# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof. H. V. R. Dias' _publ_contact_author_address ; Department of Chemistry and Biochemistry The University of Texas at Arlington Arlington, Texas 76019-0065, USA ; _publ_contact_author_email dias@uta.edu _publ_contact_author_phone 817-272-3813 _publ_contact_author_fax 817-272-3808 _publ_section_title ; Neutral Cu4N12 and Ag4N12 metallacycles with a para-cyclophane framework assembled from copper(I) and silver(I) pyrazolates and pyridazine ; loop_ _publ_author_name D.H.V.Rasika 'Himashinie V. K. Diyabalanage' 'Chammi S. Palehepitiya Gamage' data_03102 _database_code_depnum_ccdc_archive 'CCDC 257594' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((3,5-(CF3)2PzCu)4(C4H4N2)2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H12 Cu4 F24 N12' _chemical_formula_weight 613.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.3177(10) _cell_length_b 10.0414(11) _cell_length_c 11.7532(13) _cell_angle_alpha 105.928(2) _cell_angle_beta 109.526(2) _cell_angle_gamma 96.780(2) _cell_volume 969.56(18) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 2.323 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6176 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _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 1.95 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3685 _reflns_number_gt 3577 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0473P)^2^+0.8518P] 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 3685 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 1.48831(3) 0.58016(3) 0.69656(3) 0.01609(10) Uani 1 1 d . . . Cu2 Cu 1.74735(3) 0.57984(3) 0.60677(3) 0.01716(10) Uani 1 1 d . . . C1 C 1.9589(3) 0.7166(3) 0.8787(3) 0.0253(6) Uani 1 1 d . . . H1A H 2.0419 0.7113 0.8491 0.030 Uiso 1 1 calc R . . C2 C 1.9964(3) 0.7793(3) 1.0090(3) 0.0292(6) Uani 1 1 d . . . H2A H 2.1022 0.8163 1.0676 0.035 Uiso 1 1 calc R . . C3 C 1.8754(4) 0.7861(3) 1.0498(2) 0.0263(6) Uani 1 1 d . . . H3A H 1.8942 0.8281 1.1379 0.032 Uiso 1 1 calc R . . C4 C 1.7242(3) 0.7294(3) 0.9583(2) 0.0220(5) Uani 1 1 d . . . H4A H 1.6391 0.7329 0.9856 0.026 Uiso 1 1 calc R . . C13 C 1.2668(3) 0.7766(3) 0.6645(2) 0.0191(5) Uani 1 1 d . . . C16 C 1.3391(3) 0.8632(3) 0.8036(3) 0.0236(6) Uani 1 1 d . . . C23 C 1.6728(3) 0.8375(3) 0.5240(2) 0.0196(5) Uani 1 1 d . . . C26 C 1.7653(3) 0.9418(3) 0.6536(3) 0.0217(5) Uani 1 1 d . . . C33 C 1.4708(3) 0.2695(2) 0.6774(2) 0.0189(5) Uani 1 1 d . . . C34 C 1.4035(3) 0.1345(3) 0.5866(2) 0.0212(5) Uani 1 1 d . . . H34A H 1.4086 0.0448 0.5979 0.025 Uiso 1 1 calc R . . C36 C 1.5652(3) 0.3082(3) 0.8155(3) 0.0230(5) Uani 1 1 d . . . C43 C 1.8835(3) 0.3235(3) 0.5343(2) 0.0184(5) Uani 1 1 d . . . C44 C 1.8629(3) 0.2110(3) 0.4277(2) 0.0205(5) Uani 1 1 d . . . H44A H 1.9235 0.1418 0.4199 0.025 Uiso 1 1 calc R . . C46 C 2.0097(3) 0.3675(3) 0.6644(3) 0.0222(5) Uani 1 1 d . . . N1 N 1.6933(2) 0.6704(2) 0.83405(19) 0.0160(4) Uani 1 1 d . . . N2 N 1.8127(2) 0.6633(2) 0.79316(19) 0.0180(4) Uani 1 1 d . . . N11 N 1.3212(2) 0.6646(2) 0.61741(19) 0.0161(4) Uani 1 1 d . . . N21 N 1.6545(2) 0.6963(2) 0.50202(19) 0.0174(4) Uani 1 1 d . . . N31 N 1.4356(2) 0.3701(2) 0.62418(19) 0.0170(4) Uani 1 1 d . . . N41 N 1.7734(2) 0.3988(2) 0.50779(19) 0.0164(4) Uani 1 1 d . . . F16C F 1.49266(18) 0.91530(16) 0.84762(15) 0.0272(4) Uani 1 1 d . . . F16B F 1.3208(2) 0.7869(2) 0.87776(16) 0.0442(5) Uani 1 1 d . . . F16A F 1.2741(2) 0.9730(2) 0.82937(18) 0.0518(6) Uani 1 1 d . . . F26C F 1.91246(19) 0.92585(18) 0.70353(16) 0.0345(4) Uani 1 1 d . . . F26B F 1.7034(2) 0.93330(17) 0.73985(15) 0.0291(4) Uani 1 1 d . . . F26A F 1.7771(2) 1.07537(16) 0.65309(17) 0.0377(4) Uani 1 1 d . . . F36A F 1.71399(19) 0.37813(18) 0.85046(15) 0.0301(4) Uani 1 1 d . . . F36B F 1.5071(2) 0.39468(19) 0.88919(15) 0.0338(4) Uani 1 1 d . . . F36C F 1.5746(3) 0.19374(17) 0.85162(16) 0.0419(5) Uani 1 1 d . . . F46C F 1.95507(18) 0.37558(16) 0.75779(14) 0.0245(3) Uani 1 1 d . . . F46B F 2.10246(19) 0.49586(17) 0.69736(16) 0.0311(4) Uani 1 1 d . . . F46A F 2.1020(2) 0.27448(19) 0.67094(16) 0.0325(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 0.01628(17) 0.01461(16) 0.01437(16) 0.00110(12) 0.00583(12) 0.00181(11) Cu2 0.01675(17) 0.01729(16) 0.01445(16) 0.00102(12) 0.00608(13) 0.00314(12) C1 0.0163(13) 0.0275(13) 0.0223(13) 0.0005(11) 0.0021(11) 0.0045(10) C2 0.0215(14) 0.0274(13) 0.0240(14) -0.0007(11) -0.0019(11) 0.0067(11) C3 0.0366(16) 0.0207(12) 0.0159(12) 0.0017(10) 0.0057(11) 0.0102(11) C4 0.0276(14) 0.0187(12) 0.0173(12) 0.0034(10) 0.0077(11) 0.0049(10) C13 0.0208(13) 0.0172(11) 0.0220(12) 0.0050(10) 0.0132(11) 0.0031(9) C16 0.0219(13) 0.0239(13) 0.0235(13) 0.0011(11) 0.0125(11) 0.0047(10) C23 0.0214(13) 0.0162(11) 0.0224(13) 0.0027(10) 0.0134(11) 0.0027(10) C26 0.0226(13) 0.0169(11) 0.0245(13) 0.0016(10) 0.0127(11) 0.0022(10) C33 0.0212(13) 0.0166(11) 0.0215(12) 0.0055(10) 0.0120(10) 0.0047(9) C34 0.0269(14) 0.0156(11) 0.0241(13) 0.0056(10) 0.0142(11) 0.0045(10) C36 0.0292(14) 0.0200(12) 0.0239(13) 0.0090(10) 0.0134(11) 0.0070(10) C43 0.0200(12) 0.0192(11) 0.0213(12) 0.0090(10) 0.0125(10) 0.0046(10) C44 0.0205(13) 0.0196(12) 0.0252(13) 0.0069(10) 0.0136(11) 0.0059(10) C46 0.0220(13) 0.0262(13) 0.0246(13) 0.0108(11) 0.0138(11) 0.0091(10) N1 0.0178(10) 0.0123(9) 0.0151(9) 0.0020(7) 0.0055(8) 0.0020(8) N2 0.0184(10) 0.0169(9) 0.0175(10) 0.0027(8) 0.0075(8) 0.0048(8) N11 0.0170(10) 0.0156(9) 0.0160(10) 0.0041(8) 0.0079(8) 0.0028(8) N21 0.0174(10) 0.0163(9) 0.0160(10) 0.0015(8) 0.0068(8) 0.0031(8) N31 0.0178(10) 0.0155(9) 0.0152(10) 0.0017(8) 0.0066(8) 0.0025(8) N41 0.0164(10) 0.0172(9) 0.0165(10) 0.0045(8) 0.0086(8) 0.0027(8) F16C 0.0216(8) 0.0240(8) 0.0274(8) -0.0018(6) 0.0097(7) -0.0021(6) F16B 0.0500(12) 0.0503(11) 0.0195(8) 0.0029(8) 0.0147(8) -0.0182(9) F16A 0.0442(12) 0.0492(11) 0.0374(10) -0.0167(9) 0.0043(9) 0.0299(9) F26C 0.0196(8) 0.0372(9) 0.0294(9) -0.0086(7) 0.0054(7) 0.0027(7) F26B 0.0327(9) 0.0273(8) 0.0225(8) -0.0029(6) 0.0164(7) -0.0012(7) F26A 0.0575(12) 0.0128(7) 0.0323(9) 0.0008(6) 0.0136(9) -0.0032(7) F36A 0.0240(8) 0.0375(9) 0.0253(8) 0.0105(7) 0.0058(7) 0.0056(7) F36B 0.0372(10) 0.0446(10) 0.0200(8) 0.0041(7) 0.0156(7) 0.0136(8) F36C 0.0664(13) 0.0250(8) 0.0277(9) 0.0150(7) 0.0070(9) 0.0050(8) F46C 0.0260(8) 0.0309(8) 0.0201(7) 0.0100(6) 0.0117(6) 0.0077(6) F46B 0.0253(9) 0.0337(9) 0.0295(8) 0.0127(7) 0.0064(7) -0.0040(7) F46A 0.0297(9) 0.0420(9) 0.0309(9) 0.0144(7) 0.0120(7) 0.0213(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 N11 1.945(2) . ? Cu1 N1 1.951(2) . ? Cu1 N31 1.976(2) . ? Cu1 Cu2 2.9398(5) . ? Cu2 N41 1.962(2) . ? Cu2 N2 1.963(2) . ? Cu2 N21 1.987(2) . ? C1 N2 1.331(3) . ? C1 C2 1.387(4) . ? C1 H1A 0.9500 . ? C2 C3 1.367(4) . ? C2 H2A 0.9500 . ? C3 C4 1.389(4) . ? C3 H3A 0.9500 . ? C4 N1 1.331(3) . ? C4 H4A 0.9500 . ? C13 N11 1.345(3) . ? C13 C44 1.373(4) 2_866 ? C13 C16 1.493(4) . ? C16 F16A 1.331(3) . ? C16 F16C 1.330(3) . ? C16 F16B 1.346(3) . ? C23 N21 1.348(3) . ? C23 C34 1.380(4) 2_866 ? C23 C26 1.481(3) . ? C26 F26A 1.335(3) . ? C26 F26B 1.340(3) . ? C26 F26C 1.347(3) . ? C33 N31 1.345(3) . ? C33 C34 1.388(3) . ? C33 C36 1.476(4) . ? C34 C23 1.380(4) 2_866 ? C34 H34A 0.9500 . ? C36 F36C 1.332(3) . ? C36 F36B 1.345(3) . ? C36 F36A 1.348(3) . ? C43 N41 1.349(3) . ? C43 C44 1.376(3) . ? C43 C46 1.490(4) . ? C44 C13 1.373(4) 2_866 ? C44 H44A 0.9500 . ? C46 F46B 1.340(3) . ? C46 F46C 1.344(3) . ? C46 F46A 1.342(3) . ? N1 N2 1.353(3) . ? N11 N41 1.354(3) 2_866 ? N21 N31 1.357(3) 2_866 ? N31 N21 1.357(3) 2_866 ? N41 N11 1.354(3) 2_866 ? 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 N11 Cu1 N1 130.08(8) . . ? N11 Cu1 N31 113.06(8) . . ? N1 Cu1 N31 116.85(8) . . ? N11 Cu1 Cu2 116.76(6) . . ? N1 Cu1 Cu2 66.59(6) . . ? N31 Cu1 Cu2 87.83(6) . . ? N41 Cu2 N2 128.53(8) . . ? N41 Cu2 N21 114.24(8) . . ? N2 Cu2 N21 117.11(8) . . ? N41 Cu2 Cu1 119.43(6) . . ? N2 Cu2 Cu1 65.51(6) . . ? N21 Cu2 Cu1 89.00(6) . . ? N2 C1 C2 123.4(3) . . ? N2 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C3 C2 C1 117.5(3) . . ? C3 C2 H2A 121.3 . . ? C1 C2 H2A 121.3 . . ? C2 C3 C4 117.8(2) . . ? C2 C3 H3A 121.1 . . ? C4 C3 H3A 121.1 . . ? N1 C4 C3 122.8(3) . . ? N1 C4 H4A 118.6 . . ? C3 C4 H4A 118.6 . . ? N11 C13 C44 111.5(2) . 2_866 ? N11 C13 C16 120.5(2) . . ? C44 C13 C16 127.8(2) 2_866 . ? F16A C16 F16C 107.2(2) . . ? F16A C16 F16B 106.8(2) . . ? F16C C16 F16B 104.8(2) . . ? F16A C16 C13 111.1(2) . . ? F16C C16 C13 114.4(2) . . ? F16B C16 C13 112.1(2) . . ? N21 C23 C34 111.3(2) . 2_866 ? N21 C23 C26 121.1(2) . . ? C34 C23 C26 127.6(2) 2_866 . ? F26A C26 F26B 106.3(2) . . ? F26A C26 F26C 106.7(2) . . ? F26B C26 F26C 105.2(2) . . ? F26A C26 C23 111.6(2) . . ? F26B C26 C23 113.3(2) . . ? F26C C26 C23 113.2(2) . . ? N31 C33 C34 110.7(2) . . ? N31 C33 C36 121.0(2) . . ? C34 C33 C36 128.3(2) . . ? C23 C34 C33 103.0(2) 2_866 . ? C23 C34 H34A 128.5 2_866 . ? C33 C34 H34A 128.5 . . ? F36C C36 F36B 107.4(2) . . ? F36C C36 F36A 105.9(2) . . ? F36B C36 F36A 105.1(2) . . ? F36C C36 C33 111.8(2) . . ? F36B C36 C33 112.6(2) . . ? F36A C36 C33 113.5(2) . . ? N41 C43 C44 111.3(2) . . ? N41 C43 C46 120.9(2) . . ? C44 C43 C46 127.8(2) . . ? C13 C44 C43 102.9(2) 2_866 . ? C13 C44 H44A 128.5 2_866 . ? C43 C44 H44A 128.5 . . ? F46B C46 F46C 105.7(2) . . ? F46B C46 F46A 107.1(2) . . ? F46C C46 F46A 106.6(2) . . ? F46B C46 C43 112.7(2) . . ? F46C C46 C43 113.3(2) . . ? F46A C46 C43 110.9(2) . . ? C4 N1 N2 119.6(2) . . ? C4 N1 Cu1 127.18(18) . . ? N2 N1 Cu1 113.16(15) . . ? C1 N2 N1 118.9(2) . . ? C1 N2 Cu2 126.47(19) . . ? N1 N2 Cu2 114.55(15) . . ? C13 N11 N41 107.2(2) . 2_866 ? C13 N11 Cu1 132.70(17) . . ? N41 N11 Cu1 119.88(15) 2_866 . ? C23 N21 N31 107.0(2) . 2_866 ? C23 N21 Cu2 133.80(17) . . ? N31 N21 Cu2 118.73(15) 2_866 . ? C33 N31 N21 107.94(19) . 2_866 ? C33 N31 Cu1 132.16(17) . . ? N21 N31 Cu1 119.90(15) 2_866 . ? C43 N41 N11 107.10(19) . 2_866 ? C43 N41 Cu2 132.57(17) . . ? N11 N41 Cu2 119.89(15) 2_866 . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.459 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.075 #===END data_rd5001 _database_code_depnum_ccdc_archive 'CCDC 257595' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((3,5-(CF3)2PzAg)4(C4H4N2)2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H12 Ag4 F24 N12' _chemical_formula_weight 1403.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.142(2) _cell_length_b 22.807(3) _cell_length_c 10.0462(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.477(2) _cell_angle_gamma 90.00 _cell_volume 4024.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 101(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 2.071 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 101(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22956 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6991 _reflns_number_gt 6417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0430P)^2^+7.1648P] 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 6991 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.484990(15) 0.580908(12) -0.16061(3) 0.02020(9) Uani 1 1 d . . . Ag2 Ag -0.355622(15) 0.487372(11) 0.08503(3) 0.01909(8) Uani 1 1 d . . . Ag4 Ag 0.136167(15) 0.534027(12) 0.05640(3) 0.02055(9) Uani 1 1 d . . . Ag3 Ag 0.031861(15) 0.403682(12) -0.09653(3) 0.02235(9) Uani 1 1 d . . . N1 N -0.45080(17) 0.44253(13) -0.0946(3) 0.0198(7) Uani 1 1 d . . . N4 N 0.03127(17) 0.54491(13) -0.1472(3) 0.0210(7) Uani 1 1 d . . . F27C F -0.19608(13) 0.42831(11) 0.1890(2) 0.0316(5) Uani 1 1 d . . . N12 N -0.33496(17) 0.58055(12) 0.0694(3) 0.0171(6) Uani 1 1 d . . . F37C F 0.32889(14) 0.50461(11) 0.2287(3) 0.0372(6) Uani 1 1 d . . . F17C F -0.39302(13) 0.72328(10) -0.1980(2) 0.0310(5) Uani 1 1 d . . . N2 N -0.49667(17) 0.47738(14) -0.1883(3) 0.0209(7) Uani 1 1 d . . . F36C F 0.14058(15) 0.28839(11) -0.0852(3) 0.0412(6) Uani 1 1 d . . . N22 N -0.60130(17) 0.60398(13) -0.2794(3) 0.0207(7) Uani 1 1 d . . . F17B F -0.47837(13) 0.72037(11) -0.0842(3) 0.0347(6) Uani 1 1 d . . . F47C F -0.31224(14) 0.29796(12) -0.1645(3) 0.0442(7) Uani 1 1 d . . . F27B F -0.16086(13) 0.44356(11) 0.4064(3) 0.0346(6) Uani 1 1 d . . . N31 N 0.17780(17) 0.44712(13) 0.1133(3) 0.0191(6) Uani 1 1 d . . . N32 N 0.14218(17) 0.39917(13) 0.0476(3) 0.0202(7) Uani 1 1 d . . . N21 N -0.33689(16) 0.41670(13) 0.2408(3) 0.0185(6) Uani 1 1 d . . . F16C F -0.25364(15) 0.56219(13) 0.3620(3) 0.0457(7) Uani 1 1 d . . . N3 N -0.00313(18) 0.49610(14) -0.2062(3) 0.0236(7) Uani 1 1 d . . . F46C F -0.08371(16) 0.25189(14) -0.4298(3) 0.0522(8) Uani 1 1 d . . . F47B F -0.28821(14) 0.38799(11) -0.1006(3) 0.0455(7) Uani 1 1 d . . . F47A F -0.24376(14) 0.31819(13) 0.0352(3) 0.0427(6) Uani 1 1 d . . . F17A F -0.37783(16) 0.77272(10) -0.0106(3) 0.0423(7) Uani 1 1 d . . . F37B F 0.25684(15) 0.50683(12) 0.3669(3) 0.0459(7) Uani 1 1 d . . . F27A F -0.15305(13) 0.35731(10) 0.3272(3) 0.0415(7) Uani 1 1 d . . . F46B F 0.00192(15) 0.31733(11) -0.3537(3) 0.0454(7) Uani 1 1 d . . . F37A F 0.34554(16) 0.44245(12) 0.3929(3) 0.0508(8) Uani 1 1 d . . . C33 C 0.1830(2) 0.35215(16) 0.1036(4) 0.0243(8) Uani 1 1 d . . . N42 N -0.07790(17) 0.35866(13) -0.1745(3) 0.0218(7) Uani 1 1 d . . . N11 N -0.38346(16) 0.61596(13) -0.0222(3) 0.0170(6) Uani 1 1 d . . . C14 C -0.3007(2) 0.67410(16) 0.1241(4) 0.0230(8) Uani 1 1 d . . . H14A H -0.2747 0.7077 0.1684 0.028 Uiso 1 1 calc R . . F16B F -0.18073(14) 0.55219(11) 0.2285(3) 0.0391(6) Uani 1 1 d . . . C44 C -0.1695(2) 0.29041(16) -0.2358(4) 0.0225(8) Uani 1 1 d . . . H44A H -0.1974 0.2568 -0.2758 0.027 Uiso 1 1 calc R . . C13 C -0.2855(2) 0.61598(16) 0.1559(4) 0.0209(8) Uani 1 1 d . . . C34 C 0.2452(2) 0.36825(17) 0.2068(4) 0.0249(8) Uani 1 1 d . . . H34A H 0.2828 0.3437 0.2627 0.030 Uiso 1 1 calc R . . C3 C -0.5478(2) 0.45355(17) -0.2913(4) 0.0227(8) Uani 1 1 d . . . H3A H -0.5793 0.4788 -0.3569 0.027 Uiso 1 1 calc R . . C6 C -0.4581(2) 0.38438(16) -0.1076(4) 0.0214(8) Uani 1 1 d . . . H6A H -0.4255 0.3602 -0.0412 0.026 Uiso 1 1 calc R . . C25 C -0.2753(2) 0.39136(15) 0.3225(4) 0.0191(7) Uani 1 1 d . . . C15 C -0.3627(2) 0.67170(15) 0.0119(4) 0.0193(8) Uani 1 1 d . . . C23 C -0.6266(2) 0.64162(17) -0.3839(4) 0.0241(8) Uani 1 1 d . . . C24 C -0.2951(2) 0.35379(17) 0.4160(4) 0.0249(8) Uani 1 1 d . . . H24A H -0.2628 0.3306 0.4852 0.030 Uiso 1 1 calc R . . F16A F -0.17869(18) 0.63239(11) 0.3364(3) 0.0637(10) Uani 1 1 d . . . C17 C -0.4026(2) 0.72130(16) -0.0701(4) 0.0257(9) Uani 1 1 d . . . F36B F 0.21539(18) 0.25380(11) 0.0951(3) 0.0564(8) Uani 1 1 d . . . C47 C -0.2587(2) 0.33453(17) -0.0982(4) 0.0271(9) Uani 1 1 d . . . C27 C -0.1966(2) 0.40516(16) 0.3107(4) 0.0232(8) Uani 1 1 d . . . C4 C -0.5577(2) 0.39325(18) -0.3082(4) 0.0271(9) Uani 1 1 d . . . H4A H -0.5954 0.3774 -0.3827 0.033 Uiso 1 1 calc R . . F36A F 0.0978(2) 0.27435(14) 0.0898(4) 0.0741(11) Uani 1 1 d . . . C37 C 0.2921(2) 0.47035(18) 0.2980(4) 0.0267(9) Uani 1 1 d . . . F46A F -0.00306(15) 0.23905(11) -0.2390(3) 0.0432(7) Uani 1 1 d . . . N41 N -0.13538(17) 0.37386(13) -0.1164(3) 0.0214(7) Uani 1 1 d . . . F26C F -0.55387(19) 0.72683(13) -0.3879(4) 0.0611(9) Uani 1 1 d . . . F26B F -0.50540(16) 0.64727(14) -0.4293(3) 0.0564(8) Uani 1 1 d . . . C35 C 0.2397(2) 0.42848(17) 0.2093(4) 0.0215(8) Uani 1 1 d . . . C45 C -0.1898(2) 0.33250(15) -0.1539(4) 0.0202(8) Uani 1 1 d . . . F26A F -0.59938(19) 0.6831(2) -0.5776(3) 0.0833(13) Uani 1 1 d . . . C43 C -0.0986(2) 0.30890(15) -0.2458(4) 0.0217(8) Uani 1 1 d . . . C46 C -0.0459(2) 0.27988(17) -0.3178(4) 0.0294(9) Uani 1 1 d . . . C9 C 0.0116(2) 0.59631(17) -0.2101(4) 0.0268(9) Uani 1 1 d . . . H9A H 0.0360 0.6308 -0.1677 0.032 Uiso 1 1 calc R . . C5 C -0.5115(2) 0.35778(17) -0.2140(4) 0.0254(8) Uani 1 1 d . . . H5A H -0.5155 0.3163 -0.2209 0.030 Uiso 1 1 calc R . . C12 C -0.0551(3) 0.49944(19) -0.3240(5) 0.0357(10) Uani 1 1 d . . . H12A H -0.0788 0.4643 -0.3639 0.043 Uiso 1 1 calc R . . C26 C -0.5728(2) 0.6739(2) -0.4473(4) 0.0330(10) Uani 1 1 d . . . C10 C -0.0423(3) 0.60173(19) -0.3333(5) 0.0380(11) Uani 1 1 d . . . H10A H -0.0549 0.6389 -0.3754 0.046 Uiso 1 1 calc R . . C11 C -0.0768(3) 0.5519(2) -0.3924(5) 0.0468(13) Uani 1 1 d . . . H11A H -0.1144 0.5530 -0.4774 0.056 Uiso 1 1 calc R . . C36 C 0.1585(3) 0.29229(18) 0.0530(5) 0.0355(10) Uani 1 1 d . . . C16 C -0.2254(2) 0.59090(16) 0.2702(4) 0.0274(9) 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 Ag1 0.01652(15) 0.02391(16) 0.02004(16) 0.00148(11) 0.00433(12) -0.00076(10) Ag2 0.01941(15) 0.01561(14) 0.02282(16) 0.00377(10) 0.00634(12) -0.00007(10) Ag4 0.02069(16) 0.01687(15) 0.02489(17) -0.00089(11) 0.00723(12) 0.00167(10) Ag3 0.01750(15) 0.02436(16) 0.02543(17) -0.00371(12) 0.00580(12) -0.00099(11) N1 0.0166(15) 0.0215(16) 0.0229(17) 0.0002(13) 0.0079(13) -0.0006(12) N4 0.0201(16) 0.0181(15) 0.0246(18) -0.0003(13) 0.0049(14) -0.0012(12) F27C 0.0244(12) 0.0431(14) 0.0292(13) 0.0045(11) 0.0101(10) -0.0048(10) N12 0.0163(15) 0.0164(15) 0.0180(16) 0.0024(12) 0.0029(13) 0.0009(11) F37C 0.0352(14) 0.0426(14) 0.0337(14) 0.0014(11) 0.0083(12) -0.0154(11) F17C 0.0362(13) 0.0319(12) 0.0279(13) 0.0122(10) 0.0137(11) 0.0093(10) N2 0.0186(16) 0.0250(16) 0.0195(17) 0.0002(13) 0.0055(14) 0.0012(13) F36C 0.0414(15) 0.0301(13) 0.0484(17) -0.0076(12) 0.0045(13) -0.0055(11) N22 0.0200(16) 0.0198(15) 0.0228(17) 0.0036(13) 0.0062(14) -0.0002(12) F17B 0.0290(13) 0.0354(13) 0.0418(15) 0.0114(11) 0.0128(11) 0.0148(10) F47C 0.0300(14) 0.0565(17) 0.0482(17) -0.0149(13) 0.0138(12) -0.0232(12) F27B 0.0292(13) 0.0383(14) 0.0325(14) -0.0048(11) 0.0003(11) -0.0110(11) N31 0.0181(15) 0.0191(15) 0.0209(17) 0.0013(13) 0.0063(13) 0.0012(12) N32 0.0189(16) 0.0211(16) 0.0211(17) 0.0014(13) 0.0062(14) 0.0004(12) N21 0.0159(15) 0.0182(15) 0.0212(17) 0.0038(12) 0.0043(13) -0.0005(12) F16C 0.0405(15) 0.0691(19) 0.0283(14) 0.0231(13) 0.0104(12) 0.0124(13) N3 0.0220(16) 0.0210(16) 0.0261(19) -0.0019(13) 0.0026(15) -0.0016(13) F46C 0.0428(16) 0.0681(19) 0.0453(17) -0.0337(15) 0.0105(14) -0.0001(14) F47B 0.0330(14) 0.0328(14) 0.079(2) 0.0133(13) 0.0299(14) 0.0101(11) F47A 0.0421(15) 0.0572(17) 0.0322(15) 0.0063(12) 0.0155(12) 0.0029(12) F17A 0.0585(17) 0.0152(11) 0.0447(16) 0.0015(11) -0.0028(14) 0.0037(11) F37B 0.0439(16) 0.0529(17) 0.0443(17) -0.0237(13) 0.0172(13) -0.0070(13) F27A 0.0216(12) 0.0295(13) 0.074(2) 0.0061(13) 0.0131(13) 0.0065(10) F46B 0.0508(16) 0.0330(14) 0.0658(19) -0.0092(13) 0.0394(15) -0.0023(12) F37A 0.0441(16) 0.0456(16) 0.0448(17) 0.0075(13) -0.0223(14) -0.0024(13) C33 0.023(2) 0.0224(19) 0.029(2) 0.0047(16) 0.0081(17) -0.0006(15) N42 0.0187(16) 0.0199(15) 0.0270(18) -0.0026(13) 0.0061(14) 0.0006(12) N11 0.0149(15) 0.0190(15) 0.0180(16) 0.0018(12) 0.0058(13) 0.0003(12) C14 0.026(2) 0.0174(18) 0.026(2) -0.0026(15) 0.0069(17) -0.0027(15) F16B 0.0333(14) 0.0456(15) 0.0387(15) 0.0132(12) 0.0094(12) 0.0162(12) C44 0.023(2) 0.0194(18) 0.023(2) -0.0009(15) 0.0013(16) -0.0030(15) C13 0.0218(19) 0.0207(18) 0.020(2) 0.0023(15) 0.0042(16) -0.0002(15) C34 0.024(2) 0.025(2) 0.026(2) 0.0089(16) 0.0075(17) 0.0061(16) C3 0.0203(19) 0.027(2) 0.021(2) -0.0021(16) 0.0041(16) 0.0020(15) C6 0.0191(18) 0.0195(18) 0.028(2) 0.0034(15) 0.0108(17) 0.0025(14) C25 0.0197(19) 0.0170(17) 0.0188(19) -0.0002(14) 0.0017(15) 0.0004(14) C15 0.0188(18) 0.0184(18) 0.023(2) 0.0036(15) 0.0089(16) 0.0015(14) C23 0.027(2) 0.026(2) 0.020(2) 0.0042(16) 0.0060(17) -0.0024(16) C24 0.024(2) 0.029(2) 0.021(2) 0.0064(16) 0.0026(17) 0.0018(16) F16A 0.067(2) 0.0262(14) 0.068(2) 0.0020(14) -0.0407(17) -0.0075(13) C17 0.032(2) 0.0186(19) 0.028(2) 0.0033(16) 0.0097(18) 0.0023(16) F36B 0.067(2) 0.0246(14) 0.067(2) 0.0045(13) -0.0021(17) 0.0084(13) C47 0.024(2) 0.026(2) 0.029(2) 0.0007(17) 0.0049(18) -0.0007(16) C27 0.0177(19) 0.0227(19) 0.026(2) 0.0008(16) 0.0007(17) 0.0005(15) C4 0.027(2) 0.029(2) 0.025(2) -0.0102(17) 0.0066(18) -0.0034(16) F36A 0.088(2) 0.0509(18) 0.107(3) -0.0169(19) 0.068(2) -0.0408(18) C37 0.025(2) 0.032(2) 0.022(2) 0.0027(17) 0.0030(17) 0.0025(16) F46A 0.0426(15) 0.0339(14) 0.0558(18) -0.0006(12) 0.0174(13) 0.0177(12) N41 0.0188(16) 0.0207(16) 0.0252(18) -0.0024(13) 0.0062(14) 0.0016(12) F26C 0.070(2) 0.0481(18) 0.077(2) -0.0018(16) 0.0403(19) -0.0244(16) F26B 0.0447(17) 0.067(2) 0.069(2) 0.0208(16) 0.0356(16) 0.0024(14) C35 0.0202(19) 0.0275(19) 0.019(2) 0.0039(15) 0.0088(16) 0.0013(15) C45 0.0173(18) 0.0175(17) 0.023(2) 0.0013(15) 0.0006(16) -0.0005(14) F26A 0.057(2) 0.151(4) 0.0361(18) 0.041(2) 0.0007(15) -0.043(2) C43 0.0236(19) 0.0150(17) 0.025(2) -0.0020(15) 0.0037(16) 0.0028(14) C46 0.030(2) 0.025(2) 0.035(2) -0.0095(18) 0.0094(19) -0.0040(17) C9 0.026(2) 0.025(2) 0.030(2) 0.0055(17) 0.0089(18) -0.0007(16) C5 0.026(2) 0.0206(19) 0.032(2) -0.0059(16) 0.0115(18) -0.0024(15) C12 0.039(3) 0.030(2) 0.032(3) -0.0027(19) -0.003(2) -0.0075(19) C26 0.033(2) 0.041(3) 0.026(2) 0.0113(19) 0.0104(19) -0.0032(19) C10 0.038(3) 0.030(2) 0.039(3) 0.0121(19) -0.003(2) 0.0005(19) C11 0.052(3) 0.038(3) 0.034(3) 0.007(2) -0.018(2) -0.005(2) C36 0.035(2) 0.022(2) 0.048(3) 0.0087(19) 0.006(2) 0.0004(18) C16 0.030(2) 0.0180(19) 0.030(2) 0.0003(16) -0.0011(19) -0.0044(16) _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 Ag1 N11 2.165(3) . ? Ag1 N22 2.212(3) . ? Ag1 N2 2.381(3) . ? Ag2 N12 2.170(3) . ? Ag2 N21 2.213(3) . ? Ag2 N1 2.393(3) . ? Ag4 N31 2.147(3) . ? Ag4 N41 2.186(3) 3_565 ? Ag4 N4 2.433(3) . ? Ag3 N32 2.160(3) . ? Ag3 N42 2.203(3) . ? Ag3 N3 2.389(3) . ? N1 C6 1.336(5) . ? N1 N2 1.348(4) . ? N4 C9 1.337(5) . ? N4 N3 1.340(4) . ? F27C C27 1.335(5) . ? N12 C13 1.351(5) . ? N12 N11 1.367(4) . ? F37C C37 1.332(5) . ? F17C C17 1.340(5) . ? N2 C3 1.322(5) . ? F36C C36 1.347(5) . ? N22 C23 1.345(5) . ? N22 N21 1.359(4) 3_465 ? F17B C17 1.346(5) . ? F47C C47 1.326(5) . ? F27B C27 1.341(5) . ? N31 C35 1.353(5) . ? N31 N32 1.355(4) . ? N32 C33 1.344(5) . ? N21 C25 1.341(5) . ? N21 N22 1.359(4) 3_465 ? F16C C16 1.334(5) . ? N3 C12 1.318(6) . ? F46C C46 1.326(5) . ? F47B C47 1.329(5) . ? F47A C47 1.352(5) . ? F17A C17 1.341(5) . ? F37B C37 1.342(5) . ? F27A C27 1.333(4) . ? F46B C46 1.330(5) . ? F37A C37 1.339(5) . ? C33 C34 1.378(6) . ? C33 C36 1.485(6) . ? N42 C43 1.344(5) . ? N42 N41 1.361(4) . ? N11 C15 1.345(5) . ? C14 C13 1.375(5) . ? C14 C15 1.381(5) . ? F16B C16 1.335(5) . ? C44 C45 1.373(5) . ? C44 C43 1.382(5) . ? C13 C16 1.485(6) . ? C34 C35 1.378(5) . ? C3 C4 1.392(6) . ? C6 C5 1.389(6) . ? C25 C24 1.383(5) . ? C25 C27 1.496(5) . ? C15 C17 1.478(5) . ? C23 C24 1.380(5) 3_465 ? C23 C26 1.488(5) . ? C24 C23 1.380(5) 3_465 ? F16A C16 1.332(5) . ? F36B C36 1.340(5) . ? C47 C45 1.492(5) . ? C4 C5 1.363(6) . ? F36A C36 1.313(5) . ? C37 C35 1.478(6) . ? F46A C46 1.338(5) . ? N41 C45 1.349(5) . ? N41 Ag4 2.186(3) 3_565 ? F26C C26 1.352(5) . ? F26B C26 1.336(5) . ? F26A C26 1.294(5) . ? C43 C46 1.490(5) . ? C9 C10 1.378(6) . ? C12 C11 1.387(6) . ? C10 C11 1.361(7) . ? 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 N11 Ag1 N22 143.36(11) . . ? N11 Ag1 N2 118.55(11) . . ? N22 Ag1 N2 97.35(11) . . ? N12 Ag2 N21 139.97(11) . . ? N12 Ag2 N1 117.97(11) . . ? N21 Ag2 N1 100.15(11) . . ? N31 Ag4 N41 147.09(12) . 3_565 ? N31 Ag4 N4 117.85(11) . . ? N41 Ag4 N4 94.36(11) 3_565 . ? N32 Ag3 N42 145.08(11) . . ? N32 Ag3 N3 116.49(11) . . ? N42 Ag3 N3 97.75(11) . . ? C6 N1 N2 119.2(3) . . ? C6 N1 Ag2 122.2(2) . . ? N2 N1 Ag2 118.5(2) . . ? C9 N4 N3 118.7(3) . . ? C9 N4 Ag4 123.1(3) . . ? N3 N4 Ag4 117.8(2) . . ? C13 N12 N11 107.0(3) . . ? C13 N12 Ag2 129.7(2) . . ? N11 N12 Ag2 122.2(2) . . ? C3 N2 N1 119.6(3) . . ? C3 N2 Ag1 121.6(3) . . ? N1 N2 Ag1 118.8(2) . . ? C23 N22 N21 107.4(3) . 3_465 ? C23 N22 Ag1 131.8(2) . . ? N21 N22 Ag1 120.5(2) 3_465 . ? C35 N31 N32 107.7(3) . . ? C35 N31 Ag4 130.8(3) . . ? N32 N31 Ag4 121.5(2) . . ? C33 N32 N31 107.1(3) . . ? C33 N32 Ag3 129.8(3) . . ? N31 N32 Ag3 122.5(2) . . ? C25 N21 N22 107.2(3) . 3_465 ? C25 N21 Ag2 134.8(2) . . ? N22 N21 Ag2 117.6(2) 3_465 . ? C12 N3 N4 119.9(3) . . ? C12 N3 Ag3 120.9(3) . . ? N4 N3 Ag3 119.2(2) . . ? N32 C33 C34 111.4(3) . . ? N32 C33 C36 120.3(4) . . ? C34 C33 C36 128.4(4) . . ? C43 N42 N41 107.6(3) . . ? C43 N42 Ag3 133.6(2) . . ? N41 N42 Ag3 116.7(2) . . ? C15 N11 N12 107.2(3) . . ? C15 N11 Ag1 130.6(2) . . ? N12 N11 Ag1 121.0(2) . . ? C13 C14 C15 103.1(3) . . ? C45 C44 C43 103.0(3) . . ? N12 C13 C14 111.4(3) . . ? N12 C13 C16 120.5(3) . . ? C14 C13 C16 128.1(4) . . ? C33 C34 C35 103.3(3) . . ? N2 C3 C4 123.1(4) . . ? N1 C6 C5 122.8(4) . . ? N21 C25 C24 111.5(3) . . ? N21 C25 C27 121.8(3) . . ? C24 C25 C27 126.8(3) . . ? N11 C15 C14 111.4(3) . . ? N11 C15 C17 121.0(3) . . ? C14 C15 C17 127.6(3) . . ? N22 C23 C24 111.2(3) . 3_465 ? N22 C23 C26 121.1(4) . . ? C24 C23 C26 127.6(4) 3_465 . ? C23 C24 C25 102.7(3) 3_465 . ? F17C C17 F17A 106.7(3) . . ? F17C C17 F17B 105.8(3) . . ? F17A C17 F17B 106.3(3) . . ? F17C C17 C15 113.4(3) . . ? F17A C17 C15 111.0(3) . . ? F17B C17 C15 113.0(3) . . ? F47C C47 F47B 109.1(3) . . ? F47C C47 F47A 105.3(3) . . ? F47B C47 F47A 104.5(3) . . ? F47C C47 C45 111.7(3) . . ? F47B C47 C45 113.1(3) . . ? F47A C47 C45 112.6(3) . . ? F27A C27 F27C 107.3(3) . . ? F27A C27 F27B 106.3(3) . . ? F27C C27 F27B 106.6(3) . . ? F27A C27 C25 111.5(3) . . ? F27C C27 C25 112.4(3) . . ? F27B C27 C25 112.4(3) . . ? C5 C4 C3 117.6(4) . . ? F37C C37 F37A 106.4(3) . . ? F37C C37 F37B 105.8(3) . . ? F37A C37 F37B 106.3(3) . . ? F37C C37 C35 113.2(3) . . ? F37A C37 C35 111.4(3) . . ? F37B C37 C35 113.2(3) . . ? C45 N41 N42 106.7(3) . . ? C45 N41 Ag4 133.9(2) . 3_565 ? N42 N41 Ag4 114.9(2) . 3_565 ? N31 C35 C34 110.6(3) . . ? N31 C35 C37 121.4(3) . . ? C34 C35 C37 128.1(4) . . ? N41 C45 C44 111.7(3) . . ? N41 C45 C47 119.8(3) . . ? C44 C45 C47 128.4(3) . . ? N42 C43 C44 111.1(3) . . ? N42 C43 C46 120.4(3) . . ? C44 C43 C46 128.4(3) . . ? F46C C46 F46B 108.2(4) . . ? F46C C46 F46A 105.5(3) . . ? F46B C46 F46A 106.6(3) . . ? F46C C46 C43 111.6(3) . . ? F46B C46 C43 112.8(3) . . ? F46A C46 C43 111.7(4) . . ? N4 C9 C10 123.3(4) . . ? C4 C5 C6 117.7(4) . . ? N3 C12 C11 123.1(4) . . ? F26A C26 F26B 107.9(4) . . ? F26A C26 F26C 106.9(4) . . ? F26B C26 F26C 102.9(4) . . ? F26A C26 C23 113.2(4) . . ? F26B C26 C23 113.2(3) . . ? F26C C26 C23 112.0(4) . . ? C11 C10 C9 117.6(4) . . ? C10 C11 C12 117.5(4) . . ? F36A C36 F36B 109.9(4) . . ? F36A C36 F36C 105.4(4) . . ? F36B C36 F36C 104.5(4) . . ? F36A C36 C33 112.9(4) . . ? F36B C36 C33 110.7(4) . . ? F36C C36 C33 112.9(3) . . ? F16A C16 F16C 108.0(4) . . ? F16A C16 F16B 105.4(3) . . ? F16C C16 F16B 105.1(3) . . ? F16A C16 C13 111.4(3) . . ? F16C C16 C13 112.9(3) . . ? F16B C16 C13 113.5(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.369 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.133 #===END data_dias71s _database_code_depnum_ccdc_archive 'CCDC 257596' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((3,5-(CF3)2PzCu)3(C12H8N2)) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H13 Cl2 Cu3 F18 N8' _chemical_formula_weight 1064.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2674(14) _cell_length_b 15.769(2) _cell_length_c 23.946(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.060(2) _cell_angle_gamma 90.00 _cell_volume 3455.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7362 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.34 _exptl_crystal_description plates _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 2.119 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27148 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6798 _reflns_number_gt 5712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0496P)^2^+16.3200P] 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 0.00000(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6798 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 3.997 _refine_ls_shift/su_mean 0.008 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 0.40401(7) 0.12369(4) 0.22880(3) 0.02177(17) Uani 1 1 d . . . Cu2 Cu 0.36570(6) 0.13439(4) 0.35200(3) 0.02058(17) Uani 1 1 d . . . Cu3 Cu 0.16688(6) 0.24935(4) 0.26406(3) 0.02003(17) Uani 1 1 d . . . F11 F -0.1445(4) 0.3148(2) 0.28720(15) 0.0364(8) Uani 1 1 d . . . N2 N 0.5641(5) 0.1210(3) 0.33834(18) 0.0203(9) Uani 1 1 d . . . F18 F 0.0307(4) 0.3987(2) 0.19542(14) 0.0344(8) Uani 1 1 d . . . F12 F -0.1672(4) 0.3791(3) 0.36478(16) 0.0440(9) Uani 1 1 d . . . F5 F 0.6796(4) 0.2003(2) 0.45054(14) 0.0397(9) Uani 1 1 d . . . N1 N 0.5814(4) 0.1178(3) 0.28343(18) 0.0187(9) Uani 1 1 d . . . N3 N 0.2237(5) 0.2078(3) 0.37945(18) 0.0203(9) Uani 1 1 d . . . F10 F -0.0122(4) 0.4233(2) 0.31297(17) 0.0411(9) Uani 1 1 d . . . C26 C 0.1424(6) -0.0077(4) 0.3855(2) 0.0242(11) Uani 1 1 d . . . H26 H 0.2076 0.0298 0.4080 0.029 Uiso 1 1 calc R . . N4 N 0.1353(5) 0.2522(3) 0.33911(18) 0.0208(9) Uani 1 1 d . . . F16 F -0.0102(4) 0.4068(2) 0.10494(16) 0.0459(10) Uani 1 1 d . . . F6 F 0.6380(4) 0.0680(2) 0.45534(15) 0.0444(9) Uani 1 1 d . . . F8 F 0.1901(6) 0.1148(3) 0.49507(17) 0.0576(12) Uani 1 1 d . . . F9 F 0.2507(5) 0.2360(3) 0.52704(15) 0.0482(10) Uani 1 1 d . . . F4 F 0.8578(4) 0.1136(3) 0.45510(16) 0.0531(11) Uani 1 1 d . . . N6 N 0.3020(4) 0.1983(3) 0.17194(18) 0.0209(9) Uani 1 1 d . . . N8 N 0.2447(4) 0.0362(3) 0.30468(18) 0.0186(9) Uani 1 1 d . . . N5 N 0.1966(4) 0.2488(3) 0.18887(18) 0.0208(9) Uani 1 1 d . . . F17 F -0.1143(3) 0.3102(2) 0.14751(18) 0.0436(10) Uani 1 1 d . . . N7 N 0.2554(4) 0.0322(3) 0.25164(18) 0.0188(9) Uani 1 1 d . . . C23 C -0.0445(6) -0.1217(4) 0.3202(2) 0.0273(12) Uani 1 1 d . . . H23 H -0.1077 -0.1614 0.2989 0.033 Uiso 1 1 calc R . . C8 C 0.0419(6) 0.2969(4) 0.3653(2) 0.0268(12) Uani 1 1 d . . . F2 F 0.7362(5) 0.1734(3) 0.19335(18) 0.0610(13) Uani 1 1 d . . . C17 C 0.1954(6) -0.0268(4) 0.1593(2) 0.0260(12) Uani 1 1 d . . . H17 H 0.2598 0.0127 0.1461 0.031 Uiso 1 1 calc R . . C27 C 0.1477(5) -0.0172(3) 0.3274(2) 0.0201(10) Uani 1 1 d . . . F3 F 0.9280(3) 0.1132(3) 0.23523(16) 0.0402(9) Uani 1 1 d . . . C16 C 0.1752(5) -0.0263(3) 0.2160(2) 0.0200(10) Uani 1 1 d . . . C20 C 0.0029(6) -0.1424(4) 0.1972(2) 0.0258(12) Uani 1 1 d . . . H20 H -0.0627 -0.1819 0.2096 0.031 Uiso 1 1 calc R . . C18 C 0.1207(6) -0.0850(4) 0.1230(2) 0.0266(12) Uani 1 1 d . . . H18 H 0.1341 -0.0861 0.0844 0.032 Uiso 1 1 calc R . . C15 C 0.4041(6) 0.1702(4) 0.0846(2) 0.0294(13) Uani 1 1 d . . . C7 C 0.0673(6) 0.2836(4) 0.4225(2) 0.0271(12) Uani 1 1 d . . . H7 H 0.0176 0.3073 0.4506 0.033 Uiso 1 1 calc R . . C3 C 0.6995(6) 0.1183(3) 0.3700(2) 0.0227(11) Uani 1 1 d . . . C12 C 0.1989(6) 0.2762(4) 0.0970(2) 0.0255(12) Uani 1 1 d . . . H12 H 0.1772 0.2995 0.0600 0.031 Uiso 1 1 calc R . . F1 F 0.7471(5) 0.0397(3) 0.19815(18) 0.0598(13) Uani 1 1 d . . . C13 C 0.3020(6) 0.2150(4) 0.1170(2) 0.0231(11) Uani 1 1 d . . . C2 C 0.8042(6) 0.1134(4) 0.3357(2) 0.0260(12) Uani 1 1 d . . . H2 H 0.9072 0.1113 0.3468 0.031 Uiso 1 1 calc R . . C25 C 0.0411(6) -0.0535(4) 0.4091(2) 0.0265(12) Uani 1 1 d . . . H25 H 0.0355 -0.0473 0.4481 0.032 Uiso 1 1 calc R . . C11 C 0.1361(6) 0.2949(3) 0.1437(2) 0.0227(11) Uani 1 1 d . . . C14 C 0.0102(6) 0.3525(4) 0.1480(2) 0.0279(12) Uani 1 1 d . . . F13 F 0.4279(5) 0.0901(3) 0.10024(19) 0.0544(11) Uani 1 1 d . . . C19 C 0.0246(6) -0.1430(4) 0.1424(2) 0.0289(12) Uani 1 1 d . . . H19 H -0.0258 -0.1831 0.1169 0.035 Uiso 1 1 calc R . . C5 C 0.7163(6) 0.1245(4) 0.4324(2) 0.0276(12) Uani 1 1 d . . . C21 C 0.0772(5) -0.0831(3) 0.2362(2) 0.0201(11) Uani 1 1 d . . . C22 C 0.0584(5) -0.0759(3) 0.2940(2) 0.0209(11) Uani 1 1 d . . . C1 C 0.7275(5) 0.1124(3) 0.2818(2) 0.0206(11) Uani 1 1 d . . . C24 C -0.0532(6) -0.1089(4) 0.3760(2) 0.0279(12) Uani 1 1 d . . . H24 H -0.1251 -0.1385 0.3926 0.033 Uiso 1 1 calc R . . F14 F 0.5371(4) 0.2036(3) 0.0921(2) 0.0711(16) Uani 1 1 d . . . F7 F 0.3933(5) 0.1677(5) 0.48124(17) 0.086(2) Uani 1 1 d . . . F15 F 0.3581(6) 0.1710(4) 0.03063(17) 0.0796(18) Uani 1 1 d . . . C6 C 0.1842(6) 0.2268(4) 0.4294(2) 0.0230(11) Uani 1 1 d . . . C4 C 0.7821(6) 0.1103(4) 0.2275(2) 0.0250(12) Uani 1 1 d . . . C10 C -0.0707(6) 0.3539(4) 0.3329(3) 0.0277(12) Uani 1 1 d . . . C9 C 0.2572(6) 0.1864(4) 0.4830(2) 0.0300(13) Uani 1 1 d . . . Cl1 Cl 0.99165(18) 0.10232(12) 0.04221(8) 0.0468(4) Uani 1 1 d . . . Cl2 Cl 0.69847(19) 0.03011(13) 0.01966(9) 0.0547(5) Uani 1 1 d . . . C28 C 0.8361(8) 0.0728(5) 0.0716(3) 0.0434(16) Uani 1 1 d . . . H28A H 0.7972 0.1231 0.0890 0.052 Uiso 1 1 calc R . . H28B H 0.8643 0.0301 0.1016 0.052 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 0.0145(3) 0.0307(4) 0.0197(3) 0.0004(3) 0.0014(2) 0.0040(3) Cu2 0.0132(3) 0.0284(4) 0.0203(3) 0.0011(3) 0.0035(2) 0.0022(2) Cu3 0.0141(3) 0.0259(3) 0.0200(3) 0.0005(3) 0.0023(2) 0.0002(2) F11 0.0268(18) 0.040(2) 0.038(2) -0.0013(16) -0.0103(15) 0.0034(15) N2 0.016(2) 0.023(2) 0.021(2) 0.0008(18) -0.0012(17) 0.0007(17) F18 0.0319(18) 0.0354(19) 0.0349(19) -0.0065(15) 0.0028(15) 0.0064(15) F12 0.0248(18) 0.062(3) 0.046(2) -0.0034(19) 0.0087(16) 0.0189(17) F5 0.049(2) 0.040(2) 0.0289(19) -0.0091(16) 0.0012(16) 0.0003(17) N1 0.0125(19) 0.023(2) 0.022(2) -0.0034(17) 0.0058(16) 0.0013(16) N3 0.017(2) 0.026(2) 0.017(2) -0.0002(18) 0.0014(17) -0.0010(17) F10 0.0229(17) 0.0331(19) 0.065(3) 0.0094(18) -0.0003(17) 0.0040(14) C26 0.018(3) 0.027(3) 0.028(3) 0.003(2) 0.004(2) 0.001(2) N4 0.016(2) 0.025(2) 0.020(2) -0.0005(18) 0.0009(17) -0.0006(17) F16 0.052(2) 0.045(2) 0.040(2) 0.0162(18) 0.0051(18) 0.0239(19) F6 0.057(2) 0.047(2) 0.0293(19) 0.0047(17) 0.0076(17) -0.0135(19) F8 0.087(3) 0.043(2) 0.036(2) 0.0058(18) -0.010(2) -0.008(2) F9 0.073(3) 0.047(2) 0.0237(18) -0.0070(16) 0.0037(18) -0.009(2) F4 0.0224(18) 0.101(3) 0.032(2) 0.001(2) -0.0080(15) 0.016(2) N6 0.0118(19) 0.029(2) 0.023(2) 0.0037(19) 0.0040(17) 0.0005(17) N8 0.0105(19) 0.024(2) 0.022(2) 0.0021(18) 0.0038(16) 0.0015(16) N5 0.013(2) 0.026(2) 0.022(2) 0.0013(19) 0.0012(17) -0.0025(17) F17 0.0129(16) 0.045(2) 0.071(3) -0.0104(19) -0.0003(16) 0.0009(15) N7 0.0102(19) 0.023(2) 0.023(2) -0.0004(18) 0.0023(16) 0.0014(16) C23 0.015(2) 0.031(3) 0.036(3) 0.001(2) 0.003(2) -0.001(2) C8 0.014(2) 0.035(3) 0.032(3) -0.003(2) 0.005(2) 0.001(2) F2 0.060(3) 0.083(3) 0.048(2) 0.033(2) 0.032(2) 0.038(2) C17 0.016(2) 0.032(3) 0.029(3) 0.001(2) 0.000(2) 0.004(2) C27 0.012(2) 0.023(3) 0.025(3) 0.000(2) 0.0024(19) -0.0002(19) F3 0.0165(16) 0.062(2) 0.045(2) -0.0054(18) 0.0119(15) -0.0042(16) C16 0.012(2) 0.026(3) 0.021(3) 0.000(2) -0.0018(19) 0.003(2) C20 0.015(2) 0.028(3) 0.034(3) -0.004(2) 0.003(2) -0.001(2) C18 0.020(3) 0.033(3) 0.027(3) -0.006(2) 0.002(2) 0.006(2) C15 0.029(3) 0.037(3) 0.026(3) 0.004(2) 0.013(2) 0.000(2) C7 0.017(3) 0.035(3) 0.029(3) -0.007(2) 0.004(2) 0.001(2) C3 0.017(2) 0.026(3) 0.023(3) -0.002(2) -0.003(2) -0.001(2) C12 0.022(3) 0.034(3) 0.020(3) 0.003(2) -0.001(2) -0.005(2) F1 0.062(3) 0.073(3) 0.053(3) -0.039(2) 0.036(2) -0.044(2) C13 0.020(3) 0.028(3) 0.022(3) 0.003(2) 0.004(2) -0.003(2) C2 0.014(2) 0.030(3) 0.032(3) 0.001(2) -0.001(2) 0.002(2) C25 0.021(3) 0.032(3) 0.028(3) 0.005(2) 0.009(2) 0.002(2) C11 0.020(3) 0.022(3) 0.024(3) 0.002(2) -0.002(2) -0.005(2) C14 0.026(3) 0.030(3) 0.026(3) 0.001(2) 0.000(2) -0.001(2) F13 0.064(3) 0.039(2) 0.072(3) 0.007(2) 0.046(2) 0.008(2) C19 0.021(3) 0.032(3) 0.031(3) -0.007(2) -0.006(2) 0.003(2) C5 0.017(3) 0.036(3) 0.028(3) 0.002(2) -0.001(2) 0.006(2) C21 0.010(2) 0.019(2) 0.029(3) 0.000(2) -0.003(2) 0.0049(19) C22 0.010(2) 0.023(3) 0.030(3) 0.003(2) 0.003(2) 0.0012(19) C1 0.012(2) 0.023(3) 0.027(3) 0.000(2) 0.002(2) -0.0008(19) C24 0.015(2) 0.033(3) 0.036(3) 0.009(2) 0.006(2) 0.001(2) F14 0.030(2) 0.064(3) 0.128(4) -0.044(3) 0.040(3) -0.016(2) F7 0.032(2) 0.196(6) 0.034(2) 0.034(3) 0.0115(18) 0.049(3) F15 0.080(3) 0.136(5) 0.025(2) 0.005(3) 0.013(2) 0.066(3) C6 0.016(2) 0.029(3) 0.024(3) -0.004(2) 0.005(2) -0.001(2) C4 0.014(2) 0.031(3) 0.031(3) -0.002(2) 0.007(2) 0.000(2) C10 0.014(2) 0.033(3) 0.037(3) -0.003(3) 0.005(2) 0.002(2) C9 0.022(3) 0.049(4) 0.019(3) -0.002(3) 0.006(2) 0.003(3) Cl1 0.0363(9) 0.0473(10) 0.0532(10) -0.0021(8) -0.0037(7) -0.0025(7) Cl2 0.0362(9) 0.0635(12) 0.0673(12) -0.0124(10) 0.0171(8) -0.0095(8) C28 0.041(4) 0.055(4) 0.035(4) 0.002(3) 0.007(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N6 1.930(4) . ? Cu1 N1 1.936(4) . ? Cu1 N7 2.125(4) . ? Cu1 Cu2 3.0311(10) . ? Cu2 N2 1.929(4) . ? Cu2 N3 1.943(4) . ? Cu2 N8 2.130(4) . ? Cu3 N5 1.864(4) . ? Cu3 N4 1.866(4) . ? F11 C10 1.344(7) . ? N2 N1 1.351(6) . ? N2 C3 1.361(6) . ? F18 C14 1.338(7) . ? F12 C10 1.326(6) . ? F5 C5 1.333(7) . ? N1 C1 1.363(6) . ? N3 C6 1.339(7) . ? N3 N4 1.359(6) . ? F10 C10 1.342(7) . ? C26 C25 1.374(8) . ? C26 C27 1.409(7) . ? C26 H26 0.9500 . ? N4 C8 1.345(7) . ? F16 C14 1.330(7) . ? F6 C5 1.323(7) . ? F8 C9 1.341(8) . ? F9 C9 1.322(7) . ? F4 C5 1.349(6) . ? N6 C13 1.342(7) . ? N6 N5 1.371(6) . ? N8 N7 1.291(6) . ? N8 C27 1.402(6) . ? N5 C11 1.350(7) . ? F17 C14 1.331(7) . ? N7 C16 1.390(7) . ? C23 C24 1.365(8) . ? C23 C22 1.418(7) . ? C23 H23 0.9500 . ? C8 C7 1.369(8) . ? C8 C10 1.499(8) . ? F2 C4 1.316(7) . ? C17 C18 1.375(8) . ? C17 C16 1.401(8) . ? C17 H17 0.9500 . ? C27 C22 1.405(7) . ? F3 C4 1.336(6) . ? C16 C21 1.413(7) . ? C20 C19 1.359(8) . ? C20 C21 1.420(7) . ? C20 H20 0.9500 . ? C18 C19 1.406(8) . ? C18 H18 0.9500 . ? C15 F15 1.295(7) . ? C15 F13 1.326(7) . ? C15 F14 1.327(7) . ? C15 C13 1.492(8) . ? C7 C6 1.395(8) . ? C7 H7 0.9500 . ? C3 C2 1.370(8) . ? C3 C5 1.480(8) . ? C12 C11 1.371(8) . ? C12 C13 1.390(8) . ? C12 H12 0.9500 . ? F1 C4 1.327(7) . ? C2 C1 1.372(8) . ? C2 H2 0.9500 . ? C25 C24 1.393(8) . ? C25 H25 0.9500 . ? C11 C14 1.495(8) . ? C19 H19 0.9500 . ? C21 C22 1.428(8) . ? C1 C4 1.469(7) . ? C24 H24 0.9500 . ? F7 C9 1.303(7) . ? C6 C9 1.496(8) . ? Cl1 C28 1.763(7) . ? Cl2 C28 1.768(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? 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 N6 Cu1 N1 140.84(18) . . ? N6 Cu1 N7 109.28(17) . . ? N1 Cu1 N7 108.04(17) . . ? N6 Cu1 Cu2 122.23(13) . . ? N1 Cu1 Cu2 64.03(12) . . ? N7 Cu1 Cu2 66.88(12) . . ? N2 Cu2 N3 146.80(18) . . ? N2 Cu2 N8 105.45(17) . . ? N3 Cu2 N8 106.55(17) . . ? N2 Cu2 Cu1 64.41(13) . . ? N3 Cu2 Cu1 123.49(13) . . ? N8 Cu2 Cu1 64.81(11) . . ? N5 Cu3 N4 178.8(2) . . ? N1 N2 C3 107.5(4) . . ? N1 N2 Cu2 115.6(3) . . ? C3 N2 Cu2 136.7(4) . . ? N2 N1 C1 107.5(4) . . ? N2 N1 Cu1 116.0(3) . . ? C1 N1 Cu1 136.5(4) . . ? C6 N3 N4 107.5(4) . . ? C6 N3 Cu2 136.9(4) . . ? N4 N3 Cu2 115.5(3) . . ? C25 C26 C27 118.9(5) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C8 N4 N3 107.4(4) . . ? C8 N4 Cu3 132.2(4) . . ? N3 N4 Cu3 120.2(3) . . ? C13 N6 N5 106.6(4) . . ? C13 N6 Cu1 137.4(4) . . ? N5 N6 Cu1 116.0(3) . . ? N7 N8 C27 120.4(4) . . ? N7 N8 Cu2 116.3(3) . . ? C27 N8 Cu2 123.1(3) . . ? C11 N5 N6 107.5(4) . . ? C11 N5 Cu3 131.8(4) . . ? N6 N5 Cu3 120.6(3) . . ? N8 N7 C16 121.3(4) . . ? N8 N7 Cu1 111.9(3) . . ? C16 N7 Cu1 126.8(3) . . ? C24 C23 C22 120.4(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? N4 C8 C7 111.4(5) . . ? N4 C8 C10 121.3(5) . . ? C7 C8 C10 127.3(5) . . ? C18 C17 C16 119.1(5) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? N8 C27 C22 122.1(5) . . ? N8 C27 C26 116.4(5) . . ? C22 C27 C26 121.5(5) . . ? N7 C16 C17 117.3(5) . . ? N7 C16 C21 121.5(5) . . ? C17 C16 C21 121.3(5) . . ? C19 C20 C21 120.6(5) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C17 C18 C19 120.5(5) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? F15 C15 F13 107.8(6) . . ? F15 C15 F14 106.5(5) . . ? F13 C15 F14 103.3(5) . . ? F15 C15 C13 112.2(5) . . ? F13 C15 C13 113.2(5) . . ? F14 C15 C13 113.2(5) . . ? C8 C7 C6 103.0(5) . . ? C8 C7 H7 128.5 . . ? C6 C7 H7 128.5 . . ? N2 C3 C2 110.2(5) . . ? N2 C3 C5 120.1(5) . . ? C2 C3 C5 129.6(5) . . ? C11 C12 C13 103.1(5) . . ? C11 C12 H12 128.5 . . ? C13 C12 H12 128.5 . . ? N6 C13 C12 111.6(5) . . ? N6 C13 C15 121.0(5) . . ? C12 C13 C15 127.4(5) . . ? C3 C2 C1 104.7(5) . . ? C3 C2 H2 127.6 . . ? C1 C2 H2 127.6 . . ? C26 C25 C24 120.3(5) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? N5 C11 C12 111.2(5) . . ? N5 C11 C14 120.1(5) . . ? C12 C11 C14 128.5(5) . . ? F16 C14 F17 107.4(5) . . ? F16 C14 F18 106.9(5) . . ? F17 C14 F18 106.7(5) . . ? F16 C14 C11 110.8(5) . . ? F17 C14 C11 112.3(5) . . ? F18 C14 C11 112.4(4) . . ? C20 C19 C18 120.9(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? F6 C5 F5 106.5(5) . . ? F6 C5 F4 107.9(5) . . ? F5 C5 F4 105.3(5) . . ? F6 C5 C3 113.4(5) . . ? F5 C5 C3 113.4(5) . . ? F4 C5 C3 109.8(5) . . ? C16 C21 C20 117.7(5) . . ? C16 C21 C22 117.6(5) . . ? C20 C21 C22 124.7(5) . . ? C27 C22 C23 117.4(5) . . ? C27 C22 C21 116.9(5) . . ? C23 C22 C21 125.6(5) . . ? N1 C1 C2 110.0(5) . . ? N1 C1 C4 120.6(4) . . ? C2 C1 C4 129.3(5) . . ? C23 C24 C25 121.4(5) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? N3 C6 C7 110.7(5) . . ? N3 C6 C9 121.4(5) . . ? C7 C6 C9 127.8(5) . . ? F2 C4 F1 106.1(5) . . ? F2 C4 F3 106.3(5) . . ? F1 C4 F3 105.1(4) . . ? F2 C4 C1 114.2(5) . . ? F1 C4 C1 113.5(5) . . ? F3 C4 C1 111.0(4) . . ? F12 C10 F10 107.9(5) . . ? F12 C10 F11 107.7(4) . . ? F10 C10 F11 105.5(5) . . ? F12 C10 C8 111.0(5) . . ? F10 C10 C8 112.7(4) . . ? F11 C10 C8 111.7(5) . . ? F7 C9 F9 109.0(5) . . ? F7 C9 F8 107.6(6) . . ? F9 C9 F8 104.2(5) . . ? F7 C9 C6 112.2(5) . . ? F9 C9 C6 111.1(5) . . ? F8 C9 C6 112.4(5) . . ? Cl1 C28 Cl2 111.4(4) . . ? Cl1 C28 H28A 109.3 . . ? Cl2 C28 H28A 109.3 . . ? Cl1 C28 H28B 109.3 . . ? Cl2 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.107 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.131 #===END