) . . . . ? N3 C7 C8 C9 -0.6(3) . . . . ? C6 C7 C8 C9 178.41(18) . . . . ? C7 C8 C9 C10 0.0(3) . . . . ? C8 C9 C10 C11 0.2(3) . . . . ? C9 C10 C11 N3 0.2(3) . . . . ? O1 C5 N2 C6 -0.3(3) . . . . ? C4 C5 N2 C6 -177.74(15) . . . . ? O1 C5 N2 Cu1 172.78(15) . . . . ? C4 C5 N2 Cu1 -4.6(2) . . . . ? C7 C6 N2 C5 177.02(16) . . . . ? C7 C6 N2 Cu1 3.82(19) . . . . ? N50 Cu1 N2 C5 95.8(3) . . . . ? N3 Cu1 N2 C5 -176.42(15) . . . . ? N1 Cu1 N2 C5 4.81(14) . . . . ? O2 Cu1 N2 C5 -84.92(15) 2_776 . . . ? N50 Cu1 N2 C6 -90.9(3) . . . . ? N3 Cu1 N2 C6 -3.19(13) . . . . ? N1 Cu1 N2 C6 178.05(14) . . . . ? O2 Cu1 N2 C6 88.32(14) 2_776 . . . ? C8 C7 N3 C11 0.9(3) . . . . ? C6 C7 N3 C11 -178.13(17) . . . . ? C8 C7 N3 Cu1 179.01(14) . . . . ? C6 C7 N3 Cu1 0.0(2) . . . . ? C10 C11 N3 C7 -0.7(3) . . . . ? C10 C11 N3 Cu1 -178.57(15) . . . . ? N2 Cu1 N3 C7 1.69(13) . . . . ? N50 Cu1 N3 C7 167.51(13) . . . . ? N1 Cu1 N3 C7 5.8(3) . . . . ? O2 Cu1 N3 C7 -104.12(13) 2_776 . . . ? N2 Cu1 N3 C11 179.65(17) . . . . ? N50 Cu1 N3 C11 -14.53(17) . . . . ? N1 Cu1 N3 C11 -176.20(19) . . . . ? O2 Cu1 N3 C11 73.84(16) 2_776 . . . ? N4 C3 C15 O2 80.9(2) . . . . ? C4 C3 C15 O2 -97.0(2) . . . . ? N4 C3 C15 N5 -97.2(2) . . . . ? C4 C3 C15 N5 84.9(2) . . . . ? N5 C16 C17 N6 -26.5(3) . . . . ? N5 C16 C17 C18 154.85(19) . . . . ? N6 C17 C18 C19 0.3(3) . . . . ? C16 C17 C18 C19 178.95(19) . . . . ? C17 C18 C19 C20 -0.1(3) . . . . ? C18 C19 C20 C21 -0.8(3) . . . . ? C19 C20 C21 N6 1.4(3) . . . . ? O2 C15 N5 C16 2.2(3) . . . . ? C3 C15 N5 C16 -179.73(17) . . . . ? C17 C16 N5 C15 99.6(2) . . . . ? C20 C21 N6 C17 -1.2(3) . . . . ? C18 C17 N6 C21 0.3(3) . . . . ? C16 C17 N6 C21 -178.38(19) . . . . ? N5 C15 O2 Cu1 176.85(14) . . . 2_776 ? C3 C15 O2 Cu1 -1.1(3) . . . 2_776 ? N2 Cu1 N50 C50 130.0(14) . . . . ? N3 Cu1 N50 C50 44.2(15) . . . . ? N1 Cu1 N50 C50 -141.2(15) . . . . ? O2 Cu1 N50 C50 -49.3(15) 2_776 . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.626 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.050 data_l3l8cus2a _database_code_depnum_ccdc_archive 'CCDC 212608' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H60 B4 Cu4 F16 N27.50 O8' _chemical_formula_weight 2123.95 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 21.4502(5) _cell_length_b 21.4616(5) _cell_length_c 19.9220(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.156(2) _cell_angle_gamma 90.00 _cell_volume 9171.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 17369 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 26.65 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4282 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type 'Semi-empirical (SADABS)' _exptl_absorpt_correction_T_min 0.6747 _exptl_absorpt_correction_T_max 0.8225 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART area detector' _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 21082 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.1489 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.48 _reflns_number_total 15580 _reflns_number_gt 8779 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Because of the near tetragonality of the unit cell, a variety of monoclinic twin laws were tested both with and without inversion twinning (in matrix form, row by row): (0 0 1, 0 -1 0, 1 0 0); (0 1 0, 1 0 0, 0 0 -1). All led to R1 (F > 4 sig(F)) greater than 0.15. The adopted twin law (0 1 0, -1 0 0 , 0 0 -1), which led to satisfactory elaboration of the initial structure and to stable least-squares refinements, leads to four non- inversion-related twin domains with fractional sizes of the three independent components: 0.184(2), 0.112(2), 0.311(2). Reflections of the class hh0,h=2n+1 are systematically very weak. Intensity statistics (E^2^-1 = 0.708) are consistent with acentric twinned data (and with the consequences that incorrectly assigned features of Fourier maps tended to refine quite well, and missing atoms of disordered BF4- groups were not strongly differentiated from noise). Moreover, as the molecular species has 4mm symmetry and refinement in space group Cc revealed no signs of disorder, centrosymmetric monoclinic space groups, which would impose inversion symmetry, can be eliminated. Merging of data into orthorhombic or tetragonal crystal classes led to R(int) > 0.15, whereas monoclinic merging led to R(int) = 0.074. Thus, orthorhombic and tetragonal crystal classes can be eliminated also. Merging of data in triclinic symmetry was no better (or worse) than for monoclinic. Because of the near- tetragonal data symmetry and near-4mm symmetry of the complex, considerable correlation exists among formally chemically equivalent bond distances and angles, leading to patterns of unnaturally long and short interatomic distances. Therefore, bond distances that are formally chemically equivalent were refined by means of free variables. In addition tight planarity restraints were applied to appropriate rings and tight restraints to nearly spherical ellipsoids were applied to the atomic displacement parameters of B, C, N, O and F atoms. Although the flourine toms of the BF4- groups exhibited large anisotropic displacement parameters, and were flagged by SHELXL for contemplation of disorder, various disordered models applied to the BF4- groupos led to unstable refinements, despite very tight restraints on geometry and especially on atomic displacement parameters. The "amide" hydrogen atoms shared between pairs of oxygen atoms O2 and O1, O3 and O4, O5 and O6, and O7 and O8 were not observed in this structure (although in other structures they are observable, just, and are symmetrically located). As the electron density is shared between two strongly electronegative atoms, and as the hydrogen atom is formally a proton, the amount of electron density to be expected on the hydrogen atom is very small, and will only be observable in extremely well-behaved structures. Therefore, these hydrogen atoms have been inserted symmetrically between pairs of oxygen atoms to make chemical sense. Refinements converged satisfactorily; high final shift/sigma ratios are observed only for the nearly overlapping sites of the disordered acetonitrile groups, whose hydrogen atoms have been omitted. ; _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^)+(0.0150P)^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 mixed _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 -0.025(14) _refine_ls_number_reflns 15580 _refine_ls_number_parameters 1314 _refine_ls_number_restraints 1451 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.1166 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 0.117 _refine_ls_shift/su_mean 0.007 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 0.15466(9) 0.48018(9) 0.67461(10) 0.0479(5) Uani 1 1 d . . . Cu2 Cu -0.03523(11) 0.20793(10) 0.70544(11) 0.0588(7) Uani 1 1 d . . . Cu3 Cu 0.23639(10) 0.01916(9) 0.68565(10) 0.0484(6) Uani 1 1 d . . . Cu4 Cu 0.42534(11) 0.28992(10) 0.71012(11) 0.0516(6) Uani 1 1 d . . . N3 N 0.1982(2) 0.5607(4) 0.7210(5) 0.057(3) Uani 1 1 d DU . . N2 N 0.1195(5) 0.4767(5) 0.7621(6) 0.049(3) Uani 1 1 d DU . . N1 N 0.0959(3) 0.3943(4) 0.6714(4) 0.042(3) Uani 1 1 d DU . . N4 N 0.0229(3) 0.2922(4) 0.6835(5) 0.051(3) Uani 1 1 d DU . . N5 N -0.0315(5) 0.2547(5) 0.7900(5) 0.043(3) Uani 1 1 d DU . . N6 N -0.0814(2) 0.1424(4) 0.7681(6) 0.069(3) Uani 1 1 d DU . . O1 O 0.0708(5) 0.4217(5) 0.8438(5) 0.065(3) Uani 1 1 d DU . . O2 O 0.0085(6) 0.3275(5) 0.8572(5) 0.069(3) Uani 1 1 d DU . . H2A H 0.0418 0.3708 0.8539 0.104 Uiso 1 1 d . . . N9 N -0.1129(3) 0.2505(3) 0.6618(6) 0.053(3) Uani 1 1 d DU . . N8 N -0.0292(5) 0.1719(6) 0.6159(6) 0.052(3) Uani 1 1 d DU . . N7 N 0.0486(4) 0.1512(3) 0.7092(5) 0.051(3) Uani 1 1 d DU . . N10 N 0.1533(4) 0.0808(4) 0.7030(5) 0.055(3) Uani 1 1 d DU . . N11 N 0.1983(5) 0.0275(6) 0.5972(6) 0.054(3) Uani 1 1 d DU . . N12 N 0.3057(4) -0.0250(3) 0.6211(5) 0.057(3) Uani 1 1 d DU . . O3 O 0.0274(5) 0.1206(5) 0.5370(5) 0.068(3) Uani 1 1 d DU . . O4 O 0.1199(5) 0.0665(6) 0.5281(5) 0.064(3) Uani 1 1 d DU . . H4A H 0.0731 0.0943 0.5379 0.097 Uiso 1 1 d . . . N15 N 0.1928(2) -0.0618(4) 0.7337(5) 0.062(3) Uani 1 1 d DU . . N14 N 0.2712(6) 0.0261(5) 0.7765(6) 0.048(3) Uani 1 1 d DU . . N13 N 0.2918(3) 0.1037(4) 0.6812(5) 0.045(3) Uani 1 1 d DU . . N16 N 0.3686(3) 0.2060(5) 0.6899(5) 0.049(3) Uani 1 1 d DU . . N17 N 0.4212(5) 0.2488(5) 0.7948(5) 0.042(3) Uani 1 1 d DU . . N18 N 0.4707(2) 0.3570(4) 0.7678(6) 0.056(3) Uani 1 1 d DU . . O5 O 0.3143(5) 0.0836(5) 0.8574(5) 0.062(3) Uani 1 1 d DU . . O6 O 0.3756(6) 0.1798(5) 0.8670(5) 0.061(3) Uani 1 1 d DU . . H6A H 0.3459 0.1344 0.8640 0.091 Uiso 1 1 d . . . N21 N 0.5035(3) 0.2467(3) 0.6681(5) 0.039(3) Uani 1 1 d DU . . N20 N 0.4234(5) 0.3244(6) 0.6223(6) 0.052(3) Uani 1 1 d DU . . N19 N 0.3401(4) 0.3492(3) 0.7115(5) 0.056(3) Uani 1 1 d DU . . N22 N 0.2357(6) 0.4190(5) 0.6956(5) 0.051(3) Uani 1 1 d DU . . N23 N 0.1955(4) 0.4725(4) 0.5847(5) 0.041(3) Uani 1 1 d DU . . N24 N 0.0878(3) 0.5261(3) 0.6075(5) 0.046(3) Uani 1 1 d DU . . O7 O 0.3669(6) 0.3763(6) 0.5374(5) 0.071(3) Uani 1 1 d DU . . H8A H 0.3228 0.4082 0.5341 0.106 Uiso 1 1 d . . . O8 O 0.2738(6) 0.4323(6) 0.5212(5) 0.063(3) Uani 1 1 d DU . . C12 C 0.2368(4) 0.5973(5) 0.6860(7) 0.061(4) Uani 1 1 d DU . . H12 H 0.2488 0.5862 0.6417 0.073 Uiso 1 1 calc R . . C11 C 0.2581(5) 0.6496(6) 0.7139(6) 0.060(3) Uani 1 1 d DU . . H11 H 0.2859 0.6762 0.6903 0.072 Uiso 1 1 calc R . . C10 C 0.2390(4) 0.6639(6) 0.7771(6) 0.059(3) Uani 1 1 d DU . . H10 H 0.2534 0.7012 0.7976 0.070 Uiso 1 1 calc R . . C9 C 0.1980(4) 0.6243(5) 0.8133(7) 0.059(4) Uani 1 1 d DU . . H9 H 0.1848 0.6342 0.8576 0.071 Uiso 1 1 calc R . . C8 C 0.1779(4) 0.5705(5) 0.7811(6) 0.055(3) Uani 1 1 d DU . . C7 C 0.1399(7) 0.5196(6) 0.8143(7) 0.063(4) Uani 1 1 d DU . . H7A H 0.1656 0.4974 0.8480 0.075 Uiso 1 1 calc R . . H7B H 0.1034 0.5379 0.8373 0.075 Uiso 1 1 calc R . . C5 C 0.0867(7) 0.4298(6) 0.7843(6) 0.050(3) Uani 1 1 d DU . . C4 C 0.0720(3) 0.3828(4) 0.7306(6) 0.049(3) Uani 1 1 d DU . . C1 C 0.0854(3) 0.3589(4) 0.6191(6) 0.050(3) Uani 1 1 d DU . . H1 H 0.1031 0.3686 0.5767 0.060 Uiso 1 1 calc R . . C2 C 0.0490(4) 0.3086(5) 0.6268(6) 0.051(3) Uani 1 1 d DU . . H2 H 0.0417 0.2832 0.5886 0.061 Uiso 1 1 calc R . . C3 C 0.0337(4) 0.3291(5) 0.7382(6) 0.049(3) Uani 1 1 d DU . . C13 C 0.0015(7) 0.3042(6) 0.7998(6) 0.055(3) Uani 1 1 d DU . . C15 C -0.0555(6) 0.2199(5) 0.8484(6) 0.045(3) Uani 1 1 d DU . . H15 H -0.0833 0.2477 0.8743 0.053 Uiso 1 1 calc R . . H15' H -0.0199 0.2089 0.8779 0.053 Uiso 1 1 calc R . . C16 C -0.0916(3) 0.1596(5) 0.8311(6) 0.057(3) Uani 1 1 d DU . . C20 C -0.1027(4) 0.0841(6) 0.7512(8) 0.070(4) Uani 1 1 d DU . . H20 H -0.0958 0.0714 0.7062 0.084 Uiso 1 1 calc R . . C19 C -0.1328(5) 0.0423(7) 0.7918(7) 0.073(4) Uani 1 1 d DU . . H19 H -0.1459 0.0024 0.7767 0.087 Uiso 1 1 calc R . . C18 C -0.1419(5) 0.0622(6) 0.8533(8) 0.091(5) Uani 1 1 d DU . . H18 H -0.1631 0.0361 0.8842 0.109 Uiso 1 1 calc R . . C17 C -0.1210(4) 0.1217(6) 0.8750(7) 0.071(4) Uani 1 1 d DU . . H17 H -0.1277 0.1347 0.9200 0.085 Uiso 1 1 calc R . . C32 C -0.1567(6) 0.2897(5) 0.6831(8) 0.065(4) Uani 1 1 d DU . . H32 H -0.1516 0.3046 0.7277 0.078 Uiso 1 1 calc R . . C31 C -0.2076(7) 0.3113(7) 0.6496(7) 0.070(4) Uani 1 1 d DU . . H31 H -0.2360 0.3386 0.6713 0.083 Uiso 1 1 calc R . . C30 C -0.2177(6) 0.2936(5) 0.5844(7) 0.069(4) Uani 1 1 d DU . . H30 H -0.2519 0.3077 0.5580 0.083 Uiso 1 1 calc R . . C29 C -0.1722(5) 0.2527(5) 0.5614(8) 0.077(4) Uani 1 1 d DU . . H29 H -0.1754 0.2375 0.5167 0.092 Uiso 1 1 calc R . . C28 C -0.1235(5) 0.2335(5) 0.5998(6) 0.060(4) Uani 1 1 d DU . . C27 C -0.0777(6) 0.1894(7) 0.5678(7) 0.060(4) Uani 1 1 d DU . . H27A H -0.0999 0.1515 0.5523 0.072 Uiso 1 1 calc R . . H27B H -0.0584 0.2095 0.5283 0.072 Uiso 1 1 calc R . . C25 C 0.0177(6) 0.1379(7) 0.5964(6) 0.053(3) Uani 1 1 d DU . . C24 C 0.0645(4) 0.1260(3) 0.6504(6) 0.042(3) Uani 1 1 d DU . . C21 C 0.0831(5) 0.1418(4) 0.7627(7) 0.063(4) Uani 1 1 d DU . . H21 H 0.0704 0.1603 0.8037 0.075 Uiso 1 1 calc R . . C22 C 0.1375(6) 0.1060(5) 0.7628(7) 0.067(4) Uani 1 1 d DU . . H22 H 0.1618 0.0998 0.8021 0.080 Uiso 1 1 calc R . . C23 C 0.1188(5) 0.0894(4) 0.6461(6) 0.045(3) Uani 1 1 d DU . . C33 C 0.1457(6) 0.0556(7) 0.5867(6) 0.044(3) Uani 1 1 d DU . . C35 C 0.2198(6) -0.0122(7) 0.5403(7) 0.063(4) Uani 1 1 d DU . . H35A H 0.2207 0.0120 0.4980 0.075 Uiso 1 1 calc R . . H35B H 0.1918 -0.0485 0.5343 0.075 Uiso 1 1 calc R . . C36 C 0.2848(5) -0.0333(4) 0.5596(6) 0.054(3) Uani 1 1 d DU . . C40 C 0.3606(6) -0.0456(5) 0.6430(8) 0.079(4) Uani 1 1 d DU . . H40 H 0.3756 -0.0396 0.6874 0.095 Uiso 1 1 calc R . . C39 C 0.3938(8) -0.0771(6) 0.5929(8) 0.089(5) Uani 1 1 d DU . . H39 H 0.4338 -0.0926 0.6049 0.106 Uiso 1 1 calc R . . C38 C 0.3748(7) -0.0874(6) 0.5302(8) 0.092(5) Uani 1 1 d DU . . H38 H 0.4002 -0.1100 0.4997 0.111 Uiso 1 1 calc R . . C37 C 0.3157(7) -0.0639(5) 0.5098(8) 0.081(4) Uani 1 1 d DU . . H37 H 0.2994 -0.0689 0.4657 0.097 Uiso 1 1 calc R . . C52 C 0.1572(4) -0.0978(6) 0.6955(8) 0.064(4) Uani 1 1 d DU . . H52 H 0.1471 -0.0872 0.6504 0.077 Uiso 1 1 calc R . . C51 C 0.1360(5) -0.1510(7) 0.7251(7) 0.062(4) Uani 1 1 d DU . . H51 H 0.1102 -0.1791 0.7009 0.075 Uiso 1 1 calc R . . C50 C 0.1522(5) -0.1632(7) 0.7896(8) 0.082(4) Uani 1 1 d DU . . H50 H 0.1372 -0.2005 0.8096 0.098 Uiso 1 1 calc R . . C49 C 0.1900(5) -0.1234(5) 0.8284(8) 0.069(4) Uani 1 1 d DU . . H49 H 0.2010 -0.1323 0.8736 0.082 Uiso 1 1 calc R . . C48 C 0.2103(4) -0.0696(5) 0.7950(5) 0.046(3) Uani 1 1 d DU . . C47 C 0.2531(7) -0.0213(6) 0.8261(7) 0.051(4) Uani 1 1 d DU . . H47A H 0.2316 -0.0010 0.8641 0.062 Uiso 1 1 calc R . . H47B H 0.2909 -0.0421 0.8438 0.062 Uiso 1 1 calc R . . C45 C 0.3019(7) 0.0749(6) 0.7971(6) 0.044(3) Uani 1 1 d DU . . C44 C 0.3167(3) 0.1208(4) 0.7412(6) 0.043(3) Uani 1 1 d DU . . C41 C 0.3047(4) 0.1358(5) 0.6283(7) 0.055(4) Uani 1 1 d DU . . H41 H 0.2877 0.1241 0.5861 0.066 Uiso 1 1 calc R . . C42 C 0.3443(4) 0.1883(5) 0.6332(6) 0.041(3) Uani 1 1 d DU . . H42 H 0.3533 0.2114 0.5938 0.049 Uiso 1 1 calc R . . C43 C 0.3559(4) 0.1734(5) 0.7450(6) 0.041(3) Uani 1 1 d DU . . C53 C 0.3838(7) 0.2022(6) 0.8084(6) 0.043(3) Uani 1 1 d DU . . C55 C 0.4441(7) 0.2826(6) 0.8563(6) 0.048(3) Uani 1 1 d DU . . H55A H 0.4733 0.2558 0.8818 0.058 Uiso 1 1 calc R . . H55B H 0.4086 0.2932 0.8857 0.058 Uiso 1 1 calc R . . C56 C 0.4773(3) 0.3420(5) 0.8334(6) 0.057(4) Uani 1 1 d DU . . C60 C 0.4948(4) 0.4125(6) 0.7500(9) 0.073(4) Uani 1 1 d DU . . H60 H 0.4898 0.4227 0.7039 0.088 Uiso 1 1 calc R . . C59 C 0.5247(5) 0.4558(7) 0.7863(8) 0.080(4) Uani 1 1 d DU . . H59 H 0.5400 0.4939 0.7684 0.096 Uiso 1 1 calc R . . C58 C 0.5303(6) 0.4391(6) 0.8506(8) 0.087(4) Uani 1 1 d DU . . H58 H 0.5511 0.4668 0.8804 0.104 Uiso 1 1 calc R . . C57 C 0.5070(5) 0.3823(6) 0.8769(8) 0.076(4) Uani 1 1 d DU . . H57 H 0.5118 0.3723 0.9230 0.091 Uiso 1 1 calc R . . C72 C 0.5446(6) 0.2060(5) 0.6957(8) 0.070(4) Uani 1 1 d DU . . H72 H 0.5377 0.1918 0.7403 0.084 Uiso 1 1 calc R . . C71 C 0.5967(7) 0.1843(7) 0.6609(8) 0.083(5) Uani 1 1 d DU . . H71 H 0.6241 0.1553 0.6818 0.099 Uiso 1 1 calc R . . C70 C 0.6086(7) 0.2043(5) 0.5974(8) 0.072(4) Uani 1 1 d DU . . H70 H 0.6441 0.1905 0.5731 0.087 Uiso 1 1 calc R . . C69 C 0.5659(5) 0.2459(5) 0.5702(8) 0.065(4) Uani 1 1 d DU . . H69 H 0.5714 0.2614 0.5260 0.078 Uiso 1 1 calc R . . C68 C 0.5163(5) 0.2643(4) 0.6074(6) 0.045(3) Uani 1 1 d DU . . C67 C 0.4721(6) 0.3081(7) 0.5744(7) 0.053(4) Uani 1 1 d DU . . H67A H 0.4944 0.3461 0.5599 0.063 Uiso 1 1 calc R . . H67B H 0.4533 0.2883 0.5343 0.063 Uiso 1 1 calc R . . C65 C 0.3738(6) 0.3557(7) 0.5988(6) 0.048(3) Uani 1 1 d DU . . C64 C 0.3268(4) 0.3736(3) 0.6497(6) 0.042(3) Uani 1 1 d DU . . C61 C 0.3032(4) 0.3593(4) 0.7636(7) 0.056(4) Uani 1 1 d DU . . H61 H 0.3131 0.3424 0.8064 0.067 Uiso 1 1 calc R . . C62 C 0.2498(6) 0.3952(5) 0.7547(7) 0.062(4) Uani 1 1 d DU . . H62 H 0.2231 0.4027 0.7918 0.075 Uiso 1 1 calc R . . C63 C 0.2719(4) 0.4101(3) 0.6414(6) 0.048(3) Uani 1 1 d DU . . C73 C 0.2468(6) 0.4395(7) 0.5777(6) 0.043(3) Uani 1 1 d DU . . C75 C 0.1726(6) 0.5088(7) 0.5278(7) 0.052(4) Uani 1 1 d DU . . H75A H 0.1696 0.4822 0.4873 0.063 Uiso 1 1 calc R . . H75B H 0.2012 0.5438 0.5181 0.063 Uiso 1 1 calc R . . C76 C 0.1095(4) 0.5329(4) 0.5467(5) 0.039(3) Uani 1 1 d DU . . C80 C 0.0305(6) 0.5502(5) 0.6242(8) 0.066(4) Uani 1 1 d DU . . H81 H 0.0147 0.5451 0.6684 0.079 Uiso 1 1 calc R . . C79 C -0.0034(6) 0.5814(5) 0.5775(6) 0.056(3) Uani 1 1 d DU . . H79 H -0.0431 0.5977 0.5892 0.067 Uiso 1 1 calc R . . C78 C 0.0188(6) 0.5898(5) 0.5134(7) 0.065(4) Uani 1 1 d DU . . H78 H -0.0043 0.6123 0.4806 0.078 Uiso 1 1 calc R . . C77 C 0.0768(6) 0.5638(4) 0.4986(7) 0.063(4) Uani 1 1 d DU . . H77 H 0.0936 0.5678 0.4547 0.076 Uiso 1 1 calc R . . B1 B 0.0599(6) 0.3367(6) 0.4300(6) 0.060(4) Uani 1 1 d DU . . F11 F 0.0418(5) 0.3513(6) 0.3698(5) 0.128(4) Uani 1 1 d DU . . F12 F 0.1049(5) 0.3741(5) 0.4542(5) 0.106(4) Uani 1 1 d DU . . F13 F 0.0147(4) 0.3271(6) 0.4733(5) 0.111(4) Uani 1 1 d DU . . F14 F 0.0865(5) 0.2788(4) 0.4186(8) 0.176(5) Uani 1 1 d DU . . B2 B 0.5968(8) 0.3904(7) 0.4480(7) 0.097(5) Uani 1 1 d DU . . F21 F 0.5565(8) 0.4307(6) 0.4173(8) 0.255(7) Uani 1 1 d DU . . F22 F 0.6497(6) 0.4049(7) 0.4205(7) 0.212(6) Uani 1 1 d DU . . F23 F 0.5749(6) 0.3330(4) 0.4303(6) 0.107(4) Uani 1 1 d DU . . F24 F 0.5967(7) 0.3968(6) 0.5130(5) 0.140(5) Uani 1 1 d DU . . B3 B 0.2942(7) 0.3922(7) 0.9437(7) 0.093(5) Uani 1 1 d DU . . F31 F 0.2893(7) 0.3951(6) 1.0094(5) 0.144(5) Uani 1 1 d DU . . F32 F 0.3396(7) 0.4285(6) 0.9197(9) 0.235(7) Uani 1 1 d DU . . F33 F 0.2431(6) 0.4086(7) 0.9125(6) 0.174(5) Uani 1 1 d DU . . F34 F 0.3113(6) 0.3325(4) 0.9247(6) 0.103(4) Uani 1 1 d DU . . B4 B 0.3370(7) 0.8493(7) 0.9347(8) 0.088(5) Uani 1 1 d DU . . F41 F 0.3765(5) 0.8208(5) 0.9767(5) 0.103(4) Uani 1 1 d DU . . F42 F 0.3179(6) 0.8108(7) 0.8881(7) 0.225(6) Uani 1 1 d DU . . F43 F 0.3661(7) 0.8957(7) 0.9046(9) 0.248(7) Uani 1 1 d DU . . F44 F 0.2871(4) 0.8726(5) 0.9672(6) 0.097(4) Uani 1 1 d DU . . N600 N 0.969(3) 1.009(2) 0.4956(11) 0.19(2) Uiso 0.50 1 d PDU A 1 C600 C 0.974(3) 0.996(2) 0.5526(11) 0.138(19) Uiso 0.50 1 d PDU A 1 C601 C 0.9794(16) 1.0058(15) 0.6246(11) 0.078(5) Uiso 0.50 1 d PDU A 1 N60A N 0.9100(12) 1.0007(12) 0.6205(9) 0.078(5) Uiso 0.50 1 d PDU B 2 C60A C 0.9331(11) 0.9993(12) 0.5698(8) 0.040(6) Uiso 0.50 1 d PDU B 2 C60B C 0.941(2) 0.992(2) 0.4963(10) 0.092(15) Uiso 0.50 1 d PDU B 2 N610 N 0.2236(10) 0.2714(10) 0.4879(9) 0.065(7) Uiso 0.50 1 d PDU . . C610 C 0.2065(13) 0.2560(14) 0.5425(12) 0.073(9) Uiso 0.50 1 d PDU . . C611 C 0.1659(12) 0.2127(12) 0.5799(13) 0.066(8) Uiso 0.50 1 d PDU . . N620 N 0.4379(13) -0.0115(14) 0.8901(8) 0.069(9) Uiso 0.50 1 d PDU C 1 C620 C 0.449(3) -0.012(3) 0.8334(10) 0.19(3) Uiso 0.50 1 d PDU C 1 C621 C 0.4438(19) -0.0036(18) 0.7612(9) 0.069(5) Uiso 0.50 1 d PDU C 1 N62A N 0.4458(13) 0.0529(12) 0.7641(8) 0.069(5) Uiso 0.50 1 d PDU D 2 C62A C 0.4501(9) 0.0339(9) 0.8170(7) 0.022(5) Uiso 0.50 1 d PDU D 2 C62B C 0.4591(10) 0.0293(10) 0.8907(7) 0.027(4) Uiso 0.50 1 d PDU D 2 N630 N 0.1660(12) 0.2775(11) 0.8501(10) 0.080(6) Uiso 0.50 1 d PDU E 1 C630 C 0.1724(14) 0.2667(15) 0.7926(11) 0.074(10) Uiso 0.50 1 d PDU E 1 C631 C 0.201(3) 0.245(3) 0.7305(14) 0.161(16) Uiso 0.50 1 d PDU E 1 N63A N 0.2084(14) 0.2410(13) 0.8030(9) 0.079(9) Uiso 0.50 1 d PDU F 2 C63A C 0.2093(15) 0.2437(16) 0.8637(11) 0.080(6) Uiso 0.50 1 d PDU F 2 C63B C 0.1766(14) 0.2766(14) 0.9203(12) 0.074(10) Uiso 0.50 1 d PDU F 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0456(11) 0.0436(11) 0.0544(11) 0.0024(9) -0.0044(9) 0.0032(9) Cu2 0.0421(13) 0.0519(14) 0.0823(16) 0.0026(12) -0.0012(11) 0.0009(10) Cu3 0.0439(13) 0.0404(13) 0.0608(14) -0.0050(10) 0.0020(9) 0.0032(10) Cu4 0.0412(13) 0.0503(14) 0.0633(13) 0.0039(11) -0.0062(10) 0.0009(10) N3 0.058(6) 0.046(6) 0.066(5) 0.002(4) 0.009(5) 0.005(5) N2 0.045(6) 0.027(4) 0.076(6) -0.008(4) 0.009(5) 0.004(4) N1 0.049(6) 0.033(5) 0.044(5) 0.005(4) 0.004(4) -0.003(4) N4 0.042(5) 0.053(6) 0.058(5) -0.003(4) -0.013(4) -0.007(5) N5 0.043(5) 0.044(5) 0.043(5) 0.003(4) 0.013(4) -0.005(4) N6 0.058(7) 0.062(6) 0.088(6) -0.012(5) 0.012(6) -0.013(5) O1 0.076(6) 0.061(6) 0.059(5) -0.020(4) 0.030(5) -0.025(5) O2 0.079(6) 0.066(6) 0.063(5) -0.020(4) 0.021(5) -0.027(5) N9 0.045(6) 0.037(6) 0.077(5) 0.007(5) 0.009(5) 0.002(4) N8 0.039(5) 0.060(6) 0.056(6) 0.003(5) 0.000(4) 0.006(4) N7 0.044(6) 0.050(6) 0.057(5) -0.012(5) -0.002(4) 0.001(5) N10 0.047(6) 0.054(6) 0.063(5) 0.011(5) -0.006(5) 0.004(5) N11 0.035(5) 0.060(6) 0.066(6) -0.013(5) -0.006(4) 0.001(4) N12 0.052(5) 0.050(6) 0.069(5) -0.011(5) -0.007(5) -0.010(5) O3 0.064(6) 0.077(6) 0.062(5) -0.021(5) -0.024(4) 0.035(5) O4 0.065(6) 0.079(6) 0.050(4) -0.012(5) -0.008(4) 0.020(5) N15 0.063(7) 0.062(6) 0.062(5) -0.005(5) -0.004(5) -0.012(5) N14 0.051(6) 0.049(5) 0.046(5) 0.015(4) -0.014(5) -0.009(4) N13 0.042(6) 0.047(6) 0.046(5) -0.004(4) -0.003(4) -0.008(5) N16 0.052(6) 0.051(6) 0.044(5) 0.005(4) -0.012(5) 0.000(5) N17 0.045(6) 0.038(5) 0.043(5) 0.013(4) -0.014(4) -0.006(4) N18 0.056(7) 0.043(5) 0.070(5) 0.001(5) 0.003(5) 0.013(5) O5 0.063(6) 0.075(6) 0.049(4) 0.015(4) -0.014(4) -0.021(5) O6 0.074(6) 0.060(6) 0.048(4) 0.023(4) -0.022(4) -0.030(5) N21 0.038(5) 0.028(5) 0.052(5) 0.008(4) -0.011(4) -0.015(4) N20 0.044(5) 0.046(6) 0.065(6) 0.006(5) 0.001(4) 0.011(5) N19 0.048(6) 0.068(7) 0.053(5) 0.012(5) 0.000(4) 0.004(5) N22 0.043(5) 0.062(6) 0.048(5) -0.006(5) 0.000(4) 0.005(5) N23 0.048(5) 0.035(5) 0.040(5) -0.005(4) -0.006(4) 0.005(4) N24 0.043(5) 0.035(6) 0.060(5) 0.007(5) 0.003(4) 0.007(4) O7 0.068(6) 0.085(7) 0.060(5) 0.025(5) 0.015(5) 0.023(5) O8 0.064(6) 0.075(6) 0.051(5) 0.015(5) 0.012(4) 0.016(5) C12 0.050(6) 0.057(6) 0.076(7) 0.001(5) 0.017(5) 0.010(5) C11 0.050(6) 0.057(6) 0.074(6) 0.018(5) 0.004(5) 0.013(5) C10 0.056(7) 0.045(6) 0.075(6) 0.003(5) -0.012(6) -0.016(5) C9 0.056(7) 0.048(6) 0.073(7) -0.003(5) 0.010(5) -0.004(5) C8 0.050(7) 0.048(6) 0.066(6) -0.005(5) 0.003(5) -0.015(5) C7 0.069(7) 0.058(6) 0.062(6) -0.004(5) 0.015(6) -0.015(5) C5 0.053(7) 0.051(6) 0.046(5) -0.003(5) 0.011(5) 0.001(5) C4 0.057(7) 0.037(5) 0.051(5) -0.005(4) 0.002(5) 0.000(5) C1 0.060(7) 0.044(6) 0.046(5) -0.004(5) 0.009(5) 0.005(5) C2 0.058(7) 0.040(6) 0.055(6) -0.008(5) 0.000(5) 0.007(5) C3 0.037(6) 0.052(6) 0.057(5) 0.004(5) 0.006(5) -0.005(5) C13 0.051(7) 0.052(6) 0.062(5) -0.001(5) 0.004(5) -0.006(5) C15 0.044(6) 0.042(5) 0.048(6) 0.004(4) 0.006(5) 0.012(4) C16 0.051(7) 0.052(6) 0.068(6) 0.010(5) 0.001(6) -0.006(5) C20 0.059(7) 0.059(6) 0.090(7) -0.007(5) -0.003(6) -0.003(6) C19 0.065(7) 0.058(6) 0.096(7) 0.014(5) -0.018(6) -0.003(6) C18 0.095(9) 0.082(7) 0.095(7) 0.041(6) -0.008(7) -0.028(6) C17 0.073(8) 0.072(6) 0.066(6) 0.021(5) -0.012(6) -0.007(6) C32 0.056(7) 0.066(7) 0.074(7) -0.006(6) 0.005(5) -0.001(6) C31 0.061(7) 0.066(8) 0.082(7) -0.003(6) 0.008(6) 0.016(6) C30 0.059(6) 0.062(7) 0.087(7) -0.004(6) -0.017(6) 0.004(5) C29 0.068(7) 0.071(8) 0.092(7) -0.021(6) -0.009(5) 0.009(6) C28 0.052(6) 0.048(7) 0.081(6) -0.003(5) -0.003(5) 0.002(5) C27 0.049(6) 0.068(7) 0.062(7) -0.020(5) -0.016(5) -0.001(5) C25 0.049(6) 0.046(7) 0.065(6) -0.014(6) -0.009(5) 0.000(5) C24 0.039(5) 0.035(6) 0.052(5) -0.004(5) -0.007(4) -0.008(4) C21 0.068(7) 0.068(8) 0.053(6) 0.003(6) 0.002(5) 0.008(6) C22 0.064(7) 0.075(8) 0.063(6) 0.002(6) -0.012(6) 0.003(6) C23 0.032(5) 0.048(7) 0.054(5) -0.010(5) -0.005(4) -0.010(4) C33 0.032(5) 0.048(7) 0.053(5) 0.001(5) -0.003(5) -0.010(5) C35 0.069(6) 0.060(7) 0.058(7) 0.001(5) -0.005(5) 0.012(6) C36 0.060(6) 0.038(7) 0.064(6) -0.001(5) 0.013(5) 0.009(5) C40 0.061(7) 0.072(8) 0.105(7) -0.007(6) -0.011(5) 0.000(6) C39 0.069(7) 0.087(9) 0.109(7) 0.001(7) 0.011(6) -0.002(6) C38 0.087(7) 0.096(9) 0.094(7) 0.015(7) 0.037(6) 0.018(6) C37 0.089(7) 0.088(8) 0.066(6) -0.004(6) 0.026(5) 0.012(6) C52 0.049(7) 0.060(7) 0.082(7) -0.020(5) -0.009(6) 0.006(6) C51 0.035(6) 0.060(6) 0.093(7) -0.018(6) 0.002(6) 0.007(5) C50 0.073(8) 0.067(7) 0.106(7) 0.001(6) -0.003(7) -0.011(6) C49 0.063(8) 0.050(6) 0.092(7) 0.024(5) -0.010(6) -0.018(6) C48 0.040(6) 0.042(5) 0.056(6) 0.016(5) -0.006(5) 0.004(4) C47 0.051(7) 0.042(6) 0.062(6) 0.006(5) 0.000(5) -0.009(5) C45 0.036(6) 0.046(6) 0.051(5) 0.003(5) -0.003(5) -0.001(5) C44 0.043(7) 0.036(5) 0.051(5) 0.004(4) -0.010(5) 0.000(5) C41 0.056(7) 0.060(7) 0.050(6) -0.002(5) -0.018(6) -0.004(5) C42 0.044(6) 0.046(6) 0.032(5) 0.021(5) -0.008(5) 0.004(5) C43 0.034(6) 0.044(6) 0.045(5) 0.011(4) -0.009(5) -0.003(5) C53 0.042(6) 0.041(6) 0.046(5) 0.001(5) -0.010(5) -0.002(5) C55 0.050(6) 0.048(5) 0.048(6) -0.001(4) -0.019(5) 0.014(4) C56 0.046(7) 0.059(6) 0.067(6) -0.015(5) -0.007(6) -0.003(5) C60 0.056(8) 0.066(7) 0.097(7) 0.012(5) -0.010(6) 0.003(6) C59 0.079(8) 0.059(7) 0.102(7) -0.008(6) 0.012(7) 0.000(6) C58 0.089(9) 0.075(7) 0.096(7) -0.038(6) 0.020(7) -0.024(6) C57 0.086(8) 0.068(6) 0.073(7) -0.021(5) 0.007(6) -0.015(6) C72 0.061(7) 0.062(8) 0.085(7) 0.029(6) -0.012(5) -0.004(6) C71 0.074(7) 0.074(8) 0.100(7) 0.007(6) -0.019(6) 0.016(6) C70 0.057(7) 0.064(8) 0.097(7) -0.011(6) 0.001(6) 0.014(6) C69 0.052(6) 0.065(8) 0.078(7) 0.014(6) 0.007(5) 0.004(5) C68 0.039(6) 0.042(6) 0.054(6) 0.006(5) 0.005(5) -0.002(5) C67 0.049(6) 0.059(7) 0.051(6) 0.018(5) 0.009(5) 0.002(5) C65 0.045(6) 0.043(7) 0.057(5) 0.009(5) -0.004(5) 0.003(5) C64 0.038(5) 0.039(6) 0.049(5) 0.003(5) -0.011(4) 0.001(5) C61 0.058(7) 0.055(7) 0.055(6) 0.006(6) 0.006(5) 0.005(6) C62 0.059(7) 0.072(8) 0.056(6) 0.001(6) 0.004(6) 0.013(6) C63 0.039(6) 0.051(7) 0.053(5) 0.012(5) 0.004(4) 0.003(5) C73 0.035(6) 0.044(6) 0.050(5) 0.002(5) -0.004(5) 0.009(5) C75 0.057(6) 0.047(7) 0.053(6) 0.012(5) 0.009(5) 0.017(5) C76 0.042(5) 0.037(6) 0.039(5) 0.000(5) -0.011(4) 0.000(5) C80 0.058(6) 0.065(8) 0.075(6) 0.001(6) 0.015(5) -0.001(6) C79 0.030(5) 0.063(7) 0.074(6) -0.003(6) 0.006(5) 0.007(5) C78 0.051(6) 0.077(8) 0.069(6) 0.005(6) -0.006(5) 0.018(6) C77 0.061(6) 0.073(7) 0.057(6) 0.010(5) 0.001(5) 0.033(6) B1 0.055(7) 0.062(6) 0.065(7) 0.002(6) 0.003(5) -0.020(5) F11 0.117(9) 0.198(11) 0.068(6) 0.019(6) -0.001(5) -0.068(8) F12 0.103(7) 0.114(7) 0.101(7) -0.030(6) 0.009(6) -0.049(6) F13 0.070(6) 0.187(10) 0.077(6) 0.021(7) 0.021(5) -0.024(6) F14 0.124(9) 0.099(6) 0.304(15) -0.071(8) 0.002(9) -0.002(6) B2 0.105(8) 0.090(8) 0.097(7) -0.020(7) 0.008(7) -0.005(7) F21 0.355(12) 0.151(9) 0.259(13) 0.045(12) -0.052(14) 0.091(13) F22 0.201(9) 0.291(14) 0.145(10) -0.109(10) 0.075(8) -0.146(9) F23 0.110(8) 0.096(6) 0.114(8) -0.018(6) -0.040(7) -0.006(6) F24 0.167(11) 0.159(11) 0.094(6) -0.025(7) 0.023(7) -0.090(9) B3 0.098(8) 0.093(8) 0.088(7) -0.009(7) -0.011(7) 0.006(7) F31 0.190(12) 0.160(11) 0.082(6) -0.036(6) -0.051(6) 0.083(9) F32 0.242(10) 0.132(9) 0.331(16) 0.047(12) 0.046(13) -0.065(10) F33 0.178(8) 0.241(12) 0.103(7) -0.091(8) -0.058(7) 0.130(8) F34 0.136(10) 0.086(6) 0.087(7) 0.005(6) 0.022(7) 0.015(6) B4 0.076(8) 0.098(8) 0.091(8) 0.003(6) -0.006(6) 0.030(6) F41 0.101(7) 0.144(8) 0.065(6) -0.007(5) -0.024(5) 0.064(6) F42 0.168(10) 0.324(12) 0.181(10) -0.157(9) -0.098(8) 0.157(9) F43 0.143(10) 0.267(12) 0.334(17) 0.190(11) 0.069(10) 0.058(9) F44 0.070(6) 0.126(9) 0.096(8) -0.025(6) -0.020(5) 0.034(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.902(12) . ? Cu1 N23 2.002(11) . ? Cu1 N3 2.170(9) . ? Cu1 N24 2.193(9) . ? Cu1 N22 2.217(12) . ? Cu1 N1 2.232(8) . ? Cu2 N8 1.948(13) . ? Cu2 N5 1.962(11) . ? Cu2 N9 2.087(8) . ? Cu2 N6 2.128(10) . ? Cu2 N7 2.173(9) . ? Cu2 N4 2.240(9) . ? Cu3 N11 1.949(12) . ? Cu3 N14 1.962(11) . ? Cu3 N13 2.171(9) . ? Cu3 N12 2.185(9) . ? Cu3 N15 2.194(10) . ? Cu3 N10 2.248(9) . ? Cu4 N20 1.900(12) . ? Cu4 N17 1.906(10) . ? Cu4 N18 2.082(10) . ? Cu4 N21 2.094(8) . ? Cu4 N16 2.210(10) . ? Cu4 N19 2.228(9) . ? N3 C8 1.291(12) . ? N3 C12 1.339(12) . ? N2 C5 1.307(13) . ? N2 C7 1.456(14) . ? N1 C1 1.308(12) . ? N1 C4 1.311(12) . ? N4 C2 1.310(13) . ? N4 C3 1.367(13) . ? N5 C13 1.292(13) . ? N5 C15 1.477(13) . ? N6 C16 1.326(13) . ? N6 C20 1.373(13) . ? O1 C5 1.246(12) . ? O2 C13 1.258(13) . ? N9 C28 1.307(13) . ? N9 C32 1.332(13) . ? N8 C25 1.303(13) . ? N8 C27 1.461(13) . ? N7 C21 1.311(13) . ? N7 C24 1.336(13) . ? N10 C22 1.352(14) . ? N10 C23 1.364(13) . ? N11 C33 1.294(13) . ? N11 C35 1.491(14) . ? N12 C36 1.315(13) . ? N12 C40 1.330(13) . ? O3 C25 1.258(13) . ? O4 C33 1.312(12) . ? N15 C48 1.287(12) . ? N15 C52 1.326(13) . ? N14 C45 1.303(13) . ? N14 C47 1.472(13) . ? N13 C41 1.290(13) . ? N13 C44 1.357(12) . ? N16 C42 1.299(12) . ? N16 C43 1.331(12) . ? N17 C53 1.311(13) . ? N17 C55 1.505(13) . ? N18 C60 1.347(13) . ? N18 C56 1.353(13) . ? O5 C45 1.243(12) . ? O6 C53 1.275(12) . ? N21 C68 1.296(12) . ? N21 C72 1.356(12) . ? N20 C65 1.341(13) . ? N20 C67 1.459(14) . ? N19 C61 1.324(13) . ? N19 C64 1.367(13) . ? N22 C62 1.318(14) . ? N22 C63 1.346(13) . ? N23 C73 1.317(12) . ? N23 C75 1.460(13) . ? N24 C76 1.307(12) . ? N24 C80 1.374(13) . ? O7 C65 1.309(13) . ? O8 C73 1.275(13) . ? C12 C11 1.333(14) . ? C11 C10 1.361(14) . ? C10 C9 1.421(13) . ? C9 C8 1.389(13) . ? C8 C7 1.516(14) . ? C5 C4 1.503(13) . ? C4 C3 1.424(12) . ? C1 C2 1.341(12) . ? C3 C13 1.506(14) . ? C15 C16 1.546(13) . ? C16 C17 1.352(14) . ? C20 C19 1.372(14) . ? C19 C18 1.314(15) . ? C18 C17 1.419(14) . ? C32 C31 1.360(15) . ? C31 C30 1.369(15) . ? C30 C29 1.392(14) . ? C29 C28 1.357(14) . ? C28 C27 1.507(14) . ? C25 C24 1.492(13) . ? C24 C23 1.407(12) . ? C21 C22 1.396(14) . ? C23 C33 1.505(14) . ? C35 C36 1.515(14) . ? C36 C37 1.364(14) . ? C40 C39 1.401(16) . ? C39 C38 1.332(16) . ? C38 C37 1.423(16) . ? C52 C51 1.364(15) . ? C51 C50 1.354(15) . ? C50 C49 1.409(15) . ? C49 C48 1.403(14) . ? C48 C47 1.515(14) . ? C45 C44 1.521(13) . ? C44 C43 1.411(12) . ? C41 C42 1.414(13) . ? C43 C53 1.526(13) . ? C55 C56 1.531(14) . ? C56 C57 1.378(14) . ? C60 C59 1.339(15) . ? C59 C58 1.336(15) . ? C58 C57 1.419(15) . ? C72 C71 1.397(15) . ? C71 C70 1.362(15) . ? C70 C69 1.389(14) . ? C69 C68 1.357(14) . ? C68 C67 1.487(14) . ? C65 C64 1.482(14) . ? C64 C63 1.424(12) . ? C61 C62 1.392(14) . ? C63 C73 1.515(13) . ? C75 C76 1.497(13) . ? C76 C77 1.359(13) . ? C80 C79 1.355(14) . ? C79 C78 1.378(14) . ? C78 C77 1.395(14) . ? B1 F11 1.299(13) . ? B1 F13 1.315(13) . ? B1 F12 1.345(13) . ? B1 F14 1.385(13) . ? B2 F22 1.298(15) . ? B2 F24 1.303(14) . ? B2 F23 1.365(14) . ? B2 F21 1.365(16) . ? B3 F33 1.307(15) . ? B3 F31 1.314(14) . ? B3 F32 1.336(15) . ? B3 F34 1.385(15) . ? B4 F42 1.308(15) . ? B4 F43 1.320(15) . ? B4 F41 1.337(14) . ? B4 F44 1.349(14) . ? N600 C600 1.174(17) . ? C600 C601 1.453(17) . ? N60A C60A 1.128(15) . ? C60A C60B 1.482(16) . ? N610 C610 1.195(17) . ? C610 C611 1.478(17) . ? N620 C620 1.154(18) . ? C620 C621 1.453(17) . ? N62A C62A 1.133(15) . ? C62A C62B 1.484(14) . ? N630 C630 1.178(16) . ? C630 C631 1.459(17) . ? N63A C63A 1.210(17) . ? C63A C63B 1.506(18) . ? 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 N2 Cu1 N23 172.6(4) . . ? N2 Cu1 N3 79.1(4) . . ? N23 Cu1 N3 104.9(3) . . ? N2 Cu1 N24 108.4(4) . . ? N23 Cu1 N24 77.2(3) . . ? N3 Cu1 N24 100.5(3) . . ? N2 Cu1 N22 96.7(4) . . ? N23 Cu1 N22 77.0(4) . . ? N3 Cu1 N22 93.2(3) . . ? N24 Cu1 N22 153.2(4) . . ? N2 Cu1 N1 76.7(4) . . ? N23 Cu1 N1 98.9(3) . . ? N3 Cu1 N1 155.7(3) . . ? N24 Cu1 N1 89.1(3) . . ? N22 Cu1 N1 87.6(4) . . ? N8 Cu2 N5 170.4(5) . . ? N8 Cu2 N9 81.2(4) . . ? N5 Cu2 N9 99.5(4) . . ? N8 Cu2 N6 107.9(5) . . ? N5 Cu2 N6 81.5(4) . . ? N9 Cu2 N6 99.3(3) . . ? N8 Cu2 N7 75.7(4) . . ? N5 Cu2 N7 103.0(4) . . ? N9 Cu2 N7 156.8(4) . . ? N6 Cu2 N7 89.8(3) . . ? N8 Cu2 N4 95.9(5) . . ? N5 Cu2 N4 74.5(4) . . ? N9 Cu2 N4 90.6(3) . . ? N6 Cu2 N4 155.3(4) . . ? N7 Cu2 N4 89.8(3) . . ? N11 Cu3 N14 170.1(5) . . ? N11 Cu3 N13 96.6(5) . . ? N14 Cu3 N13 76.5(4) . . ? N11 Cu3 N12 78.0(4) . . ? N14 Cu3 N12 108.6(5) . . ? N13 Cu3 N12 88.0(3) . . ? N11 Cu3 N15 106.8(4) . . ? N14 Cu3 N15 79.6(4) . . ? N13 Cu3 N15 156.0(4) . . ? N12 Cu3 N15 101.8(3) . . ? N11 Cu3 N10 75.7(4) . . ? N14 Cu3 N10 96.5(5) . . ? N13 Cu3 N10 87.0(3) . . ? N12 Cu3 N10 152.5(4) . . ? N15 Cu3 N10 93.5(3) . . ? N20 Cu4 N17 173.9(5) . . ? N20 Cu4 N18 104.4(5) . . ? N17 Cu4 N18 81.6(4) . . ? N20 Cu4 N21 79.6(4) . . ? N17 Cu4 N21 100.9(4) . . ? N18 Cu4 N21 98.8(3) . . ? N20 Cu4 N16 98.0(5) . . ? N17 Cu4 N16 75.9(4) . . ? N18 Cu4 N16 157.0(4) . . ? N21 Cu4 N16 90.4(3) . . ? N20 Cu4 N19 76.8(4) . . ? N17 Cu4 N19 102.3(5) . . ? N18 Cu4 N19 88.9(3) . . ? N21 Cu4 N19 156.4(4) . . ? N16 Cu4 N19 90.9(3) . . ? C8 N3 C12 126.6(11) . . ? C8 N3 Cu1 112.3(7) . . ? C12 N3 Cu1 120.8(8) . . ? C5 N2 C7 114.0(11) . . ? C5 N2 Cu1 123.7(9) . . ? C7 N2 Cu1 120.7(8) . . ? C1 N1 C4 122.6(9) . . ? C1 N1 Cu1 126.8(7) . . ? C4 N1 Cu1 110.6(7) . . ? C2 N4 C3 117.4(10) . . ? C2 N4 Cu2 128.7(8) . . ? C3 N4 Cu2 113.9(7) . . ? C13 N5 C15 119.3(11) . . ? C13 N5 Cu2 124.8(9) . . ? C15 N5 Cu2 113.9(7) . . ? C16 N6 C20 115.6(11) . . ? C16 N6 Cu2 116.7(7) . . ? C20 N6 Cu2 127.8(9) . . ? C28 N9 C32 110.9(11) . . ? C28 N9 Cu2 114.1(7) . . ? C32 N9 Cu2 134.9(10) . . ? C25 N8 C27 119.7(12) . . ? C25 N8 Cu2 123.3(9) . . ? C27 N8 Cu2 116.7(9) . . ? C21 N7 C24 120.4(9) . . ? C21 N7 Cu2 125.5(8) . . ? C24 N7 Cu2 114.2(7) . . ? C22 N10 C23 122.8(10) . . ? C22 N10 Cu3 124.8(8) . . ? C23 N10 Cu3 112.4(7) . . ? C33 N11 C35 114.5(11) . . ? C33 N11 Cu3 123.5(9) . . ? C35 N11 Cu3 120.3(9) . . ? C36 N12 C40 124.0(11) . . ? C36 N12 Cu3 112.1(6) . . ? C40 N12 Cu3 123.7(10) . . ? C48 N15 C52 129.4(12) . . ? C48 N15 Cu3 113.2(7) . . ? C52 N15 Cu3 117.1(9) . . ? C45 N14 C47 118.6(11) . . ? C45 N14 Cu3 122.9(9) . . ? C47 N14 Cu3 117.8(8) . . ? C41 N13 C44 119.3(9) . . ? C41 N13 Cu3 126.8(8) . . ? C44 N13 Cu3 113.8(7) . . ? C42 N16 C43 118.8(10) . . ? C42 N16 Cu4 128.1(8) . . ? C43 N16 Cu4 113.0(7) . . ? C53 N17 C55 113.4(10) . . ? C53 N17 Cu4 124.5(8) . . ? C55 N17 Cu4 118.8(8) . . ? C60 N18 C56 115.2(11) . . ? C60 N18 Cu4 130.2(10) . . ? C56 N18 Cu4 114.6(7) . . ? C68 N21 C72 115.4(11) . . ? C68 N21 Cu4 114.5(7) . . ? C72 N21 Cu4 130.0(9) . . ? C65 N20 C67 117.5(11) . . ? C65 N20 Cu4 122.1(9) . . ? C67 N20 Cu4 119.6(9) . . ? C61 N19 C64 121.3(10) . . ? C61 N19 Cu4 126.5(8) . . ? C64 N19 Cu4 112.1(7) . . ? C62 N22 C63 122.1(12) . . ? C62 N22 Cu1 125.1(9) . . ? C63 N22 Cu1 112.7(8) . . ? C73 N23 C75 118.9(10) . . ? C73 N23 Cu1 120.5(8) . . ? C75 N23 Cu1 120.3(7) . . ? C76 N24 C80 120.3(10) . . ? C76 N24 Cu1 112.3(6) . . ? C80 N24 Cu1 127.3(9) . . ? C11 C12 N3 119.3(13) . . ? C12 C11 C10 118.1(13) . . ? C11 C10 C9 121.6(12) . . ? C8 C9 C10 117.0(12) . . ? N3 C8 C9 117.4(11) . . ? N3 C8 C7 118.1(10) . . ? C9 C8 C7 124.2(11) . . ? N2 C7 C8 107.7(11) . . ? O1 C5 N2 125.3(12) . . ? O1 C5 C4 121.7(11) . . ? N2 C5 C4 112.9(10) . . ? N1 C4 C3 118.5(10) . . ? N1 C4 C5 115.6(9) . . ? C3 C4 C5 125.9(10) . . ? N1 C1 C2 118.4(11) . . ? N4 C2 C1 124.4(12) . . ? N4 C3 C4 118.7(10) . . ? N4 C3 C13 111.6(9) . . ? C4 C3 C13 129.8(10) . . ? O2 C13 N5 121.9(12) . . ? O2 C13 C3 123.1(11) . . ? N5 C13 C3 114.9(10) . . ? N5 C15 C16 115.0(10) . . ? N6 C16 C17 121.4(11) . . ? N6 C16 C15 111.2(9) . . ? C17 C16 C15 126.4(11) . . ? C19 C20 N6 127.5(15) . . ? C18 C19 C20 114.1(15) . . ? C19 C18 C17 122.0(15) . . ? C16 C17 C18 119.5(14) . . ? N9 C32 C31 128.7(14) . . ? C32 C31 C30 119.8(14) . . ? C31 C30 C29 112.2(14) . . ? C28 C29 C30 123.1(14) . . ? N9 C28 C29 125.4(12) . . ? N9 C28 C27 117.5(11) . . ? C29 C28 C27 117.0(12) . . ? N8 C27 C28 110.3(11) . . ? O3 C25 N8 125.2(12) . . ? O3 C25 C24 120.9(11) . . ? N8 C25 C24 113.5(10) . . ? N7 C24 C23 119.5(10) . . ? N7 C24 C25 113.0(8) . . ? C23 C24 C25 127.4(11) . . ? N7 C21 C22 123.8(13) . . ? N10 C22 C21 115.4(13) . . ? N10 C23 C24 118.1(10) . . ? N10 C23 C33 112.3(9) . . ? C24 C23 C33 129.6(10) . . ? N11 C33 O4 126.3(12) . . ? N11 C33 C23 115.7(11) . . ? O4 C33 C23 116.8(11) . . ? N11 C35 C36 105.3(10) . . ? N12 C36 C37 125.3(12) . . ? N12 C36 C35 120.5(10) . . ? C37 C36 C35 114.1(12) . . ? N12 C40 C39 112.2(15) . . ? C38 C39 C40 126.4(17) . . ? C39 C38 C37 118.6(16) . . ? C36 C37 C38 113.4(14) . . ? N15 C52 C51 115.5(14) . . ? C50 C51 C52 119.3(15) . . ? C51 C50 C49 123.2(15) . . ? C48 C49 C50 114.7(14) . . ? N15 C48 C49 117.9(11) . . ? N15 C48 C47 118.3(10) . . ? C49 C48 C47 123.8(11) . . ? N14 C47 C48 111.1(11) . . ? O5 C45 N14 122.2(12) . . ? O5 C45 C44 124.5(11) . . ? N14 C45 C44 113.2(10) . . ? N13 C44 C43 119.8(10) . . ? N13 C44 C45 112.9(8) . . ? C43 C44 C45 127.1(10) . . ? N13 C41 C42 120.0(11) . . ? N16 C42 C41 122.2(11) . . ? N16 C43 C44 119.9(10) . . ? N16 C43 C53 113.0(9) . . ? C44 C43 C53 127.0(10) . . ? O6 C53 N17 124.2(11) . . ? O6 C53 C43 123.5(11) . . ? N17 C53 C43 112.1(10) . . ? N17 C55 C56 108.1(10) . . ? N18 C56 C57 120.3(12) . . ? N18 C56 C55 116.0(9) . . ? C57 C56 C55 123.4(12) . . ? C59 C60 N18 131.0(16) . . ? C58 C59 C60 111.9(16) . . ? C59 C58 C57 123.6(15) . . ? C56 C57 C58 118.1(14) . . ? N21 C72 C71 122.2(15) . . ? C70 C71 C72 120.6(15) . . ? C71 C70 C69 116.0(15) . . ? C68 C69 C70 119.5(14) . . ? N21 C68 C69 126.2(12) . . ? N21 C68 C67 117.4(10) . . ? C69 C68 C67 116.3(11) . . ? N20 C67 C68 108.7(11) . . ? O7 C65 N20 125.6(13) . . ? O7 C65 C64 118.5(11) . . ? N20 C65 C64 115.6(10) . . ? N19 C64 C63 119.1(10) . . ? N19 C64 C65 112.1(8) . . ? C63 C64 C65 128.8(11) . . ? N19 C61 C62 119.0(13) . . ? N22 C62 C61 121.0(14) . . ? N22 C63 C64 117.6(11) . . ? N22 C63 C73 114.2(10) . . ? C64 C63 C73 128.2(10) . . ? O8 C73 N23 122.8(12) . . ? O8 C73 C63 121.8(11) . . ? N23 C73 C63 115.4(10) . . ? N23 C75 C76 106.9(10) . . ? N24 C76 C77 121.5(10) . . ? N24 C76 C75 121.4(9) . . ? C77 C76 C75 117.1(11) . . ? C79 C80 N24 119.9(13) . . ? C80 C79 C78 121.0(13) . . ? C79 C78 C77 117.0(13) . . ? C76 C77 C78 120.4(13) . . ? F11 B1 F13 115.1(11) . . ? F11 B1 F12 113.5(11) . . ? F13 B1 F12 112.8(11) . . ? F11 B1 F14 100.8(11) . . ? F13 B1 F14 105.8(11) . . ? F12 B1 F14 107.5(11) . . ? F22 B2 F24 113.5(13) . . ? F22 B2 F23 114.1(13) . . ? F24 B2 F23 110.5(13) . . ? F22 B2 F21 102.3(13) . . ? F24 B2 F21 112.0(14) . . ? F23 B2 F21 103.7(12) . . ? F33 B3 F31 113.0(13) . . ? F33 B3 F32 106.5(13) . . ? F31 B3 F32 112.8(14) . . ? F33 B3 F34 109.9(13) . . ? F31 B3 F34 109.9(12) . . ? F32 B3 F34 104.3(12) . . ? F42 B4 F43 107.5(14) . . ? F42 B4 F41 110.5(12) . . ? F43 B4 F41 109.3(13) . . ? F42 B4 F44 109.1(12) . . ? F43 B4 F44 108.5(13) . . ? F41 B4 F44 111.8(12) . . ? N600 C600 C601 158(5) . . ? N60A C60A C60B 160(3) . . ? N610 C610 C611 145(3) . . ? N620 C620 C621 162(6) . . ? N62A C62A C62B 163(2) . . ? N630 C630 C631 160(4) . . ? N63A C63A C63B 140(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.487 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.068 data_cul3b _database_code_depnum_ccdc_archive 'CCDC 212609' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H70.5 B4 Cu4 F16 N27.5 O8' _chemical_formula_weight 2134.53 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.189(3) _cell_length_b 15.191(3) _cell_length_c 20.048(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.41(3) _cell_angle_gamma 90.00 _cell_volume 4625.8(16) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 18861 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 25.52 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2140 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8183 _exptl_absorpt_correction_T_max 0.9076 _exptl_absorpt_process_details 'X-RED 1.22 (Stoe & Cie GmbH, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24008 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 24.71 _reflns_number_total 15222 _reflns_number_gt 12059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.05 (Stoe & Cie GmbH, 2000)' _computing_cell_refinement 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_data_reduction 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_structure_solution 'XS: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'XL: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'XP: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'XCIF: SHELXTL 5.1 (Bruker AXS Inc., 1997)' _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. Because of the near tetragonality of the unit cell, a variety of monoclinic twin laws were tested both with and without inversion twinning (in matrix form, row by row): (0 0 1, 0 -1 0, 1 0 0); (0 1 0, 1 0 0, 0 0 -1). All led to R1 (F > 4 sig(F)) greater than 0.15. The adopted twin law (0 1 0, -1 0 0 , 0 0 -1), which led to satisfactory elaboration of the initial structure and to stable least-squares refinements, leads to four non-inversion-related twin domains with fractional sizes: 0.229 (2), 0.066 (2), 0.216 (2) and 0.489. Reflections of the class 00l,l=2n+1 are systematically very weak, indicating the possibility of a second screw axis (and at least intrinsic orthorhombic symmetry) or an a glide plane (noting that twinning would overlap reflections h0l and 0kl). Refinements in the monoclinic space group Pa were less successful than in P2(1). Space group P2(1)/a would impose a centre of symmetry on the cation, leading to a disordered cation, which was not observed (see below). Intensity statistics (E^2^-1 = 0.648) are consistent with an acentric twinned data (and with the consequences that incorrectly assigned features of Fourier maps tended to refine quite well, and missing atoms of disordered BF4- groups were not strongly differentiated from noise). Moreover, as the molecular species has 4mm symmetry and refinement in space group P2(1) revealed no signs of disorder, centrosymmetric monoclinic space groups, which would impose inversion symmetry, can be eliminated. Merging of data into orthorhombic or tetragonal crystal classes led to R(int) > 0.15, whereas monoclinic merging led to R(int) = 0.058. Thus, orthorhombic crystal classes can be eliminated also. Merging of data in triclinic symmetry was no better (or worse) than for monoclinic. That more than 300 reflections are flagged as inconsistent equivalents and that R(int) is significantly greater than R(sigma) is indicative of the difficulties of processing variably and partially overlapped data, consequent upon a monoclinic beta angle of 90.409 deg. Accordingly, in final cycles of refinement 22 reflections with very poor agreement between Fobs and Fcalc were eliminated. Although the extinction parameter is significantly different from zero (0.047 (2)), this is attributed to incomplete recording of reflection data, rather than to extinction itself. Data in shells with resolution better than 0.85 A were not included, as their mean I/sig(I) were less than 2. Because of the near- tetragonal data symmetry and near-4mm symmetry of the complex, considerable correlation exists among formally chemically equivalent bond distances and angles, leading to patterns of unnaturally long and short interatomic distances. Therefore, bond distances that are formally chemically equivalent were refined by means of free variables. In addition tight planarity restraints were applied to appropriate rings and tight restraints to nearly spherical ellipsoids were applied to the atomic displacement parameters of B, C, N, O and F atoms. Three of the BF4- groups are substantially disordered. Residual electron density was concentrated in the vicinity of the copper atoms. The "amide" hydrogen atoms shared between pairs of oxygen atoms O1 and O2, O3 and O4, O5 and O6, and O7 and O8 were not observed in this structure (although in other structures they are observable, just, and are symmetrically located). As the electron density is shared between two strongly electronegative atoms, And the hydrogen atom is formally a proton, the amount of electron density to be expected on the hydrogen atom is very small, and will only be observable in extremely well-behaved structures. Therefore, these hydrogen atoms have been inserted symmetrically between pairs of oxygen atoms to make chemical sense. Refinements converged satisfactorily; the highest final shift/sigma ratios are observed only for the disordered BF4- species. Hydrogen atoms on the acetonitrile moieties were included in order to conform to chemical sense, but their assigned positions lead to three poor intermolecular contacts, two with the cation and one with the disordered BF4- groups ; _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^)+(0.1176P)^2^+10.6145P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0528(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 15222 _refine_ls_number_parameters 1290 _refine_ls_number_restraints 1487 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.2204 _refine_ls_wR_factor_gt 0.1952 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.004 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 0.47956(15) 0.28133(13) 0.22674(9) 0.0527(5) Uani 1 1 d D . . Cu2 Cu 0.56134(18) 0.74307(15) 0.26836(9) 0.0626(6) Uani 1 1 d D . . Cu3 Cu 1.02513(16) 0.65792(14) 0.24701(10) 0.0565(5) Uani 1 1 d D . . Cu4 Cu 0.93863(16) 0.20034(14) 0.25946(11) 0.0627(6) Uani 1 1 d D . . O1 O 0.4477(9) 0.4203(7) 0.4007(5) 0.070(3) Uani 1 1 d DU . . H12 H 0.4675 0.4968 0.4082 0.070 Uiso 1 1 d . . . O2 O 0.4857(10) 0.5747(7) 0.4156(5) 0.067(3) Uani 1 1 d DU . . O3 O 0.7086(8) 0.7714(8) 0.1017(5) 0.060(3) Uani 1 1 d DU . . H34 H 0.7836 0.7521 0.0972 0.070 Uiso 1 1 d . . . O4 O 0.8607(8) 0.7347(9) 0.0930(5) 0.065(3) Uani 1 1 d DU . . O5 O 1.0373(10) 0.5071(8) 0.4156(5) 0.074(4) Uani 1 1 d DU . . H56 H 1.0207 0.4295 0.4172 0.080 Uiso 1 1 d . . . O6 O 1.0034(10) 0.3546(7) 0.4206(5) 0.065(3) Uani 1 1 d DU . . O7 O 0.7953(9) 0.1883(9) 0.0861(5) 0.070(3) Uani 1 1 d DU . . H78 H 0.7189 0.2049 0.0800 0.070 Uiso 1 1 d . . . O8 O 0.6450(8) 0.2220(9) 0.0726(4) 0.063(3) Uani 1 1 d DU . . N1 N 0.5046(4) 0.4252(6) 0.2275(5) 0.060(3) Uani 1 1 d DU . . N2 N 0.4490(9) 0.3208(6) 0.3142(5) 0.050(3) Uani 1 1 d DU . . N3 N 0.4448(3) 0.1569(6) 0.2694(5) 0.055(3) Uani 1 1 d DU . . N4 N 0.5413(4) 0.6009(6) 0.2440(4) 0.049(3) Uani 1 1 d DU . . N5 N 0.5266(9) 0.6911(7) 0.3530(5) 0.053(3) Uani 1 1 d DU . . N6 N 0.5822(3) 0.8516(6) 0.3331(5) 0.070(4) Uani 1 1 d DU . . N7 N 0.7037(7) 0.7179(4) 0.2740(5) 0.057(3) Uani 1 1 d DU . . N8 N 0.6018(8) 0.7753(8) 0.1807(5) 0.055(3) Uani 1 1 d DU . . N9 N 0.4401(7) 0.7758(4) 0.2223(5) 0.061(3) Uani 1 1 d DU . . N10 N 0.8813(7) 0.6826(4) 0.2655(5) 0.056(3) Uani 1 1 d DU . . N11 N 0.9787(8) 0.6961(9) 0.1608(5) 0.063(3) Uani 1 1 d DU . . N12 N 1.1348(6) 0.6363(4) 0.1830(6) 0.076(4) Uani 1 1 d DU . . N13 N 0.9962(4) 0.5184(7) 0.2409(5) 0.055(3) Uani 1 1 d DU . . N14 N 1.0530(9) 0.6173(7) 0.3353(5) 0.055(3) Uani 1 1 d DU . . N15 N 1.0611(3) 0.7812(7) 0.2916(5) 0.062(3) Uani 1 1 d DU . . N16 N 0.9636(4) 0.3434(6) 0.2450(5) 0.061(4) Uani 1 1 d DU . . N17 N 0.9712(10) 0.2445(7) 0.3474(5) 0.061(4) Uani 1 1 d DU . . N18 N 0.9137(3) 0.0835(6) 0.3165(6) 0.061(3) Uani 1 1 d DU . . N19 N 0.7960(7) 0.2305(3) 0.2597(5) 0.052(3) Uani 1 1 d DU . . N20 N 0.9026(9) 0.1753(10) 0.1692(6) 0.072(4) Uani 1 1 d DU . . N21 N 1.0596(7) 0.1654(3) 0.2185(5) 0.062(3) Uani 1 1 d DU . . N22 N 0.6201(8) 0.2560(7) 0.2469(5) 0.057(3) Uani 1 1 d DU . . N23 N 0.5267(7) 0.2468(4) 0.1390(4) 0.050(3) Uani 1 1 d DU . . N24 N 0.3685(7) 0.3028(4) 0.1660(5) 0.064(3) Uani 1 1 d DU . . C1 C 0.5326(3) 0.4744(8) 0.1773(7) 0.063(4) Uani 1 1 d DU . . H1A H 0.5401 0.4480 0.1348 0.075 Uiso 1 1 calc R . . C2 C 0.5516(5) 0.5642(8) 0.1848(6) 0.058(4) Uani 1 1 d DU . . H2A H 0.5716 0.5980 0.1480 0.070 Uiso 1 1 calc R . . C3 C 0.5133(5) 0.5548(7) 0.2966(5) 0.051(4) Uani 1 1 d DU . . C4 C 0.4948(5) 0.4645(7) 0.2872(6) 0.052(3) Uani 1 1 d DU . . C5 C 0.4649(11) 0.3993(7) 0.3397(6) 0.051(3) Uani 1 1 d DU . . C7 C 0.4204(14) 0.2562(7) 0.3648(7) 0.065(4) Uani 1 1 d DU . . H7A H 0.3619 0.2726 0.3824 0.078 Uiso 1 1 calc R . . H7B H 0.4630 0.2547 0.4024 0.078 Uiso 1 1 calc R . . C8 C 0.4160(4) 0.1678(6) 0.3315(6) 0.054(4) Uani 1 1 d DU . . C9 C 0.3824(6) 0.0939(6) 0.3650(7) 0.057(4) Uani 1 1 d DU . . H9A H 0.3614 0.0997 0.4093 0.068 Uiso 1 1 calc R . . C10 C 0.3797(7) 0.0109(7) 0.3328(7) 0.058(3) Uani 1 1 d DU . . H10A H 0.3567 -0.0388 0.3557 0.069 Uiso 1 1 calc R . . C11 C 0.4103(8) 0.0017(9) 0.2684(8) 0.070(4) Uani 1 1 d DU . . H11A H 0.4097 -0.0529 0.2454 0.084 Uiso 1 1 calc R . . C12 C 0.4422(7) 0.0792(7) 0.2398(7) 0.055(3) Uani 1 1 d DU . . H12A H 0.4638 0.0757 0.1956 0.066 Uiso 1 1 calc R . . C13 C 0.5054(13) 0.6079(8) 0.3590(5) 0.061(4) Uani 1 1 d DU . . C15 C 0.5254(14) 0.7469(8) 0.4126(5) 0.060(4) Uani 1 1 d DU . . H15A H 0.5661 0.7226 0.4468 0.072 Uiso 1 1 calc R . . H15B H 0.4654 0.7478 0.4316 0.072 Uiso 1 1 calc R . . C16 C 0.5526(5) 0.8377(7) 0.3948(6) 0.057(4) Uani 1 1 d DU . . C17 C 0.5558(7) 0.9028(8) 0.4449(7) 0.080(5) Uani 1 1 d DU . . H17A H 0.5342 0.8905 0.4882 0.096 Uiso 1 1 calc R . . C18 C 0.5911(8) 0.9860(10) 0.4301(9) 0.086(5) Uani 1 1 d DU . . H18A H 0.5935 1.0308 0.4631 0.103 Uiso 1 1 calc R . . C19 C 0.6224(9) 1.0014(10) 0.3659(8) 0.082(5) Uani 1 1 d DU . . H19A H 0.6469 1.0569 0.3545 0.098 Uiso 1 1 calc R . . C20 C 0.6170(7) 0.9325(7) 0.3178(9) 0.075(5) Uani 1 1 d DU . . H20A H 0.6380 0.9428 0.2739 0.090 Uiso 1 1 calc R . . C21 C 0.7492(9) 0.6885(4) 0.3269(6) 0.060(4) Uani 1 1 d DU . . H21A H 0.7194 0.6798 0.3678 0.072 Uiso 1 1 calc R . . C22 C 0.8382(10) 0.6704(5) 0.3237(6) 0.067(4) Uani 1 1 d DU . . H22A H 0.8689 0.6497 0.3621 0.081 Uiso 1 1 calc R . . C23 C 0.8365(8) 0.7118(5) 0.2127(5) 0.056(3) Uani 1 1 d DU . . C24 C 0.7457(8) 0.7301(5) 0.2161(5) 0.048(3) Uani 1 1 d DU . . C25 C 0.6844(9) 0.7660(8) 0.1628(6) 0.049(3) Uani 1 1 d DU . . C27 C 0.5378(9) 0.8052(12) 0.1318(8) 0.067(4) Uani 1 1 d DU . . H27A H 0.5382 0.7645 0.0932 0.080 Uiso 1 1 calc R . . H27B H 0.5552 0.8642 0.1156 0.080 Uiso 1 1 calc R . . C28 C 0.4443(9) 0.8100(5) 0.1599(6) 0.058(3) Uani 1 1 d DU . . C29 C 0.3737(10) 0.8418(6) 0.1242(9) 0.077(4) Uani 1 1 d DU . . H29A H 0.3813 0.8648 0.0805 0.093 Uiso 1 1 calc R . . C30 C 0.2900(13) 0.8396(11) 0.1535(9) 0.095(5) Uani 1 1 d DU . . H30A H 0.2375 0.8570 0.1311 0.114 Uiso 1 1 calc R . . C31 C 0.2923(13) 0.8093(11) 0.2186(9) 0.081(4) Uani 1 1 d DU . . H31A H 0.2396 0.8142 0.2436 0.097 Uiso 1 1 calc R . . C32 C 0.3644(11) 0.7725(9) 0.2507(9) 0.085(5) Uani 1 1 d DU . . H32A H 0.3582 0.7453 0.2930 0.102 Uiso 1 1 calc R . . C33 C 0.8954(9) 0.7147(11) 0.1520(6) 0.062(3) Uani 1 1 d DU . . C35 C 1.0307(10) 0.6989(10) 0.1005(7) 0.063(3) Uani 1 1 d DU . . H35A H 1.0327 0.7595 0.0825 0.075 Uiso 1 1 calc R . . H35B H 1.0053 0.6595 0.0661 0.075 Uiso 1 1 calc R . . C36 C 1.1219(9) 0.6684(5) 0.1204(6) 0.068(4) Uani 1 1 d DU . . C37 C 1.1838(10) 0.6661(7) 0.0698(8) 0.083(4) Uani 1 1 d DU . . H37A H 1.1725 0.6893 0.0265 0.099 Uiso 1 1 calc R . . C38 C 1.2658(13) 0.6263(8) 0.0878(9) 0.094(5) Uani 1 1 d DU . . H38A H 1.3110 0.6227 0.0554 0.113 Uiso 1 1 calc R . . C39 C 1.2813(13) 0.5928(9) 0.1513(8) 0.090(5) Uani 1 1 d DU . . H39A H 1.3363 0.5666 0.1622 0.108 Uiso 1 1 calc R . . C40 C 1.2139(10) 0.5984(7) 0.1994(9) 0.079(4) Uani 1 1 d DU . . H40A H 1.2234 0.5759 0.2431 0.095 Uiso 1 1 calc R . . C41 C 0.9749(3) 0.4767(8) 0.1856(6) 0.066(4) Uani 1 1 d DU . . H41A H 0.9710 0.5075 0.1444 0.079 Uiso 1 1 calc R . . C42 C 0.9581(4) 0.3854(8) 0.1882(7) 0.060(4) Uani 1 1 d DU . . H42A H 0.9427 0.3545 0.1486 0.072 Uiso 1 1 calc R . . C43 C 0.9854(5) 0.3864(7) 0.3017(6) 0.054(4) Uani 1 1 d DU . . C44 C 1.0023(5) 0.4760(6) 0.3005(5) 0.041(3) Uani 1 1 d DU . . C45 C 1.0298(13) 0.5392(8) 0.3547(6) 0.057(4) Uani 1 1 d DU . . C47 C 1.0862(12) 0.6799(7) 0.3862(7) 0.057(4) Uani 1 1 d DU . . H47A H 1.1471 0.6644 0.3995 0.068 Uiso 1 1 calc R . . H47B H 1.0487 0.6779 0.4264 0.068 Uiso 1 1 calc R . . C48 C 1.0838(4) 0.7692(7) 0.3562(6) 0.053(3) Uani 1 1 d DU . . C49 C 1.1136(6) 0.8414(8) 0.3925(9) 0.072(4) Uani 1 1 d DU . . H49A H 1.1298 0.8341 0.4380 0.087 Uiso 1 1 calc R . . C50 C 1.1201(8) 0.9254(10) 0.3628(8) 0.083(5) Uani 1 1 d DU . . H50A H 1.1404 0.9745 0.3879 0.100 Uiso 1 1 calc R . . C51 C 1.0965(8) 0.9347(11) 0.2973(8) 0.086(5) Uani 1 1 d DU . . H51A H 1.1003 0.9903 0.2758 0.104 Uiso 1 1 calc R . . C52 C 1.0663(7) 0.8592(8) 0.2619(8) 0.061(4) Uani 1 1 d DU . . H52A H 1.0495 0.8646 0.2163 0.074 Uiso 1 1 calc R . . C53 C 0.9888(12) 0.3260(7) 0.3612(6) 0.051(3) Uani 1 1 d DU . . C55 C 0.9718(13) 0.1799(7) 0.4031(6) 0.058(4) Uani 1 1 d DU . . H55A H 0.9355 0.2027 0.4400 0.070 Uiso 1 1 calc R . . H55B H 1.0328 0.1727 0.4199 0.070 Uiso 1 1 calc R . . C56 C 0.9367(4) 0.0922(6) 0.3814(6) 0.050(3) Uani 1 1 d DU . . C57 C 0.9268(7) 0.0217(8) 0.4243(8) 0.078(5) Uani 1 1 d DU . . H57A H 0.9433 0.0283 0.4698 0.093 Uiso 1 1 calc R . . C58 C 0.8929(8) -0.0599(9) 0.4020(8) 0.082(5) Uani 1 1 d DU . . H58A H 0.8861 -0.1081 0.4317 0.098 Uiso 1 1 calc R . . C59 C 0.8706(9) -0.0665(9) 0.3373(8) 0.083(5) Uani 1 1 d DU . . H59A H 0.8476 -0.1199 0.3197 0.099 Uiso 1 1 calc R . . C60 C 0.8821(7) 0.0072(7) 0.2962(9) 0.068(4) Uani 1 1 d DU . . H60A H 0.8659 0.0017 0.2505 0.082 Uiso 1 1 calc R . . C61 C 0.7531(9) 0.2511(3) 0.3145(7) 0.070(4) Uani 1 1 d DU . . H61A H 0.7817 0.2564 0.3566 0.084 Uiso 1 1 calc R . . C62 C 0.6604(10) 0.2648(5) 0.3064(6) 0.068(4) Uani 1 1 d DU . . H62A H 0.6264 0.2806 0.3441 0.082 Uiso 1 1 calc R . . C63 C 0.6669(8) 0.2360(3) 0.1921(5) 0.048(3) Uani 1 1 d DU . . C64 C 0.7578(8) 0.2222(5) 0.1988(6) 0.053(3) Uani 1 1 d DU . . C65 C 0.8224(10) 0.1920(11) 0.1473(6) 0.064(3) Uani 1 1 d DU . . C67 C 0.9696(10) 0.1450(13) 0.1203(8) 0.070(4) Uani 1 1 d DU . . H67A H 0.9735 0.1873 0.0829 0.084 Uiso 1 1 calc R . . H67B H 0.9524 0.0869 0.1019 0.084 Uiso 1 1 calc R . . C68 C 1.0567(9) 0.1380(4) 0.1548(6) 0.061(3) Uani 1 1 d DU . . C69 C 1.1255(11) 0.1064(6) 0.1153(9) 0.083(5) Uani 1 1 d DU . . H69A H 1.1179 0.0882 0.0703 0.100 Uiso 1 1 calc R . . C70 C 1.2060(13) 0.1044(9) 0.1485(9) 0.104(6) Uani 1 1 d DU . . H70A H 1.2585 0.0846 0.1277 0.125 Uiso 1 1 calc R . . C71 C 1.2043(13) 0.1337(8) 0.2149(9) 0.089(5) Uani 1 1 d DU . . H71A H 1.2594 0.1317 0.2375 0.107 Uiso 1 1 calc R . . C72 C 1.1333(11) 0.1657(8) 0.2536(9) 0.082(4) Uani 1 1 d DU . . H72A H 1.1382 0.1848 0.2986 0.098 Uiso 1 1 calc R . . C73 C 0.6107(8) 0.2360(11) 0.1298(5) 0.051(3) Uani 1 1 d DU . . C75 C 0.4656(8) 0.2471(11) 0.0806(6) 0.051(3) Uani 1 1 d DU . . H75A H 0.4603 0.1868 0.0621 0.062 Uiso 1 1 calc R . . H75B H 0.4889 0.2860 0.0453 0.062 Uiso 1 1 calc R . . C76 C 0.3771(8) 0.2791(4) 0.1024(6) 0.057(3) Uani 1 1 d DU . . C77 C 0.3083(9) 0.2831(6) 0.0568(8) 0.069(4) Uani 1 1 d DU . . H77A H 0.3188 0.2655 0.0120 0.083 Uiso 1 1 calc R . . C78 C 0.2220(11) 0.3127(8) 0.0742(9) 0.089(5) Uani 1 1 d DU . . H78A H 0.1752 0.3146 0.0426 0.107 Uiso 1 1 calc R . . C79 C 0.2106(13) 0.3388(8) 0.1406(9) 0.085(4) Uani 1 1 d DU . . H79A H 0.1560 0.3601 0.1569 0.102 Uiso 1 1 calc R . . C80 C 0.2867(10) 0.3311(7) 0.1816(9) 0.078(4) Uani 1 1 d DU . . H80A H 0.2790 0.3483 0.2268 0.094 Uiso 1 1 calc R . . B1A B 0.1997(10) 0.1823(10) 0.4838(7) 0.062(5) Uani 0.75 1 d PDU A 1 F11A F 0.1655(11) 0.0990(8) 0.4799(10) 0.127(6) Uani 0.75 1 d PDU A 1 F14A F 0.2849(7) 0.1787(11) 0.5098(8) 0.093(4) Uani 0.75 1 d PDU A 1 F13A F 0.1487(9) 0.2350(9) 0.5242(6) 0.092(4) Uani 0.75 1 d PDU A 1 F12A F 0.2015(11) 0.2202(12) 0.4206(5) 0.101(4) Uani 0.75 1 d PDU A 1 B1B B 0.2145(15) 0.2029(15) 0.5013(11) 0.062(5) Uani 0.25 1 d PDU B 2 F11B F 0.216(2) 0.2849(14) 0.5323(17) 0.127(6) Uani 0.25 1 d PDU B 2 F14B F 0.2981(14) 0.166(2) 0.506(2) 0.093(4) Uani 0.25 1 d PDU B 2 F13B F 0.1550(18) 0.1497(18) 0.5338(14) 0.092(4) Uani 0.25 1 d PDU B 2 F12B F 0.191(3) 0.212(3) 0.4348(11) 0.101(4) Uani 0.25 1 d PDU B 2 B2A B 0.2912(9) 0.7184(9) 0.5007(8) 0.051(4) Uani 0.75 1 d PDU C 1 F21A F 0.2695(12) 0.6306(7) 0.5037(10) 0.141(6) Uani 0.75 1 d PDU C 1 F24A F 0.2220(7) 0.7688(8) 0.5251(6) 0.065(3) Uani 0.75 1 d PDU C 1 F23A F 0.3676(6) 0.7369(10) 0.5366(6) 0.083(4) Uani 0.75 1 d PDU C 1 F22A F 0.3025(11) 0.7442(11) 0.4351(5) 0.093(4) Uani 0.75 1 d PDU C 1 B2B B 0.3018(14) 0.7415(14) 0.5082(11) 0.051(4) Uani 0.25 1 d PDU D 2 F21B F 0.328(2) 0.8292(13) 0.513(2) 0.141(6) Uani 0.25 1 d PDU D 2 F24B F 0.2192(13) 0.733(2) 0.5357(15) 0.065(3) Uani 0.25 1 d PDU D 2 F23B F 0.3628(16) 0.6874(19) 0.5399(16) 0.083(4) Uani 0.25 1 d PDU D 2 F22B F 0.297(3) 0.718(3) 0.4413(11) 0.093(4) Uani 0.25 1 d PDU D 2 B3 B 0.9833(12) 0.4266(11) -0.0114(8) 0.121(8) Uani 1 1 d DU . . F31 F 0.9168(11) 0.4042(10) -0.0561(9) 0.202(7) Uani 1 1 d DU . . F32 F 1.0579(12) 0.4367(10) -0.0512(10) 0.208(8) Uani 1 1 d DU . . F33 F 0.9989(12) 0.3617(9) 0.0334(6) 0.139(6) Uani 1 1 d DU . . F34 F 0.9601(10) 0.5041(8) 0.0191(7) 0.120(5) Uani 1 1 d DU . . N400 N 0.750(2) 0.5228(18) 0.1358(12) 0.097(10) Uani 0.50 1 d PDU . . C400 C 0.753(5) 0.467(3) 0.0960(15) 0.138(17) Uani 0.50 1 d PDU . . C401 C 0.7682(7) 0.4279(5) 0.0290(3) 0.20(3) Uani 0.50 1 d PDU . . H40B H 0.7423 0.4643 -0.0044 0.299 Uiso 0.50 1 calc PR . . H40C H 0.7425 0.3710 0.0272 0.299 Uiso 0.50 1 calc PR . . H40D H 0.8298 0.4235 0.0215 0.299 Uiso 0.50 1 calc PR . . B4A B 0.5151(7) 0.5135(5) -0.0025(3) 0.083(5) Uani 0.50 1 d PRDU E 1 F41A F 0.4256(7) 0.4965(5) 0.0091(3) 0.185(9) Uani 0.50 1 d PRDU E 1 F42A F 0.5270(7) 0.5255(5) -0.0710(3) 0.111(6) Uani 0.50 1 d PRDU E 1 F43A F 0.5633(7) 0.4398(5) 0.0177(3) 0.095(5) Uani 0.50 1 d PRDU E 1 F44A F 0.5444(7) 0.5860(5) 0.0331(3) 0.091(5) Uani 0.50 1 d PRDU E 1 B4B B 0.5273(7) 0.5201(5) -0.0120(3) 0.083(5) Uani 0.50 1 d PRDU F 2 F41B F 0.6137(7) 0.5475(5) -0.0200(3) 0.185(9) Uani 0.50 1 d PRDU F 2 F42B F 0.4811(7) 0.5250(5) -0.0722(3) 0.111(6) Uani 0.50 1 d PRDU F 2 F43B F 0.5254(7) 0.4321(5) 0.0093(3) 0.095(5) Uani 0.50 1 d PRDU F 2 F44B F 0.4846(7) 0.5711(5) 0.0354(3) 0.091(5) Uani 0.50 1 d PRDU F 2 N100 N 0.6934(7) 0.4626(5) 0.4857(3) 0.149(9) Uani 1 1 d RDU . . C100 C 0.6998(7) 0.4722(5) 0.4267(3) 0.125(9) Uani 1 1 d RDU . . C101 C 0.7562(7) 0.4839(5) 0.3664(3) 0.40(3) Uani 1 1 d RDU . . H10B H 0.8161 0.4889 0.3798 0.594 Uiso 1 1 d R . . H10C H 0.7388 0.5357 0.3432 0.594 Uiso 1 1 d R . . H10D H 0.7495 0.4344 0.3378 0.594 Uiso 1 1 d R . . N200 N 1.2339(15) 0.4313(14) 0.4473(7) 0.103(6) Uani 1 1 d DU . . C200 C 1.2327(16) 0.4417(15) 0.3869(8) 0.101(7) Uani 1 1 d DU . . C201 C 1.2091(17) 0.4286(16) 0.3179(8) 0.113(7) Uani 1 1 d DU . . H20B H 1.2360 0.3763 0.3020 0.169 Uiso 1 1 calc R . . H20C H 1.2287 0.4773 0.2923 0.169 Uiso 1 1 calc R . . H20D H 1.1469 0.4234 0.3139 0.169 Uiso 1 1 calc R . . N300 N 0.699(2) 1.019(2) 0.1777(11) 0.195(13) Uani 1 1 d DU . . C300 C 0.726(2) 0.997(2) 0.1259(10) 0.129(9) Uani 1 1 d DU . . C301 C 0.741(3) 0.977(2) 0.0542(10) 0.148(11) Uani 1 1 d DU . . H30B H 0.7223 1.0252 0.0277 0.222 Uiso 1 1 calc R . . H30C H 0.7077 0.9259 0.0420 0.222 Uiso 1 1 calc R . . H30D H 0.8015 0.9658 0.0473 0.222 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0651(13) 0.0380(8) 0.0550(9) -0.0026(7) -0.0040(9) -0.0077(9) Cu2 0.0968(18) 0.0449(9) 0.0459(9) -0.0027(8) 0.0004(10) -0.0035(10) Cu3 0.0670(13) 0.0344(8) 0.0679(11) -0.0005(8) -0.0062(10) -0.0063(9) Cu4 0.0738(16) 0.0358(9) 0.0784(13) 0.0039(9) -0.0104(12) -0.0039(9) O1 0.103(9) 0.053(5) 0.053(5) -0.008(4) 0.014(6) -0.039(6) O2 0.106(9) 0.056(5) 0.039(4) -0.007(4) 0.018(5) -0.010(6) O3 0.050(6) 0.076(7) 0.053(4) 0.009(5) -0.013(4) -0.002(5) O4 0.065(7) 0.088(7) 0.042(4) 0.012(5) 0.000(4) -0.009(6) O5 0.111(10) 0.054(6) 0.056(5) 0.003(4) -0.024(6) -0.017(6) O6 0.095(9) 0.038(4) 0.062(5) 0.004(4) -0.019(6) 0.006(5) O7 0.054(7) 0.091(8) 0.064(5) -0.012(6) -0.004(5) 0.000(6) O8 0.066(7) 0.093(8) 0.031(4) -0.006(5) -0.001(4) 0.001(6) N1 0.084(10) 0.045(5) 0.051(5) -0.007(4) 0.010(6) -0.003(6) N2 0.064(8) 0.020(4) 0.066(6) -0.002(4) 0.005(6) -0.001(5) N3 0.048(7) 0.050(5) 0.066(6) -0.014(5) -0.003(5) -0.017(6) N4 0.059(8) 0.056(6) 0.032(4) 0.000(4) 0.003(5) -0.001(6) N5 0.072(8) 0.046(4) 0.041(5) -0.015(4) 0.001(5) -0.010(6) N6 0.097(11) 0.045(5) 0.068(6) 0.010(5) 0.013(7) -0.020(6) N7 0.067(7) 0.057(7) 0.047(5) 0.001(5) -0.006(4) 0.006(6) N8 0.056(5) 0.034(5) 0.075(7) -0.002(5) -0.011(5) -0.005(5) N9 0.069(6) 0.059(7) 0.055(5) -0.007(5) 0.005(5) -0.027(6) N10 0.079(7) 0.047(6) 0.043(5) 0.004(4) -0.006(4) -0.007(6) N11 0.064(5) 0.056(6) 0.070(6) -0.009(6) -0.008(5) -0.013(6) N12 0.076(7) 0.076(9) 0.075(6) 0.007(6) -0.014(6) -0.008(7) N13 0.065(9) 0.056(6) 0.045(5) -0.004(4) -0.004(6) -0.011(6) N14 0.062(8) 0.042(4) 0.060(6) -0.005(4) -0.031(6) -0.004(5) N15 0.060(8) 0.062(5) 0.063(5) 0.014(5) 0.009(6) 0.002(7) N16 0.089(10) 0.032(5) 0.063(5) -0.003(4) -0.011(7) -0.005(6) N17 0.082(9) 0.039(4) 0.062(6) 0.019(4) -0.028(6) -0.033(6) N18 0.065(9) 0.037(5) 0.080(6) -0.007(5) -0.015(7) 0.004(5) N19 0.052(6) 0.042(6) 0.061(5) 0.006(5) -0.014(4) 0.005(6) N20 0.083(6) 0.065(8) 0.068(7) -0.015(6) -0.003(5) 0.026(7) N21 0.085(7) 0.031(5) 0.070(6) 0.002(5) -0.016(5) 0.012(6) N22 0.067(7) 0.046(6) 0.056(5) -0.011(5) -0.005(5) -0.017(6) N23 0.050(5) 0.055(6) 0.045(5) -0.001(5) -0.011(4) -0.002(6) N24 0.085(7) 0.041(6) 0.067(5) -0.001(5) 0.015(6) -0.002(6) C1 0.076(11) 0.056(6) 0.056(6) -0.001(5) -0.003(7) -0.014(7) C2 0.077(11) 0.053(6) 0.044(5) -0.005(5) 0.008(7) -0.001(7) C3 0.081(10) 0.036(4) 0.035(5) -0.007(4) 0.014(6) -0.002(6) C4 0.047(9) 0.045(5) 0.064(6) -0.003(4) 0.011(6) -0.011(6) C5 0.056(9) 0.038(5) 0.060(5) 0.002(4) 0.002(6) -0.019(6) C7 0.097(12) 0.028(5) 0.071(7) -0.006(5) 0.011(8) -0.021(6) C8 0.073(10) 0.023(4) 0.065(6) 0.000(4) -0.006(6) -0.026(6) C9 0.075(10) 0.020(4) 0.076(7) 0.001(4) 0.005(7) -0.007(6) C10 0.058(9) 0.021(5) 0.094(7) -0.005(5) -0.008(7) -0.009(6) C11 0.068(10) 0.049(6) 0.094(8) -0.009(6) 0.003(8) -0.010(7) C12 0.044(9) 0.040(5) 0.080(7) -0.010(5) -0.010(7) -0.012(6) C13 0.081(11) 0.065(6) 0.036(5) -0.014(5) 0.007(7) -0.008(7) C15 0.109(12) 0.049(5) 0.023(5) -0.006(4) 0.004(6) -0.004(7) C16 0.068(10) 0.053(5) 0.050(6) -0.013(5) -0.007(6) -0.010(7) C17 0.121(13) 0.054(6) 0.063(7) -0.013(5) -0.014(8) -0.028(8) C18 0.107(14) 0.051(7) 0.099(8) -0.007(7) -0.015(9) -0.011(8) C19 0.103(13) 0.046(6) 0.096(8) 0.001(6) -0.014(9) -0.013(8) C20 0.086(11) 0.036(6) 0.102(8) 0.001(6) 0.007(9) -0.028(7) C21 0.084(7) 0.066(8) 0.030(5) 0.004(5) -0.006(5) 0.004(8) C22 0.079(8) 0.093(11) 0.029(5) 0.002(6) -0.005(6) 0.010(8) C23 0.067(6) 0.061(8) 0.039(5) 0.002(5) -0.006(4) 0.008(7) C24 0.067(5) 0.033(6) 0.045(5) 0.001(5) -0.012(4) -0.008(6) C25 0.058(6) 0.027(6) 0.061(5) -0.005(5) -0.010(5) -0.003(5) C27 0.054(6) 0.067(9) 0.079(8) 0.017(7) -0.002(5) -0.011(7) C28 0.057(6) 0.054(7) 0.063(6) -0.007(6) 0.005(5) -0.006(6) C29 0.068(7) 0.066(9) 0.097(9) 0.016(8) -0.006(6) -0.003(8) C30 0.071(7) 0.081(11) 0.132(9) 0.001(9) 0.002(8) 0.002(9) C31 0.071(8) 0.057(8) 0.116(9) -0.018(7) 0.020(7) -0.022(7) C32 0.086(9) 0.071(10) 0.098(9) 0.004(8) 0.026(7) -0.016(9) C33 0.082(6) 0.056(8) 0.047(5) -0.002(6) -0.004(5) -0.013(7) C35 0.084(7) 0.037(6) 0.067(7) 0.004(6) -0.008(5) 0.012(7) C36 0.081(7) 0.060(8) 0.065(7) -0.007(6) 0.000(5) 0.007(8) C37 0.094(8) 0.082(10) 0.072(7) -0.020(7) 0.012(6) 0.005(8) C38 0.078(8) 0.118(13) 0.087(7) -0.040(8) -0.002(8) -0.005(9) C39 0.102(10) 0.061(9) 0.107(9) -0.022(8) -0.001(7) 0.011(9) C40 0.084(10) 0.057(9) 0.098(9) 0.002(8) -0.014(7) 0.012(8) C41 0.096(12) 0.056(6) 0.045(6) 0.006(5) -0.007(7) 0.004(8) C42 0.055(10) 0.057(6) 0.067(6) -0.010(5) -0.021(7) -0.008(7) C43 0.059(10) 0.039(5) 0.062(5) 0.002(4) -0.011(7) -0.010(6) C44 0.040(8) 0.032(4) 0.051(5) -0.003(4) -0.010(5) 0.000(5) C45 0.072(10) 0.043(5) 0.054(5) -0.006(5) -0.014(7) -0.012(6) C47 0.064(10) 0.030(5) 0.076(8) -0.001(4) -0.025(7) -0.001(6) C48 0.049(9) 0.032(4) 0.078(7) 0.004(5) -0.006(7) -0.008(6) C49 0.050(9) 0.038(5) 0.127(9) -0.008(5) -0.028(9) -0.019(7) C50 0.089(12) 0.051(6) 0.109(8) -0.003(7) -0.018(10) -0.016(8) C51 0.099(13) 0.055(7) 0.105(8) -0.009(7) -0.010(10) -0.012(9) C52 0.044(9) 0.046(6) 0.094(8) 0.009(5) -0.009(8) -0.018(6) C53 0.054(9) 0.029(4) 0.071(6) 0.009(4) -0.003(7) -0.001(6) C55 0.090(11) 0.039(5) 0.045(6) 0.016(4) -0.012(7) -0.006(6) C56 0.056(9) 0.027(4) 0.067(6) 0.014(4) 0.004(6) 0.007(5) C57 0.118(13) 0.043(6) 0.072(7) 0.010(5) -0.002(9) -0.017(8) C58 0.113(13) 0.031(5) 0.102(7) 0.002(6) 0.026(9) -0.009(7) C59 0.111(14) 0.032(6) 0.105(8) -0.003(6) 0.001(10) 0.006(7) C60 0.062(10) 0.033(6) 0.109(8) -0.002(5) -0.024(8) -0.015(6) C61 0.080(8) 0.070(9) 0.060(6) -0.005(7) -0.015(6) -0.017(8) C62 0.080(7) 0.090(11) 0.035(5) 0.004(7) 0.009(6) -0.002(9) C63 0.058(5) 0.048(7) 0.038(4) -0.004(5) -0.013(4) -0.016(6) C64 0.062(5) 0.034(6) 0.062(5) -0.009(5) -0.005(5) -0.008(6) C65 0.082(7) 0.044(7) 0.065(6) -0.002(6) 0.010(6) 0.004(7) C67 0.069(6) 0.068(9) 0.072(8) -0.024(7) 0.003(5) -0.003(8) C68 0.066(6) 0.043(7) 0.073(7) 0.001(6) -0.004(6) -0.002(6) C69 0.071(7) 0.081(11) 0.098(9) -0.016(9) 0.000(6) 0.009(9) C70 0.062(8) 0.111(13) 0.140(10) -0.032(11) -0.012(8) -0.016(10) C71 0.067(8) 0.075(10) 0.126(9) 0.000(9) -0.024(8) -0.033(8) C72 0.087(9) 0.058(9) 0.101(9) -0.004(8) -0.025(6) -0.029(8) C73 0.053(6) 0.055(7) 0.044(5) -0.001(6) -0.016(5) -0.004(7) C75 0.048(6) 0.067(8) 0.039(5) 0.004(6) -0.013(4) 0.007(6) C76 0.052(6) 0.056(7) 0.063(6) 0.004(6) -0.009(5) -0.001(7) C77 0.040(6) 0.073(9) 0.093(8) 0.007(8) -0.013(5) -0.007(7) C78 0.062(7) 0.103(12) 0.101(8) 0.025(9) -0.001(7) 0.014(9) C79 0.089(9) 0.058(9) 0.110(9) 0.017(8) 0.011(7) 0.012(8) C80 0.077(8) 0.067(9) 0.091(8) -0.001(8) 0.023(6) -0.027(8) B1A 0.059(9) 0.058(8) 0.068(9) -0.015(7) -0.017(8) 0.019(7) F11A 0.115(11) 0.095(8) 0.170(12) -0.017(8) -0.015(10) -0.020(7) F14A 0.055(6) 0.114(9) 0.109(8) -0.028(7) -0.016(6) 0.008(6) F13A 0.092(8) 0.109(8) 0.073(6) -0.005(7) 0.012(6) 0.043(7) F12A 0.080(8) 0.165(10) 0.057(6) 0.007(6) 0.012(6) 0.017(8) B1B 0.059(9) 0.058(8) 0.068(9) -0.015(7) -0.017(8) 0.019(7) F11B 0.115(11) 0.095(8) 0.170(12) -0.017(8) -0.015(10) -0.020(7) F14B 0.055(6) 0.114(9) 0.109(8) -0.028(7) -0.016(6) 0.008(6) F13B 0.092(8) 0.109(8) 0.073(6) -0.005(7) 0.012(6) 0.043(7) F12B 0.080(8) 0.165(10) 0.057(6) 0.007(6) 0.012(6) 0.017(8) B2A 0.022(7) 0.048(8) 0.084(8) -0.004(7) -0.020(6) -0.003(6) F21A 0.145(13) 0.061(6) 0.217(14) 0.016(8) -0.017(12) -0.030(7) F24A 0.060(6) 0.065(7) 0.069(6) 0.028(6) 0.008(5) 0.024(6) F23A 0.021(5) 0.126(10) 0.103(7) 0.014(8) -0.018(5) -0.026(6) F22A 0.089(8) 0.127(10) 0.064(5) 0.008(6) -0.004(5) 0.025(8) B2B 0.022(7) 0.048(8) 0.084(8) -0.004(7) -0.020(6) -0.003(6) F21B 0.145(13) 0.061(6) 0.217(14) 0.016(8) -0.017(12) -0.030(7) F24B 0.060(6) 0.065(7) 0.069(6) 0.028(6) 0.008(5) 0.024(6) F23B 0.021(5) 0.126(10) 0.103(7) 0.014(8) -0.018(5) -0.026(6) F22B 0.089(8) 0.127(10) 0.064(5) 0.008(6) -0.004(5) 0.025(8) B3 0.142(15) 0.095(12) 0.127(14) -0.004(10) -0.011(11) 0.012(13) F31 0.250(14) 0.118(10) 0.237(15) -0.077(10) -0.120(13) 0.088(11) F32 0.260(15) 0.097(10) 0.267(18) 0.032(11) 0.105(14) 0.034(12) F33 0.216(16) 0.119(9) 0.083(7) 0.023(7) 0.015(9) 0.059(11) F34 0.136(12) 0.095(8) 0.127(10) -0.028(7) -0.035(9) 0.017(8) N400 0.048(14) 0.111(16) 0.132(18) -0.020(14) -0.003(13) 0.003(13) C400 0.12(2) 0.15(2) 0.14(2) -0.026(17) 0.005(17) -0.013(17) C401 0.19(3) 0.21(3) 0.20(3) -0.009(18) 0.013(18) -0.017(18) B4A 0.091(10) 0.085(9) 0.075(8) -0.002(8) 0.001(8) -0.003(9) F41A 0.109(9) 0.196(16) 0.251(18) -0.005(15) 0.035(10) -0.028(10) F42A 0.176(15) 0.100(9) 0.058(5) 0.008(6) -0.018(8) 0.003(11) F43A 0.129(13) 0.079(6) 0.076(7) 0.010(6) 0.012(9) 0.022(8) F44A 0.118(13) 0.108(8) 0.048(5) -0.001(6) -0.009(8) 0.021(9) B4B 0.091(10) 0.085(9) 0.075(8) -0.002(8) 0.001(8) -0.003(9) F41B 0.109(9) 0.196(16) 0.251(18) -0.005(15) 0.035(10) -0.028(10) F42B 0.176(15) 0.100(9) 0.058(5) 0.008(6) -0.018(8) 0.003(11) F43B 0.129(13) 0.079(6) 0.076(7) 0.010(6) 0.012(9) 0.022(8) F44B 0.118(13) 0.108(8) 0.048(5) -0.001(6) -0.009(8) 0.021(9) N100 0.189(17) 0.105(12) 0.152(14) -0.036(12) 0.002(13) 0.024(13) C100 0.135(16) 0.071(11) 0.168(17) -0.003(12) 0.029(14) 0.001(12) C101 0.41(3) 0.38(3) 0.41(3) 0.005(19) 0.014(19) 0.012(19) N200 0.104(12) 0.117(11) 0.087(10) 0.005(9) 0.004(9) 0.039(10) C200 0.092(12) 0.099(12) 0.113(13) 0.008(10) 0.008(11) 0.059(10) C201 0.127(14) 0.119(12) 0.093(12) 0.006(9) 0.021(11) 0.094(11) N300 0.21(2) 0.21(2) 0.164(18) 0.005(15) 0.029(15) -0.035(16) C300 0.152(18) 0.150(16) 0.086(12) -0.016(12) 0.025(12) -0.038(14) C301 0.18(2) 0.172(18) 0.097(14) -0.020(13) 0.030(13) -0.013(15) _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 N2 1.913(10) . ? Cu1 N23 1.975(9) . ? Cu1 N24 2.098(10) . ? Cu1 N3 2.142(10) . ? Cu1 N22 2.203(12) . ? Cu1 N1 2.218(10) . ? Cu2 N8 1.929(11) . ? Cu2 N5 1.948(10) . ? Cu2 N9 2.114(10) . ? Cu2 N6 2.121(10) . ? Cu2 N7 2.198(11) . ? Cu2 N4 2.234(10) . ? Cu3 N14 1.919(10) . ? Cu3 N11 1.951(11) . ? Cu3 N12 2.136(10) . ? Cu3 N15 2.144(10) . ? Cu3 N13 2.167(10) . ? Cu3 N10 2.250(11) . ? Cu4 N20 1.925(11) . ? Cu4 N17 1.946(10) . ? Cu4 N21 2.086(11) . ? Cu4 N18 2.147(10) . ? Cu4 N19 2.215(10) . ? Cu4 N16 2.226(9) . ? O1 C5 1.294(13) . ? O2 C13 1.279(13) . ? O3 C25 1.284(13) . ? O4 C33 1.326(13) . ? O5 C45 1.319(13) . ? O6 C53 1.285(13) . ? O7 C65 1.291(14) . ? O8 C73 1.281(13) . ? N1 C1 1.326(13) . ? N1 C4 1.348(13) . ? N2 C5 1.319(13) . ? N2 C7 1.479(13) . ? N3 C12 1.322(13) . ? N3 C8 1.333(12) . ? N4 C2 1.322(13) . ? N4 C3 1.338(12) . ? N5 C13 1.311(14) . ? N5 C15 1.464(12) . ? N6 C16 1.337(13) . ? N6 C20 1.372(13) . ? N7 C21 1.339(13) . ? N7 C24 1.340(13) . ? N8 C25 1.314(14) . ? N8 C27 1.449(15) . ? N9 C32 1.288(15) . ? N9 C28 1.356(13) . ? N10 C23 1.330(13) . ? N10 C22 1.355(14) . ? N11 C33 1.307(15) . ? N11 C35 1.448(15) . ? N12 C36 1.358(14) . ? N12 C40 1.370(15) . ? N13 C41 1.316(13) . ? N13 C44 1.360(13) . ? N14 C45 1.298(13) . ? N14 C47 1.481(13) . ? N15 C52 1.328(14) . ? N15 C48 1.351(13) . ? N16 C42 1.308(14) . ? N16 C43 1.349(13) . ? N17 C53 1.297(13) . ? N17 C55 1.486(12) . ? N18 C60 1.318(13) . ? N18 C56 1.351(13) . ? N19 C61 1.319(14) . ? N19 C64 1.355(13) . ? N20 C65 1.316(15) . ? N20 C67 1.491(15) . ? N21 C72 1.318(15) . ? N21 C68 1.344(14) . ? N22 C62 1.342(14) . ? N22 C63 1.348(13) . ? N23 C73 1.300(14) . ? N23 C75 1.490(13) . ? N24 C76 1.333(13) . ? N24 C80 1.354(15) . ? C1 C2 1.401(14) . ? C3 C4 1.412(13) . ? C3 C13 1.493(13) . ? C4 C5 1.517(13) . ? C7 C8 1.501(13) . ? C8 C9 1.406(13) . ? C9 C10 1.417(13) . ? C10 C11 1.383(16) . ? C11 C12 1.398(15) . ? C15 C16 1.485(14) . ? C16 C17 1.409(14) . ? C17 C18 1.405(15) . ? C18 C19 1.394(17) . ? C19 C20 1.426(16) . ? C21 C22 1.381(16) . ? C23 C24 1.410(15) . ? C23 C33 1.517(15) . ? C24 C25 1.513(14) . ? C27 C28 1.534(16) . ? C28 C29 1.372(15) . ? C29 C30 1.405(17) . ? C30 C31 1.385(17) . ? C31 C32 1.384(17) . ? C35 C36 1.511(15) . ? C36 C37 1.390(16) . ? C37 C38 1.428(17) . ? C38 C39 1.390(17) . ? C39 C40 1.414(17) . ? C41 C42 1.410(15) . ? C43 C44 1.385(13) . ? C43 C53 1.507(14) . ? C44 C45 1.507(13) . ? C47 C48 1.484(13) . ? C48 C49 1.390(14) . ? C49 C50 1.413(16) . ? C50 C51 1.366(17) . ? C51 C52 1.423(16) . ? C55 C56 1.499(13) . ? C56 C57 1.382(14) . ? C57 C58 1.414(15) . ? C58 C59 1.343(17) . ? C59 C60 1.401(16) . ? C61 C62 1.431(16) . ? C63 C64 1.402(15) . ? C63 C73 1.507(13) . ? C64 C65 1.501(15) . ? C67 C68 1.492(16) . ? C68 C69 1.401(16) . ? C69 C70 1.387(17) . ? C70 C71 1.405(17) . ? C71 C72 1.419(17) . ? C75 C76 1.498(14) . ? C76 C77 1.386(15) . ? C77 C78 1.431(16) . ? C78 C79 1.400(17) . ? C79 C80 1.418(17) . ? B1A F11A 1.371(15) . ? B1A F13A 1.380(15) . ? B1A F14A 1.392(15) . ? B1A F12A 1.392(15) . ? B1B F13B 1.379(17) . ? B1B F12B 1.385(17) . ? B1B F14B 1.390(17) . ? B1B F11B 1.392(17) . ? B2A F21A 1.376(14) . ? B2A F22A 1.384(15) . ? B2A F23A 1.390(14) . ? B2A F24A 1.391(14) . ? B2B F24B 1.380(17) . ? B2B F23B 1.389(17) . ? B2B F22B 1.391(17) . ? B2B F21B 1.394(17) . ? B3 F33 1.354(15) . ? B3 F34 1.375(15) . ? B3 F31 1.388(16) . ? B3 F32 1.398(16) . ? N400 C400 1.162(17) . ? C400 C401 1.490(17) . ? B4A F44A 1.3829 . ? B4A F43A 1.3960 . ? B4A F42A 1.3993 . ? B4A F41A 1.4054 . ? B4B F41B 1.3864 . ? B4B F44B 1.3909 . ? B4B F42B 1.3949 . ? B4B F43B 1.4038 . ? N100 C100 1.1960 . ? C100 C101 1.4976 . ? N200 C200 1.221(14) . ? C200 C201 1.440(15) . ? N300 C300 1.164(16) . ? C300 C301 1.490(15) . ? 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 N2 Cu1 N23 172.4(5) . . ? N2 Cu1 N24 106.5(5) . . ? N23 Cu1 N24 79.6(4) . . ? N2 Cu1 N3 81.3(4) . . ? N23 Cu1 N3 102.3(3) . . ? N24 Cu1 N3 99.8(3) . . ? N2 Cu1 N22 97.3(5) . . ? N23 Cu1 N22 76.1(4) . . ? N24 Cu1 N22 155.1(4) . . ? N3 Cu1 N22 90.8(3) . . ? N2 Cu1 N1 74.2(4) . . ? N23 Cu1 N1 101.8(3) . . ? N24 Cu1 N1 89.3(3) . . ? N3 Cu1 N1 155.4(4) . . ? N22 Cu1 N1 90.3(3) . . ? N8 Cu2 N5 170.6(5) . . ? N8 Cu2 N9 79.9(4) . . ? N5 Cu2 N9 103.6(5) . . ? N8 Cu2 N6 108.2(4) . . ? N5 Cu2 N6 79.8(4) . . ? N9 Cu2 N6 102.1(3) . . ? N8 Cu2 N7 76.8(4) . . ? N5 Cu2 N7 99.1(5) . . ? N9 Cu2 N7 156.5(4) . . ? N6 Cu2 N7 87.8(3) . . ? N8 Cu2 N4 95.2(4) . . ? N5 Cu2 N4 76.2(4) . . ? N9 Cu2 N4 90.9(2) . . ? N6 Cu2 N4 154.8(4) . . ? N7 Cu2 N4 88.6(2) . . ? N14 Cu3 N11 171.5(6) . . ? N14 Cu3 N12 109.7(5) . . ? N11 Cu3 N12 78.0(5) . . ? N14 Cu3 N15 81.0(4) . . ? N11 Cu3 N15 101.5(5) . . ? N12 Cu3 N15 100.8(3) . . ? N14 Cu3 N13 77.4(4) . . ? N11 Cu3 N13 99.7(5) . . ? N12 Cu3 N13 88.5(3) . . ? N15 Cu3 N13 158.2(4) . . ? N14 Cu3 N10 96.3(5) . . ? N11 Cu3 N10 75.6(5) . . ? N12 Cu3 N10 152.5(4) . . ? N15 Cu3 N10 91.8(2) . . ? N13 Cu3 N10 88.6(2) . . ? N20 Cu4 N17 171.2(6) . . ? N20 Cu4 N21 79.9(5) . . ? N17 Cu4 N21 103.0(5) . . ? N20 Cu4 N18 106.7(6) . . ? N17 Cu4 N18 81.2(4) . . ? N21 Cu4 N18 99.1(3) . . ? N20 Cu4 N19 76.8(5) . . ? N17 Cu4 N19 99.7(5) . . ? N21 Cu4 N19 156.6(4) . . ? N18 Cu4 N19 89.6(2) . . ? N20 Cu4 N16 96.8(5) . . ? N17 Cu4 N16 74.9(4) . . ? N21 Cu4 N16 92.6(2) . . ? N18 Cu4 N16 155.2(4) . . ? N19 Cu4 N16 88.0(2) . . ? C1 N1 C4 117.5(10) . . ? C1 N1 Cu1 127.4(8) . . ? C4 N1 Cu1 115.0(7) . . ? C5 N2 C7 112.9(9) . . ? C5 N2 Cu1 126.4(9) . . ? C7 N2 Cu1 119.7(7) . . ? C12 N3 C8 121.4(10) . . ? C12 N3 Cu1 128.0(9) . . ? C8 N3 Cu1 110.3(7) . . ? C2 N4 C3 121.8(10) . . ? C2 N4 Cu2 126.0(8) . . ? C3 N4 Cu2 112.2(7) . . ? C13 N5 C15 118.6(10) . . ? C13 N5 Cu2 122.5(8) . . ? C15 N5 Cu2 118.8(7) . . ? C16 N6 C20 118.8(12) . . ? C16 N6 Cu2 113.2(7) . . ? C20 N6 Cu2 128.0(10) . . ? C21 N7 C24 119.0(11) . . ? C21 N7 Cu2 127.0(9) . . ? C24 N7 Cu2 113.9(8) . . ? C25 N8 C27 119.1(11) . . ? C25 N8 Cu2 122.2(9) . . ? C27 N8 Cu2 118.7(9) . . ? C32 N9 C28 118.1(13) . . ? C32 N9 Cu2 125.1(11) . . ? C28 N9 Cu2 116.5(9) . . ? C23 N10 C22 118.9(11) . . ? C23 N10 Cu3 114.6(8) . . ? C22 N10 Cu3 126.5(9) . . ? C33 N11 C35 114.5(11) . . ? C33 N11 Cu3 121.8(9) . . ? C35 N11 Cu3 123.5(10) . . ? C36 N12 C40 119.6(12) . . ? C36 N12 Cu3 113.0(8) . . ? C40 N12 Cu3 127.3(11) . . ? C41 N13 C44 121.8(10) . . ? C41 N13 Cu3 124.6(8) . . ? C44 N13 Cu3 113.6(7) . . ? C45 N14 C47 118.2(10) . . ? C45 N14 Cu3 120.8(8) . . ? C47 N14 Cu3 120.0(8) . . ? C52 N15 C48 122.3(11) . . ? C52 N15 Cu3 127.4(9) . . ? C48 N15 Cu3 110.1(8) . . ? C42 N16 C43 120.7(10) . . ? C42 N16 Cu4 125.4(8) . . ? C43 N16 Cu4 113.8(8) . . ? C53 N17 C55 118.0(10) . . ? C53 N17 Cu4 125.0(8) . . ? C55 N17 Cu4 117.0(7) . . ? C60 N18 C56 118.3(11) . . ? C60 N18 Cu4 128.9(10) . . ? C56 N18 Cu4 112.7(7) . . ? C61 N19 C64 124.2(11) . . ? C61 N19 Cu4 122.7(9) . . ? C64 N19 Cu4 113.0(8) . . ? C65 N20 C67 118.3(11) . . ? C65 N20 Cu4 122.1(10) . . ? C67 N20 Cu4 119.2(10) . . ? C72 N21 C68 122.0(13) . . ? C72 N21 Cu4 122.4(10) . . ? C68 N21 Cu4 115.5(9) . . ? C62 N22 C63 120.4(12) . . ? C62 N22 Cu1 125.5(10) . . ? C63 N22 Cu1 113.9(8) . . ? C73 N23 C75 119.7(10) . . ? C73 N23 Cu1 121.5(8) . . ? C75 N23 Cu1 118.1(8) . . ? C76 N24 C80 113.8(12) . . ? C76 N24 Cu1 115.4(8) . . ? C80 N24 Cu1 130.6(11) . . ? N1 C1 C2 122.3(12) . . ? N4 C2 C1 118.8(12) . . ? N4 C3 C4 117.8(9) . . ? N4 C3 C13 113.9(9) . . ? C4 C3 C13 128.3(10) . . ? N1 C4 C3 121.8(10) . . ? N1 C4 C5 111.2(9) . . ? C3 C4 C5 127.0(10) . . ? O1 C5 N2 123.4(11) . . ? O1 C5 C4 124.0(10) . . ? N2 C5 C4 112.1(10) . . ? N2 C7 C8 107.5(10) . . ? N3 C8 C9 118.1(10) . . ? N3 C8 C7 120.8(10) . . ? C9 C8 C7 121.1(11) . . ? C8 C9 C10 120.2(12) . . ? C11 C10 C9 120.4(12) . . ? C10 C11 C12 114.7(13) . . ? N3 C12 C11 125.3(14) . . ? O2 C13 N5 121.3(11) . . ? O2 C13 C3 123.4(11) . . ? N5 C13 C3 115.1(10) . . ? N5 C15 C16 109.6(9) . . ? N6 C16 C17 122.5(11) . . ? N6 C16 C15 117.8(10) . . ? C17 C16 C15 119.3(10) . . ? C18 C17 C16 119.5(14) . . ? C19 C18 C17 118.6(15) . . ? C18 C19 C20 118.8(15) . . ? N6 C20 C19 121.7(15) . . ? N7 C21 C22 122.1(12) . . ? N10 C22 C21 119.4(12) . . ? N10 C23 C24 121.6(11) . . ? N10 C23 C33 110.3(11) . . ? C24 C23 C33 128.0(10) . . ? N7 C24 C23 119.1(10) . . ? N7 C24 C25 111.5(10) . . ? C23 C24 C25 129.4(10) . . ? O3 C25 N8 122.3(12) . . ? O3 C25 C24 121.2(11) . . ? N8 C25 C24 115.4(11) . . ? N8 C27 C28 112.7(12) . . ? N9 C28 C29 125.0(13) . . ? N9 C28 C27 111.7(11) . . ? C29 C28 C27 123.2(12) . . ? C28 C29 C30 118.7(16) . . ? C31 C30 C29 112.6(18) . . ? C30 C31 C32 126.0(19) . . ? N9 C32 C31 119.0(17) . . ? N11 C33 O4 123.2(12) . . ? N11 C33 C23 117.5(11) . . ? O4 C33 C23 119.3(12) . . ? N11 C35 C36 106.0(11) . . ? N12 C36 C37 124.8(13) . . ? N12 C36 C35 118.7(11) . . ? C37 C36 C35 116.0(12) . . ? C36 C37 C38 114.8(16) . . ? C39 C38 C37 121.9(18) . . ? C38 C39 C40 119.0(19) . . ? N12 C40 C39 119.9(17) . . ? N13 C41 C42 119.1(12) . . ? N16 C42 C41 120.1(12) . . ? N16 C43 C44 120.3(10) . . ? N16 C43 C53 112.3(9) . . ? C44 C43 C53 127.4(10) . . ? N13 C44 C43 118.0(10) . . ? N13 C44 C45 110.4(9) . . ? C43 C44 C45 131.6(10) . . ? N14 C45 O5 126.3(11) . . ? N14 C45 C44 116.2(10) . . ? O5 C45 C44 117.0(10) . . ? N14 C47 C48 107.5(10) . . ? N15 C48 C49 118.4(12) . . ? N15 C48 C47 121.1(10) . . ? C49 C48 C47 120.1(11) . . ? C48 C49 C50 121.0(15) . . ? C51 C50 C49 118.7(15) . . ? C50 C51 C52 118.5(16) . . ? N15 C52 C51 121.0(15) . . ? O6 C53 N17 123.8(11) . . ? O6 C53 C43 122.2(10) . . ? N17 C53 C43 114.0(10) . . ? N17 C55 C56 111.6(10) . . ? N18 C56 C57 119.7(11) . . ? N18 C56 C55 117.1(9) . . ? C57 C56 C55 123.2(11) . . ? C56 C57 C58 121.6(14) . . ? C59 C58 C57 117.4(15) . . ? C58 C59 C60 118.5(15) . . ? N18 C60 C59 124.6(15) . . ? N19 C61 C62 115.5(13) . . ? N22 C62 C61 122.0(13) . . ? N22 C63 C64 118.8(10) . . ? N22 C63 C73 112.1(10) . . ? C64 C63 C73 129.1(10) . . ? N19 C64 C63 119.1(11) . . ? N19 C64 C65 111.8(11) . . ? C63 C64 C65 129.0(11) . . ? O7 C65 N20 126.6(13) . . ? O7 C65 C64 117.4(13) . . ? N20 C65 C64 115.9(11) . . ? N20 C67 C68 108.9(12) . . ? N21 C68 C69 128.6(14) . . ? N21 C68 C67 116.2(12) . . ? C69 C68 C67 115.2(12) . . ? C70 C69 C68 113.3(17) . . ? C69 C70 C71 115.1(19) . . ? C70 C71 C72 130.2(18) . . ? N21 C72 C71 110.7(16) . . ? O8 C73 N23 123.6(11) . . ? O8 C73 C63 120.7(11) . . ? N23 C73 C63 115.7(10) . . ? N23 C75 C76 109.1(10) . . ? N24 C76 C77 122.8(12) . . ? N24 C76 C75 117.5(10) . . ? C77 C76 C75 119.7(11) . . ? C76 C77 C78 122.7(15) . . ? C79 C78 C77 116.2(17) . . ? C78 C79 C80 115.0(18) . . ? N24 C80 C79 129.6(17) . . ? F11A B1A F13A 110.8(13) . . ? F11A B1A F14A 109.6(13) . . ? F13A B1A F14A 109.1(12) . . ? F11A B1A F12A 109.8(13) . . ? F13A B1A F12A 108.0(12) . . ? F14A B1A F12A 109.4(13) . . ? F13B B1B F12B 110.6(17) . . ? F13B B1B F14B 109.4(16) . . ? F12B B1B F14B 109.5(16) . . ? F13B B1B F11B 108.8(16) . . ? F12B B1B F11B 109.8(16) . . ? F14B B1B F11B 108.7(16) . . ? F21A B2A F22A 110.3(13) . . ? F21A B2A F23A 111.9(13) . . ? F22A B2A F23A 109.0(12) . . ? F21A B2A F24A 109.7(12) . . ? F22A B2A F24A 106.1(11) . . ? F23A B2A F24A 109.7(12) . . ? F24B B2B F23B 111.4(16) . . ? F24B B2B F22B 108.4(16) . . ? F23B B2B F22B 108.7(16) . . ? F24B B2B F21B 109.0(16) . . ? F23B B2B F21B 110.1(16) . . ? F22B B2B F21B 109.2(16) . . ? F33 B3 F34 111.8(13) . . ? F33 B3 F31 111.9(14) . . ? F34 B3 F31 108.0(13) . . ? F33 B3 F32 108.7(14) . . ? F34 B3 F32 111.8(14) . . ? F31 B3 F32 104.4(13) . . ? N400 C400 C401 157(4) . . ? F44A B4A F43A 108.8 . . ? F44A B4A F42A 111.1 . . ? F43A B4A F42A 108.5 . . ? F44A B4A F41A 111.7 . . ? F43A B4A F41A 108.1 . . ? F42A B4A F41A 108.5 . . ? F41B B4B F44B 111.1 . . ? F41B B4B F42B 110.7 . . ? F44B B4B F42B 109.1 . . ? F41B B4B F43B 110.1 . . ? F44B B4B F43B 108.2 . . ? F42B B4B F43B 107.6 . . ? N100 C100 C101 149.8 . . ? N200 C200 C201 159(3) . . ? N300 C300 C301 168(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.801 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.096